CN106672975A - Preparation method of low-cost nano-porous silica powder - Google Patents
Preparation method of low-cost nano-porous silica powder Download PDFInfo
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- CN106672975A CN106672975A CN201611185114.3A CN201611185114A CN106672975A CN 106672975 A CN106672975 A CN 106672975A CN 201611185114 A CN201611185114 A CN 201611185114A CN 106672975 A CN106672975 A CN 106672975A
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- silica flour
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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
- C01B33/02—Silicon
- C01B33/021—Preparation
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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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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
- C01P2006/16—Pore diameter
Abstract
The invention discloses a preparation method of low-cost nano-porous silica powder. The method comprises the following steps of etching of silica powder, namely etching the pretreated silica powder by using an etchant, etching for 1-600 minutes to obtain porous silicon containing nanoscale channels, wherein the apertures are 1-1,000nm and the etchant is a mixed solution prepared from HF, a metal salt, ethanol and water; and treatment of the silica powder, soaking the porous silicon containing nanoscale channels into an acid solution for soaking, and cleaning and removing impurities to obtain the nano-porous silica powder. According to the preparation method, the metal salt is introduced as the etchant, and the shape and form, the aperture, the pore-forming speed and the like of the porous silica powder can be controlled through controlling the concentration of a corrosive solution. Preparation of porous silicon is achieved by using reaction heat release at a room temperature, heating equipment is avoided, meanwhile, the reaction speed is high and the porous silicon can be prepared within a few of minutes in general.
Description
Technical field
The present invention relates to porous nano technical field of function materials, and in particular to a kind of system of inexpensive nanoporous silica flour
Preparation Method.
Background technology
When 1956, AT＆T Labs of U.S. Uhlir has found first and reports can be with by electrochemical erosion method
Form porous silicon film.After porous silicon is found, porous silicon is widely used in biology and chemical sensor, and light is urged
Change, the energy, ultracapacitor, bio-imaging, the field such as medicine delivery.
At present, the method for preparing porous silicon that the preparation method of porous silicon has domestic and international appearance has various, but totally can return
Receive as electrochemical method, photochemical corrosion method, etching method and hydrothermal etching.Current more ripe porous silicon preparation method has sun
Pole electrochemical etching method, magnesium reduction process, hydro-thermal method.But anode electrochemical etching method is only applicable to the loose structure system of silicon chip
Standby, not only silicon wafer raw material is expensive, and energy consumption is higher, and the method is not suitable for the preparation of porous silicon powder.
Tongji University Bao Zhihao et al. discloses the method (publication number that a kind of magnesium reduction process prepares porous silicon：CN
102259858A), the method is with oxide S iO of siliconx(x=0.5-2) it is raw material, silicon and oxygen is generated by magnesiothermic reduction reaction
Change the mixture of magnesium, reuse sour selective dissolution and fall magnesium oxide, the final porous silica material for obtaining self-supporting.Although the method
Compared with Anodic caustic solution process is simple, it is to avoid using expensive monocrystalline silicon piece, but its energy consumption of reaction is high, it is lazy to need
Property gas shield causes relatively costly.Therefore, the large-scale application of magnesium reduction process is limited.
Chen Qianwang et al. proposes the technology (publication number that hydro-thermal method prepares porous silicon：CN 1212989A), silica flour is placed in
In autoclave, in the aqueous solution containing 0.1~0.8mol/L fluorions, compactedness is 60%~80%, the oxic gas of regulation system
Atmosphere is 2.0-10.0N/L, is kept for 0.5~2 hour at a temperature of 100 DEG C~250 DEG C.Although this method is compared with additive method letter
Just, but heating-up temperature is higher, while hole is less, pore structure controllability is poor.
The content of the invention
It is an object of the invention to the shortcoming in the preparation of current porous silicon powder, there is provided a kind of inexpensive nanometer is more
The preparation method of hole silica flour, with silica flour as raw material, in HF/Cu (NO3)2In corrosion system, directly etching silica flour forms porous silicon
Powder, in silica flour the hole of porosity, structure-controllable is internally formed.
A kind of preparation method of inexpensive nanoporous silica flour, comprises the following steps：
1) etching of silica flour：The silica flour of pretreatment is performed etching using etching liquid, is obtained through the etching of 1-600min
Porous silicon containing nanoscale duct, aperture is in 1-1000nm；
Described etching liquid is the mixed solution being made up of HF, slaine, second alcohol and water；Described slaine be Cu, Fe,
The nitrate or chlorate of at least one in the soluble-salt of Ag ions, specially Cu, Fe, Ag plasma；
2) process of silica flour：Porous silicon containing nanoscale duct is placed in acid solution and is soaked, it is cleaned afterwards to go
The removal of impurity, obtains nanoporous silica flour.
In the present invention, using HF/ slaine corrosion systems, the etching liquid constituted using HF, slaine, second alcohol and water, draw
Enter metal ion as etching agent, by pattern, aperture, the speed of fulfiling hole of the controllable porous silicon powder of control corrosion rate liquid concentration, lead to
Cross the uniformity that ethanol controls loose structure.(100 are less than under the inventive method realizes room temperature or mild temperature using exothermic heat of reaction
DEG C) prepare porous silicon, it is to avoid expensive firing equipment.Simultaneous reactions speed is quick, can prepare generally in several minutes
Porous silicon.This method has that equipment is simple, the response time is short, easy to operate, low cost, material structure is controllable, adapt to big rule
The advantages such as mould commercial production.
Step 1) in, the preparation of the silica flour of described pretreatment includes：By the silica flour hydrogen of mass percent 5%-40%
Fluoric acid soaks 5min~90min, and afterwards cleaning, drying obtains the silica flour of pretreatment.Further preferably, the particle diameter of described silica flour
Less than or equal to 500 μm.
The concentration of HF is 0.1-25mol/L in described etching liquid, and the concentration of slaine is 0.001-15mol/L, ethanol
Mass fraction be 0.01%-100%.Further preferably, in described etching liquid HF concentration be 2-10mol/L, slaine
Concentration be 0.01-1.5mol/L, the mass fraction of ethanol is 0.2%-4%.
The temperature of described etching is 25 DEG C~100 DEG C.
The process of described etching is using mechanical agitation or magnetic agitation.
Step 2) in, described acid solution is HCl, HF, H2SO4、HNO3In one or more (including two
Kind), acid solution can be single acid or mixed acid.The time of described immersion is 1-24 hours.
Described cleaning goes the removal of impurity to include：First it is cleaned by ultrasonic, is cleaned using deionized water afterwards.
Most preferably, the preparation method of described inexpensive nanoporous silica flour, comprises the following steps：
1) by silica flour hydrofluoric acid dips 10min of mass percent 5%, afterwards cleaning, drying obtains the silicon of pretreatment
Powder；
The particle diameter of described silica flour is less than or equal to 200 μm；
2) etching of silica flour：The silica flour of pretreatment is performed etching using etching liquid, through 25 DEG C, the etching of 20min, is carved
The process of erosion adopts 300r/min magnetic agitation, obtains the porous silicon containing nanoscale duct, and aperture is in 1-1000nm；
Described etching liquid is by HF, Cu (NO3)2, second alcohol and water composition mixed solution, HF in described etching liquid
Concentration is 5mol/L, Cu (NO3)2Concentration be 0.06mol/L, the mass fraction of ethanol is 1%；
2) process of silica flour：Porous silicon containing nanoscale duct is placed in into the HNO of mass percent 10%3Middle immersion,
First it is cleaned by ultrasonic afterwards and again the removal of impurity is gone using deionized water cleaning, obtains nanoporous silica flour.
Compared with prior art, the invention has the advantages that：
The preparation method of low cost nanoporous silica flour of the invention, introduces Cu (NO3)2As etching agent, by control corrosion rate
Pattern, aperture, speed of fulfiling hole of the controllable porous silicon powder of liquid concentration etc..Remaining metal can be removed by pickling, also can be stayed in
Porous silicon powder surface protection silicon, especially can strengthen electric conductivity in lithium cell cathode material application, protect silicon not with electrolyte
Directly contact, so as to improve cyclical stability.Maintain what is corroded to occur so that whole corrosion process using oxidation reaction heat release
Carry out under the conditions of room temperature or mild temperature.This law is kept away compared to methods such as traditional Anodic etching method, magnesiothermic reductions
High energy consumption caused by high temperature, expensive high-temperature service and complex operations are exempted from.Present method be advantageous in that using exothermic heat of reaction reality
Under existing room temperature prepare porous silicon, it is to avoid firing equipment.Simultaneous reactions speed is quick, can prepare generally in several minutes many
Hole silicon.This method has that equipment is simple, the response time is short, easy to operate, low cost, material structure is controllable, adapt to extensive
The advantages such as commercial production.The method has that equipment is simple, the response time is short, processing ease, low cost, material structure are controllable, suitable
The advantages of closing scale industrial production, can be in the field exhibition such as lithium ion battery, photoelectric material, biomedicine, explosive and sensor
Existing wide application prospect.
Description of the drawings
Fig. 1 be embodiment 1 prepare the porous silicon with nano-pore SEM pictures, wherein amplification for ×
50K。
Specific embodiment
Technical scheme is discussed in detail below by instantiation, but the present invention is not limited to embodiment, below
Example is only limitted to explain the present invention that protection scope of the present invention should include all the elements in claims.
If no special instructions, the percent for occurring in the embodiment of the present invention is mass percent.
Embodiment 1
The preparation method of porous silicon described in the present embodiment, specifically includes following steps：
(1) pretreatment of silica flour：The Fluohydric acid. that silica flour (metallurgical grade silicon, particle diameter is less than or equal to 500 μm) is used into 5wt% is (i.e.
Mass percent is 5%HF aqueous solutions) soaking and washing 10min, deionized water is cleaned 3 times after filtration, drying；
(2) etching of silica flour：Silica flour is placed in into HF, Cu (NO3)2, second alcohol and water composition mixed solution in, mix it is molten
The concentration of HF is 5mol/L, Cu (NO in liquid3)2Concentration be 0.06mol/L, the mass percent of ethanol is 1%, in room temperature 25
20min is reacted at DEG C, while carrying out magnetic agitation (mixing speed is 300r/min), porous silicon grain is obtained；
(3) process of silica flour：The porous silicon grain obtained in (2) step is placed in into immersion 1 in 10% aqueous solution of nitric acid little
When (mass percent of aqueous solution of nitric acid be 10%), while carrying out ultrasonic cleaning to porous silicon goes the removal of impurity, obtain porous silicon.
(4) cleaning of porous silicon：The porous silicon deionized water obtained in (3) is cleaned 3 times, drying is to porous
Silicon.
Embodiment 2
The preparation method of porous silicon described in the present embodiment, specifically includes following steps：
(1) pretreatment of silica flour：By silica flour (metallurgical grade silicon) HF soaking and washings 10min of 5wt%, spend after filtration from
Sub- water is cleaned 3 times, drying；
(2) etching of silica flour：Silica flour is placed in into HF, Cu (NO3)2, second alcohol and water composition mixed solution in, mix it is molten
The concentration of HF is 5mol/L, Cu (NO in liquid3)2Concentration be 0.12mol/L, ethanol is 10%, is reacted at 25 DEG C of room temperature
20min, while carrying out magnetic agitation (mixing speed is 300r/min), obtains porous silicon grain；
(3) process of silica flour：The porous silicon grain obtained in (2) step is placed in 10% salpeter solution and is soaked 1 hour,
Simultaneously carrying out ultrasonic cleaning to porous silicon goes the removal of impurity, obtains porous silicon.
(4) cleaning of porous silicon：The porous silicon deionized water obtained in (3) is cleaned 3 times, drying is to porous
Silicon.
Embodiment 3
The preparation method of porous silicon described in the present embodiment, specifically includes following steps：
(1) pretreatment of silica flour：By silica flour (metallurgical grade silicon) HF soaking and washings 10min of 5wt%, spend after filtration from
Sub- water is cleaned 3 times, drying；
(2) etching of silica flour：Silica flour is placed in into HF, Fe (NO3)3, second alcohol and water composition mixed solution in, mix it is molten
The concentration of HF is 5mol/L, Fe (NO in liquid3)3Concentration be 0.24mol/L, ethanol is 15%, is reacted at 25 DEG C of room temperature
30min, while carrying out magnetic agitation (mixing speed is 300r/min), obtains porous silicon grain；
(3) process of silica flour：The porous silicon grain obtained in (2) step is placed in into immersion 1 in 10% aqueous solution of nitric acid little
When, while carrying out ultrasonic cleaning to porous silicon goes the removal of impurity, obtain porous silicon.
(4) cleaning of porous silicon：The porous silicon deionized water obtained in (3) is cleaned 3 times, drying is to porous
Silicon.
Embodiment 4
The preparation method of porous silicon described in the present embodiment, specifically includes following steps：
(1) pretreatment of silica flour：By silica flour (metallurgical grade silicon) HF soaking and washings 10min of 10wt%, spend after filtration
Ionized water is cleaned 3 times, drying；
(2) etching of silica flour：Silica flour is placed in into HF, Fe (NO3)3, second alcohol and water composition mixed solution in, mix it is molten
The concentration of HF is 10mol/L, Fe (NO in liquid3)3Concentration be 0.06mol/L, ethanol is 30%, under 50 DEG C of water-baths react
20min, while carrying out magnetic agitation (mixing speed is 300r/min), obtains porous silicon grain；
(3) process of silica flour：The porous silicon grain obtained in (2) step is placed in into 10% nitric acid and 2.5%HF mixed acid
(mass percent of nitric acid is 10% i.e. in mixed acid, and the mass percent of HF is 2.5%) middle immersion 1 hour in mixed acid,
Simultaneously carrying out ultrasonic cleaning to porous silicon goes the removal of impurity, obtains porous silicon.
(4) cleaning of porous silicon：The porous silicon deionized water obtained in (3) is cleaned 3 times, drying is to porous
Silicon.
Embodiment 5
The preparation method of porous silicon described in the present embodiment, specifically includes following steps：
(1) pretreatment of silica flour：By silica flour (metallurgical grade silicon) HF soaking and washings 60min of 10wt%, spend after filtration
Ionized water is cleaned 3 times, drying；
(2) etching of silica flour：Silica flour is placed in into HF, AgNO3, second alcohol and water composition mixed solution in, in mixed solution
The concentration of middle HF is 10mol/L, AgNO3Concentration be 0.12mol/L, ethanol is 35%, and under 50 DEG C of water-baths 10min is reacted,
Simultaneously magnetic agitation (mixing speed is 300r/min) is carried out, obtain porous silicon grain；
(3) process of silica flour：The porous silicon grain obtained in (2) step is placed in into 10% nitric acid and 2.5%HF mixed acid
(mass percent of nitric acid is 10% i.e. in mixed acid, and the mass percent of HF is 2.5%) middle immersion 1 hour in mixed acid,
Simultaneously carrying out ultrasonic cleaning to porous silicon goes the removal of impurity, obtains porous silicon.
(4) cleaning of porous silicon：The porous silicon deionized water obtained in (3) is cleaned 3 times, drying is to porous
Silicon.
Embodiment 6
The preparation method of porous silicon described in the present embodiment, specifically includes following steps：
(1) pretreatment of silica flour：By silica flour (metallurgical grade silicon) HF soaking and washings 60min of 10wt%, spend after filtration
Ionized water is cleaned 3 times, drying；
(2) etching of silica flour：Silica flour is placed in into HF, AgNO3, second alcohol and water composition mixed solution in, in mixed solution
The concentration of middle HF is 10mol/L, AgNO3Concentration be 0.24mol/L, ethanol is 5%, 1min is reacted under 50 DEG C of water-baths, together
Shi Jinhang magnetic agitation (mixing speed is 300r/min), obtains porous silicon grain；
(3) process of silica flour：The porous silicon grain obtained in (2) step is placed in into 10% nitric acid and 2.5%HF mixed acid
(mass percent of nitric acid is 10% i.e. in mixed acid, and the mass percent of HF is 2.5%) middle immersion 1 hour in mixed acid,
Simultaneously carrying out ultrasonic cleaning to porous silicon goes the removal of impurity, obtains porous silicon.
(4) cleaning of porous silicon：The porous silicon deionized water obtained in (3) is cleaned 3 times, drying is to porous
Silicon.
Claims (9)
1. a kind of preparation method of inexpensive nanoporous silica flour, it is characterised in that comprise the following steps：
1) etching of silica flour：The silica flour of pretreatment is performed etching using etching liquid, is contained through the etching of 1-600min
The porous silicon in nanoscale duct, aperture is in 1-1000nm；
Described etching liquid is the mixed solution being made up of HF, slaine, second alcohol and water, described slaine be Cu, Fe, Ag from
At least one in the soluble-salt of son；
2) process of silica flour：Porous silicon containing nanoscale duct is placed in acidic aqueous solution and is soaked, cleaned removal afterwards
Impurity, obtains nanoporous silica flour.
2. the preparation method of inexpensive nanoporous silica flour according to claim 1, it is characterised in that step 1) in, institute
The preparation of the silica flour of the pretreatment stated includes：By the silica flour hydrofluoric acid dips 5min~90min of mass percent 5%-40%,
Afterwards cleaning, drying obtains the silica flour of pretreatment.
3. the preparation method of inexpensive nanoporous silica flour according to claim 2, it is characterised in that step 1) in, institute
The particle diameter of the silica flour stated is less than or equal to 500 μm.
4. the preparation method of inexpensive nanoporous silica flour according to claim 1, it is characterised in that step 1) in, institute
The concentration of HF is 0.1-25mol/L in the etching liquid stated, and the concentration of slaine is 0.001-15mol/L, the mass fraction of ethanol
For 0.01%-100%.
5. the preparation method of inexpensive nanoporous silica flour according to claim 1, it is characterised in that step 2) in, institute
The temperature of the etching stated is 25 DEG C~100 DEG C.
6. the preparation method of inexpensive nanoporous silica flour according to claim 1, it is characterised in that step 2) in, institute
The process of the etching stated is using mechanical agitation or magnetic agitation.
7. the preparation method of inexpensive nanoporous silica flour according to claim 1, it is characterised in that step 2) in, institute
The acidic aqueous solution stated is HCl, HF, H2SO4、HNO3In one or more.
8. the preparation method of inexpensive nanoporous silica flour according to claim 1, it is characterised in that step 2) in, institute
The time of the immersion stated is 1-24 hours.
9. the preparation method of inexpensive nanoporous silica flour according to claim 1, it is characterised in that step 2) in, institute
The cleaning stated goes the removal of impurity to include：First it is cleaned by ultrasonic, is cleaned using deionized water afterwards.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108328619A (en) * | 2018-03-29 | 2018-07-27 | 昆明理工大学 | A kind of method that industrial silicon hydrometallurgy removes boron |
| CN108483448A (en) * | 2018-06-20 | 2018-09-04 | 贵州大学 | A kind of porous silicon preparation method |
| CN109422251A (en) * | 2017-08-22 | 2019-03-05 | 新特能源股份有限公司 | Silicon powder for fluidized reaction and preparation method thereof, silicon nitride and its production method |
| CN110143593A (en) * | 2019-04-29 | 2019-08-20 | 浙江大学 | Preparation method, porous silicon powder and its application of porous silicon powder |
| CN110931727A (en) * | 2019-10-25 | 2020-03-27 | 合肥国轩高科动力能源有限公司 | Preparation method of conductive polymer-coated silicon-based negative electrode material |
| CN114988413A (en) * | 2022-05-05 | 2022-09-02 | 昆明理工大学 | Method for preparing high-purity porous silicon |
| CN116162008A (en) * | 2023-01-18 | 2023-05-26 | 贵州梅岭电源有限公司 | Heating material for miniaturized rapid-activation thermal battery and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109422251A (en) * | 2017-08-22 | 2019-03-05 | 新特能源股份有限公司 | Silicon powder for fluidized reaction and preparation method thereof, silicon nitride and its production method |
| CN108328619A (en) * | 2018-03-29 | 2018-07-27 | 昆明理工大学 | A kind of method that industrial silicon hydrometallurgy removes boron |
| CN108483448A (en) * | 2018-06-20 | 2018-09-04 | 贵州大学 | A kind of porous silicon preparation method |
| CN110143593A (en) * | 2019-04-29 | 2019-08-20 | 浙江大学 | Preparation method, porous silicon powder and its application of porous silicon powder |
| CN110931727A (en) * | 2019-10-25 | 2020-03-27 | 合肥国轩高科动力能源有限公司 | Preparation method of conductive polymer-coated silicon-based negative electrode material |
| CN114988413A (en) * | 2022-05-05 | 2022-09-02 | 昆明理工大学 | Method for preparing high-purity porous silicon |
| CN114988413B (en) * | 2022-05-05 | 2024-03-15 | 昆明理工大学 | Method for preparing high-purity porous silicon |
| CN116162008A (en) * | 2023-01-18 | 2023-05-26 | 贵州梅岭电源有限公司 | Heating material for miniaturized rapid-activation thermal battery and preparation method thereof |
| CN116162008B (en) * | 2023-01-18 | 2024-04-09 | 贵州梅岭电源有限公司 | Heating material for miniaturized rapid-activation thermal battery and preparation method thereof |
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Application publication date: 20170517 |