to 3 mm) wall panel to be used for thermal insulation that contains flanges that are to be about the same thickness. An R&D effort on the development of oxidation resistance methods has just been started. Consequently, there is no information to report nor were the research approaches discussed. and a basis for starting a collaborative Program Status program. GOVERNMENT INDUSTRIAL RESEARCH INSTITUTE (GIRI), OSAKA Inorganic Materials Department The laboratory tour showed all the necessary equipment for conducting any type of chemical analysis or physical property test that might be required in the course of performing R&D investigations. This is the only industrial organization that I visited that has a small Background research effort in the field of fracture mechanics. Assessment The research, development, and production efforts appear to be well directed and coordinated with long range objectives. The Kobe efforts probably encompass the widest span of interests in the field of carbonaceous materials of any industrial organization that I visited. This is because they are in the business of not only making novel materials, including C/Cs, but selling HIP equipment for processing these materials. Consequently, there are many areas of common interests and possibilities for collaboration. Collaboration may be possible with Kobe Steel, according to Dr. Suzuki. He will recommend to the Corporate Technical Development Group that such arrangements should be made if there are technical areas of mutual interest between organizations in the United States and Kobe. It is most likely that if any efforts were started, it would be organized through Kobe's laboratory that is located in Palo Alto, California. It is recommended that communications be continued concerning the R&D efforts at Kobe Steel to be knowledgeable about their results and to determine if there are areas of technology that would be of common interest My host for this visit was Dr. I. Souma, who has recently become the head of the C/C section in the Materials Department. This laboratory has the distinction of being the place where Dr. Sindo developed the process for making the first PAN fibers many years ago. During my last visit here in 1985 I met Dr. Sindo, and he explained the activities of the laboratory at that time. Currently there are four researchers involved in the C/Ceffort, but there are no support people, which is the situation at all GIRI facilities. In general, there is more collaboration between the GIRI laboratories and industry than there is with the universities. This situation is partially brought about by the fact that the charter of these government MITI funded laboratories is to be the intermediate laboratory between the bench scale and the full scale production phase. About one-third of GIRI Osaka's budget is derived from the industrial collaboration projects. The situation is further complicated by the fact that the universities are funded by an entirely different source, the Ministry of Education, which means there is another set of ground rules and barriers similar to those that exist between the Department of Defense and the Department of Energy in the United States. The major research activities in C/Cs are being pursued by Dr. Narasawa and Mr. Tatsumi. Their areas of interest include the use of nondestructive techniques, such as ultrasonics, to study the fiber/matrix interactions while the sample is being stressed. Special unidirectional composite samples are being prepared to understand the fracturing behavior. The densification procedures for these samples involve multiple impregnations with pitch and pyrolysis at 850 °C. Sometimes this temperature is raised to 1,000 °C. In either case the impregnations are conducted at 200 atm in an autoclave. Normally coal tar pitch is used because it appears to infiltrate more thoroughly into the preform, although it is recognized as not being as graphitizable as the petroleum-based pitches. Three to five impregnation cycles are used to bring the densities of the unidirectional preforms to about 1.9 g/cc. After each impregnation and pyrolysis cycle, the next step of the process is to go to 2,400 °C to graphitize the sample and open the pores. Only unidirectional samples are used in this laboratory because the investigators believe fracturing behavior can be better evaluated. Samples of this type are not made elsewhere. This carbon effort has just been reinitiated with emphasis on C/Cs. This area is new to both of these principal investigators, Dr. Narasawa, who is trained in solid state physics, and Mr. Tatsumi, who comes from a materials science background. They have completed laying out their research program and are in the stage of getting the equipment operational. Therefore, it will be a while before there will be data and results available. However, a brief laboratory tour was conducted and it appears that there was adequate equipment to conduct their experiments and to properly characterize the samples and precursor materials for both chemical and physical characteristics. There was even equipment from previous studies to spin special fibers if the research took such a direction. Since this program is just starting, it is expected it will continue in this direction for the next 3 to 5 years. Assessment The current research work is just beginning so it is not expected to produce much information for at least a year. Studying the fiber/matrix interactions by nondestructive means is a unique approach that could be very useful from both research and industrial viewpoints. Therefore, it is recommended that some form of communication be maintained in the future. As far as collaboration is concerned, Dr. Souma believes that it is possible, especially on the university basis. HOKKAIDO UNIVERSITY Faculty of Engineering Background My host was Prof. Michio Inagoki, who leads the carbon effort in this department. He joined this faculty less than 2 years ago from Toyohashi University, where he had been for more than 18 years. Inagoki is very active in professional societies and organizations that are connected with carbon. Most recently, he was the General Chairman of the Japanese International Carbon Conference, which was held from 4-8 November 1990 in Tsukuba, Japan. Inagoki's technical interests are concerned with the chemistry, structure, and texture of ceramic and carbon systems and how these variations affect the material's properties. The two major objectives of this visit were to learn about the carbon research activities at this university and to obtain a general view of the interactions between the universities, industry, and government laboratories in furthering the total C/C research efforts of Japan. It is important to understand how effectively this research information and expertise are being used, for the answers are then integrated into the general assessment portion of this study. Carbon research at Hokkaido University has been in existence for more than 20 years in the Department of Applied Chemistry, which Inagoki now directs, and in the Coal and Carbon Laboratory, which has been directed for the past 18 years by Prof. Sanada. Inagoki supervises about 12 persons and is assisted by Assoc. Prof. Shiro Shimada. This carbon group is composed of two postdoctoral research associates, three Ph.D. candidates, two masters students, and four undergraduates. The current and primary thrusts of this group are to understand the phenomena of intercalation in thin films and oxidation in carbons and the phase changes of carbides and nitrides. Program Status Shimada's primary area of research is to understand the development of different carbide systems (TiC, ZrC, HfC, and TaC) as they are being oxidized at temperatures up to 600 °C and pressures to between 3 and 20 kPa. One of the interesting effects that has been found is evidence, by electron diffraction patterns, of a diamond phase between ZrC and Zr2O2 as the ZrC is being oxidized. Also, it appears the diamond layer is well bonded to the two adjacent Zr phases. This research is being continued to determine more precisely the exact conditions that produce the diamond film. In the course of his studies, Shimada has developed a very sensitive method for detecting changes of phases through the use of acoustic emission (AE) signals. Changes of state of these systems occur as their temperatures are raised at rates between 0.1 and 20 °C/min and AE signals are continuously being emitted. However, at certain temperatures these signals suddenly increase in their intensity and this is considered to be the temperature where a phase change is initiated. Frequently these values don't agree with those published in the literature. In such cases the experiments are rerun to be sure of the data; otherwise, the differences are attributed to the increased sensitivity of the AE method over the usual differential thermal analysis (DTA) method. Special attention is given to the manner in which the temperature of the solution is measured to be sure the AE sensor is at this same value. This AE method has been extended to be used on solids and powders up to 1,300 °C, where it detects the microcracking that occurs due to the differential thermal expansion mismatching that exists between different phases. Careful analysis of the frequency spectrums is performed to increase the sensitivity of this method. Shimada started developing the use of AE about 3 years ago and, to his knowledge, he is the originator of the technique in Japan. One possible application of this method might be for use in acquiring more insight into the initiation of the phase changes that occur in pitch as the temperature is increased through the mesophase region, coalescence, and solidification stages. Inagoki's current and primary research area is to investigate intercalation phenomena and their influence on the structures and electrical properties of graphite films and powders, but not on vapor grown carbon fibers as others are doing. The primary technical challenge at this time is to attain stability of the enhanced conductivity that is produced by intercalation so these materials can be used for switches, electric brushes, components for sound amplification systems, and other applications. Inagoki believes from his experiments that stability might be enhanced by the use of additives, like PbO. He is also conducting collaborative research with other investigators in Japan concerning the microstructure and properties of fibers and the activation of carbon fibers and how their adsorption characteristics are being altered by precursors and processing conditions. Inagoki is the head of the Japanese effort for a collaborative program with the French on the structure and properties of mesophase-based fibers. In connection with these investigations, The other half of the mission at this The laboratory equipment and analytical capabilities in both Inagoki's and Sanada's organizations appear to be very adequate for performing the desired studies for the research they are conducting. In addition, there is a central testing facility available that is run as a service by the university in the event that some piece of equipment is not available in any department. Prof. Sanada has been the director of the Coal and Carbon Laboratory for the past 18 years. This laboratory is staffed at this time by two associate technicians, nine masters candidates, and five undergraduate students. The principal directions of this laboratory's research program are to understand the phenomena of carbonization of heavy oils and petroleums and the liquid faction of coals and to develop methods for reducing the environmental pollution that occurs through the use of coals and oils. An understanding of how to modify crude oils will also provide an ability to optimize the feed stock for the spinning of fibers or for impregnating bulk graphites of C/Cs with the desired type of matrix microstructure. Half of this laboratory's efforts are devoted to pitch chemistry at temperatures <700 °C. One of the investi- Assessment gations is to model compositional structure of the coal-derived pitches by using compounds of naphthalene and anthracene and determining the influence of noncovalent bonds that are produced with a third material type of catalyst such as CF SO H. The next step of this investigation is to find a cost effective method of reclaiming this catalyst. Another portion of this laboratory's research efforts is to determine the effects of time, temperature, and pressure on the texture of the derived liquid crystal or mesophase state of the pitch. The quality of the research efforts observed at Hokkaido University is very good. This situation is expected to continue for at least the next 3 to 5 years before either Inagoki or Sanada consider retiring. The Coal and Carbon Laboratory is unique in Japan and probably in Asia. It is comparable to the laboratory at the University of Newcastle upon Tyne in England. It is expected that Inagoki's laboratory will become increasingly productive in the next few years, judging from his past record. A specific point was made by Inagoki that it is very possible that collaborative research could occur with U.S. organizations in those areas where there is a common interest. This certainly seems likely, especially in the areas of pitch chemistry and phase changes that are taking place in the mesophase transition temperature range. It is quite possible that an exchange of graduate students could be arranged. There are precedents for doing so, as Inagoki was a postdoctoral student in Prof. Mrozowski's laboratory at the University of Buffalo many years ago. It is recommended that the research at Hokkaido University be followed in the future with collaboration being a possibility. The Interactions and A discussion was held with Prof. Inagoki about how the collective research capabilities are utilized within Japan toward developing and applying their C/C technology. This topic was the second major reason for this visit, as the information was very useful in preparing the general assessment for this study. Furthermore, Inagoki's thoughts and opinions are highly valued because of his familiarity with carbon research and his professional activities and knowledge of the organizations that are involved in the carbon field throughout Japan. The overall effectiveness of research efforts depends on many factors including utilization of expertise, communication, coordination, and collaboration among the different universities, industries, and government laboratories. The utilization by industry of research information and expertise of the professional staff at the universities appears to be much less than it is in the United States or other countries, especially France. A number of factors contribute to this situation. One factor is the decision of each professor as to how much support he will accept from industry. For example, Inagoki only accepts 15% of his budget and the rest comes from his university and different funds from the Japanese Government. On the other hand, Prof. Sanada's support is >50% from industry and the rest from the university or the Government. Some professors accept no industrial support while others take >70% at other universities. So there is a wide diversity found amongst the professors visited on this survey, and it appears to depend on the professor's desire to maintain his freedom for conducting research without the constraints that are usually imposed by industry. Another factor is governmental regulations that seem to limit the utilization of university expertise by industrial organizations. Apparently industry cannot hire a professor as a consultant if he is a faculty member of a national university. The only compensation for services that the professor can receive is funds that must be sent to the professor's university for the support of his laboratory operations or for travel. Occasionally industry may ask professors to give lectures or seminars for which they receive an honorarium. This financial restriction is a real limitation because it cuts down on the flexibility of industry to utilize the expertise at universities in the most effective manner and vice versa. Communication methods for the transfer of technical information vary according to the type of organization. The maximum degree of freedom is through the dissemination of research information by publications, reports, and seminars, which are the usual modes used by the universities and the Government Industrial Research Institutes (GIRI), unless a particular research project is for an industrial organization. The least amount of freedom occurs in the industrial organizations that are very restrictive about the dissemination of any information, either orally or in writing, because of the fierce competition that exists between themselves. Very frequently the representatives of industrial organizations will not even ask questions at public seminars for fear the opposition will determine what they are doing. This situation seems to feed on itself because the companies can start to overestimate the opposition's strengths or competitors may be unnecessarily duplicating each other's research. Fortunately there exists in Japan two activities that enhance communications between the universities, government laboratories, and the industrial organizations. One of these activities is called the New Carbon Forum (NCF). Its membership consists of about 30 industrial organizations including many of the largest corporations in Japan. The purpose of the NCF is to identify new applications and uses for all forms of carbon, including C/Cs. To all forms of carbon, including C/Cs. To accomplish the objective, a great deal of effort is being expended in reviewing the literature, collating the information, and conducting study groups and seminars on specific topical areas of carbon. This information is then communicated to the organization's membership through seminars and conferences. These seminars are held every 12 to 16 weeks; guest speakers present in-depth lectures and then there are extensive discussions by the attendees concerning the current and future status of the area that is being discussed. The second means of enhancing communication in Japan is through an organization called the 117 Committee, which is a part of the Japanese Society for the Promotion of Science. This committee holds a meeting about every 6 weeks that is attended by about 40 to 60 members from the three types of laboratories: university, government, and industry. Generally, the status of different research projects that are being conducted is presented by lecturers from universities or government laboratories. However, the information is also being transmitted to the industrial representatives, who can openly ask their questions at the meeting or more discretely call the speaker by telephone at a later date. It is generally agreed by many of those that attend both the NCF and 117 Committee meetings that they serve, at a minimum, the function of communicating the status of research but, in actual fact, the direction of research is also being influenced for all three types of research laboratories, whether it is admitted or not. Furthermore, there are indications that these meetings are beginning to convince the management of some of the industrial organizations that public exchange of some of their thoughts may be advantageous for sparking new research directions. Collecting research data is of primary importance and includes information from national and international sources. Different techniques of communication are very effectively being used in Japan and these will be discussed in other portions of this report. Coordination of research activities of all three types of research organizations can be excellent, especially if the Government is providing the support for developing specific areas as defined by the Ministry of International Trade and Industry (MITI) or the Ministry of Education. Examples of this will be given in other sections of this report. Coordination is extensively used between universities and GIRI laboratories. If the process or product needs to be scaled up from a laboratory size to an intermediate scale prototype, this is a prime function of the GIRI organization. Collaboration is an essential ingredient in pursuing research activities by all three types of laboratories. This is best exemplified throughout the universities, where they will pool the necessary resources to accomplish a given objective that is of common interest. Additional Items of Interest In discussions with Prof. Inagoki, the following points were made by him: The United States is ahead of Japan in the development of C/Cs because we have a lot more experience and have made larger pieces. He admits that the opinions of the Japanese might be distorted through lack of information. It is not clear whether Japan or the United States is ahead in the science and research related to C/Cs. ⚫ The major work on developing oxidation protection is being done at GIRI Kyushu using carbides. However, the majority of the efforts in this regard are being done by many industrial organizations in Japan, although it is not clear what is being done because they are not discussing this work. Nippon Steel is making special onedimensional samples for mechanical testing by Profs. Sakai and Yasuda. This company is pushing very hard to develop two- and threedimensional C/Cs. • Kobe Steel is making 8-inchdiameter disks of C/C that have densities of about 1.8 g/cc after they had been multiply impregnated using the hot isostatic pressing (HIP) process. • Mesophase research and development is being pursued by Prof. Isao Mochida of Kyushu University, Prof. H. Yamada of Tohoku University, Kobe Steel, and Mitsubishi Chemical. The major technology thrusts last in Japan for 5 to 10 years, then they drop off to a relatively few companies. This sequence is also valid for the world of carbon, where fibers until at least 1997. Nissan is work- ⚫ A large amount of excellent equip- • There are different approaches in Prof. Morinobu Endo, who is in the Electrical Engineering Department, was my host. He is internationally known for his pioneering research on the growth of single fibers of graphite from the vapor phase. These fibers are very perfect in their crystal structure and are therefore most useful for experimental and theoretical studies such as intercalational phenomena. Endo's initial research was accomplished almost 10 years ago. In all his studies, the main theme is to use the scientific research approach to explain phenomena that can be used to enhance the properties of materials so they can be used for engineering purposes. The materials that he is generally dealing with are different forms of carbon. Endo is the head of a group that consists of 15 students (8 undergraduates, 4 graduates, and 3 from industrial organizations). |