CN211078490U - Production device for preparing spherical silicon micropowder by ultrasonic atomization - Google Patents
Production device for preparing spherical silicon micropowder by ultrasonic atomization Download PDFInfo
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Abstract
The utility model discloses a production device for preparing spherical silicon micropowder by ultrasonic atomization, which comprises a speed-control discharger, an electric heating and heat-preserving device, an ultrasonic atomizer, a water cooling reaction device, a transit tank, a diaphragm pump plate-and-frame filter press, a beater, a spray dryer, a screening device and a fan; the electric heating heat preservation device comprises an electric heating crucible and an electric heating pipe which are sequentially connected from top to bottom; the electric heating heat preservation device, the ultrasonic atomizer, the water cooling reaction device and the transit trough are sequentially connected from top to bottom; the transfer tank is connected to a plate-and-frame filter press through a diaphragm pump, and the plate-and-frame filter press is connected to a beater; the beating machine is connected to the atomizing nozzle feed inlet on the spray dryer through the delivery pump, and screening plant and fan are connected in order to the spray dryer lower extreme. The device produces the high-purity spherical silicon micropowder by utilizing ultrasonic atomization, and has a great application prospect.
Description
Technical Field
The utility model relates to an ultrasonic atomization prepares apparatus for producing of spherical silica micropowder belongs to non-metallic ore deep-processing technical field.
Background
In recent years, with the rapid development of microelectronic technology, people have higher and higher quality requirements on microelectronic elements, so that the quality requirements on silicon micropowder are higher and higher. 97% of the global Integrated Circuit (IC) packaging materials adopt Epoxy Molding Compound (EMC), and in the composition of EMC, silicon micro powder is the most used filler except the main material of novolac epoxy resin. The weight ratio of the silicon micro powder filler to the epoxy molding compound is 70-90%. Therefore, for high quality molding compounds, it is required to have ultrafine silica powder, high purity, low radioactivity elements, and in particular, to have spherical particles. This is because: (1) the surface fluidity of the ball is good, and the ball is uniformly stirred with resin to form a film, so that the addition amount of the resin is small, and the filling amount of the silicon micro powder reaches the highest, therefore, the sphericization means the increase of the filling rate of the silicon micro powder, the higher the filling rate of the silicon micro powder is, the smaller the expansion coefficient is, the lower the thermal conductivity coefficient is, the closer the thermal expansion coefficient is to the thermal expansion coefficient of monocrystalline silicon, and the better the service performance of the produced electronic component is; (2) compared with the plastic package material made of angular silicon micropowder, the spherical plastic package material has the advantages of minimum profit concentration and highest strength, and when the stress concentration of the plastic package material of the angular powder is 1, the stress of the spherical powder is only 0.6, so that the finished product rate of the manufactured microelectronic device is high, the transportation and the installation are convenient, and the mechanical damage is not easy to generate in the using process; (3) compared with angular silicon powder, the spherical powder has small friction coefficient and small abrasion to the die, so that the service life of the die can be doubled. (Ruan Jianjun 'research progress of spherical silicon micropowder' and Lijun, Jiangxing 'spherical silicon micropowder')
At present, the high-quality spherical silicon powder required by China partially depends on import, and how to prepare the high-purity and superfine spherical silicon powder is still a domestic powder research hotspot. The preparation method of the spherical silicon micro powder at the present stage mainly comprises a physical method and a chemical method.
1. Physical method
1.1, flame balling: the flame balling method comprises the steps of firstly carrying out pretreatment such as crushing, screening and purifying on quartz, then sending quartz micro powder into a high-temperature field generated by fuel gas-oxygen, carrying out high-temperature melting and cooling balling, and finally forming the high-purity spherical silicon micro powder.
Specifically, acetylene gas, hydrogen gas, natural gas and other industrial fuel gases can be used as clean pollution-free flames of molten powder as heat sources, and the method relates to the theories of thermodynamics, hydrodynamics, particle hydrodynamics and the like. Compared with plasma high-temperature flame, the method does not relate to the problems of electromagnetism theory and ion flowing and moving in an electromagnetic field, is easy to control production, is easy to realize industrialized large-scale production, and is a production process with development prospect.
The disadvantages of this method are: the industrial gas, acetylene gas and natural gas, also can bring certain pollution to the product quality in the combustion process. The danger coefficient of hydrogen is large in the using process. At present, no large-scale and mature application report of the method in industry is found.
1.2, high-temperature melt injection method: the high-temperature melting spraying method is to melt high-purity quartz into liquid at 2100-2500 ℃, and the spherical silicon micro powder is obtained after spraying and cooling. The product has smooth surface, and the sphericization rate and the amorphous rate can both reach 100 percent. According to research, the spherical silica powder in the United states is mainly produced by the method, and because of the high-performance computer technology, the spherical silica powder is tightly sealed. The high-temperature melting injection method is easy to ensure the nodularity and the amorphous rate, but is not easy to solve the problems of purity, atomized particle size adjustment and the like. At present, the research and production reports on the aspect are not seen in China.
1.3, self-propagating low-temperature combustion method: the process flow of the self-propagating low-temperature combustion method comprises the steps of preparation of sodium silicate, preparation of silicic acid sol, preparation of mixed combustion liquid, combustion reaction, annealing decarbonization, washing treatment and the like.
The technical method has the following advantages:
(1) the fused silica micro powder can be used as a raw material, and the method can also be popularized to the natural powder quartz as a raw material; (2) the process is simple, has no special equipment requirement, is convenient to operate, is easy to control and has low production cost; (3) the materials used in the production process only contain sodium ions and nitrate ions which are very soluble in water, and other impurity ions are not introduced, so that the preparation of the high-purity silicon micro powder is facilitated.
The disadvantages are that: at present, the method only stays in a laboratory stage, and large-scale production cannot be well realized.
1.4, plasma method: the basic principle of the plasma process is to use a high temperature zone of the plasma torch to deposit silicon dioxide (SiO)2) The powder is melted and spherical liquid drops are formed due to the action of the surface tension of the liquid, and spherical particles are formed in the rapid cooling process. The method has the advantages of high energy, fast heat transfer, cooling block, controllable appearance of the prepared product, high purity and no agglomeration.
The disadvantages of this method are: at present, the method only stays in a laboratory stage, and large-scale production cannot be well realized.
1.5, high-temperature calcination spheroidization: the high-temperature calcination spheroidization is generally used for preparing high-purity superfine spherical silicon powder, and the high-purity superfine spherical silicon powder is mainly prepared from mineral powder by the processes of calcination, ball milling, magnetic separation, air separation and the like.
The method has the advantages that: the high-purity superfine spherical silicon powder has the advantages of high spheroidization rate, good whiteness, high silicon content, less iron and aluminum, neutral and acidic pH value, good flowing dispersibility, small expansion and heat conductivity coefficient, low electric conductivity, corrosion resistance and low production cost.
The disadvantages of this method are: this technique is currently still in the experimental phase.
2. Chemical process
2.1, gas phase method: gas phase method of SiO2The white carbon black is a fine and special amorphous powder material prepared by hydrolyzing silicon halide at high temperature. Silane halide is subjected to high-temperature hydrolysis reaction in water generated by oxyhydrogen combustion flame, the temperature is generally up to 1200-1600 ℃, then quenching is carried out, and the SiO generated by the finished product gas phase method is obtained through post-treatment such as aggregation, cyclone separation, air jet deacidification, fluidized bed screening, vacuum compression packaging and the like2The product has high purity, average primary particle diameter of 7-40nm, and specific surface area of 50-380m2/g，SiO2The mass fraction is not less than 99.8%. The method has the disadvantages of difficult dispersion in organic matters and environmental pollution.
2.2 hydrothermal synthesis method: the hydrothermal synthesis method is a common method for preparing nano particles in a liquid phase, generally, inorganic and organic compounds are combined with water under the environment of temperature of 100-350 ℃, an improved inorganic substance is obtained by controlling an accelerated dialysis reaction and a physical process, and high-purity and ultrafine micro particles are obtained by filtering, washing and drying. The hydrothermal method has the advantage of directly generating oxides, and avoids the step of converting the oxides into the oxides by calcination in the common liquid phase synthesis method, thereby reducing the formation probability of hard agglomerates.
The disadvantages of this method are also evident: limited by the size of the reaction kettle, the current hydrothermal method for preparing SiO2But also in the laboratory phase.
2.3, sol-gel method: the sol-gel method is a method of solidifying an organic or inorganic metal compound in a solution, sol, or gel, and then forming an oxide or other compound solid by heat treatment. The method has the advantages of good chemical uniformity, fine particles, high purity, simple equipment and high powder activity. The disadvantages are that: the raw materials are expensive, the sintering property among particles is poor, the shrinkage is large during drying, and the problem of agglomeration is easy to occur.
2.4, a precipitation method: the precipitation method comprises adding surfactant into water glass and acidifying agent as raw materials, controlling reaction temperature, adding stabilizer when pH of the precipitation solution is 8, washing, drying, calcining, and collecting precipitateForming the silicon micropowder. SiO produced by precipitation2Uniform grain diameter, low cost, easy process control and contribution to industrial production, but has certain agglomeration phenomenon.
2.5, a micro-emulsion method: the microemulsion method is characterized in that two solvents which are not mutually soluble are utilized to form uniform emulsion under the action of a surfactant, so that the processes of nucleation, production, coalescence, agglomeration and the like are limited in a tiny spherical liquid drop, a solid phase is separated out from the emulsion to form spherical particles, and further agglomeration among the particles is avoided. Preparation of SiO by microemulsion method2Most of the silicon source is tetraethoxysilane, tetraethoxysilane molecules are diffused and permeate into water nuclei through a reverse micelle interface film, and then hydrolysis condensation reaction is carried out to prepare SiO2. The product prepared by the method has narrow particle size distribution, controllable particle size and good dispersibility. The disadvantages of this method are: at present, the method only stays in a laboratory stage, and large-scale production cannot be well realized.
3. Spraying method: the spraying method is a method of combining chemistry and physics in which a solution is atomized by various physical means to obtain ultrafine particles. The basic process is the preparation of solution, spraying, drying, collecting and heat treatment. The method is characterized in that the particle distribution is relatively uniform, but the particle size is submicron to 10 mu m, and the method is a novel method for synthesizing the nanoparticle oxide with controllable particle size. The disadvantages of this method are: high energy consumption, serious agglomeration of the dried micro powder and inconvenient use.
By comparing the above-mentioned methods for preparing the silica powder, we can roughly find that: the raw materials needed by the spherical silicon micropowder prepared by the physical method are cheap, but the requirements on the quality of the raw material quartz, production equipment and the like are high. The flame balling method is a process technology which can realize large-scale production and has development prospect at present, but has the problems of purity and atomized particle size adjustment.
The chemical method can prepare the spherical SiO with high purity and uniform grain diameter2However, because a large amount of surfactant is needed, the method has the disadvantages of high production cost, difficult removal of organic impurities, easy agglomeration, difficult industrialization and the like. In the economic principle, if the modification can be carried out by chemical modificationSolving a plurality of problems of the chemical method, has profound significance for the industrial production of spherical silicon micro powder and the rapid development of the electronic packaging industry in China.
At present, high-purity and ultra-pure spherical silica powder of plastic packaging materials for large-scale and ultra-large-scale basic circuits in China are imported from the countries such as the United states, Japan and the like, and although enterprises for producing the high-purity silica powder exist in China, the quality requirements of products of the high-purity silica powder still cannot meet the product quality requirements of the countries such as the United states, Japan and the like, the high-purity spherical silica powder is not fundamentally changed under the situation of people, and the high-purity spherical silica powder is always in danger of trade blockade of the countries such as the United states, Japan and the. Therefore, the advanced manufacturing process and equipment for developing high-purity and ultra-pure spherical silicon micropowder with high technical content completely having own intellectual property rights are developed, and the domestic and industrial production is carried out, so that the advanced manufacturing process and equipment are a powerful guarantee for greatly promoting and developing the high-tech electronic industry.
The Chinese patent literature is inquired, and no report about the industrial application of directly preparing the high-purity superfine silicon powder by using the high-purity liquid silicon ultrasonic atomization method and the use condition of an industrial device is found.
SUMMERY OF THE UTILITY MODEL
In order to solve the technical problem, the utility model provides an utilize high-purity liquid silicon ultrasonic atomization method to prepare device of high-purity superfine spherical silica miropowder, the device advanced process technology, design scientific and reasonable, the commonality is strong, can select the spherical silica miropowder of liquid silicon in order to produce different purity of different purity as required.
The utility model uses argon gas or helium gas or high-pressure water vapor as atomizing medium, and atomizes high-temperature liquid silicon by means of an ultrasonic atomizer to form fine spherical silicon particles; the amorphous silicon dioxide is prepared by utilizing the principle that high-temperature liquid silicon reacts with water to generate amorphous silicon dioxide. The method comprises the following specific steps: high-purity liquid silicon is atomized into a water cooling reaction device by using an ultrasonic atomizer by using high-pressure argon gas or helium gas or high-pressure steam as an atomizing medium (gas source), high-temperature liquid silicon particles with small particle size and high temperature are subjected to chemical reaction with the steam in the atomizing process to generate amorphous spherical silicon dioxide, and high-temperature liquid silicon which is not subjected to complete reactionThe particles are contacted with water and then rapidly undergo a chemical reaction to generate amorphous silicon dioxide and hydrogen; the chemical equation is as follows: si +2H2O＝SiO2+2H2(ii) a Then pressing the generated silicon dioxide slurry into a cake shape by a filter press, and then drying at high temperature to obtain the high-purity superfine amorphous spherical silicon dioxide.
The utility model provides a technical scheme as follows:
a production device for preparing spherical silicon micropowder by ultrasonic atomization comprises a speed-control feeder (1), an electric heating and heat-insulating device (2), an ultrasonic atomizer (3), a water cooling reaction device (4), a transfer tank (5), a plate-and-frame filter press (7), a beater (8), a spray dryer (10), a screening device (11) and a fan (12);
the electric heating and heat preserving device (2) comprises an electric heating crucible (21) and an electric heating pipe (22), which are sequentially connected from top to bottom;
the electric heating heat preservation device (2), the ultrasonic atomizer (3), the water cooling reaction device (4) and the transit trough (5) are sequentially connected from top to bottom; the transfer tank (5) is connected to a plate-and-frame filter press (7) through a diaphragm pump (6), and the plate-and-frame filter press (7) is connected to a beater (8); the beater (8) is connected to a feed inlet of an atomizing nozzle at the upper end of the spray dryer (10) through a feed pump (9), and the lower end of the spray dryer (10) is sequentially connected with a screening device (11) and a fan (12);
the water cooling reaction device (4) is formed by connecting a pure water reaction kettle (41) and a pure water tank (43) in parallel, and the two pure water tanks are connected through a communicating pipe (42); the pure water reaction kettle (41) is a jacket reaction kettle and is provided with a cooling water inlet and a cooling water outlet, the upper end of the pure water reaction kettle is connected to the ultrasonic atomizer (3), the lower end of the pure water reaction kettle is connected with the outlet at the lower end of the pure water tank (43) in parallel through a three-way pipeline, then the pure water reaction kettle and the pure water tank converge into a header pipe and then are connected; an electromagnetic control liquid level meter (46) is arranged on the side surface of the pure water tank, a pure water inlet (44) and an induced draft fan or a vacuum pump (45) are arranged at the upper end of the pure water tank, and the induced draft fan or the vacuum pump (45) is also connected to the pure water reaction kettle (41) through a pipeline;
the spray dryer (10) comprises a spray drying chamber (101), an electric heater (102), a blower (103) and an air filter (104), wherein the upper end of the spray drying chamber (101) is sequentially connected with the electric heater (102), the blower (103) and the air filter (104); an atomizing nozzle is arranged at the inlet of the top of the spray drying chamber (101);
the speed control hopper (1) is arranged above the electric heating and heat preservation device (2).
Specifically, the ultrasonic atomizer (3) comprises a cavity, a frequency modulation oscillator (32) and a nozzle are arranged in the cavity, and a high-pressure gas inlet (33) and a cooling water inlet and outlet are arranged on the side surface of the cavity; the high-pressure gas inlet (33) is connected to a frequency-modulated oscillator (32).
Specifically, the screening device is formed by sequentially connecting a secondary cyclone dust collector, a bag-type dust collector (113) and a fan (12).
The utility model has the advantages that:
(1) the high-purity or ultra-pure liquid silicon is utilized to be subjected to ultrasonic atomization, and the atomized particles are completely spherical and have small particle size;
(2) high-pressure argon or high-pressure helium or high-pressure steam is used as an atomizing medium, and the atomized high-temperature silicon micro-droplets react with water quickly and fully;
(3) the process is simple, the industrial production is easy, and the high-purity or ultra-pure spherical silicon dioxide micro powder can be obtained after cooling;
(4) high-temperature silicon particles with complete micro-reaction enter cooling medium water to react with water to generate amorphous silicon dioxide and hydrogen; on the other hand, water also acts as a coolant;
(5) the reaction is completed in two steps, so that the yield of the product can be greatly improved;
(6) provides a new idea for producing the silicon micropowder by ultrasonic atomization with high efficiency and simplicity, and has great industrial use value and application prospect.
Drawings
FIG. 1 is a structural view of a production apparatus of the present invention;
FIG. 2 is a partial block diagram of an electric heating device and an ultrasonic atomizer;
reference numerals: 1-speed-control blanking device, 2-electric heating heat-preserving device, 21-electric heating crucible, 22-electric heating tube, 3-ultrasonic atomizer, 31-cooling water outlet, 32-frequency-modulation oscillator, 33-oxygen inlet, 34-cooling water inlet, 4-water cooling reaction device, 41-pure water reaction kettle, 42-communicating pipe, 43-pure water tank, 44-pure water inlet, 45-induced draft fan or vacuum pump, 46-electromagnetic control liquid level meter, 5-transfer tank, 6-diaphragm pump, 7-plate-and-frame filter press, 8 beater, 9-feed pump, 10-spray drier, 101-spray drying chamber, 102-electric heater, 103-air blower, 104-air filter, 11-screening device, 111-primary cyclone dust collector, 112-secondary cyclone dust collector, 113-bag dust collector and 12-fan.
Detailed Description
The present invention will be further described with reference to specific embodiments, but the present invention is not limited thereto.
Example 1
Fig. 1 and fig. 2 show the structure of the production device of the present invention. The device comprises a speed-control blanking device 1, an electric heating and heat-preserving device 2, an ultrasonic atomizer 3, a water cooling reaction device 4, a plate-and-frame filter press 7, a pulping machine 8, a spray dryer 10, a screening device 11 and a fan 12;
the electric heating and heat preserving device 2 comprises an electric heating crucible 21 and an electric heating pipe 22 which are sequentially connected from top to bottom;
the electric heating heat preservation device 2, the ultrasonic atomizer 3, the water cooling reaction device 4 and the transfer tank 5 are sequentially connected from top to bottom; the transfer tank 5 is connected to a plate-and-frame filter press 7 through a diaphragm pump 6, and the plate-and-frame filter press 7 is connected to a beater 8; the beater 8 is connected to an inlet of an atomizing nozzle at the upper end of a spray dryer 10 through a feeding pump 9, and the lower end of the spray dryer 10 is sequentially connected with a screening device 11 and a fan 12;
the water cooling reaction device 4 is formed by connecting a pure water reaction kettle 41 and a pure water tank 43 in parallel, and the two are connected through a communicating pipe 42; the pure water reaction kettle 41 is a jacket reaction kettle and is provided with a cooling water inlet and a cooling water outlet, the upper end of the pure water reaction kettle is connected to the ultrasonic atomizer 3, the lower end of the pure water reaction kettle is connected with the outlet at the lower end of the pure water tank 43 in parallel through a three-way pipeline, and then the pure water reaction kettle is converged into a header pipe and then is connected to the; the side surface of the pure water tank 43 is provided with an electromagnetic control liquid level meter 46, the upper end of the pure water tank is provided with a pure water inlet 44 and an induced draft fan or a vacuum pump 45, and the induced draft fan or the vacuum pump 45 is also connected to the pure water reaction kettle 41 through a pipeline;
the spray dryer 10 includes a spray drying chamber 101, an electric heater 102, an air blower 103, and an air filter 104, and the upper end of the spray drying chamber 101 is connected to the electric heater 102, the air blower 103, and the air filter 104 in sequence; an atomizing nozzle is arranged at the inlet of the top of the spray drying chamber 101;
the speed-control blanking device 1 is arranged above the electric heating and heat-preserving device 2.
The ultrasonic atomizer 3 comprises a cavity, a frequency modulation oscillator and a nozzle are arranged in the cavity, and an oxygen inlet 33 and a cooling water inlet and outlet are arranged on the side surface of the cavity; the oxygen inlet 33 is connected to a frequency modulated oscillator 32.
The screening device is formed by sequentially connecting a secondary cyclone dust collector, a bag-type dust collector 113 and a draught fan 12.
The utility model discloses and the theory of operation of device thereof:
adding the molten high-purity silicon liquid into a crucible with electric heating and heat preservation, and electrically heating to ensure that the temperature is preserved between 1450 and 1550 ℃; then, high-pressure helium gas or argon gas or high-pressure steam with the pressure of 8.3-8.4Mpa is introduced from the high-pressure gas inlet 33. Starting the ultrasonic atomizer, and controlling the pulse frequency of an adjusting resonant cavity of the ultrasonic atomizer to be between 80 and 160 KHz; starting the speed-control blanking device to enable the silicon liquid to slowly flow down in an electric heating pipe with the inner diameter of 3-8mm, atomizing the silicon liquid into a pure water reaction kettle filled with electronic grade pure water through an ultrasonic atomizer under the condition, and starting jacket cooling water to cool the reaction kettle. When the atomizing gas is argon or helium, droplets of high-temperature high-purity silicon liquid drop into pure water in the atomizing process and then immediately react with the pure water to generate amorphous spherical silicon dioxide and hydrogen, the hydrogen is immediately pumped out of the reaction kettle by an induced draft fan or a vacuum pump, and the chemical reaction formulas are as follows: si +2H2O＝SiO2+H2×) ×; when the atomizing gas is high-pressure water vapor, high-temperature high-purity silicon liquid droplets in the atomizing process immediately react with the water vapor to generate amorphous spherical silicon dioxide and hydrogen when contacting with the water vapor, and the hydrogen is immediately pumped out by a draught fan; the high-temperature silicon droplets which are not completely reacted fall into pure water to perform chemical reaction with the pure water to generate amorphous spherical silicon dioxide and hydrogen, and the hydrogen is immediately pumped by a draught fan or a vacuum pumpAnd (6) discharging. And (3) slowly sinking the silicon dioxide particles generated in the reaction process to the bottom of the pure water reaction kettle, opening a discharge valve at the bottom of the pure water reaction kettle to enable the slurry to flow into a transfer tank, then sending the silicon dioxide slurry in the transfer tank into a plate-and-frame filter press by using a diaphragm pump to press the silicon dioxide slurry into a filter cake, then pulping and using spray drying or washing the filter cake by using absolute ethyl alcohol and then using vacuum drying to obtain the high-purity superfine spherical silicon micro powder product. When the reaction kettle begins to discharge materials, the liquid level will drop, and pure water is controlled to automatically flow into the pure water reaction kettle through the electromagnetic control liquid level meter on the outer side of the pure water tank until the liquid levels are equal to each other.
The method for preparing the spherical silicon micropowder by using the device comprises the following steps:
(1) adding the liquid silicon melted at high temperature into a crucible, and maintaining the temperature of the silicon liquid at 1450 and 1550 ℃ in an electric heating mode;
(2) atomizing liquid silicon into a reaction kettle by using an ultrasonic gas atomizer under the conditions of frequency of 80-160kHz and gas atomization pressure of 8.3-8.7Mpa in an atomizing medium atmosphere to react with pure water to generate an amorphous spherical silicon dioxide material, and cooling the material by using the pure water;
(3) supplementing water to the silicon dioxide slurry material generated in the reaction kettle; and (4) carrying out filter pressing on the cooled slurry, and washing and drying to obtain the spherical silicon dioxide powder.
Preferably, the liquid silicon in the step (1) is high-purity liquid silicon, and the purity is more than 4N.
Preferably, the atomizing medium in the step (2) is argon, helium or high-pressure steam.
Preferably, the concentration of the silicon dioxide slurry material after water supplement in the step (3) is 10-30%.
Preferably, the pressure filtration device in the step (3) is a pressure filter.
Preferably, the solvent washed in the step (3) is absolute ethyl alcohol.
Preferably, the drying device in the step (3) is a high-temperature vacuum dryer or a high-temperature vacuum microwave drying device.
Application example 1
Taking high-temperature silicon liquid with 99.99 percent silicon melted at high temperature as an example to prepare the silicon micro powder
1, pouring the liquid silicon with the purity of 99.99 percent and high temperature into a preheating electric heating and heat-preserving device 2, and keeping the temperature between 1450 and 1550 ℃;
2 opening a valve of a high-pressure gas inlet 33 and introducing high-pressure argon of 8.3-8.4 Mpa; opening ultrasonic nebulizer and accuse speed glassware 1 down makes silicon liquid slowly flow down in the intraductal of internal diameter 3-5mm, the pulse frequency control of ultrasonic nebulizer's regulation resonant cavity is at 80-100KHz, pass through ultrasonic nebulizer atomizing to pure water reation kettle 4 in this condition silicon liquid, it cools off to let in the cooling water for the reation kettle jacket, open draught fan 45, the high-purity silicon liquid droplet of high temperature falls into in the atomizing process and reacts with the pure water immediately and generate amorphous spherical silica and hydrogen, its chemical reaction formula is respectively: si +2H2O＝SiO2+2H2×) ×; in the process, water is used as a reactant to participate in the reaction process, and the other water plays a role in cooling and solvent; the hydrogen gas generated in the reaction process is rapidly pumped out from the pure water reaction kettle 41 and the pure water tank 43 by the induced draft fan or the vacuum pump 45.
And 3, opening a discharge valve at the bottom of the water tank to enable the generated silica slurry to flow into the transfer tank 5 for storage, and simultaneously adding pure water into the pure water tank 43 to maintain that the pure water in the tank is not less than 3/5 of the volume in the tank. And (3) conveying the silicon dioxide slurry in the transit tank into a filter press by using a diaphragm pump 6 to press the silicon dioxide slurry into a filter cake, then pulping, and drying by using a sprayer, wherein the dried powder is an amorphous spherical silicon dioxide product. The sphericity is 100%; average particle size 25 um; SiO 22The purity is more than or equal to 99.99 percent.
Application example 2
Taking high-temperature silicon liquid with 99.995 percent silicon melted at high temperature as an example to prepare the silicon micro powder
1, pouring the liquid silicon with the purity of 99.999 percent into a preheating electric heating heat preservation device 2 to keep the temperature between 1450 and 1550 ℃;
2 opening a valve of the high-pressure gas inlet 33 and introducing high-pressure helium gas of 8.3-8.4 Mpa; starting the ultrasonic atomizer and the speed control material device 1 to ensure that the silicon liquid slowly flows down in a pipe with the inner diameter of about 3-5mm and exceedsThe pulse frequency of the adjusting resonant cavity of the sound wave atomizer is controlled to be 100-plus 120KHz, silicon liquid is atomized into a pure water reaction kettle 4 through the ultrasonic atomizer under the condition, cooling water is introduced into a jacket of the reaction kettle for cooling, a draught fan or a vacuum pump 45 is started, high-temperature high-purity silicon liquid droplets fall into the pure water in the atomization process and immediately react with the pure water to generate amorphous spherical silicon dioxide and hydrogen, and the chemical reaction formulas are respectively as follows: si +2H2O＝SiO2+2H2×) ×; in the process, water is used as a reactant to participate in the reaction process, and the other water plays a role in cooling and solvent; the hydrogen gas generated in the reaction process is rapidly pumped out from the pure water reaction kettle 41 and the pure water tank 43 by the induced draft fan or the vacuum pump 45.
And 3, opening a discharge valve at the bottom of the water tank to enable the generated silica slurry to flow into the transfer tank 5 for storage, and simultaneously adding pure water into the pure water tank to maintain that the pure water in the tank is not less than 3/5 of the volume in the tank. The silicon dioxide slurry in the transit tank is sent into a filter press by a diaphragm pump 6 to be pressed into a filter cake, then the filter cake is pulped by pure water and dried by a spray dryer, and the dried powder is an amorphous spherical silicon dioxide product. The sphericity is 100%; an average particle diameter of 22 um; SiO 22The purity is more than or equal to 99.995 percent.
Application example 3
Taking high-temperature silicon liquid with 99.999 percent of silicon melted at high temperature as an example to prepare the silicon micro powder
1, pouring the liquid silicon with the purity of 99.999 percent into a preheating electric heating heat preservation device 2 to keep the temperature between 1450 and 1550 ℃;
2 opening a valve of a high-pressure gas inlet 33 and introducing high-pressure steam of 8.5-8.6 Mpa; starting an ultrasonic atomizer and a speed control material device 1 to enable silicon liquid to slowly flow down in a pipe with the inner diameter of about 3-5mm, controlling the pulse frequency of an adjusting resonant cavity of the ultrasonic atomizer to be 120-140KHz, atomizing the silicon liquid into a pure water reaction kettle 4 through the ultrasonic atomizer under the condition, introducing cooling water into a jacket of the reaction kettle 4 to cool, starting a draught fan or a vacuum pump 45, and immediately reacting high-temperature high-purity silicon liquid droplets with high-pressure steam in the atomization process to generate amorphous spherical silicon dioxide; unreacted or not completely reactedThe high-temperature silicon liquid drops into pure water to react with water to generate amorphous spherical silicon dioxide and hydrogen, and the chemical reaction formulas are as follows: si +2H2O＝SiO2+H2×) ×; in the process, water is used as a reactant to participate in the reaction process, and the other water plays roles of cooling and a solvent. The hydrogen gas generated in the reaction process is rapidly pumped out from the pure water reaction kettle 41 and the pure water tank 43 by the induced draft fan or the vacuum pump 45.
And 3, opening a discharge valve at the bottom of the water tank to enable the generated silicon dioxide slurry to flow into the transfer tank 5 for storage, and simultaneously adding pure water into the pure water tank to keep the pure water in the tank not lower than 3/5 of volume. The silicon dioxide slurry in the transit tank is sent to a filter press by a diaphragm pump 6 to be pressed into filter cakes, and the pure water is returned for use. And pulping the filter cake by using pure water, and drying by using a spray dryer, wherein the dried powder is a spherical silicon dioxide product. Sphericity is 100% average; the grain diameter is 20 um; SiO 22The purity is more than or equal to 99.999 percent.
Application example 4
Taking 99.9999% high-temperature high-purity silicon liquid as an example to prepare spherical silicon micropowder
1, pouring the liquid silicon with the purity of 99.9999 percent and the high temperature into a preheating electric heating heat preservation device 2, and keeping the temperature between 1450 and 1550 ℃;
2 opening a valve of a high-pressure gas inlet 33 and introducing high-pressure steam of 8.6-8.7 Mpa; starting an ultrasonic atomizer and a speed control material device 1 to enable silicon liquid to slowly flow down in a pipe with the inner diameter of 5-8mm, adjusting the pulse frequency of a resonant cavity to be 140-160KHz, atomizing the silicon liquid into a pure water reaction kettle 4 through the atomizer under the condition, introducing cooling water into a jacket of the reaction kettle 4 for cooling, starting an induced draft fan or a vacuum pump 45, immediately carrying out oxidation reaction on high-temperature high-purity silicon liquid droplets and water vapor to generate amorphous spherical silicon dioxide and hydrogen, and reacting the unreacted or incompletely reacted high-temperature silicon droplets with the pure water to generate amorphous spherical silicon dioxide and hydrogen; the chemical reaction formula is as follows: si +2H2O＝SiO2+H2×) ×; in the process, water is used as a reactant to participate in the reaction process, and the other water plays roles of cooling and a solvent. Hydrogen produced in the reaction process is rapidly induced by an induced draft fan or a vacuumThe air pump 45 pumps the water from the pure water reaction vessel 41 and the pure water tank 43.
And 3, opening a discharge valve at the bottom of the water tank to enable the generated silica slurry to flow into the transfer tank 5 for storage, and simultaneously adding pure water into the pure water tank to maintain that the pure water in the tank is not less than 3/5 of the volume in the tank. And (3) conveying the silicon dioxide slurry in the transfer tank into a filter press by using a diaphragm pump 6 to press the silicon dioxide slurry into a filter cake, washing the filter cake for three times by using absolute ethyl alcohol, and then conveying the filter cake into a high-temperature vacuum drier to dry, wherein the dried powder is an amorphous spherical silicon dioxide product. The sphericity is 100%; the average particle size is 15 um; SiO 22The purity is more than or equal to 99.9999 percent.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, a plurality of modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (3)
1. The utility model provides a production device of spherical silica micropowder of ultrasonic atomization preparation which characterized in that:
comprises a speed-control feeder (1), an electric heating and heat-preserving device (2), an ultrasonic atomizer (3), a water cooling reaction device (4), a transfer tank (5), a diaphragm pump (6), a plate-and-frame filter press (7), a beater (8), a spray dryer (10), a screening device (11) and a fan (12);
the electric heating and heat preserving device (2) comprises an electric heating crucible (21) and an electric heating pipe (22), which are sequentially connected from top to bottom;
the electric heating heat preservation device (2), the ultrasonic atomizer (3), the water cooling reaction device (4) and the transit trough (5) are sequentially connected from top to bottom; the transfer tank (5) is connected to a plate-and-frame filter press (7) through a diaphragm pump (6), and the plate-and-frame filter press (7) is connected to a beater (8); the beater (8) is connected to a feed inlet of an atomizing nozzle at the upper end of the spray dryer (10) through a feed pump (9), and the lower end of the spray dryer (10) is sequentially connected with a screening device (11) and a fan (12);
the water cooling reaction device (4) is formed by connecting a pure water reaction kettle (41) and a pure water tank (43) in parallel, and the two pure water tanks are connected through a communicating pipe (42); the pure water reaction kettle (41) is a jacket reaction kettle and is provided with a cooling water inlet and a cooling water outlet, the upper end of the pure water reaction kettle is connected to the ultrasonic atomizer (3), the lower end of the pure water reaction kettle is connected with the outlet at the lower end of the pure water tank (43) in parallel through a three-way pipeline, then the pure water reaction kettle and the pure water tank converge into a header pipe and then are connected; an electromagnetic control liquid level meter (46) is arranged on the side surface of the pure water tank (43), a pure water inlet (44) and an induced draft fan or a vacuum pump (45) are arranged at the upper end of the pure water tank, and the induced draft fan or the vacuum pump (45) is further connected to the upper end of the pure water reaction kettle (41) through a pipeline;
the spray dryer (10) comprises a spray drying chamber (101), an electric heater (102), a blower (103) and an air filter (104), wherein the upper end of the spray drying chamber (101) is sequentially connected with the electric heater (102), the blower (103) and the air filter (104); an atomizing nozzle is arranged at the inlet of the top of the spray drying chamber (101);
the speed-control blanking device (1) is arranged above the electric heating and heat-preserving device (2).
2. The production device for preparing spherical silicon micropowder by ultrasonic atomization according to claim 1, characterized in that: the ultrasonic atomizer (3) comprises a cavity, a frequency modulation oscillator (32) and a nozzle are arranged in the cavity, and an oxygen inlet (33) and a cooling water inlet and outlet are arranged on the side surface of the cavity; the oxygen inlet (33) is connected to a frequency modulated oscillator (32).
3. The production device for preparing spherical silicon micropowder by ultrasonic atomization according to claim 1, characterized in that: the screening device is formed by sequentially connecting a secondary cyclone dust collector, a bag-type dust collector (113) and a fan (12).
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110395739A (en) * | 2019-07-24 | 2019-11-01 | 黄冈师范学院 | A kind of ultrasonic atomization prepares the production method and device of ball-shaped silicon micro powder |
| CN114180579A (en) * | 2021-11-11 | 2022-03-15 | 苏州锦艺新材料科技有限公司 | Grading and purifying device for spherical silicon micro powder |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110395739A (en) * | 2019-07-24 | 2019-11-01 | 黄冈师范学院 | A kind of ultrasonic atomization prepares the production method and device of ball-shaped silicon micro powder |
| CN114180579A (en) * | 2021-11-11 | 2022-03-15 | 苏州锦艺新材料科技有限公司 | Grading and purifying device for spherical silicon micro powder |
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