CN106000286B - A kind of preparation method of low cost nano-structure porous silicon and silica ultrafine dust - Google Patents
A kind of preparation method of low cost nano-structure porous silicon and silica ultrafine dust Download PDFInfo
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- CN106000286B CN106000286B CN201610374292.4A CN201610374292A CN106000286B CN 106000286 B CN106000286 B CN 106000286B CN 201610374292 A CN201610374292 A CN 201610374292A CN 106000286 B CN106000286 B CN 106000286B
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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
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Abstract
The present invention relates to semiconductor and solar power silicon field of material technology, specifically a kind of preparation method of inexpensive nano-structure porous silicon and silica ultrafine dust.A kind of preparation method of low cost nano-structure porous silicon and silica ultrafine dust, for generated silicon powder aqueous solution as raw material, preparation method is as follows after cutting silicon wafer in deionized water using diamond wire：The hydration silicon particle that silicon powder aqueous solution is obtained by purification；Hydration silicon particle can be prepared into nanoporous silicon particle by chemical etching technology in hydrofluoric acid and aqueous solution of nitric acid；The nanoporous hydrated silica or silicon oxide particle material that high-specific surface area can be prepared after nanoporous silicon particle is directly heated, use as efficient absorption or filtering material.Compared with the existing technology, the preparation method for providing a kind of inexpensive nano-structure porous silicon and silica ultrafine dust converts nanometer hydrated porous silicon and silicon oxide particle for silicon particle, enables its resource utilization after production technology is improved.
Description
Technical field
The present invention relates to semiconductor and solar power silicon field of material technology, specifically a kind of inexpensive nano-structure porous silicon
With the preparation method of silica ultrafine dust.
Background technique
Porous silica material composite material, energetic material and in terms of have good application prospect；Porous oxygen
Silicon nitride material absorption, filtering, in terms of have important application value.And nano aperture（1-50 nm）Porous silicon
With silica because in its high specific surface area, function admirable, application prospect is more wide.The granularity of porous silicon particle is smaller, more
It is easy to evenly dispersed or compound with other materials, it is especially ultra-fine（Submicron order）The application surface of particle is wider.Porous silicon is general
Using monocrystalline silicon silicon wafer or silicon particle（Some tens of pm）Chemical attack or electrochemical etching are carried out in the solution such as hydrogen fluoride and are obtained
, difference is adjusted according to reaction, generally available aperture is 10-200 nm, 1-10 μm of hole depth of porous silicon chip or particle.It is more
Hole silicon oxide particle generally uses organosiloxane bead（1-100 µm）It will be obtained after its organic principle oxygenolysis at high temperature
?.This two methods is because the cost of raw material is high, and cost is more if the preparation for nano-structure porous silicon and silica ultrafine dust
Height, therefore it is generally used for laboratory research or a small amount of preparations, it is difficult to realize the industrial production of low cost mass.On the other hand,
When preparing high-purity silicon wafer of semiconductor and photovoltaic, a large amount of silicon particle materials can be generated after cutting high purity silicon rods,
Generated silicon particle accounts for the 30-40% of entire silicon rod material, generally as waste disposal.With the height of solar photovoltaic industry
Speed development, while produce a large amount of silicon wafers, along with producing a large amount of aqueous silicon particle waste material, subsequent treatment cost height and
Easily cause environmental pollution.If can be nano-structure porous silicon or silicon oxide particle by such converting waste material containing silicon particle, can significantly drop
The overall cost of low environment pollution risk and silicon wafer production, promotes the Green Development of semiconductor and solar photovoltaic industry.
Summary of the invention
The present invention in order to overcome the deficiencies of the prior art, provides a kind of inexpensive nano-structure porous silicon and silica ultrafine dust
Preparation method converts nanometer hydrated porous silicon and silicon oxide particle for silicon particle after production technology is improved, make its as a means of
Sourceization utilizes.
To achieve the above object, the preparation method for designing a kind of inexpensive nano-structure porous silicon and silica ultrafine dust, is adopted
Generated silicon powder aqueous solution is as raw material after using diamond wire to cut silicon wafer in deionized water, it is characterised in that：It is described
Preparation method it is as follows：
（1）The hydration silicon particle that silicon powder aqueous solution is obtained by purification, the size for being hydrated silicon particle is 100 ~ 1000nm；
（2）Hydration silicon particle can be prepared into nanoporous by chemical etching technology in hydrofluoric acid and aqueous solution of nitric acid
Silicon particle, nano aperture are distributed as 2 ~ 30nm；
（3）Or hydration silicon particle can be prepared in the aqueous solution of hydrofluoric acid and ethyl alcohol by electrochemical corrosive process
Nanoporous silicon particle, nano aperture are distributed as 2 ~ 50nm；
（4）The nanoporous aqua oxidation of high-specific surface area can be prepared after nanoporous silicon particle is directly heated
Silicon or silicon oxide particle material, use as efficient absorption or filtering material.
The hydration silicon particle is made of purity in 99% or more silicon particle and the hydrone of adsorption, water with
The ratio of silicon is 20 ~ 30wt%, and moist form exists.
The chemical etching technology be hydration silicon particle in be added hydrofluoric acid containing and nitric acid aqueous solution, hydrofluoric acid,
The percent concentration of nitric acid and water is 20vol%:5 vol%:100 vol%, the proportion for being hydrated silicon particle and acid solution is 10
wt%:1 wt% reacts 5 ~ 20min under ultrasonic wave effect.
The electrochemical corrosive process is being hydrated using metal platinum filament or piece as the anodic-cathodic of electrochemical capacitor
The aqueous solution of hydrofluoric acid and ethyl alcohol is added in silicon particle, the percent concentration of hydrofluoric acid, ethyl alcohol and water is 3 vol%:1 vol%:5
Vol%, the proportion for being hydrated silicon particle and acid solution is 10 wt%:3wt%；On the electrode plus pulse direct current electric field, current density 1
~30mA/cm2, 1 ~ 5min is reacted in the case where adding ultrasonic wave to act on.
The nanoporous silicon particle can be used for the energetic material of high-energy density.
The nanoporous silicon particle can be used for the rechargeable battery of high capacity and high-energy density or the electrode material of capacitor
Material.
The nanoporous silicon particle is directly in nitrogen hydrogen, N2:H2=95:1400 DEG C are heated up under 5% atmosphere to be nitrogenized
After processing, the nanoporous silicon nitride particulate material of high-specific surface area can be prepared, as high performance ceramic material.
The nanoporous silicon particle is directly containing hydrocarbon argon gas, C2H2:Ar=10:1200 are heated up under the atmosphere of 90 %
DEG C carry out carbonization treatment after, the nanoporous silicon-carbide particles material of high-specific surface area can be prepared, as high-performance ceramic material
Material.
The present invention compared with the existing technology, provides the preparation side of a kind of inexpensive nano-structure porous silicon and silica ultrafine dust
Method converts nanometer hydrated porous silicon and silicon oxide particle for silicon particle after production technology is improved, and keeps its recycling sharp
With.
The present invention is with cost of material is extremely low, is easy to large-scale production and application；Stablized using processing performance of the invention,
Consistency is good, has good cost performance；Meanwhile semi-conductor silicon chip or photovoltaic silicon wafer can be greatly reduced through the invention
Synthesis production cost, effectively facilitate industry development, for silicon materials application opened up a new application technology route.
Detailed description of the invention
The typical Electronic Speculum SEM shape appearance figure of chemical corrosion method nanoporous silicon particle Fig. 1 of the invention.
Fig. 2 is electrochemical reaction appts schematic diagram of the invention.1 is Pt electrode；2 be bipolar pulse power supply；3 be nano-silicon
The mixed solution of particle and HF；4 be supersonic generator.
Fig. 3 is the typical Electronic Speculum SEM shape appearance figure of electrochemical erosion method nanoporous silicon particle of the invention.
Specific embodiment
The invention will now be described in further detail with reference to the accompanying drawings.
Generated silicon powder aqueous solution is as raw material, preparation side after cutting silicon wafer in deionized water using diamond wire
Method is as follows：
（1）The hydration silicon particle that silicon powder aqueous solution is obtained by purification, the size for being hydrated silicon particle is 100 ~ 1000nm；
（2）Hydration silicon particle can be prepared into nanoporous by chemical etching technology in hydrofluoric acid and aqueous solution of nitric acid
Silicon particle, nano aperture are distributed as 2 ~ 30nm；
（3）Or hydration silicon particle can be prepared in the aqueous solution of hydrofluoric acid and ethyl alcohol by electrochemical corrosive process
Nanoporous silicon particle, nano aperture are distributed as 2 ~ 50nm；
（4）The nanoporous aqua oxidation of high-specific surface area can be prepared after nanoporous silicon particle is directly heated
Silicon or silicon oxide particle material, use as efficient absorption or filtering material.
Hydration silicon particle is made of purity in 99% or more silicon particle and the hydrone of adsorption, the ratio of water and silicon
Example is 20 ~ 30wt%, and moist form exists.
Chemical etching technology be hydration silicon particle in be added hydrofluoric acid containing and nitric acid aqueous solution, hydrofluoric acid, nitric acid and
The percent concentration of water is 20vol%:5 vol%:100 vol%, the proportion for being hydrated silicon particle and acid solution is 10 wt%:1
Wt% reacts 5 ~ 20min under ultrasonic wave effect.
Electrochemical corrosive process, using metal platinum filament or piece as the anodic-cathodic of electrochemical capacitor, in hydration silicon particle
The middle aqueous solution that hydrofluoric acid and ethyl alcohol is added, the percent concentration of hydrofluoric acid, ethyl alcohol and water are 3 vol%:1 vol%:5 vol%,
The proportion for being hydrated silicon particle and acid solution is 10 wt%:3wt%；On the electrode plus pulse direct current electric field, current density be 1 ~
30mA/cm2, 1 ~ 5min is reacted in the case where adding ultrasonic wave to act on.
Nanoporous silicon particle can be used for the energetic material of high-energy density.
Nanoporous silicon particle can be used for the rechargeable battery of high capacity and high-energy density or the electrode material of capacitor.
Nanoporous silicon particle is directly in nitrogen hydrogen, N2:H2=95:1400 DEG C of progress nitrogen treatment are heated up under 5% atmosphere
Afterwards, the nanoporous silicon nitride particulate material that high-specific surface area can be prepared, as high performance ceramic material.
Nanoporous silicon particle is directly containing hydrocarbon argon gas, C2H2:Ar=10:1200 DEG C of progress are heated up under the atmosphere of 90 %
After carbonization treatment, the nanoporous silicon-carbide particles material of high-specific surface area can be prepared, as high performance ceramic material.
The present invention uses improved fine diamond line, and line footpath is 30 ~ 120 microns, and cutting technique is acted in deionized water
Under to high purity silicon rods carry out cutting and grinding produce silicon wafer, while the waste water containing silicon particle generated during cutting and grinding into
After row filters pressing separates water into, aqueous silicon particle-hydration silicon particle is obtained.It is further converted using being hydrated silicon particle as raw material
For nano-structure porous silicon and silicon oxide particle, to realize the resource utilization of waste material.
Aqueous silicon particle used by method of the invention, is mainly made of the water of high-purity silicon particle and adsorption, ruler
It is very little in 100 ~ 1000 nm ranges, purity is 99% or more, and silicon particle surface will form a thin layer silica in technical process
(<1nm).Because the silicon oxide layer of formation is polar molecule, is easily combined with hydrone, form hydration silicon particle（Si-nH2O）, contain
Water is about 20 ~ 30%.It is presented wet pureed form, it is relatively stable in air.
Above-mentioned hydration sub-micron silicon particle rapid batchization preparation can be used in nano-structure porous silicon ultrafine dust of the invention.
It is specifically included in progress two kinds of reaction process of chemical attack or electrochemical etching in the solution such as hydrogen fluoride.
Method 1：Chemical corrosion method：The container made of polytetrafluoroethylene material, it is hydrogeneous by being added in hydration silicon particle
In the aqueous solution of fluoric acid and nitric acid, solution ratio HF:HNO3:H2O = 20:5:100（vol%)；Silicon particle and acid solution are matched
Than for Si-nH2O:HF-HNO3-H2O=10:1 (wt%) reacts 5 ~ 20min under ultrasonic wave effect.Main chemical reactions are such as（1）
Shown, local silicon atom can be etched to the silicon fluoride of volatile, so that forming multiple nanoscale hole holes, hole on silicon particle
Etch rate be 0.1 ~ 2nm/min.Then acid solution and impurity are cleaned with deionized water.Obtaining after filters pressing again has nanometer
The hydration silicon particle of porous structure.Nano-pore is distributed in 2 ~ 30nm range, and moisture content is 10 ~ 20%.Typical nano-structure porous silicon
SEM pattern photo as shown in Figure 1, aperture about 10nm, hole ratio about 30%.
Si+4HNO3+ 4HF=SiF4↑+4NO2↑+4H2O--------（1）
Method 2：Electrochemical etching method：The container made of polytetrafluoroethylene material, using metal platinum filament or piece as electric
The anodic-cathodic of chemical capacitor.It will be hydrated in the aqueous solution that hydrofluoric acid and ethyl alcohol are added in silicon particle, solution ratio HF:
HCH2COH:H2O=3:1:5 (vol%)；The proportion of silicon particle and acid solution is Si-nH2O：HF-HCH2COH-H2O=10:3
(wt%).After closed, on the electrode plus pulse direct current electric field (J=1-30mA/cm2, 2-12V), while adding ultrasonic oscillation, it can make
It must react uniform.Reaction time 1-5min.The schematic device of electrochemical reaction is as shown in Fig. 2, silicon particle is dispersed in two Pt electricity
In hydrofluoric acid solution 3 among pole 1, reaction chamber bottom is by there is supersonic generator 4.Ambipolar pulse direct current is connected in Pt electrode
Power supply 2, in reaction, generating positive and negative voltage can automatically switch.Main chemical reactions are such as（2）Shown, local silicon atom can be etched to
The silicon fluoride of volatile, so that forming multiple nanoscale hole holes on silicon particle, the etch rate in hole is 2 ~ 10 nm/min.One
As silicon particle surface can be oxidized generation oxide layer, main chemical reactions are such as（3）It is shown, mainly silica is generated in silicon face.
Oxide layer can be corroded after hydrofluoric acid reacts, and main chemical reactions are such as（4）It is shown, it mainly generates fluosilicic acid and removes.Instead
After the completion of answering, acid solution and impurity are cleaned using deionized water.The hydration silicon with nano-porous structure is obtained after filters pressing again
Particle.Nano-pore is distributed in 5-50nm range, and moisture content is in 10-20%.The SEM pattern photo of typical nano-structure porous silicon is such as
Shown in Fig. 3, aperture about 20nm, hole ratio about 80%.
Si+4HF=SiF4↑+2H2--------------（2）
Si+ 2H++ 2OH-=SiO2↓+H2↑ --------------（3）
SiO2+ 6HF=H2SiF6 + 2H2O --- --- --- --- --（4）
The method for preparing nanoporous silicon particle of the invention has reaction compared with traditional porous silicon preparation method
Time is short（<10 min), current density it is low (<30m A/cm2), low energy consumption, aperture it is small (<50 nm) and the features such as narrowly distributing.Such as
The general rate of the electrochemical corrosion of traditional porous silicon is 1 ~ 5 μm/min, and current density is 30 ~ 500mA/cm2, the time be 5 ~
60min.The distribution in aperture is generally in 10 ~ 200 nm ranges, and 5-100 μm of hole depth.
The nanoporous silicon particle of above method preparation can be used as original in nanoporous silica ultrafine dust of the invention
Material, the hydration submicron order porous oxidation silicon particle that further batch synthesizes.Concrete technology includes, using polytetrafluoroethylene material
Prepared nanometer hydrated porous silicon particle is heated to 100 DEG C in air, keeps the temperature 0.5 hour by the container of production；Then plus
Heat keeps the temperature 2 hours to 250 DEG C.Nanoporous silicon particle is oxidized to form nanometer hydrated porous oxidation silicon particle, water content<
10%.When temperature is heated to 600 DEG C, keeps the temperature 1 hour, particle dehydration and become nanoporous silica.According to reaction temperature
The moisture content of difference, silica generated is also different, increases with temperature, moisture content decline.The aperture master of silicon oxide nano pore
It is distributed in 5-50nm range, moisture content is in 0.1 ~ 10% range.It is general to aoxidize compared with traditional porous silicon prepares silica
Temperature is at 750 DEG C or more, and porous silica prepared by method of the invention has preparation temperature low, the small advantage of energy consumption.
Nanometer hydrated porous silicon particle, can be used for the energetic material of high capacity prepared by method of the invention.Because of nanometer
High reaction activity, the high-specific surface area of porous silicon, explosion time solid phase reaction interface is big, reactant is easy to spread and migrate.As
Energetic material, nano-structure porous silicon have many advantages, such as high-energy density and explosion product of low pollution.Perchloric acid is such as mixed in hole
The oxidants such as sodium can prepare the explosive reaction Composite Energetic Materials of high-energy density.
Nanometer hydrated porous silicon particle, can be used for the energy storage material of high capacity prepared by method of the invention.Because of silicon material
Material has very high specific capacity as the electrode material of rechargeable battery or capacitor（Theoretical value is 4200mAh/g）, but because of its body
Product expansion is larger and electric conductivity is poor, does not have practicability.Nanoporous silicon particle of the invention and conductive material such as carbon, tin, titanium
It is rear as electrode material, the porosity of Yin Qigao and good electric conductivity etc. compound, it may make the silicon based composite material of high capacity
Functionization is able in energy storage field.
Nanometer hydrated porous silica or nanoporous silicon oxide particle prepared by method of the invention can be used for efficiently
Absorption or filtering material.Because being easy to low-coat scaleization preparation, it can be used for the necks such as all kinds of water process, solution separation, filtering absorption
Domain.
Nanoporous silicon particle prepared by method of the invention can be used for the preparation of nanoporous silicon nitride material.As incited somebody to action
Nanoporous silicon particle is in nitrogen hydrogen（N2:H2=95:5%）600 DEG C are heated up under atmosphere, 30min；900 DEG C, 30min；1200 DEG C,
60min；1400 DEG C, 60min；It is taken out after being cooled to 100 DEG C, nanoporous silicon nitride material is obtained after ground crushing.
Nanoporous silicon particle prepared by method of the invention can be used for the preparation of nanoporous carbofrax material.As incited somebody to action
Nanoporous silicon particle is containing hydrocarbon argon atmospher（Such as C2H2:Ar=10:90 %）Under be heated up to 600 DEG C, 30min；900 DEG C,
30min；1200 DEG C, 60min；It is taken out after being cooled to 100 DEG C, nanoporous carbofrax material is obtained after ground crushing.
The present invention is improved because using silicon particle waste material caused by the high-purity silicon wafer of industrial-scale production through production technology
Afterwards, nanometer hydrated porous silicon and silicon oxide particle are converted by silicon particle, enables its resource utilization.With semiconductor and too
The development of positive energy photovoltaic industry, generates along with a large amount of silicon particle material, provides guarantee for raw material sources of the invention.This
Invention is with cost of material is extremely low, is easy to large-scale production and application.To be stablized using processing performance of the invention, consistency is good,
With good cost performance.Meanwhile the comprehensive life of semi-conductor silicon chip or photovoltaic silicon wafer can be greatly reduced through the invention
Cost is produced, industry development is effectively facilitated, has opened up a new application technology route for the application of silicon materials.
Claims (7)
1. a kind of preparation method of low cost nanoporous silica ultrafine dust, is cut in deionized water using diamond wire
Generated silicon powder aqueous solution is as raw material after silicon wafer, it is characterised in that：The preparation method is as follows：
（1）The hydration silicon particle that silicon powder aqueous solution is obtained by purification, the size for being hydrated silicon particle is 100 ~ 1000nm；
（2）It is micro- that hydration silicon particle is prepared into nano-structure porous silicon by chemical etching technology in the aqueous solution of hydrofluoric acid and nitric acid
Grain, nano aperture are distributed as 2 ~ 30nm；
（3）Or will hydration silicon particle to prepare nanometer by electrochemical corrosive process in the aqueous solution of hydrofluoric acid and ethyl alcohol more
Hole silicon particle, nano aperture are distributed as 2 ~ 50nm；
（4）The nanoporous silicon oxide particle material of high-specific surface area is prepared after nanoporous silicon particle is directly heated
Material, uses as efficient absorption or filtering material；
The hydration silicon particle is made of purity in 99% or more silicon particle and the hydrone of adsorption, water and silicon
Ratio is 20 ~ 30wt%, is existed in the form of moist.
2. a kind of preparation method of inexpensive nanoporous silica ultrafine dust according to claim 1, feature exist
In：The chemical etching technology be hydration silicon particle in be added hydrofluoric acid containing and nitric acid aqueous solution, hydrofluoric acid, nitric acid and
The percent concentration of water is 20vol%:5 vol%:100 vol%, the proportion for being hydrated silicon particle and acid solution is 10 wt%:1
Wt% reacts 5 ~ 20min under ultrasonic wave effect.
3. a kind of preparation method of inexpensive nanoporous silica ultrafine dust according to claim 1, feature exist
In：The electrochemical corrosive process, using metal platinum filament or piece as the anodic-cathodic of electrochemical capacitor, in hydration silicon particle
The middle aqueous solution that hydrofluoric acid and ethyl alcohol is added, the percent concentration of hydrofluoric acid, ethyl alcohol and water are 3 vol%:1 vol%:5 vol%,
The proportion for being hydrated silicon particle and acid solution is 10 wt%:3wt%；On the electrode plus pulse direct current electric field, current density be 1 ~
30mA/cm2, 1 ~ 5min is reacted in the case where adding ultrasonic wave to act on.
4. a kind of preparation method of inexpensive nanoporous silica ultrafine dust according to claim 1, feature exist
In：The nanoporous silicon particle is used for the energetic material of high-energy density.
5. a kind of preparation method of inexpensive nanoporous silica ultrafine dust according to claim 1, feature exist
In：Electrode material of the nanoporous silicon particle for the rechargeable battery or capacitor of high capacity and high-energy density.
6. a kind of preparation method of inexpensive nanoporous silica ultrafine dust according to claim 1, feature exist
In：The nanoporous silicon particle is directly in nitrogen hydrogen, N2:H2=95%:1400 DEG C of progress nitrogen treatment are heated up under 5% atmosphere
Afterwards, the nanoporous silicon nitride particulate material for preparing high-specific surface area, as high performance ceramic material.
7. a kind of preparation method of inexpensive nanoporous silica ultrafine dust according to claim 1, feature exist
In：The nanoporous silicon particle is directly containing hydrocarbon argon gas, C2H2:Ar=10%:1200 DEG C are heated up under the atmosphere of 90 %
After carrying out carbonization treatment, the nanoporous silicon-carbide particles material of high-specific surface area is prepared, as high performance ceramic material.
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| CN108147412A (en) * | 2018-01-17 | 2018-06-12 | 四川大学 | A kind of method for preparing Fluorin doped cage-shaped nano silicon carbide |
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| CN104650633A (en) * | 2015-02-10 | 2015-05-27 | 吕铁铮 | Preparation method of porous silicone coating |
| CN104701491A (en) * | 2015-03-31 | 2015-06-10 | 吕铁铮 | Nano-porous silica lithium battery anode material and preparation method and application thereof |
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