CN105818287B - A kind of method that mass prepares high-purity sub-micron hydration silicon and silicon particle - Google Patents
A kind of method that mass prepares high-purity sub-micron hydration silicon and silicon particle Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28D—WORKING STONE OR STONE-LIKE MATERIALS
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- B28D5/04—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor by tools other than rotary type, e.g. reciprocating tools
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- B28—WORKING CEMENT, CLAY, OR STONE
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- B28D5/00—Fine working of gems, jewels, crystals, e.g. of semiconductor material; apparatus or devices therefor
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Abstract
The present invention relates to semiconductor and solar power silicon field of material technology, the method that specifically a kind of mass prepares high-purity sub-micron hydration silicon and silicon particle, using fine diamond line, under deionized water auxiliary, cutting is ground to high purity silicon rods or silicon ingot, after silicon particle concentration reaches 10wt%, mixture is subjected to purification & isolation, forms press filtration water and hydration silicon particle;Press filtration water is carried out after purification, to be recycled, vacuum freeze drying is carried out to hydration silicon particle, forms high-purity silicon particle.The present invention is compared with the existing technology; using fine diamond wire cutting technology; under deionized water effect high purity silicon rods are ground with cutting and prepares high-purity silicon chip; simultaneously; deionized water after cutting and the mixture of silicon particle are purified; to prepare high-purity hydrated silicon particle or high-purity silicon particle, and it is subject to recycling.The aqueous solution after silicon particle purifies, which can be injected after purifying again in fine diamond wire cutting technology engineering, to be recycled.
Description
Technical field
The present invention relates to semiconductor and solar power silicon field of material technology, specifically a kind of mass prepares high-purity Asia
The method of micron hydration silicon and silicon particle.
Background technology
With the development of modern information industry and New Energy Industry, the semiconductor electronic technology based on high-purity silicon materials
Have evolved into the pillar industry of advanced information society;Meanwhile the solar photovoltaic technology based on high-purity silicon materials
Also the pillar industry of regenerative resource is being developed into.The demand of high-purity silicon materials and consumption are also in continual growth.
High-purity silicon materials can be divided into monocrystalline silicon and polysilicon by structure.The mainly list of semiconductor devices such as integrated circuit
Crystal silicon chip, purity is more than 99.99999%;Solar cell is according to the height of generating efficiency, and monocrystalline silicon piece and polysilicon chip are all
Use, purity is more than 99.9999%.Because the generating efficiency of monocrystaline silicon solar cell is high, reliability is high, service life length,
As technological progress will dominate solar photovoltaic industry.
The production of high-purity silicon chip is prepared by high purity silicon rods or silicon ingot by wire cutting, typically about 60% silicon rod or
Silicon ingot can be prepared as silicon chip, and remaining about 40% silicon has then been stayed in cutting liquid for powder, and silicon powder is after dehydration as at waste material
Reason.During general cutting silicon chip, made using metal wire containing silicon-carbide particles and organic matter, such as the polyethylene glycol PEG aqueous solution
Under, cutting is ground, line footpath is typically more than 250 microns.In the aqueous solution after cutting containing silicon, carborundum, organic matter,
Metal etc. is used as waste material or liquid waste processing, is not readily separated purification and recycles.
The diamond wire saw of new development, it is that the silk thread that diamond particle is coated with using metal line surface is acted in the aqueous solution
Under cutting is ground to silicon rod, line footpath can have about 65 ~ 70% silicon rod materials to be cut into silicon chip, carry typically below 250 microns
The high utilization rate of silicon rod.Simultaneously still have about 30 ~ 35% silicon rod material be ground be cut into silicon particle powder be scattered in it is water-soluble
In liquid, as waste material or liquid waste processing.
In particular with the high speed development of solar photovoltaic industry, substantial amounts of silicon powder-containing is generated when crystal silicon chip produces
Waste water, easily cause environmental pollution;Caused waste water or waste disposal are with high costs, also constrain solar photovoltaic industry
Development.
Therefore, it is necessary to design a kind of method that mass prepares high-purity sub-micron hydration silicon and silicon particle, silicon particle will be contained
Waste material further recycled after purification, to reduce the waste of water resource, reduce risk of environmental pollution, while also can be big
Width reduces the integrated cost of silicon chip production, promotes the Green Development of semiconductor and solar photovoltaic industry.
The content of the invention
The purpose of the present invention is overcome the deficiencies in the prior art, there is provided a kind of mass prepares high-purity sub-micron hydration silicon
With the method for silicon particle, will be recycled after the waste material containing silicon particle further purification, to reduce the waste of water resource, drop
Low environment pollution risk, while the integrated cost of silicon chip production can also be greatly reduced, promote semiconductor and solar photovoltaic industry
Green Development.
In order to achieve the above object, the present invention is the side that a kind of mass prepares high-purity sub-micron hydration silicon and silicon particle
Method, it is characterised in that:Prepare as follows:Step 1, using fine diamond line, under deionized water auxiliary, to HIGH-PURITY SILICON
Rod or silicon ingot are ground cutting, form high-purity silicon chip and scattered silicon particle in deionized water;Step 2, deionized water is worked as
In silicon particle concentration reach 10wt% after, the mixture of deionized water and silicon particle is discharged, and carries out purification & isolation, is formed
Press filtration water and hydration silicon particle;Step 3, press filtration water is carried out after purification, during injection fine diamond wire cutting technology to enter
Row recycles, and carries out vacuum freeze drying to hydration silicon particle, forms high-purity silicon particle.
Described fine diamond line is the silk thread that metal line surface is coated with diamond particle, and line footpath is 30 ~ 120 microns,
Diamond particle size is 5 ~ 20 microns, and described deionized water is resistivity 18M Ω high purity water.
Described purification & isolation comprises the following steps that:Step 1, using aperture<2 μm of microfiltration membranes, to deionized water and silicon
The mixture of particulate is filtered, and bulky grain or aggregate are filtered out, and forms the suspension of the water containing silicon particle, silicon particle chi
It is very little within 1 μm;Step 2, using the electrochemical catalysis electrod-array of platinum silk or platinum piece as capacitance type structure, put
Enter in suspension, it is micro in suspension under electric field action between negative electrode and anode plus direct current or pulsed dc voltage 2-24V
Carbon be oxidized in anode surface and be decomposed into carbon dioxide, micro metal ion is reduced in cathode surface and deposited, and goes the removal of impurity;
Step 3, using with aperture<The filtering equipment of 0.5 μm of microporous barrier, press filtration is carried out to the suspension after decontamination, forms liquid
Press filtration water and solid-state hydration silicon particle.
The described purifying that carried out to press filtration water includes capacitive deionization, electrodialysis, counter-infiltration, ion exchange absorption processing.
Described comprises the following steps that to hydration silicon particle progress vacuum freeze drying:Step 1, temperature control is at -10 DEG C
Hereinafter, hydration silicon particle is put into vacuum chamber, is evacuated to vacuum and reaches below 10Pa, the water liter being hydrated in silicon particle
Huawei's gaseous state, silicon particle dehydration, forms high-purity silicon particle, purity is more than 99.999%;Step 2, to high-purity silicon particle using true
Empty or filling with inert gas packaging.
Described high-purity silicon particle is melted in the case where inert gas and concentration are less than or equal to the mixed atmosphere of 5vol% hydrogen
Melt, hydrogen removes the hydrogen reduction in the silica of HIGH-PURITY SILICON microparticle surfaces, forms high purity polycrystalline silicon block materials, purity
More than 99.9999%.
Described high-purity silicon particle is under nitrogen hydrogen or ammonia atmosphere, after the nitridation heat treatment that temperature is 800 ~ 1400 DEG C, shape
Into high purity silicon nitride silicon particle, the preparation for silicon nitride ceramic material.
Described high-purity silicon particle hydrocarbon polymer is compound or hydrocarbon atmosphere under, after carbonization is heat-treated, formed high-purity
Silicon-carbide particles, the preparation for thyrite.
Described hydration silicon particle, in a solution of hydrofluoric acid, after chemical attack or electrochemical etching, form nanoporous
Silicon particle, after the oxidation of nano-structure porous silicon heat particles, form the nanoporous hydrated silica or nanoporous of high-specific surface area
Silicon oxide particle material.
Described nanoporous silicon particle, it is compound with carbon material or metal material, form high power capacity and nanoporous silicon-carbon
Or silicon metallic composite, for energy storage device.
The present invention compared with the existing technology, using fine diamond wire cutting technology, to high-purity under deionized water effect
Silicon rod is ground cutting and prepares high-purity silicon chip, meanwhile, the deionized water after cutting and the mixture of silicon particle are purified,
To prepare high-purity hydrated silicon particle or high-purity silicon particle, and it is subject to recycling.The aqueous solution after silicon particle purifies is net again
It can inject in fine diamond wire cutting technology engineering and be recycled after change.
Brief description of the drawings
Fig. 1 is the process chart of the present invention.
Fig. 2 is the structural representation of present invention hydration silicon particle.
Embodiment
The present invention is described further in conjunction with accompanying drawing.
Referring to Fig. 1, a kind of mass of the present invention prepares the method that high-purity sub-micron is hydrated silicon and silicon particle, as follows
Prepare:Step 1, using fine diamond line, under deionized water auxiliary, to high purity silicon rods that purity is more than 99.9999% or
Silicon ingot is ground cutting, is formed for semiconductor devices or high-purity silicon chip of manufacture of solar cells and is dispersed in deionized water
In silicon particle.Fine diamond line is the silk thread that metal line surface is coated with diamond particle, and line footpath is 30 ~ 120 microns, Buddha's warrior attendant
Stone particle size is 5 ~ 20 microns, and under the abrasive action of diamond particle, caused silicon particle size is below 1 micron.
The line footpath of diamond is thinner, and the silicon chip quantity of cutting is more, as used 80 microns of diamond wire saw thickness as 180 microns
High-purity silicon chip, about 70% high purity silicon rods material are cut into high-purity silicon chip, and remaining about 30% high purity silicon rods is ground as silicon particle.
Deionized water is resistivity 18M Ω high purity water, and deionized water plays cooling when high purity silicon rods are ground in fine diamond wire cutting
And lubrication, while flushing action is risen to the silicon particle of grinding.
Step 2, after the silicon particle concentration in deionized water reaches 10wt%, by deionized water and the mixture of silicon particle
Discharge, and purification & isolation is carried out, form press filtration water and hydration silicon particle.
Purification & isolation comprises the following steps that:Step 1, using aperture<2 μm of microfiltration membranes, to deionized water and silicon particle
Mixture is filtered, and bulky grain or aggregate are filtered out, and forms the suspension of the water containing silicon particle, silicon particle size is in 1 μ
Within m, outside water removal and silicon particle, concentration is also contained in suspension<0.1mg/L carbon and concentration<Two kinds of 1ppm metal ion
Impurity, the possible element of metal ion are Fe, Ni, Cr, Ti.Step 2, using platinum silk or platinum piece as electric capacity
The electrochemical catalysis electrod-array of formula structure, is put into suspension, and direct current or pulsed dc voltage 2- are added between negative electrode and anode
24V, under electric field action, micro carbon is oxidized in anode surface and is decomposed into carbon dioxide in suspension, micro metal from
Son is reduced in cathode surface and deposited, and goes the removal of impurity.Step 3, using with aperture<The filtering equipment of 0.5 μm of microporous barrier, to impurity elimination
Suspension after matter carries out press filtration, forms the press filtration water of liquid and the hydration silicon particle of solid-state.
Hydration silicon particle prepared by the present invention, is mainly made up of high-purity silicon particle and water, and HIGH-PURITY SILICON particle size is 100
~ 1000nm scopes, purity are more than 99.9999%, and silicon particle surface can be thick formed with a thin layer in cutting and grinding technical process
Degree<1nm silica.Because the silicon oxide layer of formation is polar molecule, easily combined with hydrone, form hydration silicon particle Si-
nH2O, water content is about 30%.It is hydrated the structural representation of silicon particle as described in Figure 2, granule size is in sub-micrometer scale, in table
Hydrone is adsorbed in face.The powder form that moistening is presented in silicon particle is hydrated, it is relatively stable in air.
Step 3, press filtration water is carried out after purification, injection fine diamond line is recycled, and hydration silicon particle is entered
Row vacuum freeze drying, form high-purity silicon particle.
Purifying is carried out to press filtration water includes capacitive deionization, electrodialysis, counter-infiltration, ion exchange absorption processing.
Vacuum freeze drying is carried out to hydration silicon particle to comprise the following steps that:Step 1, temperature control, will below -10 DEG C
Hydration silicon particle is put into vacuum chamber, is evacuated to vacuum and is reached below 10Pa, the water sublimate being hydrated in silicon particle is gas
State, silicon particle dehydration, forms high-purity silicon particle, and purity is more than 99.999%, and step 2, high-purity silicon particle using vacuum or is filled
Inert gas is packed.
Hydration silicon particle prepared by the present invention, it is dehydrated according to mode of heating, because silicon particle size is smaller, surface-active
Higher, when temperature is more than 60 DEG C, surface is easily oxidized so that the purity of silicon particle declines.The vacuum refrigeration that the present invention uses
Drying process, oxidation of the silicon particle in dehydration can be avoided.Because the granularity of silicon particle is submicron order, than surface compared with
Greatly, silicon particle exposure in atmosphere, is easily oxidized, or even the dangerous situations such as spontaneous combustion can occur, in order to avoid silicon particle exposes
In atmosphere, the present invention using vacuum or fills inert gas such as argon gas, is packed.
High-purity silicon particle prepared by the present invention enters in the case where such as argon gas and concentration are less than or equal to the mixed atmosphere of 5vol% hydrogen
Row melting, hydrogen remove the hydrogen reduction in the silica of HIGH-PURITY SILICON microparticle surfaces, form high purity polycrystalline silicon block materials, purity
More than 99.9999%, polysilicon block materials further prepare and form silicon single crystal rod material, available for the production of solar cell,
Recycling for silicon materials is accomplished.
High-purity silicon particle prepared by the present invention is heat-treated under nitrogen hydrogen or ammonia atmosphere through the nitridation that temperature is 800 ~ 1400 DEG C
Afterwards, high purity silicon nitride silicon particle, the preparation for silicon nitride ceramic material are formed.
High-purity silicon particle prepared by the present invention hydrocarbon polymer is compound or hydrocarbon atmosphere under, after carbonization is heat-treated, shape
Into high-purity silicon carbide particulate, the preparation for thyrite.
Hydration silicon particle prepared by the present invention, in a solution of hydrofluoric acid, after chemical attack or electrochemical etching, formation is received
Rice porous silicon particulate, nanoporous silicon particle can be as the energy storage or energetic material application of high power capacity.Nanoporous silicon particle adds
After thermal oxide, form the nanoporous hydrated silica or nanoporous silicon oxide particle material of high-specific surface area, can be used as in
Efficient absorption or filtering material use.
Nanoporous silicon particle, it is compound with the carbon material including graphene or the metal material including tin, titanium material, formed
High power capacity and nanoporous silicon-carbon or silicon metallic composite, include lithium ion and sodium ion electricity available for high-capacity secondary battery
The preparation of the negative electrode material in pond or the electrode material of energy storage super capacitor.
The present invention is because employing silicon particle material caused by the high-purity silicon chip of industrial-scale production, through the fine of the present invention
Diamond wire saw grinding production technology is improved and waste liquid purification technique, can accomplish recycling for waste water, cause simultaneously
Silicon particle resourcebility utilizes.The production cost of semi-conductor silicon chip or photovoltaic silicon chip can be greatly reduced by the present invention,
Simultaneously can low-coat scale metaplasia produce the hydration silicon and silicon particle material of high-purity submicron order, and expanded the functionalization of silicon particle
Using.By the technology application of the present invention, the development of semi-conductor industry and solar energy power generating industry can be effectively facilitated, especially
It is the acceleration application and popularization for accelerating efficient mono-crystalline silicon solar photovoltaic technology as regenerative resource, is human society
Information and energy industry structural adjustment play positive impetus.
Claims (8)
1. a kind of method that mass prepares high-purity sub-micron hydration silicon and silicon particle, it is characterised in that:Prepare as follows:
Step 1, using fine diamond line, under deionized water auxiliary, high purity silicon rods or silicon ingot is ground with cutting, is formed high-purity
Silicon chip and scattered silicon particle in deionized water;Step 2, after the silicon particle concentration in deionized water reaches 10wt%, will go
The mixture of ionized water and silicon particle is discharged, and carries out purification & isolation, forms press filtration water and hydration silicon particle;Step 3, to press filtration
Water is carried out after purification, and injection fine diamond wire cutting technology process is recycled, and it is cold to carry out vacuum to hydration silicon particle
It is lyophilized dry, high-purity silicon particle is formed, it is described that hydration silicon particle progress vacuum freeze drying is comprised the following steps that:Step 1, it is warm
Hydration silicon particle is put into vacuum chamber below -10 DEG C, is evacuated to vacuum and reaches below 10Pa, be hydrated by degree control
Water sublimate in silicon particle is gaseous state, silicon particle dehydration, forms high-purity silicon particle, purity is more than 99.999%;Step 2, to height
Pure silicon particulate is packed using vacuum or filling with inert gas, and described purification & isolation comprises the following steps that:Step 1, using aperture<2µ
M microfiltration membranes, the mixture of deionized water and silicon particle is filtered, bulky grain or aggregate are filtered out, formation contains silicon
The suspension of the water of particulate, silicon particle size is within 1 μm, step 2, using platinum silk or platinum piece as condenser type knot
The electrochemical catalysis electrod-array of structure, is put into suspension, and direct current or pulsed dc voltage 2-24V are added between negative electrode and anode,
Under electric field action, micro carbon is oxidized in anode surface and is decomposed into carbon dioxide in suspension, and micro metal ion exists
Cathode surface reduction deposition, goes the removal of impurity, step 3, using with aperture<The filtering equipment of 0.5 μm of microporous barrier, after decontamination
Suspension carry out press filtration, form the press filtration water of liquid and the hydration silicon particle of solid-state.
2. a kind of mass according to claim 1 prepares the method for high-purity sub-micron hydration silicon and silicon particle, its feature
It is:Described fine diamond line is that metal line surface is coated with the silk thread of diamond particle, and line footpath is 30-120 microns, Buddha's warrior attendant
Stone particle size is 5-20 microns, and described deionized water is resistivity 18M Ω high purity water.
3. a kind of mass according to claim 1 prepares the method for high-purity sub-micron hydration silicon and silicon particle, its feature
It is:The described purifying that carried out to press filtration water includes capacitive deionization, electrodialysis, counter-infiltration, ion exchange absorption processing.
4. a kind of mass according to claim 1 prepares the method for high-purity sub-micron hydration silicon and silicon particle, its feature
It is:Described high-purity silicon particle is melted in the case where inert gas and concentration are less than or equal to the mixed atmosphere of 5vol% hydrogen,
Hydrogen removes the hydrogen reduction in the silica of HIGH-PURITY SILICON microparticle surfaces, forms high purity polycrystalline silicon block materials, purity
More than 99.9999%.
5. a kind of mass according to claim 1 prepares the method for high-purity sub-micron hydration silicon and silicon particle, its feature
It is:Described high-purity silicon particle after the nitridation heat treatment that temperature is 800-1400 DEG C, is formed high under nitrogen hydrogen or ammonia atmosphere
Pure silicon nitride particulate, the preparation for silicon nitride ceramic material.
6. a kind of mass according to claim 1 prepares the method for high-purity sub-micron hydration silicon and silicon particle, its feature
It is:Described high-purity silicon particle hydrocarbon polymer is compound or hydrocarbon atmosphere under, after carbonization is heat-treated, form high-purity carbonization
Silicon particle, the preparation for thyrite.
7. a kind of mass according to claim 1 prepares the method for high-purity sub-micron hydration silicon and silicon particle, its feature
It is:Described hydration silicon particle, in a solution of hydrofluoric acid, after chemical attack or electrochemical etching, form nano-structure porous silicon
Particulate;After the oxidation of nano-structure porous silicon heat particles, the nanoporous hydrated silica or nanoporous oxygen of high-specific surface area are formed
SiClx microparticle material.
8. a kind of mass according to claim 7 prepares the method for high-purity sub-micron hydration silicon and silicon particle, its feature
It is:Described nanoporous silicon particle, it is compound with carbon material or metal material, form the nanoporous silicon-carbon or silicon of high power capacity
Metallic composite, for energy storage device.
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