skip to main content
OSTI.GOV title logo U.S. Department of Energy
Office of Scientific and Technical Information

Title: Microwave Sintering of Ceramic Materials for Industrial Application Final Report CRADA No. TC-1116-95

Abstract

The goal of this project was to develop the commercial capability in the US to sinter alumina oxide ceramic parts for the semiconductor manufacturing equipment industry. We planned to use the millimeter microwave (30 GHz) sintering system first developed by IAP in Russia.

Authors:
 [1];  [1];  [1]
  1. Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)
Publication Date:
Research Org.:
Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)
Sponsoring Org.:
USDOE
OSTI Identifier:
1406412
Report Number(s):
LLNL-TR-740367
DOE Contract Number:
AC52-07NA27344
Resource Type:
Technical Report
Country of Publication:
United States
Language:
English
Subject:
42 ENGINEERING; 36 MATERIALS SCIENCE

Citation Formats

Caplan, M., Tandon, R., and Callis, R.. Microwave Sintering of Ceramic Materials for Industrial Application Final Report CRADA No. TC-1116-95. United States: N. p., 2017. Web. doi:10.2172/1406412.
Caplan, M., Tandon, R., & Callis, R.. Microwave Sintering of Ceramic Materials for Industrial Application Final Report CRADA No. TC-1116-95. United States. doi:10.2172/1406412.
Caplan, M., Tandon, R., and Callis, R.. 2017. "Microwave Sintering of Ceramic Materials for Industrial Application Final Report CRADA No. TC-1116-95". United States. doi:10.2172/1406412. https://www.osti.gov/servlets/purl/1406412.
@article{osti_1406412,
title = {Microwave Sintering of Ceramic Materials for Industrial Application Final Report CRADA No. TC-1116-95},
author = {Caplan, M. and Tandon, R. and Callis, R.},
abstractNote = {The goal of this project was to develop the commercial capability in the US to sinter alumina oxide ceramic parts for the semiconductor manufacturing equipment industry. We planned to use the millimeter microwave (30 GHz) sintering system first developed by IAP in Russia.},
doi = {10.2172/1406412},
journal = {},
number = ,
volume = ,
place = {United States},
year = 2017,
month =
}

Technical Report:

Save / Share:
  • The goal of this project was to further develop and characterize the electrochemical methods originating in Russia for producing ultra high purity organometallic compounds utilized as precursors in the production of high quality electro-ceramic materials. Symetrix planned to use electro-ceramic materials with high dielectric constant for microelectronic memory circuit applications. General Atomics planned to use the barium titanate type ceramics with low loss tangent for producing a high power ferroelectric tuner used to match radio frequency power into their Dill-D fusion machine. Phase I of the project was scheduled to have a large number of organometallic (alkoxides) chemical samples producedmore » using various methods. These would be analyzed by LLNL, Soliton and Symetrix independently to determine the level of chemical impurities thus verifying each other's analysis. The goal was to demonstrate a cost-effective production method, which could be implemented in a large commercial facility to produce high purity organometallic compounds. In addition, various compositions of barium-strontium-titanate ceramics were to be produced and analyzed in order to develop an electroceramic capacitor material having the desired characteristics with respect to dielectric constant, loss tangent, temperature characteristics and non-linear behavior under applied voltage. Upon optimizing the barium titanate material, 50 capacitor preforms would be produced from this material demonstrating the ability to produce, in quantity, the pills ultimately required for the ferroelectric tuner (approx 2000-3000 ceramic pills).« less
  • This Cooperative Research and Development Agreement (CRADA) was a mutual research and development (R and D) effort among the participants to investigate a range of advanced manufacturing technologies for two silicon nitride (Si{sub 3}N{sub 4}) ceramic materials. The general objective was to identify the most cost-effective part manufacturing processes for the ceramic materials of interest. The focus was determining the relationship between material removal rates, surface quality, and the structural characteristics of each ceramic resulting from three innovative processes. These innovated machining processes were studied using silicon nitride advanced materials. The particular (Si{sub 3}N{sub 4}) materials of interest were sinteredmore » GS-44 from the Norton Company, and reaction-bonded Ceraloy 147-3. The processes studied included the following activities: (1) direct laser machining; (2) rotary ultrasonic machining; and (3) diamond abrasive grinding, including both resinoid and vitreous-bonded grinding wheels. Both friable and non-friable diamond types were included within the abrasive grinding study. The task also conducted a comprehensive survey of European experience in use of ceramic materials, principally aluminum oxide. Originally, the effort of this task was to extend through a prototype manufacturing demonstration of selected engine components. During the execution of this program, however changes were made to the scope of the project, altering the goals. The Program goal became only the development of assessment of their impacts on product strength and surface condition.« less
  • The initial work on microwave annealing of dense silicon nitride showed enhanced grain growth and improved creep resistance for materials annealed at temperatures of 1,200--1500 C. In those tests, the anneal times were on the order of 10--20 h to achieve the observed changes. To further study the effectiveness of microwave annealing, a Cooperative Research and Development Agreement (CRADA) was started in the area of microwave processing of silicon nitride with Garrett Ceramic Components/Allied-Signal (GCC/AS). The original plan was for ORNL to microwave anneal specimens of dense silicon nitride with high additive contents (> 5%) provided by GCC/AS at variousmore » times and temperatures. There were to be three sample types and 3--4 annealing conditions for a total of 9--12 annealing runs. The materials would then be characterized by both ORNL and GCC/AS to determine any changes in the properties. The objectives were: (1) to determine the effects of microwave crystallization on mechanical properties, and (2) to compare the effectiveness of microwave versus conventional heating. The mechanical properties examined that were fracture toughness, flexural strength and high temperature stress rupture. Delays, organizational changes, and other commercialization priorities resulted in a termination of this CRADA. This report contains a summary of results from one silicon nitride composition.« less
  • The progress made during the first two years of a program to study the migration of grain boundaries in ceramic oxides is reported. The principal results of the program are concerned with the structure of grain boundaries in ..cap alpha..-Al/sub 2/O/sub 3/, although important new information has also been obtained on grain boundaries in spinels and both germanlum and silicon. Attention is focused on the basal twin boundary in ..cap alpha..-Al/sub 2/O/sub 3/ which had been identified as a model interface in early work. A series of new grain boundaries exemplified by the (11anti23) twin are also discussed briefly asmore » is the rhombohedral twin interface. Earlier results on the first-order (..sigma..=3) twin in spinel have been extended with the development of models for the computer-simulation of high-resolution TEM images of these interfaces. A study of low-angle grain boundaries in spinel is giving new insight into the effect which the large size of the unit cell and the multiplicity of cations can have on structure of interfaces in ceramic materials, in general. Finally the direction of the program in examining grain boundaries in covalent materials (Ge and Si) is discussed.« less
  • The progress made during the first two years of a program to study the migration of grain boundaries in ceramic oxides is reported. The principal results of the program are concerned with the structure of grain boundaries in ..cap alpha..-Al/sub 2/O/sub 3/, although important new information has also been obtrained on grain boundaries in spinels and both germanium and silicon. Attention is focussed on the basal twin boundary in ..cap alpha..-Al/sub 2/O/sub 3/ which had been identified as a model interface in early work. A series of new grain boundaries exemplified by the (1123) twin are also discussed briefly asmore » is the rhomobohedral twin interface. Earlier results on the first-order (..sigma..=3) twin in spinel have been extended with the development of models for the computer-simulation of high-resolution TEM images of these interfaces. A study of low-angle grain boundaries in spinel is giving new insight into the effect which the large size of the unit cell and the multiplicity of cations can have on structure of interfaces in ceramic materials in general. Finally the direction of the program in examining grain boundaries in covalent materials (Ge and Si) is discussed.« less