Enthusiastically looking forward to a new chapter of high-strength powder catalyst

Abstract In the early 1990s, China's diamond industry had developed greatly. The hinged six-face press with China's independent intellectual property rights has matured. High-pressure cylinders have been expanding; the number of domestic presses is increasing. Taking iron, nickel, cobalt and manganese as...
In the early 1990s, China's diamond industry had developed greatly, and the hinged six-face press with China's independent intellectual property rights has matured. High-pressure cylinders have been expanding; the number of domestic presses is increasing. The sheet-like catalyst material with iron, nickel, cobalt and manganese as basic elements is refurbished, and the catalyst sheet is made thinner. The graphite sheet (carbon sheet) is basically stable. The main auxiliary material, the pyrophyllite block, has been pressed by the powder and is generally uniform, which can meet the requirements of diamond single crystal production. The elites in the industry are pursuing the improvement of quality, output and cost performance.

When China's superhard materials industry was born, diamond materials were still national strategic materials. Production equipment, technology, etc. are absolutely confidential internationally. Our six-face press is born under this background, but the European and American countries use a two-face press, which has a large tonnage, advanced materials, advanced sintering technology, and is controlled by a single pressure source, which is relatively stable. The diamond produced is of high quality and is a high-grade product. Our six-face top press has a small tonnage and is a six-pressure source. The control is relatively difficult, and the material has not changed much for many years. The diamond products produced are medium-low grade. In terms of compressive strength (at the time of static compressive strength), crystal form, transparency, color, particle size, and impurities, there is a big gap compared with the products of the two-face press. In the international market, the price gap between the two products is even more disparity. But many of our superhard material tools, such as saw blades for cutting stone, require medium to high grade diamonds. To develop the tool industry, we can only purchase large amounts of money and scarce foreign exchange from European and American countries. To this end, the country has spent huge sums of money to introduce multiple different types of two-sided presses. Unfortunately, due to various reasons, the indigestion has been poor, and the cost performance of the product is poor, and the expected effect has not been exerted.

How to improve the quality of domestic diamonds, adapt to the needs of domestic super-hard materials tools, and narrow the gap between diamond quality produced in Europe and the United States. It is the goal of the elite in the super-hard materials industry. There are four main factors determining the quality of diamond products. Factors: equipment, materials, cavity structure, sintering process or synthetic process. Improve the equipment, increase the hydraulic cylinder diameter, increase the pressure, expand the cavity, and indeed improve the quality and cost performance of the product. The cavity is enlarged, the temperature field inside the cavity is more uniform, and the quality of the single crystal is naturally improved. Continuous improvement of equipment, increase of tonnage of presses, and expansion of the cavity (and of course the end) are the basis and prerequisites for the development of China's superhard materials industry. However, the working form of the six-face press and the two-face press are quite different. The six pressure source determines that it is more complicated to expand, especially the hinge beam, to withstand greater stress, and put forward higher requirements in materials, manufacturing processes, error control and so on. Also affected by China's industrial infrastructure at that time, raising the tonnage of the press is not a one-off event. It can only be gradual and inconsistent. Until now, there is still a certain gap between the tonnage of the press and the tonnage of the press on both sides. Perfect cavity structure, not only meet the working needs of the press, but also achieve the effects of heat preservation, pressure transmission and sealing. It also satisfies the uniform and stable temperature field and pressure field of diamond single crystal growth, and also improves the quality of diamond. It is very important to optimize the synthesis process to ensure that the diamond crystals are nucleated and grown as needed, and some progress has been made. In addition to improving tonnage, expanding the cavity, perfecting the cavity structure, optimizing the synthesis process, whether it can make breakthroughs in materials to meet the needs of domestic saw-grade diamonds, it has become the thinking of the technicians of Beijing Jingxinlei Company. The problem. In view of the fact that researchers in China have further understood the growth mechanism of diamonds, the two-side press in Europe and the United States has begun to use powder materials. Can the use of powder catalyst, powder graphite as a raw material for the production of diamond, converted to a six-sided top press, improve the cavity structure and synthetic process to create a better environment for diamond growth, also It became the responsibility and task of the technicians of Beijing Jingxinlei Non-Metal Materials Co., Ltd.

In 1994, in Beijing Jingxinlei Non-Metallic Materials Co., Ltd., the research objective was to produce “saw-chip” synthetic diamond products on a six-face press using powdered catalyst and powdered graphite. There are many problems facing the target in the future, such as:

Selection of powder catalyst materials,
Selection of powdered graphite materials,
Selection of mixing equipment for powder materials, exploration of mixing processes,
The method of molding powder materials, and the choice of equipment and process.
Designed to match the cavity structure of the powder material.
The production method and equipment selection of the components that make up the cavity.
Optimization of the synthesis process, etc.

Of course, the most important choice of powder catalyst materials, according to their understanding of the catalyst, the technical use of the catalyst materials used in the two-side press, with reference to the composition of the sheet-like catalyst, fully take into account China's national conditions, requirements are not Under the premise of affecting product quality, try to reduce material costs, such as not using expensive cobalt metal. After repeated experiments, it was basically determined that an alloy containing Fe, Ni, and Mn as a basic element was sprayed into a powdery material as a powder catalyst. The graphite material is selected from crystalline solid graphite flakes. The Liumao mine in Heilongjiang Province is used as the main source of graphite materials. Impurities in the graphite material directly affect the quality of the product. The amount of impurities should be minimized when selecting materials. There are also the ratio of various materials, the problem of the size of the material, etc. Only through experimental optimization and selection can we draw a relatively appropriate conclusion. After several thousand experiments, Beijing Jingxinlei Non-Metallic Materials Co., Ltd. finally determined that Fe, Ni30 and Mn8 were used as catalysts, and the alloy powder was sprayed by gas atomization. The particle size ranged from 200 mesh to 300 mesh. Control is below 200PPm. The graphite material was determined to have a crystal form of relatively pure natural phosphorous flake graphite having a purity of 99.99% and a particle size of between 200 mesh and 300. The ratio of catalyst graphite is 3:7, and graphite is added. Mix well without pre-mixing with other impurities. Such a thin material, without any adhesive, is pressed into a cylinder, which is difficult under the pressure conditions of the press at that time. For the research needs, we have developed processes such as isostatic pressing, granulation and pressing. Finally, a "synthesis column" that can grow diamond single crystals can be fabricated on a four-column press.

With good materials, you must also create a good environment for the growth of single crystals. In order to match this powder material, Beijing Jingxinlei Non-Metallic Materials Co., Ltd. has done a lot of work in cavity design. For example, the steel cap has been improved, a dolomite casing has been used, and an iron belt has been added. Under the conditions at the time, this was a new thing. There were no supporting manufacturers. Except for the pyrophyllite and steel parts, all the necessary accessories were produced by themselves. With the development of the experiment, a process flow for producing accessories was gradually established. Because the production of graphite columns is almost entirely black, the production of cavity accessories is almost entirely white. At that time, employees of Beijing Jingxinlei Company dubbed our production as "black" and "white".

In the experiment, Jing Xinlei's employees have experienced too much confusion, and confusion has also led to more thinking. For example, the first process of "black road" mixes. What kind of equipment is used to mix the two kinds of fine powders with different specific gravity? How long does it take to mix evenly? How much influence the mixed material will have on the uniformity of mixing. After repeated experiments and improvements, a basic result was finally obtained. Even the mixing uniformity and mixing time of the two materials identified were found to be non-linear. To give a simple example, the "graphite column" is pressed by a four-column press, and there is a phenomenon of intermediate cracks appearing after the mold is released, and the height becomes large, which does not meet the requirements of production. What is the cause of this is that the pressure holding time is short, the pressure is insufficient, the humidity is a problem, the mold gap problem, or the size of the granulation. The problem is simple, but it leads to a series of thoughts. After repeated such a process in the experiment, problems arise - thinking - calm analysis - finding solutions - improving - good results again. The technicians of Beijing Jingxinlei Non-Metallic Materials Co., Ltd. are convinced that as long as the goal is clear, the belief in achieving the goal is firm, and the solution to the problem is done properly, Dawn is ahead. After thousands of experiments, through the repeated process of problems, analysis and problem solving, a complete set of production process and product quality standards of “black” and “white” were established.

In 1996, the experimental work was completed and passed the continuous pilot production, which achieved the expected goal. On the six-face press, the “saw-chip” synthetic diamond was produced from the powder material. The crystal form of the product is complete, which is a typical cubic octahedral shape, with good permeability, low impurity content, high yield, high particle size concentration rate, and more than 20% of single crystals with static pressure above 20 kgf . Under the microscope, the product is evenly and crystal clear. Fully meet the requirements of high quality "saw blade grade" synthetic diamond. From setting goals to reaching the goal to complete the task, the cultivators of Beijing Jingxinlei Non-Metal Materials Co., Ltd. experienced too much confusion and trouble, and also gained more excitement and joy. There is a problem, how to solve it, once or twice the adjustment has not solved the problem is trouble, the problem is finally solved is excitement, the production of crystal clear and full of high-grade diamond is joy. Jing Xinlei’s cultivators are in the alternation of trouble and excitement, in the alternation of sweat and tears, completed the production of “saw-chip” synthetic diamond on the six-sided top press with powder catalyst material. Task. In this process, the talent has also grown, and the understanding of the nucleation and growth of diamond single crystal has been deepened. The emergence of the hinged six-face press is a prerequisite for the production of synthetic diamonds in China, which has laid the foundation for China's superhard materials industry. The emergence of powder materials is a major reform compared to sheet materials. The improvement of product quality has filled the gap that cannot produce mass-produced "saw-chip" diamonds. It can also be said to be a revolution. It reduces the gap in diamond quality produced by the top presses in Europe and the United States. The excellent cavity structure provides a good environment for diamond growth. Synthetic processes are conditions that produce high quality diamonds, and they are all important. Only in the four aspects of equipment, materials, structure and technology can we produce high-quality diamond products that can meet the requirements. Based on these understandings, Jingxinlei Company has summarized the “synthesized saw blade-grade synthetic diamond blank”, that is, the powder material, “the ultra-high pressure high-temperature greenhouse for the synthesis of super-hard materials”, that is, the cavity structure, and “the synthetic synthetic diamond proprietary technology” A number of patents such as synthetic processes.

In August 1996, it cooperated with the Ministry of Metallurgy Yanjiao Diamond Industry Co., Ltd. and Mentougou Lanlong Co., Ltd., and transferred to mass industrial production, and achieved good results. There is still a gap between the success of the experiment and the continuous scale of industrial promotion. It emphasizes the improvement of the supply chain and emphasizes the stability and standardization of the products. More emphasis is placed on the reduction of material costs. For catalyst materials, it is required to reduce the impurity content as much as possible, especially the oxygen content, which is required to be limited to 150 ppm in mass production. The particle size is limited to between 200 mesh and 300 mesh. The gas atomized dusting is carried out under the protection of argon-type nitrogen . However, at that time, the domestic milling manufacturers were either full of orders, busy production, no spare time to produce such products, or production conditions were not available, and the oxygen content of the catalysts produced was too high to meet the requirements. Later, a foreign manufacturer took the order. It is guaranteed that according to the formula of Jingxinlei Company, the main component is FeNi30Mn8 (later changed to Mn4), and it produces qualified powder catalyst with trace amount of other impurities, oxygen content below 150PPm and particle size between 200-300 mesh. Graphite materials are purchased in the form of strip processing. Purchasing 99% natural phosphorus flake graphite, please use the high-temperature chlorine removal process in Shanghai Electric Furnace Factory to produce 99.99% high-purity graphite. The main material supply is continuous, the product is stable, and the “black road” product is stable. After hard work, the production of cavity attachment materials has also reached a standard and stable. The production of “White Road” has also stabilized. The production specifications and stability of “black” and “white” have laid the foundation for the industrialization of powder materials.

In May 1997, the experiment, the pilot test, and the industrial trial production were completed, and the application was officially promoted. The initial stage of promotion is also very difficult. The single crystal product is new, especially the crystal form is very complete. In the whole industrial chain, other parts have not been adjusted yet, and the product enters the market, and there will be problems in the application. To give a small example, in the early stage of application promotion, a single crystal manufacturer suddenly proposed that their downstream saw blade manufacturers reflected that the application began to be fast and good when cutting stone, but it could not be cut after a while, I don’t know. what is the reason. Beijing Jingxinlei Non-Metallic Materials Co., Ltd. sent a technician to field visit and found that there was no trace of diamond breakage on the carcass of the cutter head, all of which were pit marks left after the diamond fell. Tell them that this is not a diamond quality issue. The crystal form of the diamond is intact and basically spherical. The carcass has insufficient grip on it, and all of it is lost. Naturally, the stone cannot be cut. To solve the problem, you need to adjust the carcass formula. They bought the best diamond single crystal from GE and re-doed the secondary cutter. The result of the cutting experiment was the same. Later, they improved the carcass material, solved the problem of the inlay and achieved good results.

Beijing Jingxinlei Non-Metallic Materials Co., Ltd. began research in 1994, and after the pilot test in 1996, it was applied to the production and promotion in 1997. It has received strong support from many manufacturers in the same industry. Under the cooperation of the upstream and downstream of the industrial chain of the super-hard materials industry, since 1997, a raw material for the production of diamond single crystals, powder catalyst, has emerged in the super-hard materials industry. Adding a new wonder to China's superhard materials industry!

Since 1998, Beijing Jingxinlei Non-Metallic Materials Co., Ltd. has studied the project of “Synthesis of High-grade Diamonds of Primary Single Crystal Fine Particles”. This project was undertaken by Comrade Bian Ping, and was attended by several technicians. In June 2000, the Beijing Municipal Science and Technology Commission made a scientific and technological achievement appraisal. The appraisal opinion is “fine-grain high-grade diamond manufactured by the synthetic technology of this project. The crystal form is complete, the transparency is high, the impact resistance is good, etc. The quality index is close. The advanced level of similar foreign products."

Although we have been working in the industry for almost 20 years, it is still a recruit for China's 50th anniversary of diamond development. At present, in addition to continuing to provide diamond powder columns and fine-grade high-grade diamonds, our company has carried out some new explorations on large-scale composite films, and it has already achieved initial results! Our main goals are: respecting science, respecting talents, striving to study some high-end products, and making due contributions to China's superhard materials to fully realize the dream of a strong country. Since nearly 100 people have entered the industry, it is so fascinating, and there are so many topics that need to be constantly explored and researched, and we are determined to dedicate everything to it. Together with my colleagues, we will strive to make China's superhard materials bigger and stronger! (This article is taken from "China's Superhard Materials Industry Fifty Years")

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