CN110371989A - A kind of ultrasonic atomization prepares the production method of ball-shaped silicon micro powder - Google Patents
A kind of ultrasonic atomization prepares the production method of ball-shaped silicon micro powder Download PDFInfo
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- CN110371989A CN110371989A CN201910574714.6A CN201910574714A CN110371989A CN 110371989 A CN110371989 A CN 110371989A CN 201910574714 A CN201910574714 A CN 201910574714A CN 110371989 A CN110371989 A CN 110371989A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C01B33/181—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses the production methods that a kind of ultrasonic atomization prepares ball-shaped silicon micro powder, comprising the following steps: (1) liquid-state silicon is heated and kept the temperature, temperature maintains 1450-1550 DEG C；It (2) is being that liquid-state silicon is atomized under conditions of gas atomization pressure is 8.3-8.7Mpa to generate amorphous state preparing spherical SiO 2 material by 80-160kHZ in frequency using ultrasonic ultrasonic delay line memory under the atmosphere of the atomizing medium of high purity oxygen gas；(3) the silica material material of generation is cooled down to get preparing spherical SiO 2 powder.The present invention also provides the devices using above method production ball-shaped silicon micro powder.Prepared by the method ball-shaped silicon micro powder is high-purity or ultra-pure silicon powder, and simple process is easy to industrialization, has biggish application value and prospect.
Description
Technical field
The present invention relates to the production methods that a kind of ultrasonic atomization prepares ball-shaped silicon micro powder, belong to nonmetallic ore deep processing skill
Art field.
Background technique
In recent years, with the fast development of microelectric technique, people are higher and higher to the quality requirement of microelectronic element, make
It is also higher and higher to obtain silicon powder quality requirement.The 97% of global integrated circuit (IC) encapsulating material uses epoxy-plastic packaging material (EMC),
And in the composition of EMC, in addition to major ingredient novolac epoxy resin, silicon powder is the most filler of dosage.Silicon powder filler accounts for epoxy
Moulding compound weight ratio reaches 70%-90%.So in order to high quality plastic packaging material in addition to requiring ultra-fine silicon powder, high-purity, low putting
Outside penetrating property element, its spheroidizing of particles is also specially required.This is because: the surface mobility of (1) ball is good, form a film with resin agitating
Uniformly, so that the additive amount of resin is small, the loading of silicon powder reaches highest, therefore spheroidization means silicon powder filling rate
Increase, and the filling rate of silicon powder is higher, for the coefficient of expansion with regard to smaller, thermal coefficient is also lower, also just closer to monocrystalline silicon
The service performance of thermal expansion coefficient, resulting electronic component is also better；(2) with plastic packaging material phase made of angular silicon powder
Than, spherical plastic packaging material profit concentrates minimum, intensity highest, when it is 1 that the plastic packaging material stress of angular powder, which is concentrated, the stress of spherical powder
Only 0.6, thus manufactured microelectronic component high yield rate, is readily transported, installs, and be not likely to produce machine in use
Tool damage；(3) compared to angular silicon powder, spherical powder coefficient of friction is small, small to the abrasion of mold, so that the service life of mold
It can be improved one times.(Ruan Jianjun " progress of ball-shaped silicon micro powder " He Lijun, Jiang Shuxing " ball-shaped silicon micro powder ")
Currently, high quality ball-shaped silicon micro powder part required for China also relies on import, high-purity, ultra-fine ball how is prepared
Shape silicon powder is still domestic powder research hotspot.The preparation method of ball-shaped silicon micro powder mainly includes physical method and chemistry at this stage
Method.
1, physical method
1.1, flame spherical container shaping method: flame spherical container shaping method such as is crushed to quartz first, sieves, purifies at the pre-treatments, then will
Quartz micropowder is sent into the high-temperature field that gas-oxygen generates, and is carried out high-temperature fusion, cooling balling-up, is ultimately formed high-purity spherical shape
Silicon powder.
Clean pollution-free fire of the industrial fuels such as acetylene gas, hydrogen, natural gas gas as melting powder specifically can be used
Flame is heat source, and such method is related to the theory of thermodynamics, hydrodynamics, granule fluid mechanics etc..With plasma high-temperature
Flame is compared, and is not involved in the problems, such as that electromagnetic theory and ion are flowed and moved in electromagnetic field, produces easy to control, Yi Shixian work
Industryization large-scale production, is a kind of production technology with development prospect.
The disadvantages of this method is: industrial combustion gas -- acetylene gas and natural gas can also give product quality during burning
Bring certain pollution.Danger coefficient is big in use for hydrogen.It is industrially extensive, mature to yet there are no this method
Application report.
1.2, high-temperature fusion gunite: high-temperature fusion gunite is to melt high-purity quartz at 2100-2500 DEG C to be
Liquid obtains ball-shaped silicon micro powder by spraying, cooling.Product surface is smooth, and spherical rate and amorphous form quotient can reach
100%.According to investigation, the ball-shaped silicon micro powder in the U.S. mainly uses this method to produce, due to being related to high-performance computer technology, he
Externally bottle up.High-temperature fusion gunite easily guarantees Oxygen potential and amorphous rate, but is not easy to solve purity and atomizing particle size
The problems such as adjustment.The country is there is not yet this respect is studied and the report of production at present.
1.3, self- propagating low-temperature combustion method: the process flow of self- propagating low-temperature combustion method includes the preparation of sodium metasilicate, silicic acid
The preparation of colloidal sol, the preparation for being mixed and burned liquid, combustion reaction, annealing are except carbon, carrying out washing treatment.
The technical method has the advantage that as follows:
(1) it can also be extended to using melting silicon powder as raw material using natural powdery quartz as raw material；(2) simple process,
Easy to operate without especial equipment requirements, easily controllable, production cost is low；(3) material used in production process only includes easily
It is dissolved in the sodium ion and nitrate ion of water, other impurities ion will not be introduced, is conducive to the preparation of high purity silica powder.
Disadvantage is: this method is merely resting on laboratory stage at present, can't be mass produced well.
1.4, plasma method: the basic principle of plasma method is to utilize the high-temperature region of plasma square by silica
(SiO2) powder fusing, since the effect of surface tension of liquid forms spherical droplets, spheroidization is formed during rapid cooling
Particle.This method energy is high, heat transfer is fast, cooling block, prepared product morphology controllable, purity is high, soilless sticking.
The disadvantages of this method: this method is merely resting on laboratory stage at present, can't be mass produced well.
1.5, high-temperature calcination spheroidization: high-temperature calcination spheroidization is generally used for preparing high-purity ultra-fine sphere silicon micro-powder, mainly
It is that the processing that miberal powder is passed through the techniques such as calcining, ball milling, magnetic separation and selection by winnowing prepares high-purity ultra-fine sphere SILICA FUME.
The advantages of this method: not only Oxygen potential is high, whiteness is good, silicon content is high, iron content aluminium is few for high-purity ultra-fine sphere silicon micro-powder,
PH value is in neutrality slant acidity, flowing good dispersion, and expansion and thermal coefficient are small, and conductivity is low, and corrosion-resistant, production cost is low.
The disadvantages of this method: the technology is at present also in the experimental stage.
2, chemical method
2.1, vapor phase method: vapor phase method SiO2(being commonly called as fume colloidal silica) is to be hydrolyzed to be made at high temperature by the halide of silicon
Fine, the special amorphous powder body material of one kind.In the water that oxyhydrogen combustion flame generates high-temperature water occurs for silane halide
Solution reaction, temperature are generally up to 1200-1600 DEG C, are then quenched, using aggregation, cyclonic separation, air injection depickling, boiling
The post-processings such as bed screening, vacuum compression packaging obtain the SiO that finished product vapor phase method generates2Product purity is high, and Average primary partial size is
7-40nm, specific surface area 50-380m2/ g, SiO2Mass fraction is not less than 99.8%.The disadvantages of this method is in organic matter
It is difficult to disperse and pollutes environment.
2.2, hydrothermal synthesis method: hydrothermal synthesis method is a kind of common method that liquid phase prepares nanoparticle, generally in 100-
At 350 DEG C of temperature and hyperbaric environment, make inorganic and organic compound and hydrate, by acceleration dialysis reaction and physical process
Control, obtain improved inorganic matter, using filter, washing, drying, obtain high-purity, ultra-fine particulate.The advantages of hydro-thermal method
It is that can directly generate oxide, the step for general liquid phase synthesizing method need to be converted to oxide by calcination is avoided, to drop
The low formation probability of hard aggregation.
The shortcomings that method, is also apparent from: being limited to the size of reaction kettle, hydro-thermal method prepares SiO at present2Also it is in laboratory
Stage.
2.3, sol-gel method: sol-gel method be metal organic or inorganic compound by solution, colloidal sol, gel and
Solidification, then the method for thermally treated and formation oxide or other compound solids.The advantages of this method be chemical uniformity it is good,
Particle is thin, with high purity, equipment is simple, and powder active is high.Disadvantage is: raw material are more expensive, and particle asks that agglutinating property is poor, receive when dry
Contracting is big, agglomeration traits easily occurs.
2.4, the precipitation method: surfactant, control reaction temperature is added using waterglass and acidulant as raw material in the precipitation method in due course
Degree adds stabilizer when precipitation solution pH value is 8, and gained precipitating is washed, dry, forms silicon powder after calcining.The precipitation method are raw
At SiO2Uniform particle sizes and at low cost, technique is easy to control, is conducive to industrialized production, but there are certain agglomerations.
2.5, microemulsion method: microemulsion method is formed under the action of surfactant using two kinds of immiscible solvents
Uniform lotion is confined to the processes such as nucleation, production, coalescence, reunion in one small spherical droplets, is precipitated from lotion
Solid phase forms spheric granules, avoids and further reunites between particle.SiO is prepared using microemulsion method2Mostly with ethyl orthosilicate
It for silicon source, is spread by ethyl orthosilicate molecule, is permeated through reverse micelle interfacial film into water core, it is anti-that hydrolytic condensation then occurs
It answers, SiO is made2.The preparation of this method Granularity Distribution is narrow, size tunable, good dispersion.The shortcomings that method: this method at present
It is merely resting on laboratory stage, can't be mass produced well.
3, spray-on process: spray-on process is that solution is carried out a kind of chemistry that atomization obtains ultramicron by various physical means
The method combined with physics.Its basic process is the preparation, spraying, dry, collection and heat treatment of solution.The method feature
It is that distribution of particles is relatively uniform, but particle size is sub-micron to 10 μm, is a kind of synthesis size tunable nanoparticle oxide
New method.The shortcomings that method: energy consumption is high, and the micro mist after drying is reunited seriously, and use is very inconvenient.
By the way that the above-mentioned comparison for preparing the various methods of silicon powder, we can substantially be obtained: the spherical shape of physical method preparation
Raw material needed for silicon powder are relatively inexpensive, but more demanding to raw material quartz quality and production equipment etc..Its Flame at
Ball is currently a kind of achievable large-scale production and promising technology, but its there are purity and atomizing particle size
The problem of adjustment.
Chemical method can prepare high-purity and uniform particle sizes spherical SiOs2, but since a large amount of surfactant need to be used, because
This is not easy cleared, easy reunion there are high production cost, organic impurities and is difficult to the disadvantages of industrializing.In line with economic principle,
If the problems of chemical method can be solved by the method for chemical modification, the production of China's ball-shaped silicon micro powder will be industrialized
And the fast development of Electronic Packaging industry has profound significance.
High-purity and ultrapure ball-shaped silicon micro powder of the capsulation material of the extensive and ultra-large tandem circuit in China at present
From the U.S., Japan and other countries import, although the domestic enterprise for also having production high purity silica powder, the quality requirement of its product is also
It is the product quality requirement for being difficult to reach the U.S. and Japan and other countries, situation under one's control obtains changing for essence not yet
Become, can be blocked by the trade of the U.S. and Japan and other countries at the moment dangerous.Possess intellectual property self completely for this purpose, developing
The Advanced Manufacturing Technology and equipment of high-purity and ultrapure ball-shaped silicon micro powder of high technology content, and domesticized, industrialized production,
It is the powerful guarantee for making greater efforts to promote and developing high-tech electronic industry.
Chinese patent literature is inquired, does not find that high purity liquid state silicon ultrasonic atomization method is directly utilized to prepare high pure and ultra-fine silicon
The industrial application of micro mist and the report of industrialized unit service condition.
Summary of the invention
In order to solve the above technical problem, the present invention provides it is a kind of using high purity liquid state silicon ultrasonic atomization method prepare it is high-purity
Ultra-fine sphere silicon micro-powder, this method and above-mentioned introduced process have significant difference, and technology is advanced, device is set
Count scientific and reasonable, versatile, the spherical silicon that can select the liquid-state silicon of different purity as needed to produce different purity is micro-
Powder.
The present invention is atomizing medium using high purity oxygen gas, is atomized high-temperature liquid state silicon by ultrasonic ultrasonic delay line memory, forms it into
Tiny spherical silicon particle.The principle that generation amorphous silicon di-oxide is reacted with oxygen using high-temperature liquid state silicon prepares amorphous state
Silica.It is specific as follows: using high pressure oxygen as atomizing medium (gas source), by high purity liquid state silicon using ultrasonic ultrasonic delay line memory into
Row atomization, the high-temperature liquid state silicon particle and oxygen that partial size is tiny in atomization process, temperature is high occur chemical reaction and generate amorphous
The preparing spherical SiO 2 of state, chemical equation are: Si+O2=SiO2；Then it after cooling storehouse is cooling, can be obtained high-purity super
Thin amorphous preparing spherical SiO 2.
Technical solution provided by the invention is as follows:
A kind of ultrasonic atomization prepares the production method of ball-shaped silicon micro powder, and the technical scheme comprises the following steps:
(1) liquid-state silicon is heated and is kept the temperature, temperature maintains 1450-1550 DEG C；
(2) it is atomizing medium in high purity oxygen gas, is being 80-160kHZ, gas atomization in frequency using ultrasonic ultrasonic delay line memory
Under conditions of pressure is 8.3-8.7Mpa, liquid-state silicon is atomized to generate amorphous state preparing spherical SiO 2 material；Chemical equation
It is: Si+O2=SiO2；
(3) method according to claim 1, it is characterised in that: atomizing medium is high purity oxygen gas in the step (2).
Specifically, liquid-state silicon is high purity liquid state silicon in the step (1), purity is >=4N.
Specifically, atomizing medium is high purity oxygen gas purity >=4N in the step (2).
Another object of the present invention is to provide the process units that ball-shaped silicon micro powder is prepared using the above method, including rate controlling
Hopper, electric heater unit, ultrasonic ultrasonic delay line memory, reaction kettle, condenser pipe, feed bin and screening plant；
The electric heater unit includes electric heating crucible and electric heating tube, and the two is sequentially connected from top to bottom；
The electric heater unit, ultrasonic ultrasonic delay line memory, reaction kettle, water conservancy diversion coldplate, condenser pipe and feed bin from top to bottom according to
Secondary connection, feed bin upside are connected to screening plant；
Rate controlling hopper is set to above electric heater unit.
Specifically, the ultrasonic ultrasonic delay line memory includes chamber, frequency-modulated generator and nozzle, the side of chamber are provided in chamber
Face is provided with oxygen inlet and cooling water intake-outlet；Oxygen air inlet is connected to frequency-modulated generator.
Specifically, being provided with guide coldplate in the condenser pipe.
It is formed specifically, the screening plant is sequentially connected by a second cyclone dust extractor, bag filter and blower.
Beneficial effects of the present invention:
(1) ultrasonic atomizatio is used using high-purity or ultrapure liquid-state silicon, the particulate matter of atomization is entirely that spherical and partial size is small；
It (2) is atomizing medium using high purity oxygen gas, the high temperature silicon miostagmin reaction speed after atomization is fast and reaction is abundant；
(3) fairly simple in technique, it is easy to industrialized production, high-purity or ultrapure preparing spherical SiO 2 can be obtained after cooling
Micro mist；
It (4) is atomizing medium using high purity oxygen gas, the high temperature silicon miostagmin reaction speed after atomization is fast, with high purity；
(5) a kind of new approaches of efficient, simple ultrasonic atomization production silicon powder are provided, there is biggish industrialization
Use value and application prospect.
Detailed description of the invention
Fig. 1 is the structure chart of process units of the present invention；
Fig. 2 is the part-structure figure of electric heater unit and ultrasonic ultrasonic delay line memory；
Appended drawing reference: 1- rate controlling hopper, 2- electric heater unit, 21- electric heating crucible, 22- electric heating tube, 3- ultrasonic fog
Change device, 31- cooling water outlet, 32- frequency-modulated generator, 33- high purity oxygen gas air inlet, 34- cooling water inlet, 4- reaction kettle, 41-
Cooling water outlet, 42- cooling water inlet, 5- water conservancy diversion coldplate, 6- condenser pipe, 61- cooling water outlet, 62- cooling water inlet, 7-
Feed bin, 8-4 one cyclonic deduster, 9- second cyclone dust extractor, 10- bag filter, 11- blower.
Specific embodiment
The present invention is further described combined with specific embodiments below, and the contents of the present invention are completely without being limited thereto.
Fig. 1, Fig. 2 shows the structure charts of process units of the present invention.The present apparatus include rate controlling hopper 1, electric heater unit 2,
Ultrasonic ultrasonic delay line memory 3, reaction kettle 4, condenser pipe 6, feed bin 7 and screening plant；
The electric heater unit includes electric heating crucible 21 and electric heating tube 22, and the two is sequentially connected from top to bottom；
The ultrasonic ultrasonic delay line memory 3 includes chamber, is provided with frequency-modulated generator 32 and nozzle in chamber, the side of chamber is set
It is equipped with high purity oxygen gas import 33, cooling water outlet and inlet；High purity oxygen gas air inlet 33 is connected to frequency-modulated generator 32.
Rate controlling hopper 1 is set to 2 top of electric heater unit.Control the rate controlling that hopper 1 realizes raw material by the folding of valve.
Water conservancy diversion coldplate 5 is provided in condenser pipe, water conservancy diversion coldplate 5 is designed using ramp type, flowed downward convenient for material
And the cooling in flow process.
Screening plant is sequentially connected by a second cyclone dust extractor, bag filter and blower and is formed.
The present invention and its working principle of device are: cooling water and air-introduced machine are first opened, by air-introduced machine taking out in device
High pressure, high purity oxygen is sent into atomizer at negative pressure, then slowly, then open ultrasonic wave and adjusts the vibration in vibration cavity
Dynamic frequency is in 80-160KHz range and runs 5 minutes, and the air in device is emptied by high pressure oxygen.Later, crucible is opened
On discharging control switch, flow down the silicon liquid of molten in traditional thread binding, when high temperature silicon liquid stream arrives ultrasonic atomizing nozzle, just stand
It is 10-15um or so or thinner spherical droplet at partial size by high voltagehigh frequency oxygen atomization；The silicon droplet of high temperature at the same time
Chemical reaction occurs after contacting with high purity oxygen gas immediately and generates amorphous state, the preparing spherical SiO 2 particle without inclusion enclave, without hydroxyl.
The preparing spherical SiO 2 particle generated under the draft effect of air-introduced machine falls into the bottom coohng of cooling reactor.Then, it then flows into cold
But it the water conservancy diversion coldplate in pipe and slides downwards, is finally cooled to room temperature on the cooling plate and enters feed bin.
Embodiment 1
Silicon powder is prepared by taking the high temperature silicon liquid of 99.99% silicon high temperature melting as an example
1. purity be 99.99% high temperature liquid-state silicon pour into cool-bag, make temperature maintain 1450-1550 DEG C it
Between；
2. first open cooling water and air-introduced machine, by air-introduced machine being pumped into negative pressure in device, then slowly high pressure, high purity
Oxygen is sent into atomizer, is then opened ultrasonic wave and is adjusted the vibration frequency in vibration cavity in 80-100KHz range and transport
Row 5 minutes, the air in device is lost no time by high pressure oxygen.Later, the discharging control switch on crucible is opened, molten is made
Silicon liquid flow down in traditional thread binding, when high temperature silicon liquid stream is to ultrasonic atomizing nozzle, just immediately by high voltagehigh frequency oxygen atomization granulating
Diameter is 10-15um or so or thinner spherical droplet；The silicon droplet of high temperature occurs immediately after contacting with high purity oxygen gas at the same time
Chemical reaction generates amorphous preparing spherical SiO 2 particle.Its chemical equation is respectively as follows: Si+O2=SiO2
3. the bottom coohng that the preparing spherical SiO 2 particle generated under the draft effect of air-introduced machine falls into cooling reactor.So
Afterwards, it then the water conservancy diversion coldplate that flows into cooling tube and slides downwards, is finally cooled to room temperature on the cooling plate and enters feed bin.I.e.
Preparing spherical SiO 2 product can be obtained.Sphericity is 100% average；Partial size 30um；SiO2Purity >=99.99%.
Embodiment 2
Silicon powder is prepared by taking the high temperature silicon liquid of 99.995% silicon high temperature melting as an example
1. purity is that the liquid-state silicon of 99.995% high temperature is poured into cool-bag, temperature is made to maintain 1450-1550 DEG C
Between；
2. first open cooling water and air-introduced machine, by air-introduced machine being pumped into negative pressure in device, then slowly high pressure, high purity
Oxygen is sent into atomizer, is then opened ultrasonic wave and is adjusted the vibration frequency in vibration cavity in 100-120KHz range and transport
Row 5 minutes, the air in device is lost no time by high pressure oxygen.Later, the discharging control switch on crucible is opened, molten is made
Silicon liquid flow down in traditional thread binding, when high temperature silicon liquid stream is to ultrasonic atomizing nozzle, just immediately by high voltagehigh frequency oxygen atomization granulating
Diameter is 10-15um or so or thinner spherical droplet；The silicon droplet of high temperature occurs immediately after contacting with high purity oxygen gas at the same time
Chemical reaction generates amorphous preparing spherical SiO 2 particle.Its chemical equation is respectively as follows: Si+O2=SiO2
3. the bottom coohng that the preparing spherical SiO 2 particle generated under the draft effect of air-introduced machine falls into cooling reactor.So
Afterwards, it then the water conservancy diversion coldplate that flows into cooling tube and slides downwards, is finally cooled to room temperature on the cooling plate and enters feed bin.I.e.
Preparing spherical SiO 2 product can be obtained.Sphericity is 100% average；Partial size 25um；SiO2Purity >=99.995%.
Embodiment 3
Ball-shaped silicon micro powder is prepared by taking the high-purity silicon liquid of 99.999% high temperature as an example
1. purity is that the liquid-state silicon of 99.999% high temperature is poured into cool-bag, temperature is made to maintain 1450-1550 DEG C
Between；
2. first open cooling water and air-introduced machine, by air-introduced machine being pumped into negative pressure in device, then slowly high pressure, high purity
Oxygen is sent into atomizer, is then opened ultrasonic wave and is adjusted the vibration frequency in vibration cavity in 120-140KHz range and transport
Row 5 minutes, the air in device is lost no time by high pressure oxygen.Later, the discharging control switch on crucible is opened, molten is made
Silicon liquid flow down in traditional thread binding, when high temperature silicon liquid stream is to ultrasonic atomizing nozzle, just immediately by high voltagehigh frequency oxygen atomization granulating
Diameter is 10-15um or so or thinner spherical droplet；The silicon droplet of high temperature occurs immediately after contacting with high purity oxygen gas at the same time
Chemical reaction generates amorphous preparing spherical SiO 2 particle.Its chemical equation is respectively as follows: Si+O2=SiO2
3. the bottom coohng that the preparing spherical SiO 2 particle generated under the draft effect of air-introduced machine falls into cooling reactor.So
Afterwards, it then the water conservancy diversion coldplate that flows into cooling tube and slides downwards, is finally cooled to room temperature on the cooling plate and enters feed bin.I.e.
Preparing spherical SiO 2 product can be obtained.Sphericity is 100%；Average grain diameter 20um；SiO2Purity >=99.999%.
Embodiment 4
Ball-shaped silicon micro powder is prepared by taking the high-purity silicon liquid of 99.999% high temperature as an example
1. purity is that the liquid-state silicon of 99.999% high temperature is poured into cool-bag, temperature is made to maintain 1450-1550 DEG C
Between；
Pressure is maintained between 8.4-8.5Mpa 2. opening high pressure oxygen switch；It opens ultrasonic ultrasonic delay line memory and heat preservation is held
Switch below device flows down silicon liquid slowly in the pipe of internal diameter 3-5mm or so, the arteries and veins of the adjusting resonant cavity of ultrasonic ultrasonic delay line memory
Frequency control is rushed in 140-160KHz, silicon liquid is atomised to by ultrasonic ultrasonic delay line memory with cooling jacket and energy with this condition
In the cooling reactor for taking out tiny structure, opens cooling water and air-introduced machine is taken out and takes out tiny structure to cooling reactor, in the height of atomization process high temperature
Pure silicon liquid droplet reacts with high purity oxygen gas immediately generates amorphous preparing spherical SiO 2, and chemical equation is respectively as follows:
Si+O2=SiO2；
3. the bottom coohng that the preparing spherical SiO 2 particle generated under the draft effect of air-introduced machine falls into cooling reactor.So
Afterwards, it then the water conservancy diversion coldplate that flows into cooling tube and slides downwards, is finally cooled to room temperature on the cooling plate and enters feed bin.I.e.
Preparing spherical SiO 2 product can be obtained.Sphericity is 100%；Average grain diameter 15um；SiO2Purity >=99.999%.
The foregoing is only a preferred embodiment of the present invention, but the scope of protection of the invention be not limited thereto.
With this device can also by adjust reduce ultrasonic atomization frequency, thus obtain the thicker amorphous state of partial size, without inclusion enclave,
Preparing spherical SiO 2 emery dust without hydroxyl can be used as high-purity ultra-pure raw material of quartz glass.Any skill for being familiar with the art
Any modification that art personnel are made in the technical scope disclosed by the present invention, equivalent replacement and improvement etc., should be included in invention
Protection scope within.
Claims (7)
1. the production method that a kind of ultrasonic atomization prepares ball-shaped silicon micro powder, which comprises the following steps:
(1) liquid-state silicon is heated and is kept the temperature, temperature maintains 1450-1550 DEG C；
It (2) is being 80-160kHZ, gas in frequency using ultrasonic ultrasonic delay line memory under the atmosphere using high purity oxygen gas as atomizing medium
Under conditions of body atomizing pressure is 8.3-8.7Mpa, liquid-state silicon is atomized to generate amorphous state preparing spherical SiO 2 material；
(3) to the silica batch of generation, up to preparing spherical SiO 2 powder after poly- cooling.
2. method according to claim 1, it is characterised in that: liquid-state silicon is high purity liquid state silicon in the step (1), and purity is
4N or more.
3. method according to claim 1, it is characterised in that: atomizing medium is high purity oxygen gas in the step (2).
4. a kind of process units for preparing ball-shaped silicon micro powder using claim 1 the method, it is characterised in that:
Including rate controlling hopper (1), electric heater unit (2), ultrasonic ultrasonic delay line memory (3), reaction kettle (4), condenser pipe (6), feed bin (7)
And screening plant；
The electric heater unit (2) includes electric heating crucible (21) and electric heating tube (22), and the two is sequentially connected from top to bottom；
The electric heater unit (2), ultrasonic ultrasonic delay line memory (3), reaction kettle (4), condenser pipe (6) and feed bin (7) from top to bottom according to
Secondary connection, feed bin upside are connected to screening plant；
Rate controlling hopper (1) is set to above electric heater unit (2).
5. the apparatus according to claim 1, it is characterised in that:
The ultrasonic ultrasonic delay line memory (3) includes chamber, and frequency-modulated generator and nozzle are provided in chamber, and chamber-side setting is aerobic
Gas import (33) and cooling water intake-outlet；Oxygen air inlet (33) is connected to frequency-modulated generator (32).
6. the apparatus according to claim 1, it is characterised in that: be provided with water conservancy diversion coldplate (5) in the condenser pipe.
7. the apparatus according to claim 1, it is characterised in that: the screening plant is by a second cyclone dust extractor, cloth bag
Deduster (10) and blower (11) are sequentially connected composition.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910574714.6A CN110371989A (en) | 2019-06-28 | 2019-06-28 | A kind of ultrasonic atomization prepares the production method of ball-shaped silicon micro powder |
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| CN201910574714.6A CN110371989A (en) | 2019-06-28 | 2019-06-28 | A kind of ultrasonic atomization prepares the production method of ball-shaped silicon micro powder |
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| CN111634915A (en) * | 2020-06-12 | 2020-09-08 | 将乐三晶新材料有限公司 | Atomization powder making process for molten metal silicon |
| CN114057202A (en) * | 2021-11-29 | 2022-02-18 | 苏州西丽卡电子材料有限公司 | Preparation method and application of spherical silicon micro powder with ultrahigh purity and ultrahigh compactness |
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