Silicon micropowder production process and use

Microsilica is a pure quartz powder processed by advanced technology from fine grinding, is used widely in the inorganic non-metallic material. It has the advantages of excellent dielectric properties, low thermal expansion coefficient, high thermal conductivity and good suspension performance. Due to its excellent physical properties, high chemical stability, unique optical properties and reasonable and controllable particle size distribution, it is widely used in optical glass, electronic packaging, electrical insulation, high-grade ceramics, paint coating, precision casting. , silicone rubber, pharmaceuticals, cosmetics, electronic components and ultra-large scale integrated circuits, mobile communications, laptops, aerospace and other production areas.

Silicon micropowder is also an important raw material for the production of polysilicon. Microsilica with anhydrous hydrogen chloride (HCl) react in a fluidized bed reactor to produce trichlorosilane (SiHCl 3), SiHCl 3 reduction after further purification deposited polysilicon in hydrogen. Polysilicon is the main raw material for solar cells in the photovoltaic industry. In recent years, the continuous shortage of global energy has made the development of solar energy become the focus of energy strategies in the world. With the turbulence of the photovoltaic industry, the price of polysilicon in solar cell raw materials has skyrocketed, which has led to a rapid increase in the market demand for silicon micropowder. In short supply, silicon resource owners can enjoy amazing profits.

According to the survey, the current domestic production capacity of silicon micropowder is about 250,000 tons, mainly ordinary silicon micropowder, while high-purity ultra-fine silicon micropowder relies heavily on imports. It is initially predicted that the demand for ultrafine silicon micropowder in China will reach 60,000 tons in 2005. Among them, the rubber industry is the largest user, the coating industry is an important application field with great potential. The electronic molding compound, silicon substrate material and electronic and electrical castables all rely on imported high-purity ultra-fine silicon micro-powder raw materials, and only the price of ordinary spherical silicon micro-powder 2 - 30,000 yuan / ton, while the price of high-purity ultra-fine silicon micro-powder is as high as several hundred thousand yuan / ton.

Silicon micropowder is processed from pure quartz powder by advanced ultra-fine grinding process and is an inorganic non-metallic material with a wide range of uses. It has the advantages of excellent dielectric properties, low thermal expansion coefficient, high thermal conductivity and good suspension performance. Due to its excellent physical properties, high chemical stability, unique optical properties and reasonable and controllable particle size distribution, it is widely used in optical glass, electronic packaging, electrical insulation, high-grade ceramics, paint coating, precision casting. , silicone rubber, pharmaceuticals, cosmetics, electronic components and ultra-large scale integrated circuits, mobile communications, laptops, aerospace and other production areas. Silicon micropowder is also an important raw material for the production of polysilicon. Microsilica with anhydrous hydrogen chloride (HCl) react in a fluidized bed reactor to produce trichlorosilane (SiHCl 3), SiHCl 3 reduction after further purification deposited polysilicon in hydrogen. Polysilicon is the main raw material for solar cells in the photovoltaic industry. In recent years, the continuous shortage of global energy has made the development of solar energy become the focus of energy strategies in the world. With the turbulence of the photovoltaic industry, the price of polysilicon in solar cell raw materials has skyrocketed, which has led to a rapid increase in the market demand for silicon micropowder. In short supply, silicon resource owners can enjoy amazing profits. According to the survey, the current domestic production capacity of silicon micropowder is about 500,000 tons, mainly ordinary silicon micropowder, while high-purity ultrafine silicon micropowder relies heavily on imports. It is predicted that the demand for ultrafine silicon micropowder in China will reach 100,000 tons in 2008. Among them, the rubber industry is the largest user, the coating industry is an important application field with great potential. The electronic molding compound, silicon substrate material and electronic and electrical castables all rely on imported high-purity ultra-fine silicon micro-powder raw materials, and only the price of ordinary spherical silicon micro-powder 2 - 30,000 yuan / ton, while the price of high-purity ultra-fine silicon micro-powder is as high as several hundred thousand yuan / ton.

The ultrafine silicon micropowder has the characteristics of small particle size, large specific surface area, high chemical purity and good dispersion performance. With its superior stability, reinforcement, thickening and thixotropic properties, it has been widely used in many fields such as rubber, coatings, medicine, papermaking, and daily chemicals, and provides the basis for new materials for the development of related industrial fields. And technical guarantee, enjoy the reputation of "industrial MSG" and "the origin of material science". Since its inception, it has become one of the most adaptable and fastest-growing varieties of materials science in today's time. Developed countries have developed high-performance, highly-added fine inorganic materials as the focus of new materials in this century.

In recent years, the computer market and network information technology market have developed rapidly, the CPU set is getting bigger and bigger, the computing speed is getting faster and faster, the number of home computers and Internet users is increasing, and the requirements for computer technology and network technology are getting more and more. High, as the technology-based microelectronics industry has also achieved rapid development, PIII, PIV processors, broadband large-capacity transmission networks, are inseparable from the hardware support of large-scale, very large-scale integrated circuits.

With the rapid development of the microelectronics industry, large-scale, ultra-large-scale integrated circuits are increasingly demanding packaging materials, not only requiring ultra-fine, but also requiring high purity, low radioactive element content, especially for particles. The shape proposes a spheroidization requirement. High-purity ultra-fine molten spherical quartz powder (referred to as spherical silicon micro-powder) has large-scale, high-temperature, high heat resistance, high moisture resistance, high filling amount, low expansion, low stress, low impurity, low friction coefficient and other superior properties. In the substrate and packaging materials of VLSI, it has become an indispensable high-quality material.

Why spheroidize? First of all, the surface of the ball has good fluidity, uniform film formation with the resin, small amount of resin added, and the best fluidity, the filling amount of the powder can be the highest, and the weight ratio can reach 90.5%. Therefore, the spheroidization means silicon micropowder. The increase of the filling rate, the higher the filling rate of the silicon micropowder, the smaller the coefficient of thermal expansion, and the lower the thermal conductivity, the closer to the thermal expansion coefficient of the single crystal silicon, and the better the performance of the electronic components produced. Secondly, the viscous molding compound has the lowest stress concentration and the highest strength. When the stress concentration of the molding powder of the angular powder is 1, the stress of the spherical powder is only 0.6. Therefore, when the spherical powder molding compound encapsulates the integrated circuit chip, the yield is It is high and it is not easy to cause mechanical damage during transportation, installation and use. Third, the spherical powder has a small friction coefficient, and the wear on the mold is small, so that the service life of the mold is long. Compared with the angular powder, the service life of the mold can be doubled, and the price of the packaging mold of the plastic sealing material is high. Imports are also needed, which is also important for packaging plants to reduce costs and improve economic efficiency.

Spherical silicon micropowder, mainly used for large-scale and very large-scale integrated circuit packages, according to the degree of collection (the number of standard components per integrated circuit) to determine whether spherical silicon micropowder, when the degree of 1M to 4M, has been partially used spherical Powder, spherical powder has been used all at the 8M to 16M level. At the 250M level, the line width of the integrated circuit is 0.25 μm. When the level of 1G is set, the line width of the integrated circuit is as small as 0.18 μm. At present, the CPU chip of the computer PIV processor has reached such a level. At this time, the spherical powder used is more high-grade, and the waste material of polycrystalline silicon is mainly used to prepare ethyl silicate and silicon tetrachloride to obtain SiO2, which is also made into a spherical shape and the particle size is - (10-20) μm. . The spherical silicon micropowder synthesized by the chemical method is 10 times more expensive than the spherical powder made of the natural quartz raw material, because the powder is substantially free of radioactive alpha ray pollution, and the uranium content of 0.02 ppm or less can be achieved. When the degree of integration is large, the distance between the wires of the VLSI is very small, and when the bulk of the package material is large, the source error will occur when the integrated circuit works, which will affect the reliability of the operation of the VLSI. Therefore, it is necessary to propose radioactivity. strict requirements. The natural quartz raw material reaches (0.2 ~ 0.4) PPb is a good raw material. The spherical powder used in China is mainly spherical powder made of natural raw materials, and is also imported powder.

In general, integrated circuits are lithographically patterned on a single crystal silicon wafer, and then connected to lead wires and tube corners, and then encapsulated with epoxy plastic sealing material. The closer the thermal expansion rate of the molding compound is to the single crystal silicon, the better the thermal stability of the integrated circuit. The melting point of single crystal silicon is 1415 ° C, the expansion coefficient is 3.5 PPM, the fused silica powder is (0.3 ~ 0.5) PPM, the epoxy resin is (30 ~ 50) PPM, when the molten spherical quartz powder is added to the epoxy at a high ratio. When the molding compound is made into a resin, the coefficient of thermal expansion can be adjusted to about 8 PPM, and the more the addition, the closer it is to the single crystal silicon wafer, and the better. The crystal powder commonly known as raw powder has a coefficient of thermal expansion of 60 PPM, and the melting point of crystalline quartz is 1996 ° C, which cannot replace fused silica powder (ie, molten silicon micropowder). Therefore, when spherical powder is not used in medium and high-grade integrated circuits, molten angular silicon is also used. Micro powder. This is also the reason why the high-grade spherical powder is not successful in shaping the crystal powder into a nearly spherical shape. In the 1980s, Japan also walked through this road, and the effect was not good. It could not be achieved. Ten years ago, including China, there are still people who have taken this road. From the above theory, this method is not acceptable. That is, the high-grade plastic sealing powder cannot be replaced by crystalline powder.

Is it better to produce high-purity spherical quartz powder from fused silica (ie, high-purity quartz glass) or crystalline quartz? According to the test, experts believe that this problem is very clear, using natural quartz SiO 2 , high-temperature melt-spraying to make the ball, you can make a completely molten spherical quartz powder. A ball made of natural crystalline quartz, and then dispersed with a plasma flame is a molten ball. The ball made of flame-fired powder has a surface brilliance and a volume shrinkage. It is better to use the powder provided by Japan. X-ray spectroscopy analysis of the line is completely flat, is also a fully fused spherical quartz powder, while domestically fused quartz, such as Lianyungang fused silica spectral analysis of amorphous content of 95%, the line can still see spikes, still 5% are not melted. It can be seen that the production of spherical quartz powder, as long as the purity can meet the requirements, the natural crystalline quartz is the best raw material, the production cost is the lowest, and the process route is simpler and simpler.

First, the application of silicon micropowder in rubber products

The active silicon micropowder (treated by a coupling agent) is filled in a rubber such as natural rubber or butadiene rubber, the powder is easily dispersed, the mixing process performance is good, the calendering and extruding properties are good, and the vulcanization speed of the vulcanized rubber can be improved. It also has the effect of improving the viscosity of rubber, especially the ultra-fine grade silicon micropowder, which replaces some of the white carbon black in the rubber compound, which has a good effect on improving the physical property index of the product and reducing the production cost. -2um up to 60-70% silicon micropowder for export grade medicinal chlorobutyl rubber stoppers and for use in electrical insulation rubber shoes.

Silicon micropowder is used as a filler in the production of imitation leather. Its technical strength, elongation and flexibility are superior to those of inorganic materials such as light calcium carbonate, activated calcium carbonate and active pyrophyllite . product.

Silicon micropowder replaces the refined clay, light carbonic acid and other powder materials used in battery plastic shells, filling up to about 65%, and the process performance is good. The obtained rubber shell products have smooth and flat appearance, high hardness, acid corrosion resistance, voltage resistance, thermal deformation and impact resistance, etc., all of which meet or exceed the technical specifications of JB3076-82.

Second, the application of silicon micropowder in plastic products

Active silicon micropowder is an ideal enhancer for polypropylene, polyvinyl chloride, polyethylene and other products. It not only has a large filling capacity, but also has good tensile strength. Made of masterbatch, used in PVC floor tiles to improve the wear resistance of the product.

The silicon micropowder is applied to the olefin resin film, which has uniform powder dispersion, good film forming property and strong mechanical properties. Compared with the plastic film produced by using PCC as a filler, the infrared transmittance of the barrier is reduced by more than 10%, and the application of the agricultural greenhouse film is extremely popular. In the whole country. Can also be used in the field of wire and cable outer skin.

Third, the application of silicon micropowder in the glass and glass fiber of the melting instrument

Due to the fineness and high purity of the silicon micropowder particles, it is easy to melt in the production of glass, and the time is short. The physical and chemical properties and appearance quality of products such as borosilicate instrument glass, sodium levy instrument glass and neutral ware have reached the corresponding standards. At the same time, the energy saving effect in production is particularly significant.

Furthermore, according to the characteristics that the silicon micropowder has fine and uniform particle size and large specific surface area, it is used for a new process of direct drawing of glass fiber, which greatly improves the homogenization degree of the glass fiber batch material and accelerates the vitrification speed in the furnace. The drawing stability is superior to the glass ball drawing process, and has significant energy saving and production cost reduction effects. As an energy-saving mineral raw material, silicon micropowder is used in the ceramic industry, and it also has an ideal effect for lowering the firing temperature and improving the yield.

Fourth, silicon micropowder is good for polishing and washing abrasives.

With the development of modern technology, the surface treatment of materials is also required to be higher and more refined, and the application of grinding is becoming more and more extensive. Because of its close to round shape, the silicon micropowder is ultra-fine powder prepared by ultra-fine and graded, and then modified, it is a good washing abrasive for metal parts. For example, in the application of washing bearings, the finish can reach more than 3.0, which is better than the display. Similar products.

In addition, it is used in the semiconductor industry, precision valves, hard disks, magnetic head polishing, automotive polishing agents, and has good results.

Fifth, the application of silicon micropowder in coatings

Using the unique functionality of microsilica, substituted precipitated barium sulfate, talc, blending formulation for paint, primer, paint and the like anti-Quan (added in an amount of 6% to 15%) is filled not only as compatibilization, and The effects of improving the fineness of the paint, the leveling performance, the hardness of the paint film, the grinding time of the paint, the water resistance, the rust prevention, the corrosion resistance of the paint, the dispersibility of the pigment, and the storage stability of the paint are all remarkable. Furthermore, the melt film coating which is arranged in a certain proportion from silicon micropowder, water, surfactant and water has become a high-quality coating in precision casting due to its low viscosity, convenient use without filling and the like.

Used for cabinet finishes with excellent decorative effects and corrosion resistance.

6. Application of silicon micropowder in electrical insulation packaging materials

Electrical grade silicon micropowder is a kind of active silicon micropowder. It is used as epoxy resin insulating sealing filler for electrical products. It not only can greatly increase the filling amount but more importantly, it can reduce the viscosity of the mixture system, improve the processing performance and improve the mixture. The permeability of the high-voltage electrical coil reduces the expansion coefficient of the cured product and the shrinkage rate during the curing process, and maintains the thermal tension difference between the mixture and the coil, and improves the thermal, electrical and mechanical properties of the cured product.

As for the industry prospects of silicon micropowder, we look forward to the following aspects: In terms of market space internationally, the world's annual demand for silicon micropowder is about 100,000 tons. Japan is the country with the largest output of epoxy molding materials in the world today. The annual demand for silicon micropowder is 30,000 tons, all of which rely on imports; the United States needs 20,000 tons of silicon powder; the annual demand for silicon powder is more than 10,000 tons. Domestically, according to the statistics of relevant departments, the high-purity 300-1000 mesh ordinary silicon micropowder and ultra-fine crystalline silicon micropowder will maintain a growth rate of 20% to 35% at home and abroad every year, and the demand will increase with the expansion of the application range. Keep on increasing. In 2001, the total consumption of molten metal in China was 18,000 tons, of which 12,000 tons were imported. In 2004, the total consumption was 78,000 tons, of which 48,000 tons were imported. It is estimated that the total consumption will exceed 100,000 tons this year, and the import volume reached 25,000 tons in the first half of the year. The annual demand for silicon micropowder in the high-tech field is more than 20,000 tons. It is speculated that the domestic demand for molten silicon micropowder can reach 150,000 to 300,000 tons in 2010; in terms of electronic products, the demand for crystalline silicon micropowder is expected to exceed 700,000 tons per year; in fused silica ceramics In terms of domestic demand for silicon micropowder, the annual demand will reach 30,000 tons, and the market prospect is broad. It is understood that China's high-grade silicon micro-powder products mainly rely on imports. As China joins the WTO market and the rapid development of China's IT industry, the electronics packaging industry will gradually move to China. Experts predict that China will become the world's largest packaging country in the new century, and the market for downstream products such as high-purity ultra-fine silicon micro-powder will also expand. Although the profit margin is the same as the silicon micropowder product, the price is different by 100,000 miles. For example, the ordinary 300 mesh silicon micropowder is only 600 yuan/ton, while the 8,000 mesh to 10000 mesh ultrafine high-purity electronic product is suitable for the micropowder price up to 100,000 yuan. / ton, if you upgrade to nano-scale molten fine powder, the price is more than 200,000 yuan / ton. Product development space China's relevant units have successfully developed electronic grade high-purity ultra-fine silicon micro-powder. This is an attractive electronic material product with a promising market. High-purity ultra-fine silicon micro-powder is the main raw material for large-scale integrated circuit substrates and electronic packaging materials. It can be bonded with epoxy resin to complete the bonding and sealing of chips or components. The incorporation ratio of the ultrafine silicon micropowder in the epoxy resin determines the thermal expansion coefficient of the substrate. The higher the proportion of the silicon micropowder, the smaller the thermal expansion coefficient of the substrate, that is, the closer to the thermal expansion coefficient of the silicon wafer, so that the damage to the micron line caused by the uneven expansion can be avoided. Therefore, there are strict requirements on the purity, fineness and particle size distribution of the silicon micropowder. The above examples of enterprise examples show that silicon micropowder has attractive market prospects and broad development space. With the development of high technology, the requirements for silicon micropowder materials are getting higher and higher. Enterprises can completely adjust the product structure and develop deep processing products according to the needs of the market, and improve the competitiveness of enterprises. But these must have an indispensable premise - technological innovation. Only by relying on technology to develop high-tech products can we expand the market space and form a virtuous circle.

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