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to 3 mm) wall panel to be used for and a basis for starting a collaborative Program Status
The major research activities An R&D effort on the development GOVERNMENT INDUSTRIAL in C/Cs are being pursued by of oxidation resistance methods has RESEARCH INSTITUTE
Dr. Narasawa and Mr. Tatsumi. Their just been started. Consequently, there (GIRI), OSAKA
areas of interest include the use of is no information to report nor were
nondestructive techniques, such as the research approaches discussed. Inorganic Materials Department ultrasonics, to study the fiber/matrix The laboratory tour showed all the 1-8-31 Midorigaoka
interactions while the sample is being necessary equipment for conducting any Ikeda, Osaka 563, Japan
stressed. Special unidirectional type of chemical analysis or physical Tel: 0727-51-8351
composite samples are being prepared property test that might be required in Fax: 0727-54-1931
to understand the fracturing behavior. the course of performing R&D investi- Dates: 12-13 Jan 1991
The densification procedures for these gations. This is the only industrial orga
samples involve multiple impregnations nization that I visited that has a small Background
with pitch and pyrolysis at 850 °C. research effort in the field of fracture
Sometimes this temperature is raised mechanics.
My host for this visit was Dr. I. Souma, to 1,000 °C. In either case the
who has recently become the head of impregnations are conducted at 200 atm Assessment
the C/C section in the Materials in an autoclave. Normally coal tar pitch
Department. This laboratory has the is used because it appears to infiltrate The research, development, and distinction of being the place where more thoroughly into the preform, production efforts appear to be well Dr. Sindo developed the process for although it is recognized as not being directed and coordinated with long range making the first PAN fibers many years as graphitizable as the petroleum-based objectives. The Kobe efforts probably ago. During my last visit here in 1985 I pitches. Three to five impregnation encompass the widest span of interests met Dr. Sindo, and he explained the cycles are used to bring the densities of in the field of carbonaceous materials activities of the laboratory at that time. the unidirectional preforms to about of any industrial organization that I Currently there are four researchers 1.9 g/cc. After each impregnation and visited. This is because they are in the involved in the C/Ceffort, but there are
involved in the C/Ceffort, but there are pyrolysis cycle, the next step of the business of not only making novel no support people, which is the situa- process is to go to 2,400 °C to graphitize materials, including C/Cs, but selling tion at all GIRI
the sample and open the pores. Only HIP equipment for processing these In general, there is more collabo- unidirectional samples are used in this materials. Consequently, there are many ration between the GIRI laboratories
ration between the GIRI laboratories laboratory because the investigators areas of common interests and possi- and industry than there is with the uni- believe fracturing behavior can be better bilities for collaboration.
versities. This situation is partially evaluated. Samples of this type are not Collaboration may be possible with brought about by the fact that the made elsewhere. Kobe Steel, according to Dr. Suzuki. charter of these government MITI This carbon effort has just been He will recommend to the Corporate funded laboratories is to be the inter- reinitiated with emphasis on C/Cs. This Technical Development Group that mediate laboratory between the bench area is new to both of these principal such arrangements should be made if scale and the full scale production phase.
scale and the full scale production phase. investigators, Dr. Narasawa, who is there are technical areas of mutual About one-third of GIRI Osaka's budget
About one-third of GIRI Osaka's budget trained in solid state physics, and Mr. interest between organizations in the is derived from the industrial collabo. Tatsumi, who comes from a materials United States and Kobe. It is most ration projects. The situation is further science background. They have comlikely that if any efforts were started, it complicated by the fact that the univer
complicated by the fact that the univer- pleted laying out their research prowould be organized through Kobe's sities are funded by an entirely differ- gram and are in the stage of getting the laboratory that is located in Palo Alto, ent source, the Ministry of Education,
ent source, the Ministry of Education, equipment operational. Therefore, it California.
which means there is another set of will be a while before there will be It is recommended that communi- ground rules and barriers similar to data and results available. However, a cations be continued concerning the those that exist between the Depart
those that exist between the Depart- brief laboratory tour was conducted R&D efforts at Kobe Steel to be knowl- ment of Defense and the Department
ment of Defense and the Department and it appears that there was adequate edgeable about their results and to of Energy in the United States. equipment to conduct their experiments determine if there are areas of technol
and to properly characterize the samples ogy that would be of common interest
and precursor materials for both chemical and physical characteristics. research activities at this university and of state of these systems occur as their There was even equipment from to obtain a general view of the interac- temperatures are raised at rates between previous studies to spin special fibers iftions between the universities, indus- 0.1 and 20 °C/min and AE signals are the research took such a direction. Since try, and government laboratories in continuously being emitted. However, this program is just starting, it is expected furthering the total C/C research efforts at certain temperatures these signals it will continue in this direction for the of Japan. It is important to understand suddenly increase in their intensity and next 3 to 5 years.
how effectively this research informa- this is considered to be the tempera
tion and expertise are being used, for ture where a phase change is initiated. Assessment
the answers are then integrated into Frequently these values don't agree with
the general assessment portion of this those published in the literature. In The current research work is just study.
such cases the experiments are rerun to beginning so it is not expected to pro- Carbon research at Hokkaido Uni- be sure of the data; otherwise, the difduce much information for at least a versity has been in existence for more ferences are attributed to the increased year. Studying the fiber/matrix interac- than 20 years in the Department of sensitivity of the AE method over the tions by nondestructive means is a unique Applied Chemistry, which Inagoki now usual differential thermal analysis approach that could be very useful from directs, and in the Coal and Carbon (DTA) method. Special attention is both research and industrial viewpoints. Laboratory, which has been directed given to the manner in which the temTherefore, it is recommended that some for the past 18 years by Prof. Sanada. perature of the solution is measured to form of communication be maintained Inagoki supervises about 12 per- be sure the AE sensor is at this same in the future. As far as collaboration is sons and is assisted by Assoc. Prof. value. concerned, Dr. Souma believes that it Shiro Shimada. This carbon group is This AE method has been extended is possible, especially on the university composed of two postdoctoral research to be used on solids and powders up to basis.
associates, three Ph.D. candidates, two 1,300 °C, where it detects the micro
masters students, and four undergrad- cracking that occurs due to the differHOKKAIDO UNIVERSITY uates. The current and primary thrusts ential thermal expansion mismatching
of this group are to understand the that exists between different phases. Faculty of Engineering
phenomena of intercalation in thin films Careful analysis of the frequency specDept. of Applied Chemistry
and oxidation in carbons and the phase trums is performed to increase the Sapporo 060, Japan
changes of carbides and nitrides. sensitivity of this method. Shimada Dates: 14-15 Jan 1991
started developing the use of AE about Program Status
3 years ago and, to his knowledge, he is Background
the originator of the technique in Japan.
Shimada's primary area of research One possible application of this method My host was Prof. Michio Inagoki, is to understand the development of might be for use in acquiring more who leads the carbon effort in this different carbide systems (Tic, Zrc, insight into the initiation of the phase department. He joined this faculty less HiC, and TaC) as they are being oxi- changes that occur in pitch as the temthan 2 years ago from Toyohashi Uni- dized at temperatures up to 600°C and perature is increased through the mesoversity, where he had been for more pressures to between 3 and 20 kPa. phase region, coalescence, and solidifithan 18 years. Inagoki is very active in One of the interesting effects that has cation stages. professional societies and organizations been found is evidence, by electron Inagoki's current and primary that are connected with carbon. Most diffraction patterns, of a diamond phase research area is to investigate interrecently, he was the General Chairman between ZC and Zr,O, as the ZrC is calation phenomena and their influof the Japanese International Carbon being oxidized. Also, it appears the ence on the structures and electrical Conference, which was held from diamond layer is well bonded to the properties of graphite films and pow4-8 November 1990 in Tsukuba, Japan. two adjacent Zr phases. This research ders, but not on vapor grown carbon Inagoki's technical interests are con- is being continued to determine more fibers as others are doing. The primary cerned with the chemistry, structure, precisely the exact conditions that technical challenge at this time is to and texture of ceramic and carbon sys- produce the diamond film. In the course attain stability of the enhanced contems and how these variations affect of his studies, Shimada has developed a ductivity that is produced by intercalathe material's properties.
very sensitive method for detecting tion so these materials can be used for The two major objectives of this changes of phases through the use of switches, electric brushes, components visit were to learn about the carbon acoustic emission (AE) signals. Changes for sound amplification systems, and other applications. Inagoki believes from In connection with these investigations, next few years, judging from his past his experiments that stability might be a special high pressure electron spin record. enhanced by the use of additives, like resonance (ESR) technique (<room A specific point was made by Inagoki PbO.
temperature (RT) to 500 °C and that it is very possible that collaboraHe is also conducting collaborative <100 atm pressure in nitrogen or
tive research could occur with U.S. research with other investigators in hydrogen) is being used to study the organizations in those areas where there Japan concerning the microstructure mobility of the molecules of interest. is a common interest. This certainly and properties of fibers and the activa- For example, it has been determined seems likely, especially in the areas of tion of carbon fibers and how their that the mobility of hydrogen exceeds pitch chemistry and phase changes that adsorption characteristics are being that of nitrogen in these systems. The are taking place in the mesophase transialtered by precursors and processing life times ofsome of these radicals have tion temperature range. It is quite conditions. Inagoki is the head of the been measured at less than a millisecond,
been measured at less than a millisecond, possible that an exchange of graduate Japanese effort for a collaborative which means that the entire analysis students could be arranged. There are program with the French on the struc- must be completed in less than precedents for doing so, as Inagoki was ture and properties of mesophase-based 10 seconds. Currently the equipment a postdoctoral student in Prof. fibers.
is being modified to be able to make Mrozowski's laboratory at the UniverProf. Sanada has been the director measurements at liquid nitrogen sity of Buffalo many years ago. of the Coal and Carbon Laboratory for temperatures.
It is recommended that the research the past 18 years. This laboratory is The other half of the mission at this at Hokkaido University be followed in staffed at this time by two associate laboratory is concerned with finding the future with collaboration being a technicians, nine masters candidates, methods for burning coal with less of a possibility. and five undergraduate students. The negative impact on the environment. principal directions of this laboratory's This research is most important to Japan The Interactions and research program are to understand as more than 600,000 tons of coal are Influences of C/C Research the phenomena of carbonization of used to produce energy and metallur
used to produce energy and metallur- Organizations Within Japan heavy oils and petroleums and the liquid gical cokes. faction of coals and to develop meth- The laboratory equipment and A discussion was held with Prof. ods for reducing the environmental analytical capabilities in both Inagoki's Inagoki about how the collective pollution that occurs through the use and Sanada's organizations appear to research capabilities are utilized within of coals and oils. An understanding of be very adequate for performing the Japan toward developing and applying how to modify crude oils will also pro- desired studies for the research they their C/C technology. This topic was vide an ability to optimize the feed are conducting. In addition, there is a the second major reason for this visit, stock for the spinning of fibers or for central testing facility available that is as the information was very useful in impregnating bulk graphites of C/Cs run as a service by the university in the preparing the general assessment for with the desired type of matrix micro- event that some piece of equipment is this study. Furthermore, Inagoki's structure. Half of this laboratory's efforts not available in any department. thoughts and opinions are highly valued are devoted to pitch chemistry at tem
because of his familiarity with carbon peratures < 700 °C. One of the investi. Assessment
research and his professional activities gations is to model compositional struc
and knowledge of the organizations ture of the coal-derived pitches by using The quality of the research efforts that are involved in the carbon field compounds of naphthalene and anthra- observed at Hokkaido University is very throughout Japan. cene and determining the influence of good. This situation is expected to The overall effectiveness of research noncovalent bonds that are produced continue for at least the next 3 to 5 years efforts depends on many factors includwith a third material type of catalyst before either Inagoki or Sanada considering utilization of expertise, communisuch as CF SO,H. The next step of this retiring. The Coal and Carbon cation, coordination, and collaboration investigation is to find a cost effective Laboratory is unique in Japan and mong the different universities, indusmethod of reclaiming this catalyst. probably in Asia. It is comparable to tries, and government laboratories. Another portion of this laboratory's the laboratory at the University of The utilization by industry of research research efforts is to determine the Newcastle upon Tyne in England. It is information and expertise of the proeffects of time, temperature, and pres- expected that Inagoki's laboratory will fessional staff at the universities appears sure on the textureofthe derived liquid become increasingly productive in the to be much less than it is in the United crystal or mesophase state of the pitch.
States or other countries, especially France. A number of factors contrib- very restrictive about the dissemina- universities or government laboratories. ute to this situation. One factor is the tion of any information, either orally However, the information is also being decision of each professor as to how or in writing, because of the fierce transmitted to the industrial represenmuch support he will accept from indus- competition that exists between them- tatives, who can openly ask their questry. For example, Inagoki only accepts selves. Very frequently the represen- tions at the meeting or more discretely 15% of his budget and the rest comes tatives of industrial organizations will call the speaker by telephone at a later from his university and different funds not even ask questions at public semi- date. from the Japanese Government. On nars for fear the opposition will deter- It is generally agreed by many of the other hand, Prof. Sanada's support mine what they are doing. This situa- those that attend both the NCF and is > 50% from industry and the rest tion seems to feed on itself because the 117 Committee meetings that they serve, from the university or the Government. companies can start to overestimate at a minimum, the function of commuSome professors accept no industrial the opposition's strengths or competi- nicating the status of research but, in support while others take > 70% at tors may be unnecessarily duplicating actual fact, the direction of research is other universities. So there is a wide each other's research.
also being influenced for all three types diversity found amongst the professors Fortunately there exists in Japan of research laboratories, whether it is visited on this survey, and it appears to two activities that enhance communi- admitted or not. Furthermore, there depend on the professor's desire to cations between the universities, gov- are indications that these meetings are maintain his freedom for conducting ernment laboratories, and the indus
ernment laboratories, and the indus- beginning to convince the management research without the constraints that trial organizations. One of these activ- of some of the industrial organizations are usually imposed by industry. Another ities is called the New Carbon Forum that public exchange of some of their factor is governmental regulations that (NCF). Its membership consists of about
(NCF). Its membership consists of about thoughts may be advantageous for seem to limit the utilization of univer- 30 industrial organizations including sparking new research directions. Colsity expertise by industrial organiza- many of the largest corporations in lecting research data is of primary tions. Apparently industry cannot hire Japan. The purpose of the NCF is to importance and includes information a professor as a consultant if he is a identify new applications and uses for from national and international sources. faculty member of a national univer- all forms of carbon, including C/Cs. To Different techniques of communicasity. The only compensation for ser- accomplish the objective, a great deal tion are very effectively being used in vices that the professor can receive is ofeffort is being expended in reviewing Japan and these will be discussed in funds that must be sent to the professor's the literature, collating the informa- other portions of this report. university for the support of his labora- tion, and conducting study groups and Coordination of research activities tory operations or for travel. Occasion- seminars on specific topical areas of of all three types of research organizaally industry may ask professors to give carbon. This information is then com- tions can be excellent, especially if the lectures or seminars for which they municated to the organization's mem- Government is providing the support receive an honorarium. This financial bership through seminars and confer- for developing specificareas as defined restriction is a real limitation because ences. These seminars are held every by the Ministry of International Trade it cuts down on the flexibility of indus- 12 to 16 wecks; guest speakers present and Industry (MITI) or the Ministry of try to utilize the expertise at universi- in-depth lectures and then there are Education. Examples of this will be ties in the most effective manner and extensive discussions by the attendees given in other sections of this report. vice versa.
concerning the current and future status Coordination is extensively used Communication methods for the of the area that is being discussed. between universities and GIRI laboratransfer of technical information vary The second means of enhancing tories. If the process or product needs according to the type of organization. communication in Japan is through an to be scaled up from a laboratory size to The maximum degree of freedom is organization called the 117 Commit- an intermediate scale prototype, this is through the dissemination of research tee, which is a part of the Japanese a prime function of the GIRIorganizainformation by publications, reports, Society for the Promotion of Science. tion. and seminars, which are the usual modes This committee holds a meeting about Collaboration is an essential ingre used by the universities and the Gov- every 6 weeks that is attended by about dient in pursuing research activities by ernment Industrial Research Institutes 40 to 60 members from the three types all three types of laboratories. This is (GIRI), unless a particular research of laboratories: university, government, best exemplified throughout the uniproject is for an industrial organiza- and industry. Generally, the status of versities, where they will pool the necestion. The least amount of freedom occurs different research projects that are being sary resources to accomplish a given in the industrial organizations that are conducted is presented by lecturers from 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 oxi
dation 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.
for the world of carbon, where fibers best foundation before any of the
U.S. agreement for the exchange of
students and provides for their • A large amount of excellent equip- support while in the United States.
ment is found in industrial labora-
my host. He is internationally known
for his pioneering research on the growth • There are different approaches in of single fibers of graphite from the
the use of research for the develop- vapor phase. These fibers are very perment of materials between Japan fect in their crystal structure and are and the United States. In the for- therefore most useful for experimental mer case, research is used to build and theoretical studies such as interthe outline of the developmental calational phenomena. Endo's initial problems that are associated with research was accomplished almost manufacturing a new material. Prof. 10 years ago. In all his studies, the main Inagoki uses the analogy that the theme is to use the scientific research Japanese approach is much like approach to explain phenomena that putting up the framing structure of can be used to enhance the properties a house upon which the roof is placed, of materials so they can be used for after which the details of the house engineering purposes. The materials are filled in. But in the United States, that he is generally dealing with are his impression is extensive develop- different forms of carbon. Endo is the ment is used to understand all the head of a group that consists of 15 phenomenology of the material, students (8 undergraduates, 4 graduates, which is analogous to building the and 3 from industrial organizations).
• Nippon Steel is making specialone
dimensional 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-inch
diameter 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 develop
ment is being pursued by Prof.
• 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