Abstract I was born in 1965, two years later than the birth of my first synthetic diamond. Write a pen for the "Chinese Diamond 50 Years Commemorative Anthology", the heart of his heart is real, and looking back on the past, always want to write the impulse of the moment is also true! ...
I was born in 1965, two years later than the birth of my first synthetic diamond. Write a pen for the "Chinese Diamond 50 Years Commemorative Anthology", the heart of his heart is real, and looking back on the past, always want to write the impulse of the moment is also true! I. Origin
Domestic doctoral thesis of engineering is usually "quality and quantity are equal", "process and theory coexist" - no quality without theory seems to be no level, no quantity without process and difficult to reflect the workload; and the technicality of synthetic diamond research is obvious And once it is not synthesized (unsuccessful), there is a risk that a word cannot be written. The reason why the choice of powder catalyst synthetic diamond as the research direction of my doctoral thesis is not only my personal choice, but also its origin: my undergraduate and postgraduate students are all materials science, and assigned to Changsha Research Institute of Mining and Metallurgy in 1989. The material works. At that time, the Changsha Institute of Mining and Metallurgy was the main production unit of flake catalyst for diamond synthesis in China, but I did not engage in related work. The first contact with the catalyst material was purely accidental. At that time, the material was divided into two pieces: one piece was Do material research in the research building; one is to do catalyst production, in the workshop. Due to the good production situation at the time, the employees working in the workshop were very well treated, and there were cold drinks in the summer; while the workers working in the research building seemed to have gaps, sometimes boiling water was lacking; I was the general secretary of the regiment, and I was led by young indignation. More than 20 people working in the research building (mostly new graduate students) participated in the film selection work. I still remember the working scene of the film selection: put a bucket of original film between the two feet, put two basins beside the right foot, and put a basin on the left foot; the first, second and third grades are handed out. This is my first contact with the catalyst - it is the beginning of the primary. Of course, the reason why diamond synthesis is mainly because I have learned powder metallurgy and I also know that the world's first diamond is synthesized with metal powder catalyst.
2. Zigzag
In 1992, I returned to the doctoral thesis of powder metallurgy research at Central South University. The Powder Metallurgy Institute has never conducted such research, and there are no synthetic equipment and related conditions, so the first problem I encountered was to find equipment.
At that time, the first thing we looked for was Changsha 233 Factory (now Hunan UFO Superhard Material Co., Ltd.). It should be the presence of Professor Lu Haibo. The responsible comrades of Changsha 233 Factory were also very enthusiastic; then I went to contact but could not. The reason is that the production task of everyone was very busy at the time, and the second was the risk of powder catalyst synthesis.
So we thought of the director of Yang Yongke. Yang Changchang worked in the Changsha Research Institute of Mining and Metallurgy and later resigned to contract the diamond workshop of the Central South University Machinery Plant. After a few twists and turns, Academician Ma Fukang was the director of the Education Bureau of China Nonferrous Metals Industry Corporation. He also personally came forward; Yang Director not only agreed to use our six-face press to do synthetic experiments, but also gave me knowledge about the diamond industry. "universal".
It was originally thought that as long as the temperature and pressure conditions were met, graphite could be converted into diamond by thermodynamics. After the first synthesis, it was observed that the color of the composite block did not change - black and black, and it was considered that the temperature was not added. Thus, the heating sheet was added a second time, and the modification of the composite block was also carried out for the third time. It is heartbreaking that the first three experiments not only did not synthesize a diamond, but even worse, they broke the top hammer every time (sometimes two times at a time); it is impossible to continue because the workshop is the director of Yang. Contracted, here is his personal loss.
It is well known that the six-sided top press is very specific and directly related to their respective economic benefits; and there is almost no open literature at the time; I also have a general enrollment (the child was born in 1993). No salary). The inner depression is not light!
Academician Ma Fukang is one of my thesis supervisors. He has always been concerned with guiding my work. Upon learning about my situation, he directly found the Director of the Geological Survey Bureau of China Nonferrous Metals Industry Corporation. Director Tang arranged for me to go to Beijing Jindi Superhard Materials Co., Ltd. (hereinafter referred to as Jindi Company) under the Geological Survey Bureau to conduct experiments. It can be carried out until it is completed.
Three pieces
Outing
Jindi Company is located in a new industrial area in Mentougou, Beijing. At that time, there were few enterprises entering the area, so the company was alone in the open loess and thatch. In addition to the on-duty and on-duty staff, everyone is going back to the city after work; the company was established shortly, and there was no time to establish the corresponding cultural and sports facilities; I really went back to the dormitory-shoproom-canteen "three points and one line" university life. The company specially arranged a press for me and was free to experiment. At the beginning of several experiments, I could not synthesize diamonds. Although there is no re-sharp hammer (it is really dare not!), but the pressure in my heart is heavy! Mr. Bian Kezheng, the general manager of the company, is an old comrade who has been over 60 years old. He was the head of the Beijing Nonferrous Metals Exploration Bureau and has a red BMW. Every time I went, he arranged for people to send me to the surrounding area with a BMW car; so I went to Tanzhe Temple in Beijing, Panshan in Tianjin and other places. In the circumstances at the time, I did not have the mood to go (the open Northland, where is your moving landscape), and the old gentleman's love is always unforgettable.
Dangerous situation
I haven't been able to synthesize diamonds, and the pressure is getting bigger (the pressure in my heart is sinking, and where is the success)! Once, I thought it was because of the porous characteristics of the powder that the synthetic block could not be compacted; so the mold of the composite rod was placed directly in a six-sided press to pressurize it to obtain more pressure to obtain more High synthetic block density. My right hand is on the console, my eyes are on the mold - I press it to the expected position and stop; I don't want my finger to press the "jog" button, but the "auto" button. I have to wait for the pressure, I want to stop it. I only heard a muffled sound, and the mold burst, because I was nearsighted and my head was close. Any piece of lobes has a great chance to fly to my head, and any piece of iron that flies to my head can kill me. I picked one of them and marked it with the date: August 10, 1994 - still in my study! When I was doing the experiment, the staff at the workshop always had to look around "fresh", and everyone would never come again.
Surprise
After the failure of the experiment, I made some improvements in the processing of the powder, the assembly and processing of the synthetic block, and the synthesis process (now these are basically common, and at that time, one person groping without any information); from black Black (under-temperature) and bright (over-temperature) see the sporadic diamonds, the brilliance of diamonds in full-section, to the multi-grain diamonds, the inner surprise is beyond words! I was the first to tell Ma Fukang that Teacher Ma also put down his busy work and came to the workshop for the first time. I also clearly remember that Teacher Ma leaned over and placed his eyes on the microscope lens. He kept saying: Jianhong, okay! Jianhong, okay!
Splash
Gemdale's equipment is matched with production; therefore, post-processing of synthetic blocks is carried out at Central South University. In the pickling and purifying diamond process, there is a large amount of sulphur dioxide-containing smoke emission, which is very inappropriate in the school laboratory; I always secretly carry out in the middle of the night. I remember the first time, because the time was very late, in order to speed up, I knocked the synthetic rod into powder and placed it in a beaker. The beaker was also placed on an electric stove to heat it. It was prepared to be "sour boiled"; summer Changsha Very hot, I bare upper body, wearing shorts; when the king water poured into the beaker, suddenly the solution in the beaker splashed; some of them splashed on the body, so far I have a small print on it, it is also a commemoration.
Painting vegetables
During my time at Gemdale, I liked the dish of the company cafeteria called “painting dishesâ€. One is because it is cheap, about two cents a piece, only five cents more than green vegetables, sometimes there is meat inside; the second is because this dish is salty, the content is also very rich, very suitable for my heavy taste of Hunan people So, I have to play one every night. The "painting dishes" in the canteen are often placed on the far side, and there are very few people waiting in line to buy them. I become conspicuous; for a long time, I always feel that young masters are pointing out. I was surprised to ask, I only know when I asked: The so-called "painting dish" is that the remaining dishes are not used every day at noon, and mixed with heated dishes at night.
teacher
My instructor started with Professor Huang Peiyun and Professor Lu Haibo, and Ma Fukang was later joined. Academician Huang Peiyun was over 80 years old. I only met during the doctoral interview; he asked me a question about concentration and activity. After graduating from my Ph.D., I worked as an academic secretary for more than 10 years, but these are all words. Professor Lu Haibo gave a lot of guidance - I remember that Hebei Province wanted to introduce WINTER's powder catalyst technology, and the other party issued a tens of millions of dollars in technology transfer fees; because the project of more than 10 million US dollars at that time was approved by the State Planning Commission. Therefore, we must organize expert argumentation; WINTER provided a video material that was “precisely prepared†for technical confidentiality. I saw the glittering diamond on the cross section of the composite block that was pressed from both sides in the video. Academician Ma Fukang cares about my work from beginning to end: at the beginning of the work, he invited two professors from the Moscow Iron and Steel Institute to Changsha for a lecture on synthetic diamonds (I also know Professor Jiang Rongchao), and the powder catalyst I used was also personally contacted. Provided by Tula Metals of Russia; even after the writing of the thesis, he is revised word by word; I remember that he wrote a sentence on the first page of my manuscript: the doctoral thesis should write something that he can be gratified in his life!
worker
Before I started this research, I have not only seen relevant information and scenes, even even a diamond single crystal has never been seen, it is all from scratch! Everything is the result of the help of many people, and I can't thank them all by name. I remember that the director of the Synthetic Workshop of Jindi Company was surnamed Ma. Director Ma was slightly larger than me and had a lot of practical experience. He not only taught me a lot of machine operation knowledge, but also, when I was depressed, our two bachelors exchanged. Also gave me a lot of comfort. The workshop has a squad leader, very young, and is also talking about the object; the appearance is somewhat black and thin, and it is also recruited from other places; he also often helps me to do synthetic experiments. In the exchange, I knew that he would compose music, so we also cooperated one time: I wrote the words, he compose music.
Result
After more than three years of work, I realized the synthesis of diamonds of different varieties (crystal form and particle size) and different conversion rates on a six-face press using Mn-based powder catalyst. After the paper is written, it is necessary to ask the experts to review. Unlike most of the students' paper review experts, the mentor is different. My paper review experts are my own. Nearly 20 experts have given a high affirmation (most of them have not been seen so far). Mr. Qi Qingquan not only gave the comments affirmation, but also sent me his related monographs; Professor Hao Zhaoyin not only gave good comments, but also sent me letters twice, pointing out the mistakes and shortcomings in my thesis. I also hope that I will go to Jilin University to study as a postdoc. In July 1996, my dissertation passed a defense organized by Mr. Xu Zhongyu and Mr. Ma Rongjun. The result was rated as excellent.
Here, I briefly talk about the main paper results of the paper:
Synthesis of powder catalyst: The homogenization of powder material and the control of oxygen content are solved by the choice and treatment of solvent. The uniformity of heating and temperature field is solved by the improvement of assembly method of synthesis block. Different varieties are synthesized by process optimization. Diamond with different conversion ratios; and through the technical and economic comparison between the powder catalyst and the sheet catalyst, it is pointed out that the powder catalyst is a preferred catalyst form for synthetic diamond.
Internal stress mechanism: The stability and accuracy of temperature field and pressure field control in the synthesis chamber under high temperature and high pressure are the key to synthetic diamond technology, and the internal stress in the synthesis chamber directly affects the pressure field distribution; the sheet catalyst itself is deformed. The uneven distribution of internal stresses causes unevenness in the synthetic diamond. In addition, the temperature change during the synthesis of the flake catalyst can be greatly reduced in the synthesis of the powder catalyst.
Metastable gap solid solution theory: The phenomenon and law of the change of catalyst composition in the diamond single crystal inclusions were found, and the relevant data were directly tested. On the basis of the analysis, the graphite SP2 carbon atoms to the diamond SP3 carbon atoms were proposed. The transformation process can be described as follows: Graphite SP2 is melted into the catalyst solvent in the form of atomic groups to form a metastable interstitial solid solution, and precipitates in the thermodynamically stable region of diamond with diamond SP3; thus, the analysis catalyst has two main types of carbon and bond formation. effect.
V. Conclusion
The development of each cause is the result of the unremitting efforts of many people. The reason why I want to write my own experience is to remember that Academician Huang Peiyun passed away in 2010. Academician Ma Fukang (I witnessed in Russia the scene of his academician of the Russian Academy of Sciences, he is also the winner of the Russian Presidential Friendship Award) Passed away in 2011, no help from Mr. Ma will not have this paper! Second, in order to learn, there is uncertainty in research, how to boldly envisage, and careful verification, although they are different, but the inner spirit can be learned and learned.
Yi Jianhong: Born in 1965, Zhuzhou, Hunan; currently a second-level professor at Central South University and Kunming University of Science and Technology, and vice president of Kunming University of Science and Technology. The main academic part-time jobs are: executive director of China Materials Research Society, secretary general of China Powder Metallurgy Federation, vice chairman of National Materials Science Experimental Teaching Committee, vice chairman of China Iron and Steel Association Powder Metallurgy Branch, China Institute of Nonferrous Metals, Powder Metallurgy and Cermet Vice Chairman of the Committee, Secretary General, Member of the Materials Science and Engineering Committee of the China Nonferrous Metals Society and the Precious Metals Committee, Vice Chairman of the China Mechanical Engineering Powder Metallurgy Branch, Director of the China Tungsten Industry Association, Member of the Expert Advisory Committee of China Nonferrous Metals Processing Association, China Member of the Association of Powder Metallurgy Experts of the Association, Member of the National Superhard Materials Expert Committee, Vice Chairman of the Hunan Mechanical Engineering Society; Deputy Editor-in-Chief of Powder Metallurgy Technology and Powder Metallurgy Industry, Progress of China Materials, Precious Metals and Editorial Board of "China Tungsten Industry" magazine.
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