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(7) Discussion on the method of sample addition (8) Discussion on heating method of sample (9) Analysis of pressure heating process 5 Yes, D is that we have carried out experimental research based on the calculated graphite-diamond balance curve. After arduous exploration of failure, improvement, failure, and improvement, it was finally synthesized on the night of December 6, 1963 in the high-pressure laboratory of Beijing General Machinery Research Institute, which was designed and manufactured on the 61-type double-faced ultra-high pressure device designed and manufactured in China. The first synthetic diamond in China. The participants in the test were: Hu Enliang, Xu Jinfeng, Zhang Yonghua and Du Fuchang of the General Machinery Research Institute, Wang Guangzu, Lu Feixiong and Li Jinbao of the Abrasives Grinding Research Institute. I remember that this evening in a group of programs numbered in the 32nd experiment, it was found that the shiny crystals in the synthetic rods appeared mysteriously. When the glass was scratched with this crystal, the ears smelled crisp and humming. It is a signal that diamonds are coming to the land of China. After the crystal is subjected to acid treatment and separation by heavy liquid, yellow-green crystals having a particle diameter of 20 to 30 μ are obtained. X-ray analysis proves that the synthesized sample has the same spectral line as the natural diamond and the synthetic diamond sample lines of the United States and Japan, indicating that the yellow-green crystal is diamond, and the detailed data are listed in Table 1. Table 1 Comparison of synthetic samples in China with foreign and natural diamond spectral data
Because the diamond developed by the subject is kept secret, if there is diamond in the sample synthesized, the joint code is D, which is the first letter of Diamond. On December 10, 1963, we received a telegram from Hongchang. The message was not translated. It was already 9:00 pm. Hu Enliang and Tang Yujing went to the Tianqiao Post Office to find the interpreter. When they saw the translated message, they found D. When we were on the line, we were very happy. The hard work of three years saw the dawn. The laboratory once again cheered, we succeeded! We succeeded! It is the great victory of Mao Zedong Thought, the great victory of Chairman Mao’s revolutionary line, and the result of the great cooperation of socialism. The Abrasives Grinding Research Institute reported the above results to the Ministry of Science and Technology. In order to be cautious, the director of the Science and Technology Department should instruct the National Authority to conduct a re-inspection. So he appointed Wang Huarong to go to Beijing to help his steel research institute teacher, his teacher. After the identification results came out, I said to Wang Huarong, your result is not wrong, it is D! Congratulations on making a big contribution to the country! 6. Conclusion The National Science and Technology Commission officially issued the "synthetic diamond test research" in October 1963. The project is given to a machine department. Because it is a cutting-edge technology with strong confidentiality, it is named "121". The "121" of Zhengzhou Abrasives Grinding and Grinding Research Institute is determined by 121 of the "121" subject. After the research institute of Abrasives Grinding and Grinding moved to Zhengzhou National High-tech Development Zone, the number of the license plate was still 121, which was of far-reaching significance. On December 6, 1963, the birth of China's first synthetic diamond was achieved under the careful organization and care of the country. It was jointly researched by the above three research institutes and obtained in the underground laboratory of Beijing General Machinery Research Institute. It is a multidisciplinary course. The crystallization of synergy and the crystallization of collective wisdom. After a synthetic diamond came out, the collaboration between the three families was drawn to a full stop. We know that this is only the first step in the long-term journey of man-made diamond industry. The road of artificial diamond production is waiting for us to create. (Text / Wang Guangzu Zhengzhou Abrasives Grinding Research Institute) References (omitted)
Wang Guangzu: Birth of synthetic diamond
1. The charm of diamonds Since ancient times, diamonds (also known as diamonds) have attracted people's attention. This extremely rare mineral was discovered in India around 3,000 BC, but was actually known to the ancient Greeks before the 5th century BC. "Diamond" - derived from the Arabic word al-mas ("hardest") and the Greek word "aδ aμas", meaning "uncontrollable", "invincible", "indestructible". Diamond is not only much harder than Other substances, but also has many other "firsts". For example, the hardness of diamond is three times that of cubic silicon carbide, the wear resistance is five times that of alumina, the compressive strength is 20 times that of tungsten carbide, the sound transmission rate is three times that of steel, and the heat transfer rate is four times that of silver. The hole movement rate is 2.5 times that of the silicon crystal. The light transmission area and chemical inertness (below 500 ° C) of diamond also greatly exceed other materials. In addition, diamond has extremely high resistivity, refractive index, radiation resistance, and extremely low coefficient of thermal expansion, coefficient of friction, specific heat, and the like. Thanks to these unparalleled championship qualities, diamonds are an irreplaceable product in every application. Diamond is not only the most common material in the universe, it is also the most useful material for humans. In the future, diamond will become the most effective heat sink for electronic components, the brightest see-through window for radiation sources, the most stable protective film for chemical containers, the most slippery bearing surface for mechanical seals, the most suitable media for biomedical materials, and even the most information transfer. Fast semiconductors. Therefore, we expect that humans can use rich diamonds to build a more splendid material civilization and bring our children and grandchildren into the eternal "diamond era." Who wants to open up such a beautiful future, we! Because we need it! 2, a century of quest for success. Although diamond was discovered in India as early as 3,000 BC, its nature has always been a mystery. It was not until the end of the 17th century that diamonds were found to have flammable properties. As a result, British chemists and German physicists have all appeared on the scene. Unfortunately, in the past test conditions for the conversion of graphite to diamond, only high temperatures and lack of high enough pressure, therefore, graphite is impossible to transform into diamond. Although many attempts in the past have failed, these research efforts have pointed the way for later success. It is clear that the process of manufacturing diamond is a high-pressure and high-temperature process, that is, the conversion of graphite into diamond can only be achieved under the condition that both ultra-high pressure and high temperature exist simultaneously. In 1938, Rossini and Jessup published their calculated diamond (D)-graphite (G) equilibrium line; in 1939, Liepumsky published his calculated DG balance line; in 1947, PWBrigman published his calculated DG balance line. It solves the theoretical problem that synthetic diamond needs ultra-high pressure and high temperature, which provides a theoretical basis. Because of the maturity of synthetic diamond growth theory and high temperature and high pressure technology, it is indicated that the birth of synthetic diamond has been noisy in the mother's womb and is about to come to the world. In 1954, GE Corporation of the United States announced the successful synthesis of synthetic diamonds. Sweden announced that diamonds were synthesized in 1953. In 1959, South Africa, the Soviet Union and Japan in 1960 successively announced the synthesis of synthetic diamonds. Foreign achievements indicate that manual production of diamonds is no longer an insurmountable issue. At the time, this technology was completely closed to China. However, the success of the pioneers, for China to try in this regard, is no longer an infeasible thing, the synthesis of China's own diamonds to strengthen the determination and confidence of science and technology workers. 3. Mission is glorious and responsible. China's work in developing synthetic diamonds began in the early 1960s. In the same battlefield, there are two legions, that is, the Academy of Sciences (national level) and the ministerial two-level army are almost in the same era, indiscriminately fighting the rare and precious synthetic diamond technology. One is to fight for the development of the discipline, and the other is to fight for the urgent need for such products. The process of our development work cannot be as distant as the Chinese Academy of Sciences, and our battle is "100,000 points of fire", requiring quick fixes, the shorter the development process, the better! Ten thousand years is too long, only Fighting for the day! Our team ended the battle after more than a thousand days and nights. To this end, we won the 1978 National Science Conference Award. 3.1 The members of the national team of the Academy of Sciences team are: Institute of Physics, Chinese Academy of Sciences and Institute of Geology, Chinese Academy of Sciences. The member units of the ministerial level team include: First Machinery Department, General Machinery Research Institute, One Machine Department Abrasives Grinding Research Institute and Geological Department Geological Science Research Institute. The team of the Academy of Sciences is led by Professor He Shouan and Professor Zhang Yuanlong. Shen Shen, in the article "Several Progress in the Study of Synthetic Diamonds in China", pointed out that since the middle and late 1950s, internationally reported the use of static high-pressure synthetic methods to obtain abrasive grade diamonds in the laboratory. Therefore, the high-pressure method has received great attention from scientists and technicians. Therefore, the high-pressure phase transformation and synthesis project has become a key project in the discipline of China's physics and high-voltage physics in the development of the 12-year discipline development of natural sciences. This is also the important content of the artificial diamond project of the Institute of Physics of the Chinese Academy of Sciences in the late 1950s as a branch of high-voltage physics. When the high-pressure physics laboratory was established in 1962, the project became the background of the key project team. Li Daming, Liu Guangzhi told us in the article "Thirty Years of History": The direction of the Mineral Research Laboratory of the Institute of Geology of the Chinese Academy of Sciences focuses on applied basic research. Under the leadership of Professor Zhang Yuanlong, a number of intraocular lens growth projects began in 1960. . At that time, the diamond project was called one of the “five golden flowers†​​by the Chinese Academy of Sciences. It is the five most difficult projects. After analyzing the advantages and disadvantages of several types of ultra-high pressure high-temperature devices reported internationally, Mr. Zhang came up with a "one-way loading four-pair oblique sliding surface cube (hexahedron) ultra-high pressure with a 450-inch sliding surface in 1962. High temperature device". Due to the weak processing power of the Institute of Geology, the device was successfully developed and produced in 1965. 3.2 Departmental team 1960 international situation mutation. The severance of diamond sources has seriously affected the process of socialist construction in China. As is well known, in countries where natural diamond resources are extremely scarce, solving the problem of the source of diamonds has become an important issue that needs to be solved urgently. Thus, in October of this year, the country issued the task of developing synthetic diamonds. This task was carried out in collaboration with the General Machinery Research Institute of the Ministry of Machinery Industry, the Abrasives Grinding Research Institute and the Geological Science Research Institute of the Ministry of Geology. The super-hard abrasive diamond falling abrasive is completely consistent with the development of new abrasives and new abrasive tools in one of the basic tasks of the institute, and is consistent with its objective abrasive-abrasive-grinding, ie, material-product-application. After picking up the task, we immediately formed a strong team of codenamed 121. Among them, Yu Hongchang and I studied chemistry, and studied basic theory courses in material structure, chemical thermodynamics and chemical kinetics in the university. Such a knowledge structure is the first advantage of its work in diamond research. The two practical advantages of Yu Hongchang and my sister are that they have studied silicon carbide smelting technology in the Soviet Union and East Germany. In the process of silicon carbide smelting, there is a kind of decomposed graphite called silicon carbide. The purity of this kind of graphite is very high, and the metallurgical coke and pitch coke used for smelting silicon carbide are all carbon materials. This knowledge comes in handy when we are involved in the research of synthetic diamond synthesis technology. General Machinery Research Institute: responsible for the design and manufacture of high temperature and high pressure equipment, pressure measurement and organization work. Institute of Geological Sciences: responsible for the selection and temperature measurement of pressure-transmitting insulation materials. Abrasives Grinding Research Institute: responsible for the synthesis process and analysis. The principle of cooperation: division of labor does not separate home. Members involved in joint research: General Machinery Research Institute: Lian Yuanjian, Hu Enliang, Xu Jinfeng, Zhang Yonghua, Jin Qiuye, Liu Kaizhong and Du Fuchang; Institute of Geological Sciences: Yao Yucheng, Xiong Wensong, Zhou Jitang, Sun Rongchuan; Institute of Abrasives Grinding : Yu Hongchang, Wang Guangzu, Lu Feixiong, Yu Zhengmin and Li Jinbao. Experimental site: Underground laboratory of the office building of Beijing General Machinery Research Institute. Since then, I have had a lifelong relationship with the diamond industry. I am studying chemistry, but I don’t know anything about the synthesis of diamond technology, and there is a blank in my mind. We are responsible for the hardships of the country! We are engineers and technicians trained in the new China. We are worried about the country and the people of our generation. Who are we to bear? We quickly launched investigations and research, collected and read a lot of relevant The data on diamond growth, the "Foundation of Synthetic Diamond Synthesis Process" was written for the implementation of the test. Through the analysis of the data, the following questions are clarified: (1) Graphite and diamond are allotropes of carbon. From their crystal structure analysis, they have internal factors of mutual transformation, that is, in specific Under the conditions, not only in theory, it is feasible to use graphite as raw material to obtain diamond, and this has been proved by GE's experiment; (2) Graphite can only be diamond to the condition of ultrahigh pressure and high temperature. transition; (3) participating in the absence of a catalyst, while the graphite can be converted to diamond, but required much higher pressure and temperature conditions at high pressure and temperature with a catalyst participation. Obviously, the former is not advisable. How to solve the above problem? It is what we need to design and explore. 4 Theoretical basis for the implementation of the outline According to the requirements of the draft of the "synthetic basis of synthetic diamond technology", we focus on the analysis of thermodynamic conditions in the graphite-diamond transformation process and the discussion of the equilibrium curve, the analysis of the dynamic conditions in the graphite-diamond transformation process, The catalysis of the graphite-diamond conversion process, the discussion of the sample heating method and the analysis of the heating and pressurization process. In the process of analyzing the above problems, Professor Sun Chengwei from the Department of Chemistry of Peking University and Professor Chen Meihua from the Department of Chemistry of the East China Textile Institute of Technology consulted on theoretical issues. Several considerations have been put forward on the principles for the preparation of the "Foundation of Synthetic Diamond Synthetic Process": 1. Provide theoretical basis for the first stage experiment of synthetic diamond crystal growth; 2. Pass the thermodynamic and kinetic conditions of the graphite-diamond transformation process, And the preliminary analysis of the role of the catalyst in this transformation process to understand the general law of diamond crystal growth; 3, the details of diamond crystal growth, such as activation energy, calculation of reaction rate and other issues in the preparation of synthetic diamond process basis ( The first stage) is not considered at the moment, but it must be pointed out that this theoretical work must be done. At a group meeting before the start of the battle, I gave a detailed explanation to the members of the research team on the “Implementation Plan for Synthetic Diamond Synthesis Processâ€. Participants are: Yu Hongchang Lu Feixiong Hu Enliang Jin Qiuye Xu Jinfeng Yu Zhengmin Zhou Jitang Yao Yucheng Liu Kaizhong Xiong Wensong Zhang Yonghua. The report is divided into three parts: 1. Preface According to the published information, the research center of synthetic diamond synthesis technology has been established in many countries, and research work in this area is being vigorously carried out, and remarkable results have been achieved. Although the technical outline has been revealed, the key details are still confidential and need to be studied and solved by Chinese scientists. Therefore, we believe that: (1) natural diamond can not meet the requirements of scientific and technological development, must take the road of artificial synthesis; (2) from the domestic natural resources are small, the demand is large, we must quickly master the new diamond crystal growth technology. 2, a brief history of synthetic diamond research 1880 British chemist Hannery, 1894 French famous physicist Moissan and 1935 ~ 1940 American outstanding high-pressure physics researcher PWBridgman and other famous figures led by several experiments, the 1950s People have mastered the synthetic diamond synthesis technology. It is clearly proved that the synthetic process of synthetic diamond must be a process of simultaneous super-high pressure and high temperature, that is, diamond formation is only possible under the condition that both ultra-high pressure and high temperature exist simultaneously. 3. Analysis of thermodynamic conditions during graphite-diamond transformation and discussion of equilibrium curve Thermodynamic principles and data are the basis for calculating and discussing the graphite-diamond equilibrium curve. That is to say, in the study of graphite-diamond transformation, the first Considering the thermodynamic problem, because the calculation of thermodynamics allows us to predict the direction of the graphite gold-gangue transformation process, it provides a theoretical basis for studying this transformation process. (1) Thermodynamic basis (2) Calculation of equilibrium curve (3) Discussion of equilibrium curve (4) Analysis of kinetic conditions during graphite diamond transformation (5) Catalysis of graphite-diamond transformation process (6) About selection of catalyst problem consider.