CN113149016A - Preparation method of high-purity spherical nano silicon powder with adjustable particle size - Google Patents
Preparation method of high-purity spherical nano silicon powder with adjustable particle size Download PDFInfo
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- CN113149016A CN113149016A CN202110205670.7A CN202110205670A CN113149016A CN 113149016 A CN113149016 A CN 113149016A CN 202110205670 A CN202110205670 A CN 202110205670A CN 113149016 A CN113149016 A CN 113149016A
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 160
- 239000005543 nano-size silicon particle Substances 0.000 title claims abstract description 133
- 239000002245 particle Substances 0.000 title claims abstract description 84
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 90
- 238000004519 manufacturing process Methods 0.000 claims abstract description 63
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000001816 cooling Methods 0.000 claims abstract description 36
- 239000011261 inert gas Substances 0.000 claims abstract description 32
- 230000009471 action Effects 0.000 claims abstract description 21
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims description 48
- 238000000034 method Methods 0.000 claims description 43
- 239000012535 impurity Substances 0.000 claims description 42
- 229910052710 silicon Inorganic materials 0.000 claims description 39
- 239000010703 silicon Substances 0.000 claims description 39
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 22
- 238000000227 grinding Methods 0.000 claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000011575 calcium Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 230000001105 regulatory effect Effects 0.000 claims description 11
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 10
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 10
- 229910052791 calcium Inorganic materials 0.000 claims description 10
- 238000005520 cutting process Methods 0.000 claims description 10
- 229910052742 iron Inorganic materials 0.000 claims description 10
- 229910052698 phosphorus Inorganic materials 0.000 claims description 10
- 239000011574 phosphorus Substances 0.000 claims description 10
- 229910052782 aluminium Inorganic materials 0.000 claims description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 6
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 5
- 229920000570 polyether Polymers 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 238000012546 transfer Methods 0.000 claims description 3
- 238000005563 spheronization Methods 0.000 claims 1
- 230000005674 electromagnetic induction Effects 0.000 abstract description 11
- 239000007787 solid Substances 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 5
- 230000005284 excitation Effects 0.000 abstract description 4
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 4
- 239000007789 gas Substances 0.000 abstract description 2
- 239000004005 microsphere Substances 0.000 description 50
- 238000006243 chemical reaction Methods 0.000 description 39
- 230000007613 environmental effect Effects 0.000 description 25
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 24
- 229910052786 argon Inorganic materials 0.000 description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 239000004576 sand Substances 0.000 description 8
- 230000006698 induction Effects 0.000 description 7
- 230000001276 controlling effect Effects 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000011324 bead Substances 0.000 description 3
- 238000003801 milling Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000007158 vacuum pyrolysis Methods 0.000 description 3
- 239000004484 Briquette Substances 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 229910021417 amorphous silicon Inorganic materials 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 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
- 230000008020 evaporation Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000005389 magnetism Effects 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
- 229910000077 silane Inorganic materials 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
- 239000010406 cathode material Substances 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000000383 hazardous chemical 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
- 239000007858 starting material Substances 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
- 238000001238 wet grinding Methods 0.000 description 1
Images
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 and 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 and sent into an electromagnetic induction cavity, resonance effect generated by microwave acts on the inert gas, the gas is partially ionized under the excitation action of electromagnetic induction to generate higher temperature, and heat is transferred to the surface of the silicon powder, so that the surface of the silicon powder reaches a solid-liquid coexisting state, a spherical shape is formed under the action of surface tension, and then the spherical nano silicon powder is rapidly cooled after entering a cooling cavity to form solid spherical nano silicon powder with uniform particle size; and 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 microwave. 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 two allotropes, amorphous and crystalline silicon. The crystalline silicon is grey black and the amorphous silicon is black. Silicon is a raw material for manufacturing glass, quartz glass, water glass, optical fiber, important parts of the electronic industry, optical instruments, artware and refractory materials, and is also an important material for scientific research, and particularly, in recent years, with the rapid development of the electronic industry, the silicon industry is also developed vigorously. The spherical nano 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 high-purity spherical silicon powder is a interdisciplinary high-difficulty project, and the existing method for preparing the nano silicon powder mainly comprises a mechanical ball milling method, a gas-phase chemical deposition method, a plasma evaporation and condensation method and the like. However, for spherical nano silicon powder, especially for high-purity spherical nano silicon powder with precisely controllable particle size, the methods which can achieve low cost and large-scale yield are few at present.
In the prior art, the mechanical ball milling method has lower cost, but the granularity is reduced mainly by physical milling, 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 that the method has larger potential safety hazards and environmental hazards; the plasma evaporation condensation method generally uses an arc plasma method and a radio frequency induction (RF) plasma method; in the arc plasma method, as disclosed in patent publication No. CN102910630A, the power electrode contacts the heat source during heating, so that the prepared material is polluted to some extent; the rf induction plasma method, such as CN203333311U, adopts an electrodeless method, so as to avoid the contact between the electrode and the heat source, and although the prepared material is not polluted, the discharge process will generate a high voltage sheath and the sputtering pollution of the ion wall caused by the high voltage sheath, and considering that the rf induction frequency is generally MHz level, the frequency is low, so the working power of the power supply is generally high, the power consumption is large in the mass production, and the cost is relatively high.
Therefore, how to find a more suitable method for preparing spherical nano-silicon, which can prepare spherical nano-silicon with higher purity and controllable granularity and is more beneficial to industrial realization, has become one of the problems to be solved by many front-line researchers in the field.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a method for preparing nano-silicon, and in particular, a method for preparing spherical nano-silicon, which avoids the silicon powder from being contaminated by impurities during the preparation process, has uniform and adjustable particle size, and the prepared spherical nano-silicon has higher purity, and the preparation method is simple, environment-friendly, high in production efficiency, lower in power consumption and production cost, and more suitable for large-scale production and application.
The invention provides a preparation method of spherical nano-silicon, which comprises the following steps,
a) under the action of electromagnetic waves and under the condition of nitrogen and/or inert gas, the suspended silicon powder is spheroidized and then cooled to obtain the spherical nano silicon.
Preferably, the electromagnetic wave includes one or more of microwave, ultrashort wave and shortwave;
the pressure of the nitrogen and/or the 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/m3。
Preferably, the electromagnetic wave specifically functions to ionize nitrogen and/or inert gas;
the 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 0.1-3 s;
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 spheroidization process comprises the following specific steps:
the suspended silicon powder forms a solid-liquid coexisting state and forms a spherical shape under the action of surface tension;
the cooling mode comprises one or more of water cooling, air cooling and natural cooling;
the concrete steps of cooling include air cooling and water cooling.
Preferably, the silicon powder is prepared by grinding and removing impurities 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 sanding and wet line cutting grinding.
Preferably, the raw material silicon comprises silicon blocks;
the iron content of the raw material silicon is less than or equal to 0.01 percent;
the aluminum content of the raw material silicon is less than or equal to 0.01 percent;
the phosphorus content of the raw material silicon is less than or equal to 50 ppm;
the calcium content of the raw material silicon is less than or equal to 0.01 percent.
Preferably, the particle size 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 removing impurities through a magnetic field and at a high temperature 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 by the magnetic field is 0.1-3 s;
the temperature for high-temperature impurity removal is 500-1000 ℃;
and the time for removing impurities at high temperature 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 and 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 invention aims at the problems that the purity and the grain diameter 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.
The invention creatively disperses the nanoscale silicon powder from inert gas and sends the nanoscale silicon powder into the electromagnetic induction cavity, utilizes the resonance effect generated by microwave to act on the inert gas, is excited by the electromagnetic induction of the microwave, partially ionizes the inert gas to generate higher electronic temperature, and transfers heat to the surface of the silicon powder, so that the nanoscale silicon powder reaches a solid-liquid coexisting state, forms a sphere due to the action of surface tension, and then, after entering the cooling cavity, the spherical nanometer silicon powder is rapidly cooled to form solid spherical nanometer silicon powder with uniform granularity. And 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 spherical nano silicon powder prepared by the invention avoids the silicon powder from being polluted by impurities in the preparation process, has higher purity, uniform and adjustable granularity 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 and is 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%, impurity elements Fe is less than 100ppm, Al is less than 100ppm, P is less than 30ppm, Ca is less than 60ppm, and the impurity content is not 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 invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.
All of the starting materials of the present invention, without particular limitation as to their source, may be purchased commercially or prepared according to conventional methods well known to those skilled in the art.
All the raw materials of the invention are not particularly limited in purity, and the invention is preferably prepared by adopting the conventional purity of analytically pure or high-purity spherical nano silicon.
All the raw materials, the marks and the acronyms thereof belong to the conventional marks and acronyms in the field, each mark and acronym is clear and definite in the field of related application, and the raw materials can be purchased from the market or prepared by a conventional method by the technical staff in the field according to the marks, the acronyms and the corresponding application.
In all the processes of the invention, the abbreviations thereof belong to the common abbreviations in the art, each abbreviation is clearly clear in the field of its associated use, and the ordinary process steps thereof can be understood by those skilled in the art from the abbreviations.
The invention provides a preparation method of spherical nano-silicon, which comprises the following steps,
a) under the action of electromagnetic waves and under the condition of nitrogen and/or inert gas, the suspended silicon powder is spheroidized and then cooled to obtain the spherical nano silicon.
The invention has no special limitation on the types and parameters of the electromagnetic waves in principle, 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 0.001-10 m (meter), more preferably 0.005-8 m, more preferably 0.01-5 m, more preferably 0.05-3 m, more preferably 0.08-2 m, and particularly 0.1-1 m.
The specific action of the electromagnetic wave is not particularly limited in principle, and a person skilled in the art can select the electromagnetic wave according to actual production conditions, quality requirements and product requirements.
The invention is an integrated and refined preparation industry, and aims to improve the purity of spherical nano silicon microspheres, ensure that the spherical nano silicon microspheres have more uniform particle size, ensure that the particle size and the reaction process are controllable, increase the environmental protection and safety, and more easily realize large-scale low-cost mass production.
The invention has no particular limitation on the pressure of the nitrogen and/or the inert gas in principle, and a person skilled in the art can select the pressure according to the actual production condition, the quality requirement and the product requirement, in order to improve the purity of the spherical nano silicon microspheres, ensure that the spherical nano silicon microspheres have more uniform particle size, ensure the particle size and the reaction process to be controllable, increase the environmental protection and the safety, and more easily realize large-scale low-cost mass production, the pressure of the nitrogen and/or the 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, more preferably 1-3 Kpa.
The invention is in principle directed toThe concentration of the silicon powder suspended in the nitrogen and/or inert gas is not particularly limited, and a person skilled in the art can select the silicon powder according to actual production conditions, quality requirements and product requirements, in order to improve the purity of the spherical nano-silicon microspheres, ensure that the spherical nano-silicon microspheres have more uniform particle size, ensure that the particle size and the reaction process are controllable, increase environmental protection and safety, and more easily realize large-scale low-cost mass production, the concentration of the silicon powder suspended in the nitrogen and/or inert gas is preferably 0.1-1 g/m3More preferably 0.3 to 0.8g/m3More preferably 0.5 to 0.6g/m3。
The invention has no special limitation on the spheroidization time in principle, and a person skilled in the art can select the spheroidization time according to the actual production condition, the quality requirement and the product requirement, in order to improve the purity of the spherical nano silicon microspheres, ensure that the spherical nano silicon microspheres have more uniform particle size, ensure the particle size and the reaction process to be controllable, increase the environmental protection and the safety, and more easily realize large-scale low-cost mass production, the spheroidization time is preferably 0.1-3 s, more preferably 0.5-2.5 s, and more preferably 1-2 s.
The temperature for the spheroidization is not particularly limited in principle, and a person skilled in the art can select the temperature according to actual production conditions, quality requirements and product requirements, in order to improve the purity of the spherical nano-silicon microspheres, so that the spherical nano-silicon microspheres have more uniform particle size, the particle size and the reaction process are controllable, the environmental protection and safety are improved, the large-scale low-cost mass production is easier to realize, and the temperature for the spheroidization is preferably 500-2500 ℃, more preferably 700-2000 ℃, and more preferably 900-1800 ℃.
The specific selection of the silicon powder is not particularly limited in principle, 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 integral preparation scheme, and in order to improve the purity of the spherical nano silicon microspheres, ensure that the spherical nano silicon microspheres have more uniform particle size, ensure that the particle size and the reaction process are controllable, increase the environmental protection and the safety, and more easily realize large-scale low-cost mass production, the particle size of the spherical nano silicon can be regulated and controlled by regulating the power of the electromagnetic waves, and the particle size of the spherical nano silicon can be regulated and controlled by regulating the power of the electromagnetic waves and/or the particle size of the silicon powder.
The invention is a complete and refined integral preparation process, better improves the purity of the spherical nano silicon microspheres, ensures that the spherical nano silicon microspheres have more uniform particle size, ensures that the particle size and the reaction process are controllable, increases the environmental protection and the safety, is easier to realize large-scale low-cost mass production, and preferably adopts the following specific processes of sphericization:
the suspended silicon powder forms a solid-liquid coexisting state and forms a spherical shape under the action of surface tension.
In the present invention, the suspended silicon powder is in a solid-liquid coexisting state, and preferably means that the surface of the suspended silicon powder is in a molten state. That is, the suspended silicon powder is solid inside and molten on the surface, and is in a state of coexistence of solid and liquid.
The cooling method 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, in order to improve the purity of the spherical nano-silicon microspheres, so that the spherical nano-silicon microspheres have more uniform particle size, the particle size and the reaction process are controllable, the environmental protection and safety are improved, and the large-scale low-cost mass production is easier to realize.
The invention is a complete and refined integral preparation scheme, better improves the purity of the spherical nano silicon microspheres, ensures that the spherical nano silicon microspheres have more uniform particle size, ensures the particle size and the reaction process to be controllable, increases the environmental protection and the safety, is easier to realize large-scale low-cost mass production, and the specific steps of cooling can be air cooling firstly and then water cooling, and specifically can be as follows:
the nano silicon particles are cooled by dispersed air (air cooling) and then further cooled by water.
The time for the dispersion air cooling is preferably 5 to 10 seconds, more preferably 6 to 9 seconds, and still more preferably 7 to 8 seconds. The temperature for cooling the dispersion gas is preferably 200 ℃ or higher, and may be 180 ℃ or higher or 160 ℃ or higher. The water cooling is specifically cooling to below 20 ℃.
The invention has no particular limitation on the source of the silicon powder in principle, and a person skilled in the art can select the silicon powder according to the actual production condition, the quality requirement and the product requirement.
The purity of the raw material silicon is not particularly limited in principle, and a person skilled in the art can select the raw material silicon according to actual production conditions, quality requirements and product requirements, in order to improve the purity of the spherical nano-silicon microspheres, so that the spherical nano-silicon microspheres have more uniform particle size, the particle size and the reaction process are controllable, the environmental protection and safety are improved, and 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 shape of the raw material silicon is not particularly limited in principle, and a person skilled in the art can select the shape according to actual production conditions, quality requirements and product requirements.
The iron content of the raw material silicon is not particularly limited in principle, and a person skilled in the art can select the iron content according to actual production conditions, quality requirements and product requirements, in order to improve the purity of the spherical nano-silicon microspheres, ensure that the spherical nano-silicon microspheres have more uniform particle size, ensure the particle size and the reaction process to be controllable, increase the environmental protection and safety, and more easily realize large-scale low-cost mass production, 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 aluminum content of the raw material silicon is not particularly limited in principle, and a person skilled in the art can select the raw material silicon according to actual production conditions, quality requirements and product requirements, in order to improve the purity of the spherical nano-silicon microspheres, ensure that the spherical nano-silicon microspheres have more uniform particle size, ensure that the particle size and the reaction process are controllable, increase environmental protection and safety, and more easily realize large-scale low-cost mass production, 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 phosphorus content of the raw material silicon is not particularly limited in principle, and a person skilled in the art can select the phosphorus content according to actual production conditions, quality requirements and product requirements, in order to improve the purity of the spherical nano-silicon microspheres, ensure that the spherical nano-silicon microspheres have more uniform particle size, ensure the particle size and the reaction process to be controllable, increase the environmental protection and safety, and more easily realize large-scale low-cost mass production, the phosphorus content of the raw material silicon is preferably less than or equal to 50ppm, more preferably less than or equal to 40ppm, and more preferably less than or equal to 30 ppm.
The calcium content of the raw material silicon is not particularly limited in principle, and a person skilled in the art can select the calcium content according to actual production conditions, quality requirements and product requirements, in order to improve the purity of the spherical nano-silicon microspheres, ensure that the spherical nano-silicon microspheres have more uniform particle size, ensure that the particle size and the reaction process are controllable, increase environmental protection and safety, and more easily realize large-scale low-cost mass production, 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 purity of the silicon powder is not particularly limited in principle, 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% to 99.999%, more preferably 99.95% to 99.995%, and still more preferably 99.97% to 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, in order to improve the purity of the spherical nano-silicon microspheres, so that the spherical nano-silicon microspheres have more uniform particle size, the particle size and the reaction process are controllable, the environmental protection and safety are improved, and large-scale low-cost mass production is easier to realize, wherein the grinding mode preferably comprises one or more of wet ball milling, wet sand milling and wet linear cutting grinding, and more preferably comprises wet ball milling, wet sand milling or wet linear cutting grinding.
The particle size of the ground raw silicon powder is not particularly limited in principle, and a person skilled in the art can select the particle size according to actual production conditions, quality requirements and product requirements, in order to improve the purity of the spherical nano-silicon microspheres, so that the spherical nano-silicon microspheres have more uniform particle sizes, the particle sizes and the reaction process are controllable, the environmental protection property and the safety are improved, the 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 more preferably 400-600 nm.
In order to improve the purity of the spherical nano-silicon microspheres, ensure that the spherical nano-silicon microspheres have more uniform particle size, ensure the particle size and the reaction process to be controllable, increase the environmental protection and safety, and more easily realize large-scale low-cost mass production, the specific steps of impurity removal are preferably as follows:
and mixing the ground raw material silicon powder with a solvent, and removing impurities through a magnetic field and at a high temperature to obtain the silicon powder.
The specific selection of the solvent is not particularly limited in principle, and a person skilled in the art can select the solvent according to actual production conditions, quality requirements and product requirements, in order to improve the purity of the spherical nano-silicon microspheres, so that the spherical nano-silicon microspheres have more uniform particle size, the particle size and the reaction process are controllable, the environmental protection and safety are improved, and the large-scale low-cost mass production is easier to realize, wherein the solvent preferably comprises one or more of water, ethanol, acetone, isopropanol, polyethylene glycol and polyether, and more preferably comprises water, ethanol, acetone, isopropanol, polyethylene glycol or polyether.
The magnetic field intensity of the magnetic field impurity removal is not particularly limited in principle, and a person skilled in the art can select the magnetic field intensity according to actual production conditions, quality requirements and product requirements, in order to improve the purity of the spherical nano-silicon microspheres, the spherical nano-silicon microspheres have more uniform particle size, the particle size and the reaction process are controllable, the environmental protection and safety are improved, large-scale low-cost mass production is easier to realize, and the magnetic field intensity of the magnetic field impurity removal is preferably 1-10 tesla, more preferably 3-8 tesla, and more preferably 5-6 tesla.
The time for removing impurities by the magnetic field is not particularly limited in principle, and a person skilled in the art can select the time according to actual production conditions, quality requirements and product requirements, in order to improve the purity of the spherical nano-silicon microspheres, so that the spherical nano-silicon microspheres have more uniform particle size, the particle size and the reaction process are controllable, the environmental protection and safety are improved, the large-scale low-cost mass production is easier to realize, and the time for removing impurities by the magnetic field is preferably 0.1-3 s, more preferably 0.5-2.5 s, and more preferably 1-2 s.
The temperature of the high-temperature impurity removal is not particularly limited in principle, and a person skilled in the art can select the high-temperature impurity removal temperature according to actual production conditions, quality requirements and product requirements, in order to improve the purity of the spherical nano-silicon microspheres, so that the spherical nano-silicon microspheres have more uniform particle size, the particle size and the reaction process are controllable, the environmental protection and safety are improved, the large-scale low-cost mass production is easier to realize, and the high-temperature impurity removal temperature is preferably 500-1000 ℃, more preferably 600-900 ℃, and more preferably 700-800 ℃.
The time for high-temperature impurity removal is not particularly limited in principle, and a person skilled in the art can select the high-temperature impurity removal time according to actual production conditions, quality requirements and product requirements, in order to improve the purity of the spherical nano-silicon microspheres, so that the spherical nano-silicon microspheres have more uniform particle size, the particle size and the reaction process are controllable, the environmental protection and safety are improved, large-scale low-cost mass production is easier to realize, and the high-temperature impurity removal time is preferably 30-60 min, more preferably 35-55 min, and more preferably 40-50 min.
The particle size of the spherical nano silicon is not particularly limited in principle, and a person skilled in the art can select the spherical nano silicon according to actual production conditions, quality requirements and product requirements, in order to improve the purity of the spherical nano silicon microspheres, ensure that the spherical nano silicon microspheres have more uniform particle sizes, ensure that the particle sizes and the reaction process are controllable, increase the environmental protection and safety, and more easily realize large-scale low-cost mass production, 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 purity of the spherical nano silicon is not particularly limited in principle, and a person skilled in the art can select the spherical nano silicon according to actual production conditions, quality requirements and product requirements, and in order to improve the purity of the spherical nano silicon microspheres, the spherical nano silicon microspheres have more uniform particle size, the particle size and the reaction process are controllable, the environmental protection and safety are improved, and 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 more preferably 99.97-99.99%.
The invention is a complete and refined integral preparation scheme, better improves the purity of the spherical nano-silicon microspheres, ensures that the spherical nano-silicon microspheres have more uniform particle size, ensures the particle size and the reaction process to be controllable, increases the environmental protection and the safety, is easier to realize large-scale low-cost mass production, and the preparation method of the spherical nano-silicon can specifically comprise 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 50 ppm.
2. Grinding: grinding the raw material silicon block by a wet method by using a linear cutting or sand mill, or crushing by using 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 cutting linear diameter or the bead particle size of the sand mill and the grinding or crushing time;
3. impurity removal: the ground silicon powder passes through a high-intensity magnetic field pipeline in a liquid environment, and a super-conduction strong magnet with the magnetic field intensity within 10 Tesla is selected to remove metal impurities; and decomposing the organic matters at 500-1000 ℃ through vacuum pyrolysis reaction to remove the organic matters.
4. Spheroidizing: the nano-scale silicon powder is dispersed and sent into an electromagnetic induction cavity by inert gas or nitrogen for high-temperature spheroidization.
5. And (3) cooling: cooling the spheroidized silicon nanoparticles for 5-10 s in a dispersing air cooling mode, further cooling the spheroidized silicon nanoparticles to below 20 ℃ by water cooling when the temperature is reduced to below 200 ℃, and obtaining the spherical nano silicon.
The invention obtains silicon powder with solid-liquid coexistence in high-temperature reaction, and spherical particles are formed under the action of surface tension, so that the spherical nano silicon is obtained. The resonance effect generated by the microwave in the high-temperature reaction cavity acts on the inert gas, the inert gas is partially ionized under the excitation action of electromagnetic induction to generate higher electronic temperature, heat is transferred to the surface of the silicon powder, the nanoscale silicon powder reaches a solid-liquid coexisting state, the spherical nanometer silicon powder is formed into a sphere under the action of surface tension, and then the spherical nanometer silicon powder is rapidly cooled after entering the cooling cavity to form solid spherical nanometer silicon powder with uniform granularity. The invention can obtain the spherical nano silicon powder with controllable granularity by adjusting the grain diameter of the introduced nano silicon powder and controlling the input power of the microwave source.
The steps of the invention provide a preparation method of high-purity spherical nano silicon powder with adjustable particle size. The method adopts three steps to obtain spherical nano silicon powder with controllable granularity, high purity and low cost; firstly, crushing and wet grinding a silicon block material with the purity of 99.9-99.9999% to obtain nano-scale silicon powder with a certain particle size; 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 nanoscale silicon powder into an electromagnetic induction cavity by inert gas, acting the resonance effect generated by the microwave on the inert gas, under the excitation action of the electromagnetic induction of the microwave, partially ionizing the inert gas to generate higher electronic temperature, transferring heat to the surface of the silicon powder to enable the nanoscale silicon powder to reach a solid-liquid coexisting state, forming a spherical shape due to the action of surface tension, and then rapidly cooling the spherical nano silicon powder after entering a cooling cavity to form solid spherical nano silicon powder with uniform particle size.
The invention does not use a chemical method to wash the raw materials, thereby reducing the pollution to the environment in the production process. 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: the invention utilizes the resonance effect generated by microwave to heat the inert gas and the nano silicon powder at the periphery of the nano silicon powder simultaneously, the inert gas is partially ionized under the excitation action of the electromagnetic induction of the microwave to generate higher electronic temperature, and the heat is transferred to the surface of the silicon powder, so that the nano silicon powder reaches a solid-liquid coexisting state, a spherical shape is formed under the action of surface tension, and then the spherical nano silicon powder is rapidly cooled after entering a cooling cavity to form solid spherical nano silicon powder with uniform granularity.
The spherical nano silicon powder prepared by the method avoids impurity pollution in the preparation process, has higher purity, uniform and adjustable granularity 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 and is 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%, impurity elements Fe is less than 100ppm, Al is less than 100ppm, P is less than 30ppm, Ca is less than 60ppm, and the impurity content is not increased in the reaction process.
For further illustration of the present invention, the following detailed description of the method for preparing spherical nano-silicon according to the present invention is provided in conjunction with the following examples, but it should be understood that these examples are implemented on the premise of the technical solution of the present invention, and the detailed embodiments and specific procedures are given, only for further illustration of the features and advantages of the present invention, and not for limitation of the claims of the present invention, and the scope of the present invention is not limited to the following examples.
Example 1
1. Raw materials: the raw material silicon briquette 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 30 ppm.
2. Grinding: grinding a raw material silicon block by a wet method by using a linear cutting or sand mill to obtain 150-200 nm silicon powder, wherein the particle size can be regulated and controlled by controlling the cutting linear diameter or the grinding bead particle size of the sand mill and the grinding time;
3. impurity removal: the ground silicon powder passes through a high-intensity magnetic field pipeline in a liquid ethanol environment, and a superconducting strong magnet with the magnetic field intensity of 10 Tesla is selected to remove metal impurities; and carrying out vacuum pyrolysis reaction for 30min, and decomposing the organic matters at 800 ℃ to remove the organic matters.
4. Spheroidizing: the nano-scale silicon powder is dispersed and sent into an electromagnetic induction cavity by inert gas or nitrogen for high-temperature spheroidization.
Specifically, the silicon powder after impurity removal is added into an electromagnetic reaction device at the speed of 1 g/s, the introducing speed of argon is 0.002 cubic meter/s, and the silicon powder is fully contacted with the argon; wherein the argon pressure in the reaction chamber is 0.1Mpa, and the concentration of the silicon powder suspended in the argon is 0.5-1 g/m3. Setting the wavelength of electromagnetic waves to be 0.33m, starting the electromagnetic waves, enabling silicon powder suspended in argon to pass through an electromagnetic wave region under the action of the electromagnetic waves in the reaction cavity with the power of 15KW, heating the silicon powder by argon plasma, and passing through the region after 2 seconds to obtain spherical nano-silicon powder.
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 the spherical nano silicon powder prepared by the invention.
As shown in FIG. 1, the spherical nano-silicon is prepared by the method, 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 show that the spherical nano-silicon powder has a purity of > 99.9%, an iron content of 70ppm, an aluminum content of 66ppm, a phosphorus content of 27ppm and a calcium content of 49 ppm. 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 briquette 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 40 ppm.
2. Grinding: grinding a raw material silicon block by a wet method by using a linear cutting or sand mill to obtain 150-200 nm silicon powder, wherein the particle size can be regulated and controlled by controlling the cutting linear diameter or the grinding bead particle size of the sand mill and the grinding time;
3. impurity removal: the ground silicon powder passes through a high-intensity magnetic field pipeline in a liquid ethanol environment, and a superconducting strong magnet with the magnetic field intensity within 8 Tesla is selected to remove metal impurities; and carrying out vacuum pyrolysis reaction for 50min, and decomposing the organic matters at 800 ℃ to remove the organic matters.
4. Spheroidizing: the nano-scale silicon powder is dispersed and sent into an electromagnetic induction cavity by inert gas or nitrogen for high-temperature spheroidization.
Specifically, the silicon powder after impurity removal is added into an electromagnetic reaction device at the speed of 0.8 g/s, the introducing speed of argon is 0.002 cubic meter/s, and the silicon powder is fully contacted with the argon; wherein the argon pressure in the reaction chamber is 0.05Mpa, and the concentration of the silicon powder suspended in the argon is 0.5-1 g/m3. Setting the wavelength of electromagnetic waves to be 0.125m, starting the electromagnetic waves, enabling silicon powder suspended in argon to pass through an electromagnetic wave region under the action of the electromagnetic waves in the reaction cavity with the power of 10KW, heating the silicon powder by argon plasma, and passing through the region after 3 seconds to obtain spherical nano-silicon powder.
The spherical nano-silicon powder prepared in example 2 of the present invention was examined.
The results show that the spherical nano-silicon powder has a purity of > 99.9%, an iron content of 52ppm, an aluminum content of 73ppm, a phosphorus content of 25ppm, and a calcium content of 55 ppm. 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 method for preparing spherical nano silicon powder with adjustable particle size according to the present invention has been described in detail, and the principle and embodiments of the present invention are illustrated herein by using specific examples, which are only used to help understand the method of the present invention and its core ideas, including the best mode, and also to enable any person skilled in the art to practice the present invention, including making and using any device or system, and implementing any combination of methods. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention. The scope of the invention 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 approximate the literal language of the claims, or if they include equivalent structural elements with insubstantial differences from the literal languages 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 and under the condition of nitrogen and/or inert gas, the suspended silicon powder is spheroidized and then cooled to obtain the spherical nano silicon.
2. The method according to claim 1, wherein the electromagnetic wave includes one or more of microwave, ultrashort wave, and shortwave;
the pressure of the nitrogen and/or the 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/m3。
3. The method according to claim 1, characterized in that the electromagnetic waves act in particular to ionize nitrogen and/or inert gases;
the 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.
4. The method according to claim 1, wherein the time for the spheronization is 0.1 to 3 seconds;
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.
5. The preparation method according to claim 1, wherein the spheroidization is carried out by the following specific processes:
the suspended silicon powder forms a solid-liquid coexisting state and forms a spherical shape under the action of surface tension;
the cooling mode comprises one or more of water cooling, air cooling and natural cooling;
the concrete steps of cooling include air cooling and water cooling.
6. The preparation method according to claim 1, wherein the silicon powder is obtained by grinding and removing impurities from a 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 sanding and wet line cutting grinding.
7. The production method according to claim 6, wherein the raw material silicon comprises a silicon ingot;
the iron content of the raw material silicon is less than or equal to 0.01 percent;
the aluminum content of the raw material silicon is less than or equal to 0.01 percent;
the phosphorus content of the raw material silicon is less than or equal to 50 ppm;
the calcium content of the raw material silicon is less than or equal to 0.01 percent.
8. The preparation method according to 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 removing impurities through a magnetic field and at a high temperature to obtain silicon powder;
the solvent comprises one or more of water, ethanol, acetone, isopropanol, polyethylene glycol and polyether.
9. The preparation method according to claim 8, wherein the magnetic field intensity for removing impurities in the magnetic field is 1-10 Tesla;
the time for removing impurities by the magnetic field is 0.1-3 s;
the temperature for high-temperature impurity removal is 500-1000 ℃;
and the time for removing impurities at high temperature is 30-60 min.
10. The preparation method according to any one of claims 1 to 9, wherein the spherical nano-silicon has a particle size of 20 to 700 nm;
the purity of the spherical nano-silicon is 99.9-99.999%.
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