CN113149016B - Preparation method of high-purity spherical nanometer silicon powder with adjustable particle size - Google Patents
Preparation method of high-purity spherical nanometer silicon powder with adjustable particle size Download PDFInfo
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- CN113149016B CN113149016B CN202110205670.7A CN202110205670A CN113149016B CN 113149016 B CN113149016 B CN 113149016B CN 202110205670 A CN202110205670 A CN 202110205670A CN 113149016 B CN113149016 B CN 113149016B
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 168
- 239000011863 silicon-based powder Substances 0.000 title claims abstract description 95
- 239000002245 particle Substances 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 104
- 238000004519 manufacturing process Methods 0.000 claims abstract description 56
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000001816 cooling Methods 0.000 claims abstract description 36
- 239000011261 inert gas Substances 0.000 claims abstract description 34
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 21
- 230000009471 action Effects 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims description 48
- 239000002994 raw material Substances 0.000 claims description 48
- 229910052710 silicon Inorganic materials 0.000 claims description 42
- 239000010703 silicon Substances 0.000 claims description 42
- 239000012535 impurity Substances 0.000 claims description 38
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 20
- 238000000227 grinding Methods 0.000 claims description 19
- 239000002904 solvent Substances 0.000 claims description 13
- 239000011575 calcium Substances 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 9
- 229910052782 aluminium Inorganic materials 0.000 claims description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 9
- 229910052791 calcium Inorganic materials 0.000 claims description 9
- 229910052742 iron Inorganic materials 0.000 claims description 9
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 8
- 238000005520 cutting process Methods 0.000 claims description 8
- 229910052698 phosphorus Inorganic materials 0.000 claims description 8
- 239000011574 phosphorus Substances 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- 239000004576 sand Substances 0.000 claims description 8
- 238000012546 transfer Methods 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 4
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229920000570 polyether Polymers 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 230000006870 function Effects 0.000 claims description 2
- 238000003801 milling Methods 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 230000005674 electromagnetic induction Effects 0.000 abstract description 11
- 230000000694 effects Effects 0.000 abstract description 9
- 239000007789 gas Substances 0.000 abstract description 7
- 239000007787 solid Substances 0.000 abstract description 7
- 230000005284 excitation Effects 0.000 abstract description 5
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 description 33
- 239000004005 microsphere Substances 0.000 description 30
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 24
- 230000007613 environmental effect Effects 0.000 description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 12
- 229910052786 argon Inorganic materials 0.000 description 12
- 239000000463 material Substances 0.000 description 9
- 230000001105 regulatory effect Effects 0.000 description 9
- 230000006698 induction Effects 0.000 description 7
- 230000001276 controlling effect Effects 0.000 description 5
- 230000005389 magnetism Effects 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- 239000011324 bead Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229910000077 silane Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000006978 adaptation Effects 0.000 description 2
- 229910021417 amorphous silicon Inorganic materials 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 229910021419 crystalline silicon Inorganic materials 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000007158 vacuum pyrolysis Methods 0.000 description 2
- 238000010146 3D printing Methods 0.000 description 1
- -1 3D printing Substances 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910021418 black silicon Inorganic materials 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
Classifications
-
- 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
- C01B33/037—Purification
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention provides a preparation method of spherical nano silicon, which comprises the following steps of under the action of electromagnetic waves, under the condition of nitrogen and/or inert gas, spheroidizing suspended silicon powder, and cooling to obtain the spherical nano silicon. According to the invention, nanoscale silicon powder is dispersed from inert gas into an electromagnetic induction cavity, the resonance effect generated by microwaves is utilized to act on the inert gas, the gas is partially ionized under the excitation action of electromagnetic induction, a higher temperature is generated, heat is transferred to the surface of the silicon powder, the surface of the silicon powder reaches a solid-liquid coexisting state, the silicon powder forms a sphere due to the action of surface tension, and then the spherical nano silicon powder is rapidly cooled after entering a cooling cavity, so that solid spherical nano silicon powder with uniform granularity is formed; and the spherical nanometer silicon powder with controllable granularity can be obtained by adjusting the particle size of the introduced nanometer silicon powder and controlling the input power of microwaves. The invention has high production efficiency, lower power consumption and production cost and is more suitable for large-scale production and application.
Description
Technical Field
The invention belongs to the technical field of preparation of spherical nano silicon materials, relates to a preparation method of spherical nano silicon, and particularly relates to a preparation method of high-purity spherical nano silicon powder with adjustable particle size.
Background
Silicon is a very common element, with both amorphous and crystalline silicon allotropes. Crystalline silicon is gray black and amorphous silicon is black. Silicon is an important material for manufacturing glass, quartz glass, water glass, optical fibers, important parts of the electronic industry, optical instruments, artworks and refractory materials, and is also an important material for scientific research, particularly in recent years, along with the rapid development of the electronic industry, the silicon industry also develops vigorously. The spherical nanometer silicon powder is mainly used in the fields of lithium battery cathode materials, 3D printing, electronic materials and the like, and has wide market prospect. However, the preparation of the high-purity spherical silica powder is a interdisciplinary high-difficulty engineering, and the existing method for preparing the nano silica powder mainly comprises a mechanical ball milling method, a vapor phase chemical deposition method, a plasma evaporation condensation method and the like. However, for spherical nano silicon powder, particularly high-purity spherical nano silicon powder with precisely controllable particle size, the current method capable of realizing low-cost large-scale production is less.
In the prior art, the mechanical ball milling method has lower cost, but the granularity is reduced mainly by physical grinding, so spherical nano silicon powder cannot be obtained; the vapor deposition method takes silane as a raw material and is generated by reaction in a vapor environment, but the silane has stronger toxicity, so the silane has larger safety and environmental hidden trouble; plasma evaporative condensing methods generally use arc plasma methods and radio frequency induction (RF) plasma methods; according to the arc plasma method, as disclosed in the patent publication No. CN102910630A, a power electrode contacts a heat source in the heating process, so that a certain pollution is generated to the prepared material; the rf induction plasma method, such as CN203333311U, adopts an electrodeless method, avoids contact between the electrode and the heat source, and although the electrode and the heat source do not pollute the prepared material, the discharge process generates a high-voltage sheath layer and ion wall sputtering pollution caused by the high-voltage sheath layer, and the rf induction frequency is generally MHz-level, so that the frequency is lower, the power supply working power is generally higher, the power consumption is higher in mass production, and the cost is relatively higher.
Therefore, how to find a more suitable preparation method of spherical nano-silicon, which can prepare spherical nano-silicon with higher purity and controllable granularity, is more beneficial to industrialized implementation, and is one of the problems to be solved by a plurality of first-line researchers in the field.
Disclosure of Invention
In view of the above, the technical problem to be solved by the invention is to provide a preparation method of nano silicon, in particular to a preparation method of spherical nano silicon.
The invention provides a preparation method of spherical nano-silicon, which comprises the following steps,
a) Under the action of electromagnetic waves, under the condition of nitrogen and/or inert gas, the suspended silicon powder is sphericized and cooled to obtain spherical nano silicon.
Preferably, the electromagnetic wave includes one or more of microwave, ultrashort wave and short wave;
the pressure of the nitrogen and/or inert gas is 10 Pa-0.12 Mpa;
the concentration of the silicon powder suspended in the nitrogen and/or inert gas is 0.1-1 g/m 3 。
Preferably, the electromagnetic wave has the function of ionizing nitrogen and/or inert gas;
ionized nitrogen and/or inert gas can generate corresponding electron temperature and transfer heat to the surface of the silicon powder;
the wavelength of the electromagnetic wave is 0.001-10 m.
Preferably, the spheroidization time is 0.1 to 3s;
the temperature of the spheroidization is 500-2500 ℃;
the silicon powder comprises nanoscale silicon powder;
the particle size of the spherical nano-silicon can be regulated and controlled by regulating the power of the electromagnetic wave.
Preferably, the specific process of sphericizing is as follows:
the suspended silicon powder forms a solid-liquid coexisting state and forms a sphere under the action of surface tension;
the cooling mode comprises one or more of water cooling, air cooling and natural cooling;
the specific steps of cooling comprise air cooling and water cooling.
Preferably, the silicon powder is ground and decontaminated from raw material silicon;
the purity of the raw material silicon is 99.9-99.9999%;
the silicon powder comprises high-purity silicon powder;
the purity of the silicon powder is 99.9% -99.999%;
the grinding mode comprises one or more of wet ball milling, wet sand milling and wet wire cutting grinding.
Preferably, the raw silicon includes a silicon block;
the iron content of the raw material silicon is less than or equal to 0.01%;
the aluminum content of the raw material silicon is less than or equal to 0.01%;
the phosphorus content of the raw material silicon is less than or equal to 50ppm;
the calcium content of the raw material silicon is less than or equal to 0.01 percent.
Preferably, the granularity of the ground raw material silicon powder is 50-1000 nm;
the specific steps of impurity removal are as follows:
mixing the ground raw material silicon powder with a solvent, and performing magnetic field impurity removal and high-temperature impurity removal to obtain silicon powder;
the solvent comprises one or more of water, ethanol, acetone, isopropanol, polyethylene glycol and polyether.
Preferably, the magnetic field intensity of the magnetic field impurity removal is 1-10 tesla;
the time for removing impurities in the magnetic field is 0.1-3 s;
the high-temperature impurity removal temperature is 500-1000 ℃;
the high-temperature impurity removal time is 30-60 min.
Preferably, the particle size of the spherical nano silicon is 20-700 nm;
the purity of the spherical nano silicon is 99.9-99.999%.
The invention provides a preparation method of spherical nano silicon, which comprises the following steps of under the action of electromagnetic waves, under the condition of nitrogen and/or inert gas, spheroidizing suspended silicon powder, and cooling to obtain the spherical nano silicon. Compared with the prior art, the preparation method aims at the problems that the purity and the particle size are difficult to control, the process is not environment-friendly, the cost is high and the like in the existing preparation method of the spherical nano silicon.
According to the invention, nanoscale silicon powder is creatively sent into the electromagnetic induction cavity from inert gas, the resonance effect generated by microwaves is utilized to act on the inert gas, the inert gas is partially ionized under the excitation of electromagnetic induction of the microwaves, higher electron temperature is generated, heat is transferred to the surface of the silicon powder, the nanoscale silicon powder reaches a solid-liquid coexisting state, the nanoscale silicon powder forms a sphere due to the action of surface tension, and then the spherical nanoscale silicon powder is rapidly cooled after entering the cooling cavity, so that solid spherical nanoscale silicon powder with uniform granularity is formed. And the spherical nanometer silicon powder with controllable granularity can be obtained by adjusting the particle size of the introduced nanometer silicon powder and controlling the input power of a microwave source. The spherical nanometer silicon powder prepared by the method avoids the pollution of impurities to the silicon powder in the preparation process, has higher purity, uniform granularity, adjustable size and good sphericity. Meanwhile, the preparation method provided by the invention is simple and environment-friendly, and the microwave has high frequency and short wavelength, and compared with radio frequency induction and the like, the microwave induction temperature is lower, generally about 500-2500 ℃, so that the preparation method has high production efficiency, lower power consumption and production cost and is more suitable for large-scale production and application.
Experimental results show that the purity of the spherical nano silicon prepared by the method can reach more than 99.9%, the impurity elements Fe <100ppm, al <100ppm, P <30ppm and Ca <60ppm, and the impurity content can not be increased in the reaction process.
Drawings
FIG. 1 is a scanning electron microscope image of spherical nano silicon powder prepared by the invention.
Detailed Description
For a further understanding of the present invention, preferred embodiments of the invention are described below in conjunction with the examples, but it should be understood that these descriptions are merely intended to illustrate further features and advantages of the invention and are not limiting of the invention claims.
All the raw materials of the present invention are not particularly limited in their sources, and may be purchased on the market or prepared according to conventional methods well known to those skilled in the art.
All raw materials of the present invention are not particularly limited in purity, and the present invention is preferably prepared with conventional purity of analytically pure or high-purity spherical nano-silicon.
All raw materials of the invention, the brands and abbreviations of which belong to the conventional brands and abbreviations in the field of the related application are clear and definite, and the person skilled in the art can purchase from the market or prepare by the conventional method according to the brands, abbreviations and the corresponding application.
In all processes of the present invention, the abbreviations thereof are conventional in the art, each abbreviation is clearly understood in the art of its associated use, and the skilled artisan will understand the conventional process steps thereof based on the abbreviations.
The invention provides a preparation method of spherical nano-silicon, which comprises the following steps,
a) Under the action of electromagnetic waves, under the condition of nitrogen and/or inert gas, the suspended silicon powder is sphericized and cooled to obtain spherical nano silicon.
The invention is in principle not particularly limited to the types and parameters of the electromagnetic waves, and a person skilled in the art can select the electromagnetic waves according to actual production conditions, quality requirements and product requirements. The wavelength of the electromagnetic wave is preferably 0.001 to 10m (meter), more preferably 0.005 to 8m, still more preferably 0.01 to 5m, still more preferably 0.05 to 3m, still more preferably 0.08 to 2m, and particularly may be 0.1 to 1m.
The invention is in principle not particularly limited to the specific effect of the electromagnetic wave, and a person skilled in the art can select according to actual production conditions, quality requirements and product requirements.
The invention is in the whole and refined whole preparation industry, in order to improve the purity of the spherical nano-silicon microsphere, ensure the spherical nano-silicon microsphere to have more uniform particle size, ensure the controllable particle size and the reaction process, increase the environmental protection and the safety, and be easier to realize large-scale low-cost mass production, preferably, ionized nitrogen and/or inert gas can generate corresponding electron temperature and transfer heat to the surface of silicon powder, and more preferably, ionized nitrogen or inert gas can generate corresponding electron temperature and transfer heat to the surface of silicon powder.
The pressure of the nitrogen and/or inert gas is not particularly limited in principle, and can be selected by a person skilled in the art according to actual production conditions, quality requirements and product requirements, so that the spherical nano-silicon microsphere has more uniform particle size, controllable particle size and reaction process are ensured, environmental protection and safety are improved, and large-scale low-cost mass production is easier to realize, wherein the pressure of the nitrogen and/or inert gas is preferably 10 Pa-0.12 Mpa, more preferably 0.05-50 Kpa, more preferably 0.1-10 Kpa, more preferably 0.5-5 Kpa, and more preferably 1-3 Kpa.
The concentration of the silicon powder suspended in the nitrogen and/or inert gas is not particularly limited in principle, and can be selected by a person skilled in the art according to actual production conditions, quality requirements and product requirements 3 More preferably 0.3 to 0.8g/m 3 More preferably 0.5 to 0.6g/m 3 。
The invention is not particularly limited in principle, the spheroidization time can be selected by a person skilled in the art according to actual production conditions, quality requirements and product requirements, and the invention aims to improve the purity of the spherical nano-silicon microsphere, ensure that the spherical nano-silicon microsphere has more uniform particle size, ensure controllable particle size and reaction process, increase environmental protection and safety, and be easier to realize large-scale low-cost mass production, wherein the spheroidization time is preferably 0.1-3 s, more preferably 0.5-2.5 s, and more preferably 1-2 s.
The invention is in principle not particularly limited to the spheroidization temperature, and a person skilled in the art can select according to actual production conditions, quality requirements and product requirements, and in order to improve the purity of the spherical nano-silicon microsphere, the spherical nano-silicon microsphere has more uniform particle size, ensures controllable particle size and reaction process, increases environmental protection and safety, and is easier to realize large-scale low-cost mass production, the spheroidization temperature is preferably 500-2500 ℃, more preferably 700-2000 ℃, and even more preferably 900-1800 ℃.
The method is in principle not particularly limited to the specific selection of the silicon powder, and a person skilled in the art can select the silicon powder according to actual production conditions, quality requirements and product requirements.
The invention is a complete and refined whole preparation scheme, and in order to improve the purity of the spherical nano-silicon microsphere, the spherical nano-silicon microsphere has more uniform particle size, the controllable particle size and the controllable reaction process are ensured, the environmental protection and the safety are improved, the large-scale low-cost mass production is easier to realize, the particle size of the spherical nano-silicon can be regulated and controlled by preferably regulating the power of the electromagnetic wave, and the particle size of the spherical nano-silicon can be regulated and controlled by preferably regulating the power of the electromagnetic wave and/or the particle size of silicon powder.
The invention is a complete and refined integral preparation process, the purity of the spherical nano-silicon microsphere is better improved, so that the spherical nano-silicon microsphere has more uniform particle size, the controllable particle size and the controllable reaction process are ensured, the environment friendliness and the safety are improved, the large-scale low-cost mass production is easier to realize, and the specific process of sphericizing is preferably as follows:
the suspended silicon powder forms a solid-liquid coexisting state and forms a sphere under the action of surface tension.
In the present invention, the suspended silicon powder is brought into a solid-liquid coexisting state, and preferably, the surface of the suspended silicon powder is brought into a molten state. That is, the suspended silicon powder is solid inside and molten liquid on the surface, and the solid-liquid coexisting state is established.
The method of cooling is not particularly limited in principle, and a person skilled in the art can select according to actual production conditions, quality requirements and product requirements, so that the spherical nano-silicon microsphere has more uniform particle size, controllable particle size and reaction process are ensured, environmental friendliness and safety are improved, and large-scale low-cost mass production is easier to realize.
The invention is a complete and refined whole preparation scheme, the purity of the spherical nano-silicon microsphere is better improved, so that the spherical nano-silicon microsphere has more uniform particle size, the controllable particle size and the controllable reaction process are ensured, the environment friendliness and the safety are improved, the large-scale low-cost mass production is easier to realize, the specific steps of cooling can be firstly air cooling and then water cooling, and the specific steps can be as follows:
the nano silicon particles are cooled by dispersing air (air cooling) and then further cooled by water.
The cooling time of the dispersion gas is preferably 5 to 10 seconds, more preferably 6 to 9 seconds, and still more preferably 7 to 8 seconds. When the temperature of the cooling of the dispersion gas is preferably 200 ℃ or higher, it may be 180 ℃ or higher or 160 ℃ or higher. The water cooling is specifically cooling to below 20 ℃.
The method is characterized in that the silicon powder is prepared from silicon powder, silicon powder and a solvent, wherein the silicon powder is prepared from silicon powder, a solvent and a solvent, and the solvent is selected from silicon powder, a solvent and a solvent according to the actual production condition, quality requirements and product requirements.
The method is in principle not particularly limited to the purity of the raw material silicon, and a person skilled in the art can select the raw material silicon according to actual production conditions, quality requirements and product requirements, so that the spherical nano-silicon microsphere has more uniform particle size, controllable particle size and reaction process are ensured, environmental friendliness and safety are improved, large-scale low-cost mass production is easier to realize, and the purity of the raw material silicon is preferably 99.9% -99.9999%, more preferably 99.95% -99.9995%, 99.99% -99.999% and 99.993% -99.997%.
The invention is in principle not particularly limited to the morphology of the raw material silicon, and a person skilled in the art can select the raw material silicon according to actual production conditions, quality requirements and product requirements.
The invention is in principle not particularly limited to the iron content of the raw material silicon, and a person skilled in the art can select the raw material silicon according to actual production conditions, quality requirements and product requirements, and in order to improve the purity of the spherical nano-silicon microsphere, the spherical nano-silicon microsphere has more uniform particle size, ensures controllable particle size and reaction process, increases environmental protection and safety, and is easier to realize large-scale low-cost mass production, wherein the iron content of the raw material silicon is preferably less than or equal to 0.1%, more preferably less than or equal to 0.05%, and more preferably less than or equal to 0.03%.
The method is in principle not particularly limited to the aluminum content of the raw material silicon, and a person skilled in the art can select the raw material silicon according to actual production conditions, quality requirements and product requirements, and in order to improve the purity of the spherical nano-silicon microsphere, the spherical nano-silicon microsphere has more uniform particle size, controllable particle size and reaction process are ensured, environmental protection and safety are improved, and large-scale low-cost mass production is easier to realize, wherein the aluminum content of the raw material silicon is preferably less than or equal to 0.1%, more preferably less than or equal to 0.05%, and more preferably less than or equal to 0.03%.
The invention is in principle not particularly limited to the phosphorus content of the raw material silicon, and a person skilled in the art can select the raw material silicon according to actual production conditions, quality requirements and product requirements.
The method is in principle not particularly limited to the calcium content of the raw material silicon, and a person skilled in the art can select the raw material silicon according to actual production conditions, quality requirements and product requirements, and in order to improve the purity of the spherical nano-silicon microsphere, the spherical nano-silicon microsphere has more uniform particle size, ensures controllable particle size and reaction process, increases environmental protection and safety, and is easier to realize large-scale low-cost mass production, wherein the calcium content of the raw material silicon is preferably less than or equal to 0.01%, more preferably less than or equal to 0.008%, and more preferably less than or equal to 0.005%.
The method is in principle not particularly limited to the purity of the silicon powder, and a person skilled in the art can select the silicon powder according to actual production conditions, quality requirements and product requirements. Specifically, the purity of the silicon powder is preferably 99.9% -99.999%, more preferably 99.95% -99.995%, and even more preferably 99.97% -99.99%.
The grinding mode is not particularly limited in principle, and can be selected by a person skilled in the art according to actual production conditions, quality requirements and product requirements, so that the spherical nano-silicon microsphere has more uniform particle size, controllable particle size and reaction process are ensured, environmental friendliness and safety are improved, and large-scale low-cost mass production is easier to realize.
The particle size of the ground raw silicon powder is not particularly limited in principle, and can be selected by a person skilled in the art according to actual production conditions, quality requirements and product requirements, so that the spherical nano silicon microsphere has more uniform particle size, controllable particle size and reaction process are ensured, environmental friendliness and safety are improved, and large-scale low-cost mass production is easier to realize, and the particle size of the ground raw silicon powder is preferably 50-1000 nm, more preferably 200-800 nm, and even more preferably 400-600 nm.
The specific steps of the impurity removal are not particularly limited in principle, and can be selected by a person skilled in the art according to actual production conditions, quality requirements and product requirements, and the specific steps of the impurity removal are preferably as follows:
mixing the ground raw material silicon powder with a solvent, and performing magnetic field impurity removal and high-temperature impurity removal to obtain the silicon powder.
The specific choice of the solvent is not particularly limited in principle, and a person skilled in the art can choose the solvent according to actual production conditions, quality requirements and product requirements, so that the spherical nano-silicon microsphere has more uniform particle size, controllable particle size and reaction process are ensured, environmental friendliness and safety are improved, and large-scale low-cost mass production is easier to realize.
The invention is in principle not particularly limited to the magnetic field intensity of the magnetic field impurity removal, and a person skilled in the art can select the magnetic field intensity according to actual production conditions, quality requirements and product requirements.
The invention is in principle not particularly limited to the time for removing impurities in the magnetic field, and a person skilled in the art can select the magnetic field according to actual production conditions, quality requirements and product requirements.
The high-temperature impurity removal temperature is not particularly limited in principle, and can be selected by a person skilled in the art according to actual production conditions, quality requirements and product requirements, so that the spherical nano-silicon microsphere has more uniform particle size, controllable particle size and reaction process are ensured, environmental friendliness and safety are improved, large-scale low-cost mass production is easier to realize, the high-temperature impurity removal temperature is preferably 500-1000 ℃, more preferably 600-900 ℃, and more preferably 700-800 ℃.
The invention is in principle not particularly limited to the high-temperature impurity removal time, and a person skilled in the art can select according to actual production conditions, quality requirements and product requirements.
The particle size of the spherical nano-silicon is not particularly limited in principle, and can be selected by a person skilled in the art according to actual production conditions, quality requirements and product requirements, so that the spherical nano-silicon microsphere has more uniform particle size, controllable particle size and reaction process are ensured, environmental friendliness and safety are improved, and large-scale low-cost mass production is easier to realize, wherein the particle size of the spherical nano-silicon is preferably 20-700 nm, more preferably 70-600 nm, more preferably 80-500 nm, and more preferably 120-400 nm.
The method is in principle not particularly limited to the purity of the spherical nano silicon, and a person skilled in the art can select the spherical nano silicon microsphere according to actual production conditions, quality requirements and product requirements, so that the spherical nano silicon microsphere has more uniform particle size, controllable particle size and reaction process are ensured, environmental friendliness and safety are improved, large-scale low-cost mass production is easier to realize, and the purity of the spherical nano silicon is preferably 99.9% -99.999%, more preferably 99.95% -99.995%, and even more preferably 99.97% -99.99%.
The invention is a complete and refined whole preparation scheme, the purity of the spherical nano-silicon microsphere is better improved, so that the spherical nano-silicon microsphere has more uniform particle size, the controllable particle size and the reaction process are ensured, the environmental protection and the safety are improved, the large-scale low-cost mass production is easier to realize, and the preparation method of the spherical nano-silicon comprises the following steps:
1. raw materials: the silicon block material with the purity of 99.9-99.9999 percent is used, the iron content is less than 0.1 percent, the aluminum content is less than 0.1 percent, the calcium content is less than 0.01 percent, and the phosphorus content is less than 50ppm.
2. Grinding: grinding raw material silicon blocks by a wet method by utilizing a wire cutting or sand mill, or crushing the raw material silicon blocks by utilizing a jet mill to obtain silicon powder with the particle size of 50-1000 nm, wherein the particle size can be regulated and controlled by controlling the particle size of cutting wire diameter or grinding beads of the sand mill and the grinding or crushing time;
3. removing impurities: the ground silicon powder passes through a strong magnetic field pipeline in a liquid state environment, and superconducting strong magnetism with the magnetic field strength within 10 Tesla can be selected to remove metal impurities; and through vacuum high temperature cracking reaction, decomposing organic matter at 500-1000 deg.c to eliminate organic matter.
4. Spheroidizing: and dispersing the nanoscale silicon powder into an electromagnetic induction cavity by inert gas or nitrogen for high-temperature spheroidization.
5. And (3) cooling: and cooling the spheroidized silicon nano particles for 5-10 s by adopting a dispersing air cooling mode, and cooling the silicon nano particles to below 20 ℃ after the temperature is reduced to below 200 ℃ by further water cooling, so as to obtain the spherical nano silicon.
The invention obtains silicon powder with coexisting solid and liquid in high temperature reaction, and spherical particles are formed under the action of surface tension, so that spherical nano silicon is obtained. The resonance effect generated by microwaves in the high-temperature reaction cavity is used for acting on inert gas, the inert gas is subjected to excitation of electromagnetic induction, partial ionization of the inert gas is performed, high electron temperature is generated, heat is transferred to the surface of silicon powder, the nano silicon powder reaches a solid-liquid coexisting state, the nano silicon powder forms a sphere due to the action of surface tension, and then after the nano silicon powder enters the cooling cavity, the spherical nano silicon powder is rapidly cooled, so that solid spherical nano silicon powder with uniform granularity is formed. According to the invention, the spherical nano silicon powder with controllable granularity can be obtained by adjusting the particle size of the introduced nano silicon powder and controlling the input power of the microwave source.
The invention provides a preparation method of high-purity spherical nanometer silicon powder with adjustable particle size. The spherical nanometer silicon powder with controllable granularity, high purity and low cost is obtained by adopting a three-step process; firstly, crushing and wet grinding a silicon block material with the purity of 99.9-99.9999% to obtain nano-grade silicon powder with a certain granularity; secondly, removing metal elements in the silicon powder by using superconducting strong magnetism, and removing organic substances such as ethanol, polyether and the like added in the wet crushing or grinding process by using a high-temperature vacuum heating method; and thirdly, dispersing the nano-grade silicon powder into an electromagnetic induction cavity from inert gas, applying the resonance effect generated by microwaves to the inert gas, and partially ionizing the inert gas under the excitation of electromagnetic induction of the microwaves to generate higher electron temperature and transfer heat to the surface of the silicon powder so that the nano-grade silicon powder reaches a solid-liquid coexisting state, and forming a sphere under the action of surface tension, and then rapidly cooling the spherical nano-silicon powder after entering a cooling cavity to form the solid spherical nano-silicon powder with uniform granularity.
The invention does not use chemical method to wash the raw materials, thereby reducing the pollution of the production process to the environment. The invention adopts superconducting strong magnetism to remove metal impurities from raw materials, removes organic matters through high-temperature pyrolysis, does not use chemical methods and chemical agents, and reduces the pollution to the environment in the production process. And: according to the invention, the resonance effect generated by microwaves is utilized to heat the inert gas and the nano silicon powder at the periphery of the nano silicon powder at the same time, the inert gas is partially ionized under the excitation effect of electromagnetic induction of the microwaves, a higher electron temperature is generated, heat is transferred to the surface of the silicon powder, so that the nano silicon powder reaches a solid-liquid coexisting state, and the spherical nano silicon powder is formed due to the effect of surface tension and then enters a cooling cavity, and then the spherical nano silicon powder is rapidly cooled to form solid spherical nano silicon powder with uniform granularity.
The spherical nanometer silicon powder prepared by the method avoids impurity pollution in the preparation process, has higher purity, uniform granularity, adjustable size and good sphericity. Meanwhile, the preparation method provided by the invention is simple and environment-friendly, and the microwave has high frequency and short wavelength, and compared with radio frequency induction and the like, the microwave induction temperature is lower, generally about 500-2500 ℃, so that the preparation method has high production efficiency, lower power consumption and production cost and is more suitable for large-scale production and application.
Experimental results show that the purity of the spherical nano silicon prepared by the method can reach more than 99.9%, the impurity elements Fe <100ppm, al <100ppm, P <30ppm and Ca <60ppm, and the impurity content can not be increased in the reaction process.
For further explanation of the present invention, the following describes in detail a preparation method of spherical nano-silicon provided by the present invention with reference to examples, but it should be understood that these examples are implemented on the premise of the technical solution of the present invention, and detailed implementation and specific operation procedures are given, only for further explanation of the features and advantages of the present invention, and not limitation of the claims of the present invention, and the scope of protection of the present invention is not limited to the following examples.
Example 1
1. Raw materials: the raw material silicon block material with the purity of more than 99.9 percent is used, the iron content is less than 0.01 percent, the aluminum content is less than 0.01 percent, the calcium content is less than 0.01 percent, and the phosphorus content is less than 30ppm.
2. Grinding: grinding raw material silicon blocks by a wet method by utilizing a wire cutting or sand mill to obtain silicon powder with the particle size of 150-200 nm, wherein the particle size can be regulated and controlled by controlling the cutting wire diameter or the grinding bead particle size and the grinding time of the sand mill;
3. removing impurities: the ground silicon powder passes through a strong magnetic field pipeline in a liquid ethanol environment, and superconducting strong magnetism with the magnetic field strength of 10 Tesla is selected to remove metal impurities; and performing vacuum pyrolysis reaction for 30min, decomposing organic matters at 800 ℃, and removing the organic matters.
4. Spheroidizing: and dispersing the nanoscale silicon powder into an electromagnetic induction cavity by inert gas or nitrogen for high-temperature spheroidization.
Specifically, adding the silicon powder subjected to impurity removal into an electromagnetic reaction device at a speed of 1 g/s, wherein the argon gas is introduced at a speed of 0.002 cubic meters/s, and the silicon powder is fully contacted with the argon gas; wherein the argon pressure in the reaction cavity is 0.1Mpa, and the concentration of silicon powder suspended in the argon is 0.5-1 g/m 3 . Setting the wavelength of electromagnetic wave to be 0.33m, starting the electromagnetic wave, enabling silicon powder suspended in argon to pass through an electromagnetic wave area under the action of the electromagnetic wave in a reaction cavity with the power of 15KW, heating the silicon powder by argon plasma, and obtaining spherical nano silicon powder after 2 seconds of passing through the area.
The spherical nano-silicon powder prepared in example 1 of the present invention was characterized.
Referring to fig. 1, fig. 1 is a scanning electron microscope image of spherical nano silicon powder prepared by the invention.
As can be seen from FIG. 1, the present invention prepares spherical nano silicon, wherein the particle size of the nano silicon is 150-200 nm.
The spherical nano-silicon powder prepared in example 1 of the present invention was examined.
The results showed that the purity of the spherical nano silicon powder was >99.9%, the iron content was 70ppm, the aluminum content was 66ppm, the phosphorus content was 27ppm, and the calcium content was 49ppm. This shows that the purity of the spherical nano silicon prepared by the invention is basically the same as that of the raw material silicon powder.
Example 2
1. Raw materials: the raw material silicon block material with the purity of more than 99.9 percent is used, the iron content is less than 0.01 percent, the aluminum content is less than 0.01 percent, the calcium content is less than 0.01 percent, and the phosphorus content is less than 40ppm.
2. Grinding: grinding raw material silicon blocks by a wet method by utilizing a wire cutting or sand mill to obtain silicon powder with the particle size of 150-200 nm, wherein the particle size can be regulated and controlled by controlling the cutting wire diameter or the grinding bead particle size and the grinding time of the sand mill;
3. removing impurities: passing the ground silicon powder through a strong magnetic field pipeline in a liquid ethanol environment, and selecting superconducting strong magnetism with magnetic field strength within 8 tesla to remove metal impurities; and performing vacuum pyrolysis reaction for 50min, decomposing organic matters at 800 ℃, and removing the organic matters.
4. Spheroidizing: and dispersing the nanoscale silicon powder into an electromagnetic induction cavity by inert gas or nitrogen for high-temperature spheroidization.
Specifically, adding the silicon powder subjected to impurity removal into an electromagnetic reaction device at a speed of 0.8 g/s, wherein the argon gas is introduced at a speed of 0.002 cubic meters/s, and the silicon powder is fully contacted with the argon gas; wherein the argon pressure in the reaction cavity is 0.05Mpa, and the concentration of silicon powder suspended in the argon is 0.5-1 g/m 3 . Setting the wavelength of electromagnetic wave to be 0.125m, starting the electromagnetic wave, and obtaining spherical nano silicon powder after silicon powder suspended in argon passes through an electromagnetic wave area and is heated by argon plasma for 3 seconds and passes through the area under the electromagnetic wave effect in a reaction cavity with the power of 10 KW.
The spherical nano-silicon powder prepared in example 2 of the present invention was examined.
The result shows that the purity of the spherical nano silicon powder is more than 99.9%, the iron content is 52ppm, the aluminum content is 73ppm, the phosphorus content is 25ppm, and the calcium content is 55ppm. This shows that the purity of the spherical nano silicon prepared by the invention is basically the same as that of the raw material silicon powder.
The above description of the preparation method of the high-purity spherical nano silicon powder with adjustable particle size provided by the invention is provided in detail, and specific examples are applied herein to illustrate the principles and embodiments of the invention, and the above examples are only used to help understand the method and core ideas of the invention, including the best mode, and also to enable any person skilled in the art to practice the invention, including making and using any device or system, and implementing any combined method. It should be noted that it will be apparent to those skilled in the art that various modifications and adaptations of the invention can be made without departing from the principles of the invention and these modifications and adaptations are intended to be within the scope of the invention as defined in the following claims. The scope of the patent protection is defined by the claims and may include other embodiments that occur to those skilled in the art. Such other embodiments are intended to be within the scope of the claims if they have structural elements that do not differ from the literal language of the claims, or if they include equivalent structural elements with insubstantial differences from the literal language of the claims.
Claims (10)
1. A preparation method of spherical nano-silicon is characterized by comprising the following steps,
a) Under the action of electromagnetic waves, under the condition of nitrogen and/or inert gas, the suspended silicon powder is sphericized and cooled to obtain spherical nano silicon;
the pressure of the nitrogen and/or inert gas is 10 Pa-0.12 MPa;
the concentration of the silicon powder suspended in the nitrogen and/or inert gas is 0.1-1 g/m 3 ；
The electromagnetic wave has the functions of ionizing nitrogen and/or inert gas;
ionized nitrogen and/or inert gas can generate corresponding electron temperature and transfer heat to the surface of the silicon powder;
the wavelength of the electromagnetic wave is 0.001-10 m;
the silicon powder is nano-scale silicon powder;
the specific process of sphericizing is as follows:
the suspended silicon powder forms a solid-liquid coexisting state and forms a sphere under the action of surface tension.
2. The method according to claim 1, wherein the spheroidization time is 0.1 to 3s;
the spheroidization temperature is 500-2500 ℃.
3. The method according to claim 1, wherein the particle size of the spherical nano-silicon can be controlled by adjusting the power of the electromagnetic wave.
4. The method of claim 1, wherein the cooling means comprises one or more of water cooling, air cooling and natural cooling.
5. The method of claim 1, wherein the cooling comprises air cooling and then water cooling.
6. The method of claim 1, wherein the silicon powder is ground and purified from raw silicon;
the purity of the silicon powder is 99.9% -99.999%;
the grinding mode comprises one or more of wet ball milling, wet sand milling and wet wire cutting grinding.
7. The method of manufacturing according to claim 6, wherein the raw material silicon comprises a silicon block;
the iron content of the raw material silicon is less than or equal to 0.01%;
the aluminum content of the raw material silicon is less than or equal to 0.01%;
the phosphorus content of the raw material silicon is less than or equal to 50ppm;
the calcium content of the raw material silicon is less than or equal to 0.01 percent.
8. The method of claim 6, wherein the particle size of the ground raw silicon powder is 50-1000 nm;
the specific steps of impurity removal are as follows:
mixing the ground raw material silicon powder with a solvent, and performing magnetic field impurity removal and high-temperature impurity removal to obtain silicon powder;
the solvent comprises one or more of water, ethanol, acetone, isopropanol, polyethylene glycol and polyether.
9. The preparation method of claim 8, wherein the magnetic field strength of the magnetic field impurity removal is 1-10 tesla;
the time for removing impurities in the magnetic field is 0.1-3 s;
the high-temperature impurity removal temperature is 500-1000 ℃;
the high-temperature impurity removal time is 30-60 min.
10. The preparation method of any one of claims 1 to 9, wherein the particle size of the spherical nano-silicon is 20 to 700nm;
the purity of the spherical nano silicon is 99.9% -99.999%.
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Denomination of invention: A method for preparing high-purity spherical nano silicon powder with adjustable particle size Granted publication date: 20230922 Pledgee: Hangzhou United Rural Commercial Bank Co.,Ltd. Haining sub branch Pledgor: Zhejiang Jiaxing Xinghan Nano Technology Co.,Ltd. Registration number: Y2024980005351 |