Ceramic Industry April 2011

April 2011 | Volume 161 | Issue Number 4 www.ceramicindustry.com

Microwave

Sintering

³ Toll Firing ³ Flexible Ceramic Membranes ³ Glass Frit MEMS Wafer Bonding

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New, super-efficient microwave assist firing. In 2007, Harrop, under license from Ceralink, designed and built this 27 ft3 1600°C atmosphere elevator kiln, the first large scale kiln with microwave assist technology.

Only from Harrop! • Heating times reduced up to 80% • Energy use cut by up to 60% • Lower processing temperatures • Smaller carbon footprint • Enhancement of properties These are the benefits of Microwave Assist Technology (MAT), proven after years of field testing. MAT combines conventional gas or electric radiant heat with a relatively small amount of microwave energy. The microwaves

target the core of the product, while the conventional heat provides thermal balance and uniformity to the product surface. Harrop is the exclusive North American licensee of industrial microwave assisted kilns and furnaces. To learn more about the potential of this patented and highly promising process, call us at 614-231-3621.

Fire our imagination

www.harropusa.com

³ TABLEOFCONTENTS April 2011 | Volume 161 | Issue Number 4

15

21

27

DEPARTMENTS

FEATURES

Inside CI . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6

³ Case Study: Renewable Resource R&D Harper International has designed a furnace system with dual functionality for carbon-related R&D . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11

International Calendar . . . . . . . . . . . . . . . . . 7 Ceramics in the News . . . . . . . . . . . . . . . . . . 8 People in the News . . . . . . . . . . . . . . . . . . 10 Kiln Connection . . . . . . . . . . . . . . . . . . . . . . 12 IP in Depth . . . . . . . . . . . . . . . . . . . . . . . . . . 13

³Case Study: Consistent Firing Results Ross Ceramics uses Bullers Rings as an essential part of its statistical process control procedure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15 ³Industrial-Scale Microwave Sintering Industrial microwave furnaces are now available that exploit the advantages of microwave sintering for zirconia-based dental restorations. . . . . 17

Product Spotlight: Burner Control System. . . . . . . . . . . . . . . 36 What’s New . . . . . . . . . . . . . . . . . . . . . . . . . 36 Services Marketplace . . . . . . . . . . . . . . . 37 Classified Advertisements . . . . . . . . . . . 45 Advertiser Index . . . . . . . . . . . . . . . . . . . . 46

³Toll Firing Success Several important factors should be considered when selecting a toll firing provider . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21 ³Measuring Fuel Energy The continuous monitoring of the calorific value of mixed gaseous fuels is on the rise . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24

SPECIAL SECTION | ADVANCED CERAMICS/GLASS ³Flexible Ceramic Membranes for Green Applications The huge global demand for clean and efficient energy, stable food, and clean water and air will spawn boundless opportunities for fuel cell technologies . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27 ³A Better Bond Lead-free glass pastes can offer multiple bonding advantages in MEMS wafer level packaging . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30

SPECIAL REPORT | RESOURCE MANAGEMENT ³Advances in Video Collaboration Manufacturers are now taking video collaboration outside of the boardroom and onto the plant floor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33  Denotes articles with global emphasis

ON THE COVER: Photo courtesy of Spheric Technologies Inc. CERAMIC INDUSTRY (ISSN 0009-0220) is published 12 times annually, monthly, by BNP Media, 2401 W. Big Beaver Rd., Suite 700, Troy, MI 48084-3333. Telephone: (248) 362-3700, Fax: (248) 362-0317. No charge for subscriptions to qualified individuals. Annual rate for subscriptions to nonqualified individuals in the U.S.A.: $178.00 USD. Annual rate for subscriptions to nonqualified individuals in Canada: $216.00 USD (includes GST & postage); all other countries: $228.00 (Int’l mail) payable in U.S. funds. Printed in the U.S.A. Copyright 2011, by BNP Media. All rights reserved. The contents of this publication may not be reproduced in whole or in part without the consent of the publisher. The publisher is not responsible for product claims and representations. Periodicals Postage Paid at Troy, MI and at additional mailing offices. POSTMASTER: Send address changes to: CERAMIC INDUSTRY, P.O. Box 2145, Skokie, IL 60076. Canada Post: Publications Mail Agreement #40612608. GST account: 131263923. Send returns (Canada) to Pitney Bowes, P.O. Box 25542, London, ON, N6C 6B2. Change of address: Send old address label along with new address to CERAMIC INDUSTRY, P.O. Box 2145, Skokie, IL 60076. For single copies or back issues: contact Ann Kalb at (248) 244-6499 or [email protected].

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³ INSIDECI by Susan Sutton | Editor-in-Chief, Integrated Media

Too Good to Be True? A representative from my cell phone company recently called and excitedly told me that I could upgrade my phone for FREE if I changed my plan and paid $20 more each month. I ran through a number of responses in my head, ranging from “You’ve got to be kidding,” and “Do you take me for a fool?” to “Please define free for me.” In the end, I decided it was one of those “if you don’t have anything nice to say, don’t say anything at all” kind of moments. I just laughed and said, “No, thank you.” On the surface, the concept of offshoring might seem like a great deal: moving operations overseas can enable manufacturers to dramatically slash costs and improve their profitability. But according to Harry Moser, founder of the Reshoring Initiative, when companies look deeper into the details of offshoring—particularly the logistics involved—additional costs become readily apparent. “According to a 2009 survey by Archstone Consulting, 60% of manufacturers use only rudimentary calculation methods to determine what it costs them to offshore,” he says. “On average, they miss about 20% of the total costs of offshoring.” Additional costs typically come in the form of travel, packaging, shipping and inventory, to name just a few. To help manufacturers calculate the true costs of offshoring, The Reshoring Initiative has developed a spreadsheet that includes a number of variables, both tangible and intangible. Moser will discuss these issues in detail when he delivers the keynote address at Tech ManufactureXPO, a live virtual event that will be held May 4. Co-sponsored by ASI, our sister publication, the free event will enable attendees to save on travel costs while gathering information and networking with peers—all from the comfort of their office. Learn more in “Bringing It All Back Home,” online at www.ceramicindustry.com.

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EDITORIAL ADVISORY BOARD Surinder Maheshwary, Director, Quality Assurance/Process Improvement, Dal-Tile International; William Babik, Technical Sales Manager, Nabertherm Inc.; Charles Semler, Ph.D., Refractories Consultant, Semler Materials Services; Gary Childress, General Manager, Orton Ceramic Foundation; Matthew Centa, Technical Support Manager - Ceramics & Glass, Rio Tinto Minerals; James E. Houseman, Ph.D., President, Harrop Industries, Inc.

ONLINE EXTRA: BRINGING IT ALL BACK HOME The Reshoring Initiative aims to educate manufacturers about the true costs of outsourcing.

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April 2011 ³ WWW.CERAMICINDUSTRY.COM



³INTERNATIONALCALENDAR April 4-8 2011 Industrial Combustion Seminars ³ Lebanon, Pa., www.hauckburner.com April 5-7 AeroDef Manufacturing ³ Anaheim, Calif., http://aerodef.sme.org April 18-20 4th Annual Tactical Vehicles Summit ³ Alexandria, Va., www.TacticalVehiclesSummit.com

May 17 NESHAP Subpart HHHHHH “6H” Training Program ³ Toledo, Ohio, www.owens.edu/workforce_cs/spray2011flier.pdf May 18-20 Spray Finishing Technology Workshop ³ Toledo, Ohio, www.owens.edu/workforce_cs/spray2011brochure.pdf May 18-21 PowderMet 2011 ³ Chicago, Ill., www.mpif.org

April 25-27 CISILE2011 ³ Beijing, China, www.cisile.com.cn

JUNE 6-9 ArmorCon ³ Vienna, Va., www.ArmorConExpo.com

April 26-28 Kitchen & Bath Industry Show ³ Las Vegas, Nev., www.nkba.org May 2-4 INTERTECH 2011 ³ Chicago, Ill., www.intertechconference.com May 4 Tech ManufactureXPO virtual trade show ³ www.techmanufacturexpo.com

JUNE 9-10 13th Small Fuel Cells 2011 ³ Boston, Mass., www.knowledgefoundation.com/viewevents. php?event_id=258&act=evt JUNE 28-July 1 European Fuel Cell Forum ³ Lucerne, Switzerland, www.efcf.com

May 9-11 Construction, Corrosion & Infrastructure Conference ³ Las Vegas, Nev., http://www.goeshow.com/acma/CCI/ ereg497293.cfm?clear

JULY 15-15 COMPOSITES CHINA ³ Shanghai, China, [email protected]

May 10-12 Pneumatic Conveying Course ³ Houston, Texas, www.asme.org/education

AUG 10-12 8th China (Beijing) International Metallurgy Industry Expo 2011 ³ Beijing, China, (86) 10-8168 0380

* Look for Ceramic Industry magazine at these events! For a more detailed listing, visit our website at www.ceramicindustry.com.

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CERAMIC INDUSTRY 6/5/08 ³ April 2011 2:30:33 PM

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³ INTHENEWS KYOCERA and Japan Medical Materials Open U.S.-Based Orthopedic Design Center Kyocera Industrial Ceramics Corp.’s Orthopedic Division has opened its new Orthopedic Design Center in Somerset, N.J., formed in collaboration with Japan Medical Materials Corp. (JMM), a Kyocera Group company. The JMM Design Center will expand Kyocera’s relationships and partnerships in support of JMM’s implant and medical device business. The facility offers the extensive medical field experience and time-proven materials technologies of both companies. Ceramic-based orthopedic implants are growing in demand due to rising awareness of the excellent wear-resistant properties of ceramic materials. Ceramic heads are expected to mate more smoothly with the polyethylene cup in hip and knee replacements, helping to prevent “wear debris.” Visit http://global.kyocera.com for details.

ments in manufacturing processes, upgrades in enterprise systems, textbooks, and more. For additional information, visit www.americanpiezo.com.

Thermal Technology Receives Orders for Sapphire Crystal Grower Thermal Technology announced it recently received 59 orders for its model K1 90 kg sapphire crystal grower from customers in Taiwan, Korea and China. These growers will produce a total of 5.2 million two-in-equivalents (TIE) per year. The sapphire crystal grower advances beyond the traditional kyropoulos process and out-performs other sapphire crystal growth methods currently being marketed, such as HEM or Bridgman, according to the company. The model K1 grower is intended for LED substrate production. The tool’s short cycle time reportedly makes it the most productive grower commercially available. For additional details, visit www.thermaltechnologyinc.com.

Crossville Selects Sacmi Press Crossville Inc., a producer of technical and glazed granito, has reportedly been running the highest tonnage press in the U.S. for more than a year. The Sacmi-made PH7500 press was purchased to produce large tiles, a product segment that is steadily gaining ground in the U.S. market. The press has a width of 2450 mm, with a 1360 mm maximum filling depth. Crossville recently decided to boost production of 600 x 600 tiles and start large-scale production of 600 x 900 mm tiles. Additional goals include the production of even larger tiles, up to 1200 x 1200 mm. Additional information is available at www.sacmi.com or www.crossvilleinc.com.

Ceradyne Receives $56.6 Million ESAPI Body Armor Order Ceradyne Inc. recently announced that it has received a delivery order for approximately $56.6 million for enhanced small arms protective insert (ESAPI) ceramic body armor plates. The company will begin shipping this ESAPI production release in the second quarter of this year, with full shipment expected to be completed late in the third quarter. The release was issued under the $2.37 billion indefinite delivery/indefinite quantity (ID/IQ) contract originally issued in October 2008 and scheduled to expire in September 2013. A balance of approximately $2.1 billion remains on the ID/IQ contract. “We are extremely pleased to have been awarded this ESAPI contract,” said David P. Reed, president of North American Operations. “We anticipate meeting the government’s quality and delivery requirements with this delivery order shipped complete in the third quarter 2011.” For additional details, visit www.ceradyne.com.

APC International Celebrates 25 Years February 3 marked the 25th anniversary for APC International Ltd. The company began in 1986 and, over the years, has had changes in location, new divisions, new facilities, improve8

April 2011 ³ WWW.CERAMICINDUSTRY.COM

Owens Corning to Divest Brazil Glass Reinforcements Plant Owens Corning recently announced that it has reached a definitive agreement to sell its Capivari, Brazil, glass fiber reinforcements plant to Chongqing Polycomp International Corp. (CPIC). The transaction, which is expected to close during the second quarter, is subject to regulatory approval and other customary conditions. For more information, visit the company’s website at www.owenscorning.com.

Engis to Double Headquarters Engis Corp. recently announced expansion plans that will nearly double the size of its world headquarters in the Chicago suburb of Wheeling, Ill. The company will expand its state-ofthe-art manufacturing and warehouse facilities and create space for the new Engis Technology Center. The 54,000-sq-ft, multi-million-dollar expansion will bring total space to 121,500 sq ft and enable the company to consolidate all engineering, process development labs, manufacturing, warehousing, and administrative offices into one facility. In conjunction with this project, Engis will add new manufacturing, process development, and testing and measurement equipment. Construction will start this month and is expected to be complete by this fall. “This expansion demonstrates our long-term commitment to customers as a leading-edge provider of superabrasive solutions,” said Stephen Griffin, president. “For example, new automated manufacturing equipment will enable us to increase our ability to support global markets, while the Engis Technology Center will enhance our capability to develop turnkey manufacturing solutions. It also demonstrates our commitment to keep and generate future jobs in Wheeling and in the U.S.” For additional details, call (800) 993-6447 or visit www.engis.com.

Bennu Glass to Reopen Washington Factory Bennu Glass LLC recently announced plans to reopen the idle wine bottle manufacturing facility located in Kalama, Wash. The factory was previously owned by Cameron Family Glass Packaging LLC. Bennu purchased most of Cameron’s assets through foreclosure after Cameron filed Chapter 7 bankruptcy in 2009. “To restart the factory, Bennu will make a significant investment in the existing facility,” said Jerry Lemieux, CEO. “This will include removal of the inoperable electric glass furnace that was blamed

Corning Cable Systems to Provide Solutions to Kazakhstan Corning Cable Systems GmbH & Co KG, part of Corning Inc.’s Telecommunications segment, will supply its passive optical solutions to Astanatelecom for an initiative to bring fiber to the home (FTTH) to the residents of Astana, the capital and second-largest city of Kazakhstan. Astanatelecom plans to connect 1000 single-family units in the growing city of Astana. Corning’s flexible, interchangeable Evolant® Solutions for FTTx networks help to make SFU deployments easier and faster with preterminated solutions, no-epoxy/no-polish connectors, and Corning’s bend-insensitive ClearCurve® single-mode fiber. For more information, call (49) 800267-64641 or visit the website at www.corning.com/cablesystems.

in large part for Cameron’s failure. In its place, a new, state-of-theart oxygen-fuel furnace will be installed.” Nikolaus Sorg GmbH & Co. KG was chosen to design, engineer and install the new furnace. The company is hopeful that the factory will be in full production by early 2012. At full capacity, the facility will produce over 100 million wine bottles per year. Within the next several months, Bennu will begin hiring the employees necessary for the factory and business operations. For additional information, visit www.bennuglass.com.

ments with local authorities, and will initially create 300 new jobs. “We appreciate the outstanding support we received from Rostov Governor Golubev and his administration,” said Russell Ebeid, president of Guardian Glass group. “It is evident that they view new investment as a priority, and the government works hard to streamline the development process to attract new projects that will create new jobs.

Guardian is bullish on Russia, given the excellent growth at our first plant in Ryazan and the customers we have in the country. The timing is right for the region and for Guardian.” For additional details, visit the company’s website at www.guardian.com.

EPA Awards $5.5 Million to Support Nanotechnology Research The U.S. Environmental Protection

Thermo. Dynamic.

Guardian to Build Second Float Glass Plant in Russia Guardian Industries Corp. has announced plans to build a float glass manufacturing plant in Krasny Sulin (Rostov region), Russia. The $220 million plant will be the company’s largest, producing 900 tons of glass per day, and will include a technologically advanced glass coater. The Rostov plant w ill produce Guardian’s ClimaGuard® (residential) and SunGuard® (commercial) glass products for the construction of homes, offices, retail, health care, and other facilities. The plant is expected to begin operation in mid-2012, based on the fulfillment of all incentives and agree-

Harper’s innovative thermal processing systems help ceramic manufacturers meet the needs of emerging applications, to reach newer, greater heights.

Spark the future.

TM

© 2011 Harper International

harperintl.com 716.684.7400

CERAMIC INDUSTRY ³ April 2011

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IN THE NEWS

NETZSCH to Host HI TEMP Conference NETZSCH Instruments recently announced it will host the inaugural HI TEMP 2011 Conference September 20-22 in Boston. The two-and-a-half-day conference will focus on the latest trends in high-temperature thermal analysis and thermal properties measurement of advanced materials. The conference will offer 10 keynote speakers, 30 oral presentations and a poster session. The deadline for papers is April 10. For additional details, visit www.hitemp2011.com.

Agency (EPA) has awarded $5.5 million to three consortia to support innovative research on nanotechnology. The EPA, in collaboration with the UK’s Natural Environment Research Council, is leading this scientific research effort to better understand the potential risks to people’s heath and the environment. The scientific information developed from the research can help guide the EPA and other agencies in decisions about the safety of new materials and products that are made using nanotechnology. “The responsible development of nanotechnology can play a major role in sustaining a positive, healthy environment, a vibrant and growing economy, and a high standard of living,” said Paul Anastas, assistant administrator of the EPA Office of Research and Development. “Understanding the risks posed by engineered nanomaterials is a global challenge that is best met through international collaboration, drawing on the combined expertise of researchers from diverse backgrounds.” Visit www.epa.gov/nanoscience for more information.

FCHEA Launches Energy Network Campaign The Fuel Cell and Hydrogen Energy Association (FCHEA) has launched a campaign calling on Congress to continue funding fuel cell and hydrogen programs, which are critical to preserving U.S. leadership in the evolving clean energy network. The FCHEA launched a new website for the campaign through which it expects to engage an army of grassroots proponents of fuel cells and hydrogen energy. The FCHEA is calling on the U.S. government to acknowledge in its rhetoric, policies and government purchases what energy experts and leaders across the globe have already acknowledged: all clean energy options, including fuel cells and hydrogen, are necessary to reach the country’s economic growth, environmental and energy security goals. The organization is calling on industry to lend support to this cause. For more information, visit www.fchea.org. 

DAILY UPDATES For the latest industry news and information, visit us online at www.ceramicindustry.com. 10

April 2011 ³ WWW.CERAMICINDUSTRY.COM

³ PEOPLEINTHENEWS Owens-Illinois Inc. (O-I) announced that Deborah Hockman, Ph.D., has been named vice president of global environment, health and safety (EHS). In the newly created position, she will lead the company’s global efforts to enhance its safety, environment compliance and health processes, and standards and metrics. She also will serve as global safety program leader, driving the company’s worldwide efforts to create an accident-free workplace. The Supervisory Board of RHI AG has appointed Henning E. Jensen CEO. Jensen previously served as chief financial officer and spokesman for the Management Board of RHI AG. The Supervisory Board has also appointed Mark J. Eckhout chief financial officer. Eckhout has held numerous senior financial positions in various telecommunications companies. He has also served as a member of the Supervisory Board of RHI AG. NYCO recently announced the appointment of Li Wanghua (Jack Lee) as managing director, NYCO China. Lee will continue to reside full time in China and will work closely with other sales and operations managers from NYCO’s North American operations. Eric Marcotte has been appointed the new southern U.S. regional sales manager for Stedman and Innovative Processing Solutions. Marcotte’s responsibilities will include selling crushing equipment and systems to Stedman customers. He has over three years of experience in the mining industry, plant operations, and size reduction equipment. Marcotte received a bachelor’s degree in mining engineering from the University of Kentucky. John F. Meier, chairman and CEO of Libbey Inc., has announced his intention to retire by the end of 2011. The Nominating and Governance Committee of the Board of Directors, along with an internationally recognized executive search firm, will lead a comprehensive search process to determine his successor. Du-Co Ceramics Co. has appointed Josh Rupp to the newly created position of process engineer. Rupp will assist in the development and design of automation systems, as well as the improvement of overall efficiencies. The company has also proRupp moted Jim Shaner to the position of ceramic process engineer at its Saxonburg, Pa., facility. Shaner’s experience will be optimized in production, R&D, product improvement, cost reduction and material management. Anthony W. Thornton, director of Product Integrity and Performance and a senior product scientist for Micromeritics Instrument Corp., has been elected to serve a three-year term on the ASTM International board of directors. 

³ CASESTUDY Renewable Resource R&D Harper International has designed a furnace system with dual functionality for carbon-related R&D.

H

arper International Corp. recently developed a furnace system with dual functionality for a national laboratory that is engaged in the research, development and commercialization of new advanced materials. The laboratory is researching the development of a wide range of carbon materials from renewable resources. Advanced carbon materials derived from renewable sources would replace products currently derived from petroleum. The objective is to provide products with similar functional quality at a lower cost, thereby increasing the applications for these advanced carbon materials.

Project Requirements To simulate the commercial production of carbon materials, a continuous thermal processing system was selected by the lab’s research team. Precursor materials planned for this development project vary widely in both particle sizes and shapes. These variations in precursor materials would require two distinctive types of furnace systems: a rotary furnace for one type of material and a mesh belt furnace system for other materials. The laboratory, which had limited floor space available, contacted Harper International for assistance in designing a single, continuous thermal processing system that could satisfy both requirements. The Harper team designed a multi-functional thermal processing system that can be transformed from a rotary tube furnace to a mesh belt furnace while using a single thermal platform. “The design of this custom furnace system demonstrates the commitment Harper makes to provide solutions, investments and new concepts to achieve the needs of our valued customers,” says Rick Rehrig, vice president of Sales for Harper. “The world of advanced materials continues to change at an accelerated pace. The engineers and scientists here at Harper International provide custom solutions and technical assistance for economical commercialization in the advanced materials industry.”

charge h collection ll i to maintain i i atmospheric h i iintegrity. i F Four zones of control allow for adjustments to heat-up rate, soak period and cooling rate. Process capacity is controlled by adjusting the angle of the system’s inclination, along with the rotational speed of the tube and the feeder system screw. The rotary tube may be removed from the system, allowing for the installation of a mesh belt within the same thermal section of the furnace. The mesh belt thermal system is also atmospherically controlled, with purge chambers located at both the entrance and exit end of the furnace system. Four zones of control allow for adjustments to the thermal profile. The internal alloy muffle was designed with several exhaust ports at key locations for the removal of corrosive off-gases. A water jacket installed around the muffle assists with the cooling of material prior to its exit from the furnace. Both furnace systems have been designed to be gas tight and operate with a variety of atmospheric gases, including reactive and corrosive gases. The systems can operate in the 1000°C range with thermal processing cycle variations from 30 minutes up to 10 hours. The laboratory will have the flexibility to test and develop new carbon materials from a variety of sources, including renewables. 

System Features The single thermal processing system features a clam-shell design that allows the top half of the furnace to open, exposing the furnace’s internal section. The rotary tube furnace features a completely sealed rotary tube system and enclosed dis-

For additional information, contact Harper International Corp. at 100 W. Drullard Ave., Lancaster, NY 14086-1698; call (716) 684-7400; fax (716) 684-7405; e-mail [email protected]; or visit www.harperintl.com. CERAMIC INDUSTRY ³ April 2011

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³ KILNCONNECTION by Ralph Ruark | Senior Technical Editor

Understanding Variability

“V

ariability is the enemy of quality.” This has become the battle cry for manufacturing excellence in many facilities that I visit. After engineers measure the range of process parameters, they analyze the required operational changes necessary to narrow the range and standard deviation of specific values. Control limits are established, and considerable effort is expended to minimize the variations. But like the many programs for quality, consistency, and yield that have come before it, the process of measuring variations and subsequent discussion is often confused for progress. A surprising number of plants spend significant funds in an effort to improve processes through adjustment but, after a few years, the resulting progress is limited; yield improvements are modest, at best.

Variation Types Quality experts separate variations into two types. The first type is common cause; these are variables inherent within the process. Hundreds of such variables can exist, and they generally cannot be eliminated without changing the process in some significant manner.

Fixing common-cause problems will often provide the largest window for successful firing. The other types of variables are defined as special cause, and this class of variable is far more discernable: something happened within the process, often abruptly, that caused properties to deviate widely. These kinds of variations normally provoke instant action and firefighting in order to determine “what went wrong.” Frequently, a ceramic factory will spend much of its time trying to eliminate the special-cause variables through the establishment of control charts, standard procedures, etc., while the common-cause issues are noted—but rarely addressed. Fixing special-cause problems is often easy; better monitoring, adjustments and procedures usually allow things to resume ‘normal operation.’ Sometimes, however, it is the common-cause variation that must be addressed before lasting and continuous improvements can be made.

Figure 1. The differences in temperature and the relative heating rates in this kiln are completely location-dependent.

Fixing Common-Cause Variations As an example, take a look at the Datapaq curve shown in Figure 1, which displays the temperatures in the preheating zone of a tunnel kiln in several locations on a single kiln car. In the case of this kiln, the differences in temperature and the relative heating rates are completely location-dependent. The top levels of the kiln car are hot, and the bottom levels and car interior are cold. For this particular kiln, no amount of adjustment will fix the problem. Occasionally, losses will occur due to cracking or insufficient oxidation; these problems are usually caused by heating that is either too fast or too slow in certain locations. Such high losses can and do result in futile kiln adjustments until the yield problem goes away. Instead, the focus should be shifted to the common-cause problem root—poor temperature uniformity—and the kiln’s design should be modified to eliminate the problem. This is a ma nagement f u nc t ion (not a n operator’s responsibility), yet few companies address these inherent problems. Fixing common-cause problems will often provide the largest window for successful firing, even when upstream variations are a little out of kilter. The goal in kiln operations should be to provide the best chance of success, even when the greenware coming to the kiln might be imperfect. Variability truly is the enemy of quality. Recognizing the difference between inherent common-cause problems and special problems—and addressing both—can make the difference between continuous improvements of quality/yield, and the standard firefighting of special problems alone that does nothing but fix the occasional bad yield issue. 

Ralph Ruark is a registered professional engineer with degrees in ceramic engineering and business, and 37 years of experience in the ceramic industry. He formed Ruark Engineering Inc. several years ago and serves as a technical consultant to a number of ceramic manufacturers and kiln companies. He is dedicated to assisting ceramic companies with a variety of kiln and firing needs, leading kiln analysis efforts, providing training expertise, and improving operations. Ruark can be reached at (941) 730-2253, fax (888) 370-2546, e-mail [email protected] or online at www.ruarkengineering.com. Any views or opinions expressed in this column are those of the author and do not represent those of Ceramic Industry, its staff, Editorial Advisory Board or BNP Media.

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³ IPINDEPTH by Michael Gzybowski | Counsel, Brinks Hofer Gilson & Lione

Pilot Program Options

T

he U.S. Patent and Trademark Office (USPTO) is facing a growing backlog of more than 700,000 patent applications. On average, it currently takes about 25 months after the filing of an application for examination to begin. Once examination begins, an additional 10-36 months may be necessary for an application to issue as a patent. In cases where an application must go through the appeals process within the USPTO, the process can take as long as 53 additional months. The USPTO has initiated a number of pilot programs and other proposals that are geared toward reducing both the backlog and pendency of application processing. These include the following: • First-Action Interview Pilot Program • Ombudsman Pilot Program • Green Technology Pilot Program • Peer Review Pilot Program • Patent Prosecution Highway Pilot Program • Missing Parts Pilot Program • Patent Application Backlog Reduction Stimulus Plan • Proposal to Extend Terms of Provisional Applications • Proposed Three-Track System These programs and proposals each present different options to accelerate the examination process and reduce the number of applications that enter examination.

First-Action Interview Pilot Program The First-Action Interview Pilot Program allows applicants to conduct an interview with examiners before a First Office Action is prepared (normally the beginning of examination). Initially launched in April 2008 and limited to computer-related inventions, the program was enhanced and extended to additional technologies in October 2009. Under the enhanced program, an eligible applicant can file a request to participate in the program. Approval is at the discretion of the examiner; once approved, the examiner will conduct a prior art search and provide the applicant with a pre-interview communication, which is a condensed preview of objections or rejections proposed against the claims. Within 30 days from the issue date of the pre-interview communication, the applicant must either choose not to have a firstaction interview with the examiner or schedule the interview. If an interview is conducted and agreement is reached, the applica-

tion will be allowed. If an agreement is not reached or an interview is not conducted, a First-Action Interview Office Action will be entered and the applicant will have a limited time to reply.

Ombudsman Pilot Program The Ombudsman Pilot Program allows applicants experiencing problems during the processing of applications to contact an ombudsman representative “if the normal channels have not been successful.” The ombudsman representative will call the applicant within one day for assistance in resolving the problem. As stated in a USPTO press release, “The Ombudsman Pilot Program does not replace other existing resources available to patent applicants, attorneys or agents…. The ombudsman should only be contacted if an applicant, attorney or agent feels that examination has stalled and that their efforts to move their application forward through the normal channels (e.g., contacting the examiner or supervisory patent examiner) have not been effective.”

Green Technology Pilot Program The Green Technology Pilot Program allows applicants to accelerate the examination of unexamined applications that pertain to “green technologies.” To participate in the program, an applicant must file a petition (no fee required) and substantiate that the invention pertains to environmental quality, energy conservation, development of renewable energy resources or greenhouse gas. If the applicant’s petition is granted, the application will be accorded special status and advanced out of turn for examination.

Peer Review Pilot Program The Peer Review Pilot Program involves the use of an Internetbased review process in which the public is allowed to review volunteered published patent applications and submit technical references and comments on what they believe to be the best prior art to consider during the examination. Patent examiners can then use (and supplement) the submitted prior art to evaluate patentability of an application during the examination process. This program was initially limited to computer-related inventions when it launched in June 2007. It was expanded in October 2010 to include applications in biotechnology, bioinformatics, telecommunications and speech recognition. continued on p. 14

Michael Gzybowski is an intellectual property attorney with Brinks Hofer Gilson & Lione. He has over 25 years of experience, including serving as a patent examiner at the U.S. Patent and Trademark Office prior to entering private practice. He can be reached at [email protected].

Any views or opinions expressed in this column are those of the author and do not represent those of Ceramic Industry, its staff, Editorial Advisory Board or BNP Media.

CERAMIC INDUSTRY ³ April 2011

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IP IN DEPTH

Patent Prosecution Highway Pilot Program

a non-provisional application that claims priority to a provisional application.

The Patent Prosecution Highway (PPH) Pilot Program is based on the recognition that many large companies file corresponding patents in several countries simultaneously. The PPH program allows participating patent offices in different countries to benefit from work that was previously done by another country’s patent office, with the goal of reducing examination workload. Under the PPH program, when an applicant obtains a favorable examination in an office of first filing, they can request that the other participating countries accelerate the examination of the corresponding claims.

Missing Parts Pilot Program The Missing Parts Pilot Program allows an applicant to delay the payment of non-provisional application search and examination fees (currently $760 for a large entity) for up to 12 months from the filing date of

Patent Application Backlog Reduction Stimulus Plan The Patent Application Backlog Reduction Stimulus Plan allows a small entity inventor who has more than one pending, unexamined application to abandon one application in exchange for another application being advanced out of turn (accorded special status).

Proposal to Extend Terms of Provisional Applications

to create a three-track process from which applicants can choose how quickly they want their applications processed. One track will give applicants a “prioritized examination.” The fee for this track will be set to cover the cost of expediting the examination and be high enough to deter inventors from using this track for all their patent applications. The second track will be the USPTO’s traditional examination timeline. The third track would allow applicants to delay examination for up to 30 months.

Careful Consideration

The Proposal to Extend Terms of Provisional Applications seeks to extend the term of a provisional application to 24 months. Currently, a provisional application has to be converted into a non-provisional application within 12 months.

Proposed Three-Track System The Proposed Three-Track System seeks

Each of these pilot programs and proposals has benefits and disadvantages. In view of the fact that a number of the pilot programs that were initiated some time ago have repeatedly been extended and expanded, it is reasonable to believe that at least some of these programs will be available for patent applicants for some time to come. 

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³ CASESTUDY Consistent Firing Results Ross Ceramics uses Bullers Rings as an essential part of its statistical process control procedure.

W

ith 40 years of experience in the manufacture of ceramic cores, Ross Ceramics Ltd. (RCL) is continually at the forefront of advanced ceramic core technology. As a wholly owned Rolls Royce subsidiary, RCL has particular expertise in the manufacture of the complex geometry ceramic cores that are used in the investment casting of high-performance, directionally solidified and single-crystal gas turbine engine components for aerospace and industrial applications. RCL’s materials are developed to give stability at high casting temperatures, no adverse core to alloy reactions, and dimensional consistency. The use of Bullers Rings is a critical part of RCL’s routine quality assurance procedures.

Ross Ceramics’ ceramic cores are used in the investment casting of high-performance, directionally solidified and single-crystal gas turbine engine components. (Photograph reproduced with the permission of Rolls Royce plc, © Rolls Royce plc 2010.)

What are Bullers Rings? Bullers Rings are pyrometric devices that are used to accurately measure the effects of heatwork within a kiln firing environment. (Heatwork is the action and effect of temperature over time on a ceramic product. If the product receives too much or too little time at the correct thermocouple temperature, it may be under- or over-fired.)

Bullers Rings are used to verify consistent heat distribution between firing cycles. UK-based Taylor Tunnicliff Ltd. specializes in the manufacture of Bullers Rings, which are used by many of the world’s leading tableware, sanitaryware, brick, refractories and technical ceramics manufacturers to measure the amount of heatwork that has taken place in the kiln. Bullers Rings provide an independent, accurate, reliable and essential indication that the firing of the product is correct and unaffected by any variations in temperature and kiln loading.

Bullers Rings are pyrometric devices that are used to accurately measure the effects of heatwork within a kiln firing environment.

How are Bullers Rings Used? The physical properties of the ceramic core are of paramount importance for RCL and, indeed, Rolls Royce. To help ensure that the finished parts meet quality requirements, RCL bases its statistical process control (SPC) charts directly on Bullers Ring readings. Bullers Rings are first placed on and around the setter blocks and saggars on the kiln cars. Readings are taken after the firing, and these readings are inputted directly to the SPC chart. As can be seen in Figure 1 (p. 16), the readings are plotted against an average and a range, per kiln side. Over time, CERAMIC INDUSTRY ³ April 2011

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CASE STUDY

In addition to providing essential SPC data, RCL has found Bullers Rings particularly useful when products need to be fired on an alternative kiln. For example, a new kiln may have a more powerful or efficient burner. The use of Bullers Rings enables the firing profile for the new kiln to be set up accurately and efficiently.

Summary

Figure 1. Bullers Ring readings are inputted directly to SPC charts.

Ross determined the appropriate Bullers Ring range for its firing parameters. Close monitoring of the SPC charts ensures that corrective action can be taken immediately, should the Bullers Rings readings fall outside the acceptable parameters. For a Type 55 Bullers Ring on a firing of 960-980°C, a typical range of 10 to 14 can be expected.

Bullers Rings are used to verify consistent heat distribution between firing cycles without the expense of extensive testing. The use of Bullers Rings provides a clear indication that the correct properties have been achieved, resulting in RCL’s ceramic cores performing as expected in the casting process. This cannot be achieved using thermocouples alone, since they only measure temperature. If Bullers Rings were not used, extensive, costly and destructive thermal expansion testing would be required to ensure that the ceramic cores are fit for their purpose.  For additional information, contact Taylor Tunnicliff Ltd., Normacot Rd., Longton, Stoke-on-Trent, England, ST3 1PA; call (44) 1782-501174; fax (44) 1782-328807; e-mail [email protected]; or visit www.taylortunnicliff.com.

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Europe

Tokuyama Europe GmbH Oststrasse 10,40211 Dusseldorf Germany Tel: +49-211-1754480

Japan

Tokuyama Corporation Shapal Sales Department, Specialty products Business Division Shibuya Konno Bldg. 3-1, Shibuya 3-chome, Shibuya-ku, Tokyo 150-8383 Tel: +81-3-3597-5135 e-mail: [email protected] URL http://www.shapal.jp/index.html

Industrial-Scale Microwave Sintering

I

t is widely recognized that the microwave-enhanced processing of materials offers several advantages o v e r c o nv e n t i o n a l h e a t i n g , including shorter processing times, energy savings, improved product yield, decreased manufacturing costs, unique microstructure and properties, and new materials synthesis routes. These advantages result from the basic difference between microwave heating and other conventional bulk heating mechanisms.

Process Basics In conventional heating, conduction, convection and/or radiation mechanisms deliver thermal energy to the surface of the sample. The conduction mechanism then transfers the thermal energy into the bulk of the sample. In microwave heating, the heating mechanism is different. Molecular interaction with the electromagnetic field helps deliver microwave energy directly and simultaneously into the sample’s whole bulk. During microwave heating, electromagnetic energy is converted to thermal energy within the sample; the mechanism is therefore essentially one of energy conversion, not just heat transfer. When microwaves penetrate and are converted to thermal energy within the material, heat energy is generated throughout the volume of the material; this results in volumetric heating and rapid, uniform heat-up of the bulk material. The thermal gradient profile in a conventionally heated sample could be thought of as the reverse of that in microwave heating, in that the center could be slightly less hot than the outside because the thermal energy flows inward.

➤ Industrial microwave furnaces are now available that exploit the advantages of microwave sintering for zirconiabased dental restorations. by Kuruvilla (Karl) Cherian, Director of Applied Research, and Michael Kirksey, Vice President, Spheric Technologies, Inc. In microwave heating, however, the center may be slightly hotter due to the internal energy conversion mechanisms, coupled with heat losses from the surfaces. If necessary, additional external susceptors placed strategically nearby could help neutralize any such thermal nonuniformity to achieve uniform and rapid temperature ramp-up in suitable material phases. It has been reported that, in addition to the radiant heat produced by nearby external microwave susceptors, a direct microwave effect on the sample occurs that could increase the sintering kinetics by 1-2 orders of magnitude. This could result in increased heating rates, lowered sintering temperatures, reduced sintering times and improved mechanical properties. Since microwaves can lead to energy transfer at the molecular level and rapidly generate heat throughout the volume of the material, the potential exists to reduce overall processing time with enhanced product quality in the case of predominantly thermal processes such as sintering. When microwaves pass through a composite/ mixture in which the constituents have different dielectric properties, they will selectively couple and heat up the higher loss tangent constituent. This effect can facilitate the selective heating of materials and could enable rapid “anisothermal heating reactions”

to occur. These microwave-enhanced rapid reaction processes have been found to have interesting applications in the sold-state chemical synthesis of materials with specific characteristics that are needed for various commercial/ industrial applications. Microwave processing offers several advantages over conventional methods in various application areas. These include significant enhancements in reaction and diffusion kinetics, much shorter process cycle times, substantial energy savings, finer microstructures that result in better performance products, eco-friendly processing, and more. In microwave-enhanced synthesis and sintering, enhancements in reaction kinetics and materials diffusion have been reported. The general observation has been that microwave-sintered products have finer microstructures and certain other features that result in considerable improvements in mechanical properties, leading to overall improvement in the quality and performance of the processed parts. Various ceramic materials and composites have been produced to advantage through microwave processing techniques. This article deals with one of microwave sintering’s real-world application products: zirconia-based dental restorations. CERAMIC INDUSTRY ³ April 2011

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ADS Temp Profile Temp (C) 1800 1600 1400 1200 1000 800 600 400 200 0

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An ADS microwave batch furnace for sintering zirconia-based dental restorations.

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Figure 1. An AMPS-9 continuous microwave furnace schematic with a temperature-time processing profile from an ADS batch sintering (top), and its conversion to temperature-distance profile for AMPS continuous microwave processing (bottom).

Material Characteristics Stabilized zirconia was introduced as “ceramic steel” in 1975 and was incorporated in biomedical applications as an alternative to brittle alumina. Since then, stabilized zirconia has been used in applications ranging from replacement femoral head implants to dental implants and restorations. The addition of 2-7 vol% yttria improves the strength of zirconia by changing the crystalline structure from monoclinic to tetragonal. While this provides increased fracture resistance, it can also make the material susceptible to an ageing effect called “low-temperature hydrothermal degradation.” Yttria can react with water vapor to form a hydroxide, which can, in turn, produce instability of the tetragonal phase and lead to the material reverting back to its original monoclinic structure. Such a structural transformation would be associated with an approximately 4.5% volume expansion, which can lead to the formation of microcracks and decreased grain adhesion strength in the material, and thus a loss of structural integrity and possible component failure. This process may take a few decades if the component is exposed to typical ambient temperatures, but it could be accelerated to a few hours if the exposure temperatures are in the 300-400°C range. According to research investigations, this hydrothermal degradation can be reduced or even eliminated by: • Adding another material (e.g., alumina or ceria) in small quantities to the 3 vol% yttria-stabilized zirconia (3YTZP) composition 18

• Controlling the microstructure during sintering • Decreasing the sintered grain size to ~ 0.42 microns

Microwave Sintering Advantages It is in this context that the microwave sintering of zirconia-based dental restorations assumes great practical significance. As mentioned earlier, microwave sintering could lead to finer microstructures in ceramics. Such characteristics in microwave-sintered, zirconia-based dental restorations could not only improve the strength of the material but, if the resulting grain size is comparable or less than the reported critical value of 0.42 microns, may also help reduce or eliminate the hydrothermal aging effect. The fine microstructure may provide an additional aesthetic advantage in greater translucency of the finished restoration, which helps achieve a more natural appearance for the end user (patient). Comparative analytical studies were undertaken of several different zirconiabased material samples sintered through conventional and microwave techniques. A 3Y-TZP composition was used for a detailed scientific study (“Flexure Strength and Hydrothermal Degradation of Yttria-Stabilized Zirconia: Microwave vs. Conventional Sintering”) by Arizona State University researchers Professor Pedro Peralta and Kirk Wheeler of the Department of Mechanical and Aerospace Engineering. The resulting samples were tested according to standards established

April 2011 ³ WWW.CERAMICINDUSTRY.COM

A crucible used to load the zirconia-based samples for microwave sintering in the ADS.

by the American Dental Association. Postsintered flexure strengths were measured and correlated with the sintering method and resulting microstructure. It was found that microwave-sintered samples had increased average flexure strength compared to identically prepared samples that were sintered in a conventional furnace. This was attributed to a sintering process that facilitates rapid densification due to enhanced sintering kinetics, as well as substantially smaller grain sized microstructure, through microwave processing. Long-term degradation effects were also studied through an accelerated ageing test that was performed to simulate the long-term degradation of 3Y-TZP in a humid environment. Samples sintered by microwave and conventional techniques were tested in a steam environment at approximately 125°C and 200 kPa pressure for 75 hours. Flexure strength decreased by around 43% for conventionally sintered samples, while the decrease of flexural strength was only about 14% for microwaves i n te re d s a m p l e s . T h e d e c re a s e d degradation of the microwave-sintered material was also attributed to much smaller grain size; the ageing effect is

AMPS Continuous Microwave Processing Furnace Specifications MW frequency Power Maximum temperature Control system An AMPS continuous microwave furnace, shown from the sample input side.

Data output Temperature measurement Atmosphere control System type Speed Crucible size Footprint Output

Control cabinets and an AMPS furnace, shown from the sample exit side.

decreased with decreasing grain size and is expected to be eliminated for grain size of around 0.43 microns. Though the grain size had not decreased to this critical size in the current microwave sintering trials, a decreased level of hydrothermal degradation was nevertheless observed. Additional improvements to the sintered grain size may be made by using starting materials of specific characteristics and using suitably modified sintering profiles.

Commercial Systems The results of the scientific study clearly reveal the advantages of microwave sintering over conventional sintering for dental zirconia-based materials. To take advantage of these findings on the commercial level, advanced microwave sintering furnaces specially designed for the dental restorations industry are now available in the U.S. One such furnace, the HAMiLab ADS* microwave batch furnace, is specifically designed to meet the low-volume production throughput requirements of individual dental labs. The ADS system is an air-cooled microwave furnace and offers an effective uniform heating volume of approximately 100 × 100 × 60 *Private labeled as the MicroSinterWave A1614.

2450 MHz 0.9-9.0 kW (variable) 1550°C Programmable, 8-in. digital input touch-pad, temperature, time, power inputs Calculated power, real power, temperature, time to data port Four thermocouples Two-channel gas flow meter (air, N2, Ar, mix) Pusher 15-600 mm/hr (adjustable) 150 x 100 x 60 mm (boats) 4 m long x 1 m wide x 1.5 m high (13 ft long x 3.1 ft wide x 5 ft high) 50-100 kg/day (size-dependent components)

mm within an applicator of around 265 × 265 × 315 mm. These ADS systems, with a maximum microwave power output of 1.1 kW, feature built-in computer capabilities for temperature programming and control in the range 250-1650°C. Temperature measurement and control is achieved through an IR pyrometer, while a touchpad control panel provides overall system programming and control. The system includes factory preset programs for automatic mode operation that would enable zirconia-based material sintering runs to be completed in about 90 minutes. Various operator-defined temperature ramp-up rates, temperature hold stages (up to about 1550°C) and hold times may also be programmed, if necessary. Test samples (sintered under conditions similar to those used in the previously mentioned scientific study) revealed increased flexural strength and decreased ageing effects in microwavesintered samples. For dental labs and establishments with higher volume production throughput requirements, the Spheric/SynoTherm AMPS continuous microwave furnace could be a viable option. Efficient and completely automated, this system is being used in high-temperature sintering, high-temperature reactions, and hightemperature heat treatment of various ceramic and non-ceramic parts and

compositions. Having an upper sinter zone operating limit of 1550°C, the furnace can be configured for sintering zirconia-based dental restoration parts as well. The AMPS-9 continuous system is a pusher-type furnace with rectangular crucibles of approximately 150 × 100 × 60 mm and a lateral system speed of 15-600 mm/h. The system, which is designed to provide microwave power output of 0.9-9 kW or higher (up to 100 kW, depending on customer needs and specifications), features built-in computer capabilities for temperature programming and control in the range of 100-1550°C. (See the specifications sidebar for additional details.) The system can be programmed for operation with various temperature ramp-up rates to predetermined temperature hold stages (up to around 1550°C) and hold times. Predetermined stages provide the system with the versatility required to develop processing regimes and profiles of relevance to various materials in general and zirconia-based dental restoration parts, in particular. Preliminary trials on an AMPS continuous microwave furnace have shown encouraging results for the successful industrial-scale, largethroughput microwave sintering of zirconiabased dental restoration products.

Scale-Up from Batch to Production Expanding from ADS batch microwave systems to AMPS continuous microwave CERAMIC INDUSTRY ³ April 2011

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MICROWAVE SINTERING

systems would enable larger throughputs for dental establishments that may have larger volume production needs. Once the best temperature-time profile for the zirconia-based composition of interest is established through ADS batch processing trials, this knowledge can be adapted to develop the AMPS continuous processing routine for larger production throughputs. This would mean transfer of the preferred processing profile in time from the ADS batch microwave furnace to a processing profile in space for the AMPS continuous microwave furnace. A schematic of the AMPS-9 continuous microwave furnace is shown in the middle of Figure 1. A total of 28 pusher boats are in the processing area at any time during the continuous operation. The furnace processing area is divided into three sections: preheat zone, sinter-heat zone and cooling zone. Four temperature monitoring points (T1, T2, T3 and T4) are included. Of these, the first three are active and provide feedback for microwave power regulation (and therefore temperature) at their locations. T1 can reach a maximum of 700°C, whereas T2 and T3 can reach around 1550°C. Each monitoring point can be used to program predetermined set temperatures in their respective locations. Shown above the AMPS schematic is the best time-temperature processing profile (ramp rates, holding temperature and holding time) obtained from successful sintering runs of zirconia-based dental restorations in an ADS microwave batch furnace. The AMPS system is then programmed for suitable set temperatures at T1, T2, and T3 to achieve a profile in the AMPS-9 system similar to that shown below the AMPS schematic. Both T2 and T3 are programmed to reach the required sintering temperature so there is a maximum temperature plateau in the T2-T3 section. A boat push-through rate is then chosen for the AMPS system that, when multiplied by the number of boats at the required temperature in the sinter-heat zone, corresponds to the optimized hold/soak time of the ADS microwave batch processing profile. 20

The hot zone and an exiting boat in an AMPS furnace, shown through the exit throat.

This enables each pusher boat to traverse the constant sintering temperature plateau region (or be in the sintering temperature region) for a period corresponding to the hold/soak period in the ADS batch microwave furnace sintering profile. Thus, a preliminary “temperature variation in time” profile can be used to obtain a corresponding “te m p e r a t u re v a r i a t i o n i n s p a ce (distance)” profile for optimum AMPS continuous microwave furnace operation. Such a strategy has been successfully implemented for the processing of certain types of ceramic materials in an AMPS continuous microwave furnace currently operating in the U.S. The results show that the broad, major challenges of scale-up from limited throughput batch production to larger throughput continuous production levels can be met using the advanced microwave continuous pusher furnace. The AMPS’ advanced capabilities, including programming and control capabilities for time-temperature, lateral material movement rate, and microwave power input—combined with the system’s continuous feed-through operation mode—help achieve the commercial-level, large-throughput microwave sintering of various dental restoration components.

flexure strength compared to samples sintered in a conventional furnace. This was attributed to a reduced grain size and a sintering process that encourages rapid densification due to the enhanced sintering kinetics produced by the microwaves. Samples tested in a steam environment at around 125°C and 200 kPa pressure for 75 hours showed a reduction of flexure strength by about 43% for conventionally sintered samples and only 14% for microwave-sintered samples. It was estimated that this corresponded to about 10 years of simulated testing in the mouth, after which microwave-sintered zirconia does not deteriorate significantly and is nearly 50% stronger than traditionally sintered zirconia. Industrial microwave furnaces are now available to exploit the advantages of microwave sintering for zirconiabased dental restorations. A batch-type ADS microwave sintering furnace has been specially designed for relatively smaller throughput dental labs, while an AMPS continuous microwave pusher furnace is available for larger throughput requirements. The processing profiles obtained in a microwave batch furnace can be a helpful step in the subsequent scaling-up of the process for larger production throughput with the AMPS continuous microwave furnace. 

Conclusions The microwave sintering of ceramics offers several advantages over conventional sintering methods. A detailed scientific study carried out by university researchers revealed that samples sintered in a suitable microwave furnace had an increased

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For more information, contact Spheric Technologies Inc. at 4708 E. Van Buren St., Phoenix, AZ 85008; call (602) 218-9292; fax (602) 218-9299; e-mail mkirksey@ spherictech.com; or visit the website at www.spherictechnologies.com.

➤ Several important factors should be considered when selecting a toll firing provider.

Toll Firing Success

by Dan Binz, Senior Sales Associate, Ceramics Division, Ipsen Inc., Pecatonica, Ill.

A

t oll firing service provider’s (TFSP) success is measured by its ability to provide timely and consistent service to its customers. Toll firing services mean different things to different customers, depending on their needs. However, services could include defining kiln schedules, determining availability, choosing temperatures or soak times, testing fired material, or simply responding positively to customer inquiries. Regardless of the services needed, several important factors should be considered when selecting a toll firing provider.

Material Expectations At the start of the selection process, familiarize yourself with the material you need to have fired. In these beginning stages, the TFSP is primarily going to be interested in the material itself, so it is a good idea to know if any potential dangers will be present before, during or after the firing. To that end, it is a good practice to supply a Material Safety Data Sheet (MSDS) with your quote request so the TFSP can review potential environmental, carcinogenic or handling concerns before proceeding.

It is also important to relay your expectations of success to your TFSP, who needs to know what you are trying to achieve with the material through the firing. Some of the common gauges of success include a specific surface area, bulk density, weight or color. In addition, you will want to have an idea of what you consider an acceptable yield. Initial sample testing can usually determine whether or not the expected yield can be achieved. All of this information will be helpful to the TFSP because it lets them compare results to their previous experiences and gives them a preliminary idea of the kiln requirements.

Firing Capabilities Once the material expectations are understood, the focus can be placed on the actual firing. Each toll firing service provider has different capabilities regarding the available kiln type(s), atmosphere, kiln capacity and firing cycles. However, each of these individual factors is important. Kilns Since different kilns have different capabilities, making the correct match is vital to the end result. A good TFSP should have a variety of kilns available to enhance customers’ options. Typical kiln varieties might include periodic (or batch) kilns, continuous roller hearth kilns, tunnel kilns, elevator kilns, rotary kilns or pit kilns. The TFSP should be able to provide technical information, including atmosphere, maximum temperature, minimum temperature, ramp rate capabilities and hot zone details, for each of its kilns. Outlining your temperature and soak time expectations to the potential TFSP is typically the easiest way for them to make a match. Atmosphere A firing project sometimes calls for a specific firing atmosphere, such as hydrogen or nitrogen. Each TFSP has distinctive CERAMIC INDUSTRY ³ April 2011

21

TOLL FIRING

capabilities for these types of requests. For example, some kilns run strictly on natural gas, which means that it is not possible to add any type of atmosphere to the firing. Depending on their resources, different facilities, kilns and TFSPs may have those options available. Capacity Interestingly, the required capacity changes for every individual project. Some R&D-type projects might include two pieces of 2 x 1 x 1-in. bar, while a separate project may require 40 tons of material to be pushed through a kiln each month. Kiln capacity can be dictated by several factors, including kiln type, dimensions, firing cycle and soak times. An additional consideration should be given to the size of the sagger or other ceramic vehicle used to transport the material through the fire.

Loaded kiln cars.

Firing Cycle Perhaps one of the biggest misconceptions that potential customers often have involves the firing cycle. Every kiln is different, which means that every new firing has the potential for issues to arise. Many customers ask for a recommendation about a soak time or ramp rate on a particular provider’s kilns, but the answer depends entirely on the material that needs to be fired.

Hi-Temp Microwave Furnaces This loaded kiln car is ready to be pushed into a tunnel kiln.

While the TFSP’s expertise is not with the material itself, they should certainly be willing to assist in answering any technical questions related to kiln operation. The fastest way to ensure success is to use a thorough sample testing program. With such a wide range of materials, it is important to work closely with your TFSP during this stage. Adjustments to soak times, ramp rates and temperature during testing will ultimately yield the end product you desire.

Other Considerations • Up to 80% reduced Spheric Technologies sells and energy use services systems in the Western • Up to 90% reduced Hemisphere utilizing the latest processing time microwave processing advances for ceramics, cermets, and powder • Finer grain and greater density metals. Benefits include: • Temperatures to 1600ºC

SPHERIC TECHNOLOGIES, INC.

4708 East Van Buren • Phoenix, Arizona 85008-6924 602-218-9292 Info@SphericTech Catalog available at www.SphericTech.com

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April 2011 ³ WWW.CERAMICINDUSTRY.COM

One of toll firing’s key components is the ceramic sagger or kiln furniture that holds the material during the firing. Some TFSPs manufacture their own saggers; these are usually included in the price of the firing. In other cases, customers might want to provide their own saggers or use a material formula that the TFSP does not have. Either way, an effective TFSP should be willing to work with customers to reach a solution. If the customer is not going to provide their own saggers, some consideration should be given to the content of the saggers to ensure that they will not contaminate the product. Generally speaking, the TFSP should be able to work with you on your ceramic needs. You may want to consider the cost of shipping the material to and from your customer. Selecting a TFSP located near your

facility may save a significant amount of time, as well as money on shipping costs. You can also discuss warehousing options with your TFSP. Warehousing can be advantageous if you have large quantities (perhaps a truckload) that need to be shipped together to save shipping costs. Ask prospective TFSPs about their capabilities for packaging. Some common forms of deliverable materials include sacks, supersacks, barrels or drums. It is important to know that your TFSP has the capabilities to process each of these. You should also discuss how the material is to be shipped back. For instance, if the material is sent in a drum, will a second, empty drum be included to return the material? While these may not seem like major logistical issues, it is best to know all of the potential “hidden” costs. It is also a good practice to ask the TFSP what has been fired previously in the kiln. After prolonged or consistent use, the

lining of a kiln can become sponge-like and retain particles of previous material, especially if the material is very fine and susceptible to being airborne. If a material is held in the kiln lining and the kiln blower adds air circulation, your product could easily become contaminated. Another factor to contemplate, albeit to a much lesser degree, is the cleanliness around the vicinity of that particular kiln. While it may be a difficult variable to control, a good TFSP should strive for a very clean facility in and around its kilns. There have been documented instances in which a material was contaminated because adjacent kilns had a loose powder, unnoticed by anyone, that was blowing around the facility. Some TFSPs will be able to put up shields or dividers; however, as mentioned previously, this can sometimes be a difficult factor to control. Finally, some parts require post-firing services, tests or additional processes.

Most TFSPs are generally able to screen, sift or break down the material to a specific grain size. Keep in mind that these services usually incur additional costs, which should be weighed against performing the process in-house.

Successful Production Choosing the best TFSP for your company should not be an overwhelming task. Find an experienced company with which you are comfortable—one that makes economic sense and offers the capabilities you need. Remember that the best way to determine whether or not a process will be successful is through a significant sample testing program. Once testing success is achieved, you are better assured of success in production.  For more information, contact Ipsen at P.O. Box 420, Pecatonica, IL 61063; call (815) 2392385; fax (815) 239-2387; or visit the website at www.ipsenceramics.com.

CERAMIC INDUSTRY ³ April 2011

23

Measuring Fuel Energy

➤ The continuous monitoring of the calorific value of mixed gaseous fuels is on the rise. by Chris Schaeffer, President, Control Instruments Corp., Fairfield, N.J.

I

t is becoming increasingly important to measure fuel energy, which is formed by complex mixtures of combustible and non-combustible gases, and vapors. These gases and vapors can vary in concentration and composition over time. Whether a non-traditional fuel source is an undesirable byproduct of chemical processes (and therefore should be destroyed before it is released into the atmosphere) or a potential alternative energy source from a landfill or biomass, it will likely present some measurement challenges. Possible challenges can stem from the rate of change or the presence of a wide range of water vapor at different process temperatures. Perhaps the combustibles vary in composition under different process conditions. Maybe the heating value itself even varies from very lean at some times to very rich at others. In any case, measuring the calorific value can often be difficult. For fuel mixtures, the measurement should be fast and continuous, with a universal response to any gaseous fuels over a wide measurement range. A heated sample handling system is essential.

Note that for gaseous fuels, two calorific values are defined: the lower heating value excludes the heat energy present in the water formed by combustion, and the higher heating value includes that energy. This is necessary because, in addition to heat energy, fuels that contain hydrogen atoms create hot water vapor as a byproduct of combustion. (Calorific values that involve the effects of moisture and ashproducing substances on the amount of energy released by burning—“as received,” “dry,” “ash-free,” “dry and ash-free,” etc.— can be important for solid and liquid fuels, particularly wood and coal, but they are not pertinent to most gaseous fuels.) For the higher heating value, the heat energy present in hot water vapor (known as heat of vaporization or heat of condensation) that is produced by combustion can be 5-15% of the total energy released by the fuel. If this can be recaptured and put to use in the process (e.g., by condensation back into liquid), it can be an important contribution to the total energy available from the fuel. Processes that do Table 1. Calorific values of pure fuel gases.

Background Calorific value, also known as heating value, is the energy density of a fuel or the amount of heat energy released when a given amount of fuel burns (see Table 1). For gaseous fuels, common units of measurement include BTU per cubic foot or megajoules per cubic meter (26 BTU/ft3 = 1 MJ/m3). 24

April 2011 ³ WWW.CERAMICINDUSTRY.COM

not recapture this heat only realize the lower heating value of the fuel. It is important to note that all hydrocarbon fuels produce some water vapor, which contains about 5-10% of the energy yield, but there are exceptions. Carbon monoxide (CO) has no hydrogen and burns without producing water vapor, so its higher and lower heating values are equal. Hydrogen, which produces proportionally more water vapor than other fuels, has a larger difference between its higher and lower heating values than other fuels; about 15% of the energy from burning hydrogen is contained in hot water vapor.

Measurement Processes In non-conventional fuels, significant and varying amounts of water vapor might be present in a gaseous fuel mixture before it is burned. This may mean that a wetbasis measurement should be made; a wet-basis measurement involves analyzing a sample of the fuel without removing any water vapor through condensation

Table 2. Response factor for a number of fuel gases.

from temperature or pressure changes. Otherwise, the loss of water vapor erroneously increases the concentrations of the remaining gases in the mixture before reaching the analyzer, thereby producing a large error. (It is possible, but not preferable or practical, to recover and measure the removed water vapor to correct for dry basis measurement error.) At atmospheric pressure, saturated water vapor may constitute up to 20% of the mixture’s volume at 60ºC (140ºF), but only 2% at 20ºC (68ºF). As shown in Figure 1 (p. 26), if a sample saturated with water vapor is taken at 60ºC and is allowed to cool to 20ºC prior to measurement, 18% of the sample volume turns to liquid. When the remaining gases are measured at 20ºC, the concentrations are 22% higher in the partially dried sample than in the true 60ºC mixture. Measurements taken on partially dried samples have large errors. Under most conditions, keeping all parts of the sampling system and analyzer at 120ºC (250ºF) prevents this error. In addition, a heated analyzer prevents condensation of heavier, less volatile hydrocarbons. Keeping all sample-wetted parts of the sampling system and analyzer at a high temperature ensures that these combustible vapors are properly measured. A related effect occurs in a sample pump system (see Figure 2, p. 26). Even without a drop in temperature, the pump’s pressure rise lowers the dew point and condenses out water, thus unintentionally increasing the concentration of the remaining gases. For a 60ºC mixture saturated with water vapor at atmospheric pressure, a 15+ psig pressure rise condenses half of its water

volume. The concentrations of the remaining gases increase, which causes an error of about 10%. Since many fuel mixtures contain a variety of combustibles gases and vapors, along with nitrogen, carbon dioxide, and water vapor, it is important to consider the response of the analyzer to each component. An analyzer’s response to a particular gas relative to a standard reference gas is known as the response factor. The response often varies. A calibration procedure can be used to correct the reading for a single gas or specific mixture, but it is not practical for mixtures that change composition or are not well known. In an ideal analyzer, all response factors would be identical. In practice, no analyzer is ideal, but it is possible to have response factors that are close enough to minimize errors. Because it actually burns a sample to determine the calorific value, a micro-combustion calorimeter is a direct measurement and provides good response factors (see Table 2). In addition, an analyzer should feature a fast response time so that it can quickly respond and activate controls for gas-blending optimization. Applications include flare stacks, biofuels, turbine engines and feed-forward control.

Accurate Performance The performance and measurement of a combustion calorimeter can be greatly improved by adding a known, controlled amount of hydrogen to the sample stream prior to combustion. This stabilizes the flame and keeps the measurement accurate over a wide range of calorific values. The

flame would then be lit and measured accurately even when the calorific value is zero. By necessity, the flame in a hydrogenfueled combustion calorimeter is small, and the hydrogen fuel requirement low. Careful control and compensation for fuel and sample flow allows a precise measurement from a small flame size in an apparatus that is small enough to be thermostatically heated to a high temperature.

The performance and measurement of a combustion calorimeter can be greatly improved by adding a known, controlled amount of hydrogen to the sample stream prior to combustion. The small flame responds quickly to changes in concentration by using temperature detectors with low thermal mass. This analyzer has the characteristics needed to quickly and continuously measure the heating value of a variety of combustible gases over a wide range of measurement.

Summary Several key points should be considered when designing a system for the continuous monitoring of the calorific value of mixed gaseous fuels: • Heating prevents errors that result from the condensation of water vapor. The sample stays intact during measurement. • Heating allows combustible gases with low vapor pressure (high boiling CERAMIC INDUSTRY ³ April 2011

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MEASURING FUEL ENERGY

•

• Figure 1. Temperature effects on process readings.

•

•

Figure 2. Pressure effects on process readings.

points) to be measured without losses in the sampling system. False low readings are avoided. The aspirated system does not increase pressure above the process conditions, which prevents condensation of water vapor or combustible gas that would otherwise condense. The sample is not affected. Combustion calorimeters provide good response factors, which is especially useful for unknown mixtures or “anything that burns.” The use of hydrogen fuel stabilizes the flame and widens the measurement range (including zero). The flame is always ready to measure. The instrument’s speed provides a continuous measurement that is useful when process conditions can change quickly. Speed can sometimes be as important as accuracy. 

For more information, contact Control Instruments Corp. at 25 Law Dr., Fairfield, NJ 07004; call (973) 575-9114; fax (973) 5750013; e-mail [email protected]; or visit www.controlinstruments.com.

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special section | advanced ceramics/glass

Flexible Ceramic Membranes for Green Applications

by John Olenick, President, ENrG Inc., Buffalo, N.Y.

O

ur planet is changing as a result of higher levels of carbon dioxide (CO2) in the atmosphere. According to the National Oceanic and Atmospheric Administration (NOAA), which has measured the CO2 level since 1960, the current level of 390 ppm represents a 26% increase over that of 1960.1 Similar increases over the next 50 years will bring the CO2 level to nearly 500 ppm. Since a direct relationship exists between the CO2 level and the earth’s temperature variations, many expect that a level exceeding 450-500 ppm will be extremely uncomfortable—if not life changing—for humans and other species. In Hot, Flat, and Crowded, Thomas Friedman states that the earth’s six billion people are split into three distinct groups: one billion live very comfortably with an abundance of energy, food, clean water and air; two billion are about to join those comfortable one billion; and the remaining three billion have little to none of these four basic needs. Today’s unserved energy markets, particularly in the emerging economies of China, India, Africa and much of South America, will provide tomorrow’s opportunities. The huge global demand for clean and efficient energy, stable food, and clean water and air will spawn boundless opportunities for new production and distribution solutions.

➤ The huge global demand for clean and efficient energy, stable food, and clean water and air will spawn boundless opportunities for fuel cell technologies. Today’s commercialization efforts for fuel cell technology and other advanced energy methods will be an important part of the overall solution.

Electrolyte-Supported Fuel Cells ENrG Inc. worked w ith Corning Incorporated for five years to integrate ultra-thin, flexible ceramic sheets into the fabrication of electrolyte-supported fuel cells (ESCs). ENrG established a state-ofthe-art fabrication line to focus on the printing, handling, sintering and testing of the thin and robust fired electrolyte (U.S. patent number 5089455). In 2008, ENrG licensed the membrane technology for fabrication of the thin electrolyte and, in the following year, successfully demonstrated a proprietary green tape process to produce highly flexible 25-40 μm thick fired electrolytes. (Electrode inks were developed with Heraeus Inc.) Also in 2009, ENrG introduced its Thin E-Strate™ and ThinESC™ (thin electrolyte-supported cell) products in Europe and provided substrate samples and initial button cells to system manufacturers for evaluation. Flexible ceramic membranes are required for today’s new high-

temperature fuel cell systems. These systems, operating at > 700°C, subject the membrane to an extremely harsh environment. The tri-layer membrane, a combination of thin electrolyte with electrodes on both sides, produces energy through an electrochemical process that combines hydrogen and oxygen into water across the membrane. Over a 5000-40,000 hour operating life, these membranes typically lose their electrochemical ability to produce energy. To achieve a broader level of market acceptance, a high-temperature fuel cell system must retain > 80% of its original capacity at 40,000 hours of life. The system-level power performance degradation is directly attributable to the fuel cell stack and the membrane in each electrochemical cell of the stack. The thicker (100-150 microns) and typically weaker membranes currently in use can microcrack or completely fracture over time. They can also become electrochemically poisoned due to contaminants from other system components, or the fuel and/or air streams. Microcracking or fracturing is the direct result of the thermo-mechanical issues that result from cycling the system CERAMIC INDUSTRY ³ April 2011

27

FLEXIBLE CERAMIC MEMBRANES

Figure 1. Cross-section of a dense, 40 μm thick electrolyte coated with a thin anode and cathode on opposing sides.

and membranes from room temperature to the > 700°C operating temperature while the system is sealed within a metal cassette. Electrochemical contamination results from the effects of longer-term operation within a steam atmosphere, which can lead to chemical contamination from the many materials within the system, including the Cr within the stainless steel components.

Potential Applications The role of ceramic materials and flexible ceramic membrane manufacturing processes is becoming increasingly important in the cleantech market space and its many applications. In the past several years, cleantech has garnered a tremendous increase in funding and venture capital attention. In some cases, key system components such as solid oxide fuel cell (SOFC) stacks are nearly entirely composed of ceramic materials and could not function without them. Ceramic membranes provide functions across the cleantech landscape, including ion transport, thermal management, catalysis of gases and liquids, power generation, energy storage, hydrogen purification and storage, generation of light, and energy from waste processes, among many others. The high performance of ceramic membranes makes them strong candidates to fill critical technology gaps in many applications and industries, including advanced nuclear energy, air pollution control, solar energy, biofuels and biorefining, carbon sequestration, high-capacity energy storage, the hydrogen infrastructure, solid-state lighting, thermoelectric, thin-film solar, waste-to-energy, water remediation, harsh environment sensors, and wind power. Increased production volumes and their resulting cost reductions are a prerequisite for the commercialization of many clean energy technologies. Using the same technology, component and/or manufacturing process to meet the 28

April 2011 ³ WWW.CERAMICINDUSTRY.COM

requirements of many cleantech applications will help reach cost targets and accelerate commercialization. Electrolytesupported SOFCs typically use a zirconia-based membrane for the substrate. This same membrane product has volume opportunities outside of SOFC applications in areas such as sensors (gas or vibration), gas separation, gas generation and electrolysis, to name a few. The same properties required for the membrane in electrolyte-supported SOFCs are often the same properties of value in other markets. The density, high strength and chemically inert properties of thin 3YSZ substrates result in gas-tight membranes that are excellent choices for severe environment and/or hightemperature applications. These ultra-thin membranes have the ability to flex in and out of the plane of sealing such that they stress relief during system operations. Other applications can benefit from the membranes’ ionic conductivity, superior mechanical properties and low thermal mass. Functional coatings are applied using thick or thin film, spraying, direct writing, or other standard deposition methods.

Flexible and Robust While most people think about ceramics in terms of brittle, inflexible materials that easily break if dropped or hit, ceramics can be formulated and processed as thin membranes that yield flexible, translucent sheets that can nearly be rolled around the circumference of a pencil. These membranes with coated electrodes are desirable in the production of highly efficient, low-resistant SOFC systems. Since they can be produced in thin supports, thereby reducing the resistance and increasing the power output, they help reduce the system cost by reducing the number of cells in the stack (or producing more power for the same number of cells in the stack). The market price for micro-combined heat and power (CHP) energy systems in the U.S. is $1000/kilowatt (using the residential market as the benchmark). The price is higher in Europe, but much smaller systems are required there. Current SOFC systems are beyond this figure by a factor of 8-20x. Significant design improvements and manufacturing cost reductions are required to reach the < $1000/kilowatt cost target. The fuel cell stack is approximately 40-60% of the system cost; the remainder is the balance of plant. The demonstration of new manufacturing technology that significantly reduces the cost of cell manufacturing while increasing the surface area on thin membranes is key to reaching these price figures. Critical system components in a SOFC system include a fuel reformer, fuel cell stack, controls and power conditioning. The fuel cell stack is the heart of the system, serving as the source of electricity and heat. Key SOFC technology challenges include the demonstration of stable long-term performance, the need for larger area cells/stack designs that can withstand thermal cycling, and cost reductions for stack components and stack assembly. While many companies focus on improving the stability of their longer term stack performance, few have focused on

Table 1. Thin membrane properties and applications. Gas Tight Flexible Thermal Mechanical Low Thermal or Thin Shock Strength Conductivity Resistant SOFCs • • • • • Sensors • • • • • High-temperature • • • • membrane separation Electrochemical energy • • • • • generation Electronic substrate • • • • Energy storage • • • • • Advanced materials • • • • Cryogenics • • • • Bioceramics • • •

A 40 μm thick membrane folded into nearly a figure eight.

ways to simultaneously achieve thermal cycle survivability, stable performance and low manufacturing costs. Thermal cycle survivability is an often overlooked “make-or-break” requirement for many CHP applications. Without thermal cycling tolerance, SOFC-based systems must be left on at all times, even in the summer when little or no waste heat is needed, or while the building occupants

Electrically Insulating

Lightweight

Ionic Conductivity

Chemical Resistance

•

• • •

• •

• • •

•

•

•

•

• • • • •

• • •

• •

• •

•

•

•

are away on vacation. This significant waste of energy detracts from the positive aspects of SOFC technology. Table 1 shows the thin membrane properties for ENrG’s Thin E-Strate™ and ThinESC™ technology, as well as potential applications for this technology. The ability to relieve stress through flexing provides thermal shock tolerance and the cycling durability required for CHP applications. As a “substrate,” this thin ceramic sheet is strong enough for handling and additional processes such as applying electrodes and current conductors through an inexpensive screen-printing process. Figure 1 shows a cross-section of a dense 40 μm thick electrolyte coated with a thin anode and cathode on opposing sides. The electrolyte technology is based on 3YSZ. Most electrolyte-supported fuel cell designs are based on 8YSZ, 10YSZ, ScSZ, YbSZ and other exotic materials. While the latter materials have higher oxygen ionic conductivity and therefore higher power performance, they are much weaker than 3YSZ. The minimum thickness of these electrolytes is about 110-150 μm, and durability has been sacrificed for performance. One key to increasing the power p e r f o r m a n ce o f t h e l ower i o n i c conductivity of 3YSZ is to fabricate as thin a membrane as possible, thereby reducing electrical resistance. The 2009 introduction of the 40 μm thick electrolyte (~65 μm overall with electrodes) was a major first step; prototype quantities

were achieved through single caster runs. The next target is 25 μm thick electrolytes in 2011, and thinner beyond that. With the 40 μm thick electrolyte and inks developed so far, a power density of 250 mW/cm2 at 850ºC has been achieved; it is expected that the power density will exceed 400 mW/cm2 by mid-2011.

Summary SOFC technology has a ways to go before reaching the target 40,000 hour lifetime for commercialized systems. Many system manufacturers now require early adopters to absorb the cost of a second stack within the 40,000 hour lifetime warranty of a purchased system. Ultra-thin-film ceramic membranes offer unique design and performance advantages that make them well-suited to meet the demanding requirements of many new energy and environmental technologies in the emerging cleantech market space. Low-resistance, ultra-thin membranes that can be tailored to many different functions, and applications can aid in solving global energy and environmental challenges.  For more information, contact ENrG Inc. at 155 Rano St., Suite 300, Buffalo, NY 14207; call (716) 390-6740; e-mail [email protected]; or visit www.enrg-inc.com.

Reference 1. Earth System Research Laboratory, Global Monitoring Division, www.esrl.noaa.gov/gmd/ccgg/trends/. CERAMIC INDUSTRY ³ April 2011

29

➤ Lead-free glass pastes can offer multiple bonding advantages es in MEMS wafer level packaging.

d n Bo r e t t e B A

by S. Sridharan, Global R&D/AT Manager for Electronic & Specialty Glasses;* V. Dragoi, Chief Scientist;** B. Gardner, Senior Applied Technologist;† J. Holthus, Senior Technician;† and D. Gnizak, Analytical Microscopist*

D

ue to rapid advances in consumer electronics, automotive electronics and mobile communication, the microelectromechanical systems (MEMS) market is growing rapidly.1 Applications for MEMS cover diverse fields, including automotive, aeronautics, consumer, defense, industrial, medical and life science, and telecommunications. Various MEMS devices require a vacuum level or controlled atmosphere operation to ensure either good performance or an acceptable operation lifetime. Different wafer bonding technologies are commercially used for MEMS packaging.2-7 Among these, glass frit bonding7 offers multiple advantages, such as superior hermeticity, less stringent surface roughness requirements and tailored expansion matching to the materials being joined.

achieve the required hermetically sealed assembly. The quality of the resultant seal (or bonding) is both a function of the seal glass material used and the process variables employed in both glazing and frit bonding. The interactions between these variables are important to improve the quality of the seal. A study was undertaken to discover the effect of seven process-related factors

(pre-glaze temperature, back fill type, peak temperature, time at peak temperature, ramp rate, force applied during bonding, and cool-down rate) in the frit bonding process while keeping the glazing conditions constant. Additional attention was directed at the effect of two types of pastes (leadfree pastes DL11-205 and HT753 vs. leadbased paste FX11-036) on the quality of the bonding as measured by bond strength

Table 1. DOE Taguchi L18 design matrix.

Process Basics In glass frit wafer bonding, sealing glass paste is screen-printed into the desired geometry. This layer is dried in an infrared (IR) oven, and then fired in a furnace to burn the binder and pre-fuse the sealing glass layer. Called glazing, this process is usually done in either a belt or box furnace under atmospheric conditions. In a process known as frit bonding, the pre-glazed wafer is placed in a wafer bonder and bonded to a cap wafer in a temperature/time/pressure cycle under the desired vacuum or backfill level to 30

April 2011 ³ WWW.CERAMICINDUSTRY.COM

*Ferro Corp., ECGM Division, Independence, Ohio **EV Group, Florian, Austria † Ferro Corp., ECGM Division, Vista, Calif.

special section | advanced ceramics/glass

Table 2. Responses vs. effects for experiments in Table 1. Optimum conditions for each paste type are coded in blue.

Table 3. Inferences that could be deduced from the study.

and uniformity, the size and type of voids in the bond lines, and metal (lead or bismuth) precipitation at the interface.

Experiment Details The study used a Taguchi L18 screening d e s i g n 8 w i t h e i g h t f a c to r s — o n e qualitative material variable (B) and seven quantitative bonding variables (A and C to H), as well as four responses (see Table 1). The sealing glass pastes used in this study included the lead-based FX11-036 and the lead-free DL11-205 and HT753 (all manufactured by Ferro Corp.). The pastes were screen-printed on 6-in.-diameter (thickness, 675 μm; weight, 28.14 ± 0.50 g), borondoped silicon (Si) wafers. The sealing glass pattern was printed using 325 mesh screen (45° mesh angle/1.1 mil diameter/1.2 mil emulsion thickness) using a 0.3 in./min squeegee speed and 80 mil snap-off distance.

For both cases, the average dry print thickness was 27 μm; the average fired thickness was 17 μm after glazing and 9 μm following the final frit bonding step. After screen printing, the wafers were dried in an IR belt dryer with a 120°C peak temperature. The wafers were then randomized for additional processing steps. The sealing glass patterns on the bottom wafers were fired in the glazing profile shown in Figure 1(a), 295°C (40 min) binder burnout and 410°C (15 min) glazing, in a four-hour box furnace cycle with adequate air flow. After the glazing step, the cap wafers were sealed to the bottom wafers (glazed sealing glass pattern) in an EVG520IS wafer bonder. Figure 1(b) shows the typical glass frit wafer bonding cycle that was used. All of the experiments in Table 1 were performed in random order with one repeat for each experiment. The resulting bond lines were examined by SAM and

Figure 1. Processing details for the time-temperature cycle used in the glazing step (a) and the time-temperature-piston force-backfill cycle in glass frit bonding (b).

cross-sectional SEM, as well as EDAX analysis, for adherence to the wafers, size and location of voids, cracks, metal (lead or bismuth), and other precipitates. These observations were quantified into four responses as shown in Table 1 for analysis in DOE, similar to an earlier publication for lead-based MEMS sealing glass pastes.9

Results Figure 2 (p. 32) shows the SAM surface CERAMIC INDUSTRY ³ April 2011

31

A BETTER BOND

Figure 3. Marginal means plot and Pareto chart for metal precipitates response.

Figure 2. SAM and SEM cross-section images of the lead-free paste (a) and lead paste (b).

image and SEM cross-sectional images for optimum processing conditions for the two different types of pastes considered for this study. The SAM images depict the quality of the bond lines across the entire wafer. More sharp and uniformly dark (distinguishable) bond lines indicate a higher quality bond. The cross-sectional SEM images in Figure 2 provide information on voids, debonding tendency, cracks, metal (lead or bismuth) and other precipitates in the seal. The criteria outlined in Table 1 were used to quantify the responses from each experiment. A summary of the responses for each experiment is shown in Table 2 (p. 31). Lower numerical scores for each response indicate a better quality of the frit-bonded seal with respect to that defect. A combined minimum for all four responses signifies the best condition for glass frit bonding. The marginal means plot and Pareto chart for the measure of metal precipitates at the glass/Si interface response is shown in Figure 3. The steeper the line in the marginal means plot and the higher the bar in the Pareto chart, the more significant the variable is for that response. Figure 3 shows that the paste type has the strongest influence on metal precipitation. 32

Although not shown here, similar plots for the other three responses were obtained and analyzed. In general, lower peak temperatures led to smaller voids and smaller and fewer lead precipitates at the interface for the lead paste (FX11-036), and no metal precipitates for the lead-free paste (DL11-205). Although not plotted here, interaction plots (between variables) showed that peak time must increase as the peak temperature decreases in order to produce a good glass frit-bonded microstructure. Table 3 (p. 31) includes a summary of inferences that could be deduced from this study. All four responses that affect MEMS seal quality are optimized by using a lead-free glass paste with a lower preglaze temperature (410°C) and air or no gas used as back fill. A peak temperature of ) 450°C for 15-30 min eliminates metal precipitates and reduces debonds, voids and cracks. Defects in SEM were also minimized with a ramp rate of 18°C/min and a bonding force of 4000 N. A cool-down rate of 20°C/min helped to eliminate metal precipitates and defects in SAM. From the DOE, the optimum processing conditions for the lead-free glass paste (DL11-205) include: • Glazing: 410°C (15 min) • Backfill: Vacuum or partial air • Bonding: 450 ± 15°C (15-30 min) • Ramp and cool-down rates of ~ 20°C/min • Bonding force: 4000 ± 800 N for 6-in. wafer

For more information, contact Ferro Corp. at 7500 E. Pleasant Valley Rd., Independence, OH 44136; call (216) 750-6947; fax (216) 750-6915; e-mail [email protected]; or visit www.ferro.com.

References

Conclusions

1. Market Forecast, Yole Development, France, www.yole.fr. 2. R. Stengl, T. Tan, and U. Gösele, J. Appl. Phys., 28, 1735 (1989). 3. C. H. Tsau, S. M. Spearing, and M. A. Schmidt, J. of Microelectromech. Systems, 11, 641 (2002). 4. G. Wallis and D. Pommerantz, J. Appl. Phys., 40, 3946 (1969). 5. V. Dragoi, T. Glinsner, G. Mittendorfer, B. Wieder, P. Lindner, SPIE Proc. Series, vol. 5116, p. 160, Bellingham, WA (2003). 6. J.-W. Yang, S. Hayes, J.-K. Lin, and D. Frear, J. of Appl. Phys., 95, 6077 (2004). 7. M. Petzold, C. Dresbach, M. Ebert, J. Bagdahn, M. Wiemer, K. Glien, J. Graf, R. Muller-Fiedler, and H. Hofer, Proc. of “10th Intersociety Conf. on Thermal and Thermomech. Phenom. in Electronics Syst., ITHERM ’06,” IEEE Proc. Series, 1343 (2006). 8. S.R. Schmidt, and R.G. Launsby, “Understanding Industrial Designed Experiments,” pp. 3-47 Air Academy Press & Associates, Colorado Springs, CO 80920 (2005); DOE software SPC XL2000, licensed from Air Academy Associates LLC was used for this study. 9. S. Sridharan et.al., “Effect of Process Variables on Glass Frit Wafer Bonding in MEMS Wafer Level Packaging,” Paper 1139-GG03-35 in Mater. Res. Soc. Symp. Proc. Vol. 1139, (2009), Materials Research Society.

Both lead-free and lead-based glass pastes can be used in the glass frit bonding of MEMS wafers for MEMS wafer level packaging. A lead-free paste was shown to offer a wide processing window. In addition, metal precipitates at the Si/glass interface are absent with the lead-free paste, while they are prevalent with the lead-based paste. 

Editor’s note: This article is based on a poster paper presented at the 11th International Symposium on Semiconductor Wafer Bonding: Science, Technology & Applications at the 218th ECS Meeting, Las Vegas, Nev., October 10-15, 2010. The information has been reproduced with the permission of The Electrochemical Society.

April 2011 ³ WWW.CERAMICINDUSTRY.COM

➤ Manufacturers are now taking video collaboration outside of the boardroom and onto the plant floor.

special report | resource management

Advances

in Video Collaboration by Marieke Wijtkamp, Vice President of Marketing and Client Services, Librestream Technologies Inc., Winnipeg, Manitoba, Canada

V

ideo conferencing has become a standard form of communication across enterprises. In fact, video conferencing is expected to become a $10.8 billion industry by 2015. The standard form of video collaboration facilitates faceto-face meetings in video conferencing meeting boardrooms. For manufacturers, though, the heart of their business is often the plant floor—where traditional video conferencing doesn’t reach.

Secure Mobile Video With the development of new mobile technologies, the opportunity for video collaboration has expanded. Manufacturers are now taking video collaboration outside of the boardroom and onto the plant floor, to a supplier location, or into the field where the problems are occurring. These mobile technologies generally include wireless video devices for use on

the plant floor and collaboration software for the remote experts’ desktops. Plant workers use the mobile device to share video, voice, telestration (i.e., onscreen drawing) and images with the experts who interact live through the collaboration PC software. Remote experts can also share images or pre-recorded videos to play on the touchscreen panel of the device. By sharing this visual content, the experts can provide plant floor personnel or field technicians with visual instructions. For many manufacturers, their plant floor operation contains competitive and sensitive information; for this reason, cameras are typically not allowed on the plant floor. In many Fortune 1000 companies, potentially “rogue” video devices such as smart phones must be checked at security. New video conferencing mobile devices overcome that concern by providing tight security over the wireless communication, media content and device usage. Security,

encryption, authentication and even centralized administrator control have become tablestakes for mobile video collaboration products.

Reduced Downtime For one major consumer packaged goods (CPG) manufacturer, this kind of mobile collaboration has helped in various operational situations, including production line equipment maintenance and repair, supply chain interaction, and OEM vendor communication. Video collaboration was first used on the CPG manufacturer’s plant floor to help maintain and repair critical production line equipment. If a machine was down and the right engineer was not available onsite to troubleshoot the problem, downtime rapidly escalated. By using the mobile video device to show a remote expert the failed equipment, the manufacturer was able to remove costly delays from the repair CERAMIC INDUSTRY ³ April 2011

33

VIDEO COLLABORATION

process. Together, the production line engineer and remote specialist can now collaborate to identify immediate corrective action plans. Production equipment downtime costs can be staggering. With downtime costs averaging from $500 for a standalone machine, $1500-8500/hour for a production cell or even as much as $3500/ minute for an entire auto factory line, reducing downtime is critically important. Trying to troubleshoot an equipment problem through pictures via e-mail or waiting for an offsite specialist to travel to the problem site adds costly hours that can be easily avoided with mobile collaboration technologies. Much of this delay can be reduced or eliminated by bringing the problem to the expert, as opposed to the other way around.

to perform live visual communication when needed. The camera optics within these mobile devices are so advanced that remote experts can see detailed design aspects where even a fraction of a millimeter matters. In some cases, third-party cameras such as microscopes or borescopes can also be attached to the mobile device to show the remote experts even more detailed visuals. By interacting live with suppliers on the plant floor, this manufacturer has accelerated product delivery, reduced travel costs, and leveraged scarce expert resources in their own company and that of their supply chain partners. The CPG manufacturer also uses mobile collaboration with its OEM vendors to perform acceptance test processes on new production line

The off-site expert views video, photos and drawings to help plant personnel find a solution.

with the mobile collaboration device to stream video and interact with colleagues to perform the acceptance test. Expense savings in this application alone have been as high as €50,000 (approximately $67,500) in just one use.

Remote Process Reviews

Plant personnel share video of problematic equipment and discuss solutions with off-site experts.

Improved Supplier Interaction The CPG manufacturer also uses mobile collaboration to streamline supply chain interaction. Design reviews and first-run production samples are an ongoing part of standard communication with suppliers. Normally, team members would travel to the supplier locations for live interactions, introducing delays into the process. Instead of travel, the mobile devices are now kept or shipped to major suppliers 34

equipment. The process was traditionally conducted at the supplier site. Multiple skill sets were required to adequately inspect and test the new production line equipment, which equated to teams of people travelling to the supplier’s facility. In many cases, the OEM vendors were not just in the next state, but in another country or continent. Instead of sending a team of people, this manufacturer now sends one person

April 2011 ³ WWW.CERAMICINDUSTRY.COM

For global manufacturers with internal or supplier locations around the world, the importance of visual communication becomes even more important to overcome language and cultural barriers. For one supplier to the automotive, aerospace and medical industry, mobile video collaboration has helped visually connect engineers in technical centers with plants in locations such as Mexico. In one instance, the manufacturer experienced an abnormally high scrap rate for one of its products. Language barriers and the inability to capture movement made e-mail and phone communication insufficient to resolve the detailed process issues. Instead of sending specialized engineers to Mexico, the manufacturer held a live collaboration session. The team in Mexico streamed video from the plant floor using the mobile device to show the engineering team the existing production process. By seeing the process live, the specialists identified numerous process errors. They then communicated the problems and corrective action steps during the live collaboration session. To make sure the feedback was clear, the production team in Mexico then showed the remote engineering team

Screen shot of the video collaboration software.

the revised process. This collaboration took three hours instead of the estimated three or four days that typically resulted from attempts to correct problems over e-mail or travel. As a result, the scrap rate immediately decreased by 25% after the new process was implemented.

networks through mobile Wi-Fi hotspot devices such as the MiFi or Cradlepoint. By using a hotspot device, a wireless network can be created for the mobile device anywhere there is adequate cellular coverage. For example, heavy industrial equipment manufacturers use cellular connectivity to perform live collaboration from the field when they need help repairing equipment. Deferred collaboration is another possible alternative to a live video session. When access to the Internet isn’t available or other challenges arise, such as problems in connecting with experts due to time zone differences, the video devices can record to a local SD card. The recording can be uploaded to a shared directory for the remote expert to access later, or the device operator can share the recording in a deferred live collaboration session with a remote expert. While the recording is playing, both parties can still talk, telestrate and share images in a fully interactive deferred session.

Internal Education With the emerging problem of aging workforces, leveraging scarce expert resources can also be a major concern. For one manufacturer of industrial equipment, this was their top concern. This manufacturer had more people in their company over the age of 50 than under the age of 30. Within five to 10 years, their top experts would retire, leaving their business without adequately trained resources. Mobile video collaboration provided this organization with a way to leverage its scarce expert pool and effectively mentor staff in the field to develop new experts.

Network Requirements While many benefits and cost savings opportunities are related to using mobile video collaboration on the plant floor, it is important to consider the infrastructure requirements. The main requirement is that the mobile devices have either an Ethernet or wireless network connection to access the Internet. Wireless connectivity (i.e., 802.11 b/g) is the most common method used at a manufacturing plant to keep the device mobility level high. While manufacturers have often invested in wireless networks to share equipment sensor data, these networks were not always constructed with video in mind. As a rule of thumb, most manufacturers use video settings for their mobile devices that require approximately 500 kbps of bandwidth at the plant. However, this mobile video collaboration can be successful with less than 500 kbps as well. In other industries, such as oil and gas or mining operations, it is more common to see bandwidth consumption below 128 kbps due to narrow bandwidth backhaul connections. Even with only 128 kbps, mobile collaboration can include live video, voice, telestration, and image sharing between the field technician and the remote expert. For manufacturing plants, though, the additional bandwidth capacity is typically worth the investment.

Wireless Alternatives Another alternative to consider is the use of 3G or 4G cellular

Extend Existing Video Infrastructure For organizations with investments in meeting room video infrastructure such as Cisco TelePresence suites or Tandberg videoconferencing rooms, mobile collaboration solutions become immediate extensions. The mobile devices and collaboration software use the same industry-standard protocols and media Codecs as the room-based video technologies. For manufacturers, that means that these mobile devices can immediately deliver a “live feed” from the plant floor or the field to add value to traditional face-to-face video meetings. In addition to face-to-face video rooms, mobile collaboration sessions can also be shared with multiple experts on their desktop computers. This “one-to-many” experience can be provided in many ways. One method is to simply call another desktop that has the collaboration software loaded. In this case, the additional experts can interact fully with capabilities like telestration and image sharing. Another way is to launch an online meeting tool such as Cisco WebEx. With this method, colleagues, suppliers or customers can be brought in to a collaboration session for ad-hoc meetings very quickly.

Multiple Benefits With the advent of mobile technologies, securely extending the power of video collaboration across a manufacturing enterprise is now a reality. Manufacturers have proven that mobile video helps reduce downtime, drive quality improvements, accelerate product delivery, leverage experts and eliminate unnecessary travel. Video is now an essential component of interaction between manufacturing facilities, suppliers, customers and OEM vendors. For many manufacturers, engaging in a video collaboration session has become as simple as making a phone call.  For more information, contact Librestream Technologies Inc. at 895 Waverley St., Suite 110, Winnipeg, Manitoba, Canada, R3T 5P4; call (800) 849-5507; e-mail [email protected]; or visit www.librestream.com. CERAMIC INDUSTRY ³ April 2011

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³PRODUCTSPOTLIGHT

Burner Control System A new relay-logic control panel provides flame supervision, temperature control and sequencing for single-burner combustion control applications.

T

he new SBC 1.0A control system is a configurable singleburner combustion control panel. The relay-logic panel provides flame supervision, temperature control and sequencing for single-burner combustion control applications. The core of the system is the Kromschröder IFD 258 automatic burner control unit. The SBC 1.0A can be configured to meet specific application requirements. Potential combustion applications for the SBC 1.0A include rotary dryers, oxidizers, incinerators, air heaters, fluidized bed dryers, and package burners, as well as ovens and furnaces.

The core of the system is the automatic burner control unit. Temperature control is selectable between 4-20 mA or position proportional control actuators (and three position step). Users may select either direct spark ignition (gas only application) or pilot ignition (combination gas/oil application). In addition, the SBC 1.0A can be configured with combustion air blower start/stop switches, a panel heater and nozzle purge circuits (for heavy oil applications). Other selectable 36

³WHAT’SNEW AMETEK LAND Arc Radiometric Thermal Imager Arc is a range of general-purpose thermal imaging cameras able to withstand heavy industrial applications, while being compact enough for use in R&D and automation. The high-resolution radiometric thermal imager can provide detailed thermal images with temperature accuracy. The system is available with two temperature ranges (-20 to 500°C and 100 to 1000°C), four lenses, two frame rates, and three software variants to meet user requirements. Visit www.ametek-land.com.

MORGAN THERMAL CERAMICS

configurations include thermocouple (type K or J) and ultraviolet (UV) or flame-rod flame detection (gas only). Additional features include a standard NEMA 4-rated enclosure; fullfeatured ¼ DIN temperature controller with set-point ramp capability; 1/16 DIN high-temperature limit instrument; adjustable purge timer; and low-fire hold circuit and indicators for purging, limits set, and control on. SBC 1.0A control systems can be used with most industr y-accepted actuators, including Kromschröder IC-40, GT-50, and IC-20; Honeywell Herculine and Modutrol; Barber Colman EA series; and Siemens SQM series. Additional actuator control types are also available.  For more information, contact Hauck Manufacturing Co. at P.O. Box 90, Lebanon, PA 17042; call (717) 272-3051; fax (717) 2739882; e-mail [email protected]; or visit www.hauckburner.com.

April 2011 ³ WWW.CERAMICINDUSTRY.COM

Furnance Lining Material This company’s experts presented information on an improved furnace lining material at the TMS 2011 Annual Meeting and Exhibition in February. The speakers discussed a new monolithic material for lining aluminum holding and melting furnaces. The new material reportedly performs better than existing materials and is suitable for use in the critical metal contact areas of aluminum furnaces. Visit www.thermalceramics.com.

GEA NIRO Spray Drying System A set of spray drying systems has been developed for the production of highperformance Li-ion battery materials. The systems are tailored to specific applications and specifications. With the company’s rotary and nozzle atomization systems, particle sizes from a few to several hundred microns can reportedly be obtained in a single compact, energy-efficient spray drying plant. Visit www.niro.com. 

Have Product News to Share with the Industry? E-mail news releases to Teresa McPherson at [email protected].

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Ruark Engineering, Inc. Customer Oriented Expert Kiln Assistance • • • •

Ralph Ruark, PE 10506 Cypress Point Drive Bradenton, FL 34202

38

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CONTINUOUS IMPROVEMENT OF KILN OPERATIONS KILN UPGRADE AND MODIFICATIONS NEW KILN PROCUREMENT SPECIALIZED TRAINING ON SITE P: 941-730-2253 F: 941-360-3211 [email protected] http://www.ruarkengineering.com

April 2011 ³ WWW.CERAMICINDUSTRY.COM

CoorsTek is the largest US-owned technical ceramics manufacturer in the world. Call 303-271-7006 or email [email protected] for expert assistance on your next project. Visit us on the web www.coorstek.com

SERVICESMARKETPLACE

³CONTRACT MANUFACTURING SERVICES / FINISHING & MACHINING SERVICES

WORLD LEADER IN PRECISION CERAMICS

Over a Quarter Century of Precision Ceramic Machining Process Development, has resulted in hundreds of satisfied customers. Put our experience and knowledge to work for you and become one of our satisfied customers.

719-687-0888 • [email protected] • www.okeefeceramics.com

³FINISHING & MACHINING SERVICES

YOUR OU U ULTRASOURCE SOU C FOR MACHINING HARD & BRITTLE MATERIALS

www.bullentech.com 1301 Miller Williams Rd. Eaton, Ohio 54320 USA Phone: (937) 456-7133 • Fax: (937) 456-2779 Email: [email protected]

EBL PRODUCTS, INC.

28 Years of Precision Ceramic Grinding

PIEZOCERAMICS

• Custom forming of technical ceramics * Built to customer print * • Prototype, short run and high volume production quantities • Multiple C.N.C. Capabilities

Serving our customers for over 50 years PRECISION CUSTOM DESIGN for:

• • • •

piezoceramic tubes piezo composites lead zirconate titanates matching layers & wearplates

EBL Products, Inc. 22 Prestige Park Circle, E Hartford CT 06108 Phone: 860-291-2537 • Fax: 860-291-2533 www.eblproducts.com [email protected]

Phone: 714-538-2524 Fax: 714-538-2589 Email: [email protected] Website: www.advancedceramictech.com

CERAMIC INDUSTRY ³ April 2011

39

³FINISHING & MACHINING SERVICES / FIRING & DRYING SERVICES ³FIRING & DRYING SERVICES

ISOSTATIC PRESSING

Contract Machining Company and Ceramic Component Supplier

Specializing in

• ISO 9001:2000 & AS9100B • CAD/CAM CNC Machining • Extensive Material Inventory • Material/Technical Support • Over 40 Years of Service

HIP, CIP, Service and Equipment Visit us on the Web: www.aiphip.com Call toll free: 800-375-7108

Specializing in BN, SiC, Macor, Si N , Al O , ZrO , Quartz, Ferrites and other related materials 3

4

2

3

2

American Isostatic Presses 1205 S. Columbus Airport Rd. Columbus, Ohio 43207 Phone (614) 497-3148 Fax (614) 497-3407

TEVTECH, LLC MATERIALS PROCESSING SOLUTIONS

di n i Gr & i o n Machining fC era ls m eria

ng

Pre o cis

t ics & Advanced Ma

PremaTech Advanced Ceramics is a highly respected, world leader in advanced custom machining and grinding for the Semiconductor, Aerospace & Defense, Research, Life Sciences and Commercial industries. For all your ceramic needs, please call 508.791.9549

Advanced Ceramic Machining & Components

Grinding of Hard and Ultrahard Materials: Alumina, Boron Nitride, Ferrite, Quartz, Silicon Carbide, Silicon Nitrides and Zirconia

100 Billerica Ave., N. Billerica MA 01862 Tel. (978) 667-4557 • Fax. (978) 667-4554 www.tevtechllc.com

TOLL FIRING SERVICES

NEW Lapping & Polishing Capabilities

Engineering and Design Support

Custom Vacuum Furnaces & Hot Zone Refurbishment for Sintering • CVD • Purification • Brazing

ISO 9001-2008 Certified ITAR & CCR Registered WBENC Certified

www.prematechac.com

• Sintering, calcining, heat treating to 1700°C • Bulk materials and shapes • R&D, pilot production • One-time or ongoing EQUIPMENT

• Atmosphere electric batch kilns to 27 cu. ft. • Gas batch kilns to Columbus, Ohio • 614-231-3621 57 cu. ft. www.harropusa.com e-mail: [email protected]

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April 2011 ³ WWW.CERAMICINDUSTRY.COM

SERVICESMARKETPLACE

³FIRING & DRYING SERVICES / GLASS SERVICES BUS.: (608) 783-4455 ALLIED FAX: (608) 783-4420 KILN EMAIL: [email protected] SERVICE INC. TIMOTHY J. TOBIN

New Kiln Design and Manufacturing Roller Hearth - Shuttle - Car Bottom - Tunnel • Installations • Combustion

• Refractory/Fiber • Electrical

• Instrumentation • Profile/Balancing

www.alliedkilnservice.com 1349 Moorings Dr. • La Crosse, WI 54603

³GLASS SERVICES

ALBERT LEWIS PRESIDENT

GLASS

INCORPORATED INTERNATIONAL 14055 LAURELWOOD PL • CHINO, CA 91710 email: [email protected] website: www.glassint.com Phone 909-628-4212 TOLL FIRING and CERAMIC REFRACTORIES

• Multiple kilns and furnaces for optimal firing options • Screening, surface area, and bulk density testing available • Custom and standard ceramic refractories • Alumina and Fused Silica formulas • Shapes include saggers, tiles, crucibles, kiln furniture [email protected] • (815)239-2385 ext. 105 www.ipsenceramics.com

I SQUARED R ELEMENT CO., INC. AKRON, NY USA

• Custom Designed Silicon Carbide & Molybdenum Disilicide Heating Elements for Your Application • Engineering Assistance & Trouble Shooting • Customized Accessories

Visit our Web Site: www.isquaredrelement.com Phone: (716) 542-5511 • Fax: (716) 542-2100

Fax 909-628-2771

SEM•COM

COMPANY, INC.

SPECIALTY & ELECTRONIC GLASS MANUFACTURING We provide the following services:

Q GLASS MELTING Q GLASS FABRICATION Q COMPOSITION DEVELOPMENT Q CONSULTING Contact us for further information:

Ph: 419-537-8813 Fax: 419-537-7054 E-mail: [email protected] www.sem-com.com

Refractory Repair Specialists • Ceramic Welding & Periscope Surveys • Port & Checker Cleaning • Hot Refractory Sawing & Drilling • Furnace Overcoating • Hot & Cold Refractory Repair

• Standard, Custom, Proprietary Glass and Glass-Ceramic compositions • Available in frit, powder (wet/dry milling), rod, or will develop a process to custom form • Fused Silica crucibles and Refractory lined tanks • Electric & Gas melting up to 1650°C • Research & Development • Pounds to Tons Phone (813) 855-5779 • Fax (813) 855-1584 Website: www.sgiglass.com • E-mail: [email protected]

CERAMIC INDUSTRY ³ April 2011

41

³GLASS SERVICES / INDEPENDENT AGENTS / LABORATORY & TESTING SERVICES ³LABORATORY & TESTING SERVICES

Electronic and Specialty Glass Frits & Powders • • • • • • • • • •

Standard compositions Custom melt capacity Glass development Calcinations Toll processing Test sample availability Production volumes Tailored particle sizes Press-ready granulation ISO 9001:2008 registered

G E L L E R M I C ROA NA LY T I C A L LABORATORY Analytical Services & NIST Traceable Magnification Standards SEM/X-ray, Electron Mircoprobe, Surface Analysis (Auger), Metallography, Particle Size Counting, and Optical Microscopy for Ceramics and Composite Materials Specializing in quantitative analysis of boron, carbon, nitrogen, oxygen, etc. in micrometer sized areas. Elemental mapping, diffusion studies, failure analysis, reverse engineering and phase area determinations. IS O 9 0 0 1 & 1 7 0 2 5 C ert i fi ed Put our years of experience to work on your specimens! 426 Boston St. Topsfield, MA 01983 Tel: 978-887-7000 Fax: 978-887-6671 www. gellermicro.com Email: [email protected]

Your Partner in Ceramics Analysis

GLASS TECHNOLOGY Design • Development • Manufacturing

6701 Sixth Ave. S. Seattle, WA 98108 (206) 763-2170 E-mail: [email protected] www.viox.com

³ INDEPENDENT AGENTS

Experiennced analysis of Advanced Experienced Advaanceed ceramic cerramicc m materials atterialss in including ncluudi ding alumina, magnesia, zirconia, carbides, nitrides, and oxides. Specialized Testing Capabilities Compositional Analysis Elemental and Chemical Analysis Microscopy and SEM Thermal Analysis

Analytical Expertise

BULLERS RINGS • Improve Kiln Yields • Reduce Loss • Improve Production Profits • Guarantee Consistent Firings

USA McCuen & Associates Ph: 330 482-1074 Fax: 330 482-4560 Email: [email protected] www.davemccuen.com UK Taylor Tunnicliff Limited. Normacot Road Longton Stoke-on-Trent ST3 1PA

w w w.t ayl o r tunni clif f.co m

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April 2011 ³ WWW.CERAMICINDUSTRY.COM

Trace Level Analysis Bulk Composition Thermal Conductivity Contaminants Inclusions Failure Analysis

www.nslanalytical.com

NSL Analytical Services, Inc. 4450 Cranwood Parkway, Cleveland, Ohio 44128 4OLL&REEsMRJS$RWPEREP]XMGEPGSQ

Trust

|

Technology

|

Turnaround

SERVICESMARKETPLACE

³LABORATORY & TESTING SERVICES / MAINTENANCE SERVICES

Thermal Analysis Materials Testing • Dilatometry • ASTM Testing • Glass Testing

• Thermal Gradient • Custom Testing • Clay Testing

• Firing Facilities • Refractories Creep • DTA/TGA

Columbus, Ohio • 614-231-3621 www.harropusa.com e-mail: [email protected]

JTF Microscopy Services, LLC Microscopy, Petrographic Analysis, Training & Consulting • Glass defect analysis and source identification • Furnace refractory failure investigations • Glass technology support services related to glass defect issues • Training seminars – on-site, on your own equipment

• Raw material contaminant identification • Trouble-shooting and correction of microscope equipment problems • Consulting for equipment purchases: microscope, camera & sample preparation • Expert witness services in legal actions

phone: 607.292.6808 • mobile: 607.731.8863 email: [email protected] • website: www.jtfmicroscopy.com

³MAINTENANCE SERVICES • Mill Lining Installation • Ball & Pebble Mill Parts ISO 17025 Compliant • cGMP compliant • FDA registered

Particle Size • Particle Shape BET Surface Area • Pore Size Analysis • Density

www.particletesting.com [email protected] 770.662.3630 PRINT, DIGITAL & ONLINE! TRIPLE EXPOSURE! CI’s Services Marketplace ads keep your services accessible in the customer’s preferred format 24/7 for 12 full months.

2011 RATES $950/unit . . . . . . . . . .black and white $1325/unit . . . . . . . . .4-color Contact Ginny Reisinger with questions: 614-760-4220 or [email protected]

• Field Service & Installation • Thickness Testing • Mill Doors & Gaskets • Grinding Media • Buy/Sell Used Process Equipment

Ceram

ic Maintenance Services, In

MILL LINING INSTALLATION GRINDING MEDIA

c.

Providing Quality Service for Over 25 Years PO Box 119 • Conneaut PA 16316 • Cell: 412-818-1379 Email: [email protected] • www.ceramicservicesonline.com

place your ad here!

CONTACT GINNY REISINGER @ 614/760.4220 or reisingerg@ bnpmedia.com to place yours today.

CERAMIC INDUSTRY ³ April 2011

43

³PROCESSING SERVICES

LOWER COST MILLING SOLUTIONS Holding off on capital purchases? Union Process still has several low cost options for you to get the job done economically and efficiently using the finest size reduction equipment on the market.

TOLL MILLING Save on capital equipment, personnel and space. Let Union Process toll grind your product in our Pilot Plant.

ENGINEERED PARTICLES Custom Particle Processing featuring: • • • • •

Spray Drying Particle Coating & Surface Modification Wet & Dry Ball Milling Bead Milling Research & Development

Our approach: • • • •

Innovation Collaboration Exceptional Customer Service Quality

"EFORE

REBUILDING Got a used Attritor in need of an update? Talk to Union Process about our 8-step refurbishing process using all OEM parts.

!FTER

[email protected] ISO 9001: 2008 Registered 2045 Wooddale Drive Woodbury, MN 55125 For more information visit: www.aveka.com 651-730-1729 | FAX 651-730-1826 or Call Toll Free: 1-888-317-3700

SPARE PARTS Make sure your Attritor is performing at peak efficiency. Order critical OEM spare parts today. Union Process stocks many parts ready for immediate shipping.

Partner with Union Process.

0HONEsWWWUNIONPROCESSCOM

Expanding the Possibilities for Size Reduction

Your Source for Powder Processing We specialize in: • Spray Drying • Wet and Dry Milling • Calcining and Sintering Typical Applications: • Catalysts • Electronics • Ceramics • Fuel Cells For more information, please contact Alan Sukovich at 219-462-4141 x224 or [email protected] 5103 Evans Avenue | Valparaiso, IN 46383

www.pptechnology.com

PRINT, DIGITAL & ONLINE! TRIPLE EXPOSURE! CI’s Services Marketplace ads keep your services accessible in the customer’s preferred format 24/7 for 12 full months.

2011 RATES $950/unit . . . . . . . . . .black and white $1325/unit . . . . . . . . .4-color Contact Ginny Reisinger with questions: 614-760-4220 or [email protected]

44

April 2011 ³ WWW.CERAMICINDUSTRY.COM

place you!r ad here

CONTACT GINNY REISINGER @ 614/760.4220 or reisingerg@ bnpmedia.com to place yours today.

³REFACTORY SERVICES

Refractory Repair Specialists • Ceramic Welding & Periscope Surveys • Port & Checker Cleaning • Hot Refractory Sawing & Drilling • Furnace Overcoating • Hot & Cold Refractory Repair

SERVICESMARKETPLACE

³PROCESSING SERVICES / RECYCLING SERVICES

Nth Degree PRODUCTS Reduce Your Refractory Costs NOW! We want to understand your current process and manufacturing needs. Our knowledgeable team will match your operating requirements with the right materials to meet your goals. We redesign and provide free samples to test concepts that provide better product quality, longer refractory life, and significant cost savings that will impact your overall bottom line. Higher quality and longer life refractories lead to smoother plant operating conditions, reduced scrap rates and improved end product quality.

³ RECYCLING SERVICES

RECYCLE! Eliminate Disposal

Wanted: ceramics, refractories, abrasives, kiln furniture, SiC and hi alumina ceramic scrap

9SPECIALIZING IN 9 CORDIERITE PRODUCTS Call us today: 609-518-9447 • Fax: 609-518-9445 [email protected] • www.nthdegreeproducts.com

A-TEN-C, INC. Call: 412-821-5566 • [email protected] • www.ceramicrecycling.com

Continuing to introduce innovative products to help improve your bottom line.

NEW RIBBON BLENDERS PRICED 30% LESS

World’s #1 Manufacturer! • All stainless, highest quality! • Sizes 1 to 500 cu.ft. • Many sizes in stock! Call now!

1-800-243-ROSS

USA Tel: 631-234-0500 • Fax: 631-234-0691 www.ribbonblenders.com

Quality & Service First BUY & SELL MACHINERY 586-790-1717 • [email protected] WWW.AADVANCEDMACH.COM

³POSITIONS AVAILABLE

Assistant Plant Manager Well-established brick and tile clay products manufacturer seeks assistant plant manager. Must have 5+ years experience with extrusion process, Mechanical, engineering, supervisory and computer skills required, Successful candidate will be trained for plant manager’s position. Small private company offers competitive package including generous retirement contributions.

BUY & SELL MACHINERY Detroit Process Machinery TOM SUHY: 586-469-0323 www.detroitprocessmachinery.com

³POSITIONS AVAILABLE

OPERATIONS MANAGER for a 24x7 glass manufacturing company. This company is a dynamic and profitable multi-billion dollar company that is driven by excellence. The ideal candidate will be a strong leader, open geographically, and who is capable of moving into a Plant Manager position as his/her next career step. Please call or email for more information. Cynthia Simpson, JT Nelson & Assoc. 800 848-0133 [email protected]

CLASSIFIEDADVERTISEMENTS

³BUY & SELL

Send resume to: Marion Ceramics PO Box 1134, Marion SC 29571 or [email protected] CERAMIC INDUSTRY ³ April 2011

45

³ ADVERTISERINDEX

³BUY & SELL

ADVERTISER

LINK

PAGE NO.

Carbolite Inc. . . . . . . . . . . . . . . . . . . . . . . . . . . . www.carbolite.us . . . . . . . . . . . . . . . . . . . . . 7 Ceramic Industry House Ads . . . . . . . . . . . . . www.ceramicindustry.com . . . . . . . . . . . IBC Ceramic Industry House Ads . . . . . . . . . . . . . www.ceramicindustry.com . . . . . . . . . . . IFC Clear Seas Research . . . . . . . . . . . . . . . . . . . . www.clearseasresearch.com . . . . . . . . . . . 3 Deltech Inc. . . . . . . . . . . . . . . . . . . . . . . . . . . . . www.deltechfurnaces.com . . . . . . . . . . . .BC Harper International Corp. . . . . . . . . . . . . . . . www.harperintl.com . . . . . . . . . . . . . . . . . . 9 Harrop Industries, Inc. . . . . . . . . . . . . . . . . . . . [email protected]. . . . . . . . . . . . . . . . . 4 Keith Co., Inc. . . . . . . . . . . . . . . . . . . . . . . . . . . www.KeithCompany.com . . . . . . . . . . . . .14 LignoTech USA . . . . . . . . . . . . . . . . . . . . . . . . . www.lignotech.com . . . . . . . . . . . . . . . . . . 23 Mohr Corp.. . . . . . . . . . . . . . . . . . . . . . . . . . . . . www.mohrcorp.com. . . . . . . . . . . . . . . . . .46 Spheric Technologies, Inc. . . . . . . . . . . . . . . . www.SphericTech.com . . . . . . . . . . . . . . . 22 Tokuyama America Inc. . . . . . . . . . . . . . . . . . . [email protected] . . . . . . . . . . . . 16 * See our ad in the 2010-2011 Ceramic Industry Data Book & Buyers’ Guide. This index is a feature maintained for the convenience of the advertiser. It is not part of the advertiser’s contract, and Ceramic Industry assumes no responsibility for its accuracy.

! e r e h d a our

y e c pla 46

April 2011 ³ WWW.CERAMICINDUSTRY.COM

CONTACT GINNY REISINGER @ 614/760.4220 or reisingerg@ bnpmedia.com to place yours today.

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