WO2021221234A1 - Procédé de fabrication de nouvelles nanoparticules de silicium - Google Patents

Procédé de fabrication de nouvelles nanoparticules de silicium Download PDF

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WO2021221234A1
WO2021221234A1 PCT/KR2020/010577 KR2020010577W WO2021221234A1 WO 2021221234 A1 WO2021221234 A1 WO 2021221234A1 KR 2020010577 W KR2020010577 W KR 2020010577W WO 2021221234 A1 WO2021221234 A1 WO 2021221234A1
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silicon
average particle
particle diameter
silicon particles
pulverizing
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PCT/KR2020/010577
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English (en)
Korean (ko)
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정영운
오정훈
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주식회사 엘피엔
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Publication of WO2021221234A1 publication Critical patent/WO2021221234A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/02—Silicon
    • C01B33/021—Preparation
    • 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
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

Definitions

  • the present invention relates to a novel method for manufacturing silicon nanoparticles, and more particularly, to a method for manufacturing silicon nanoparticles using a high-speed mechanical milling apparatus and a microfluidizer.
  • Silicon is attracting attention as a lithium ion secondary battery for portable electronic devices such as mobile phones and laptops that require high capacity due to its lithium ion storage capacity greater than graphite when charging, and as an anode material for solar cells.
  • Silicon is used in the form of nanoparticles in order to solve the problem of deterioration of repeated charge/discharge characteristics caused by large volume expansion and contraction during insertion and release of lithium.
  • silicon nanoparticles having various commercial applications, such as a solar cell device and a high-performance light emitting device, as well as as an anode material for such a lithium ion secondary battery.
  • Patent Document 1 silicon nanoparticles are produced by bead milling and filtering of silicon pieces, and in Patent Document 2, plasma arc discharge is used for the production of silicon nanoparticles, and in Patent Document 3, laser and plasma are used.
  • Patent Document 4 uses a thermal decomposition reaction of silicon to produce silicon nanopowder
  • Patent Document 5 uses a method of ultrasonically treating porous silicon prepared by reduction of silicon oxide
  • Patent Documents 6 and 7, respectively A method for preparing silicon nanoparticles by electric explosion and using a basic buffer solution is disclosed.
  • Patent Documents 3, 6, and 7 disclose a mass production method.
  • An object of the present invention is to provide a method for manufacturing silicon nanoparticles that can be mass-produced due to low cost and easy manufacturing.
  • an object of the present invention is to provide a method for mass-producing silicon nanoparticles of 500 nm or less in a short period of time.
  • step b) preparing silicon nanoparticles having an average particle diameter of 500 nm or less by using a microfluidizer at a constant pressure with the mixture of the silicon particles and the organic solvent of step a).
  • the silicon granules according to an embodiment of the present invention may have an average particle diameter of 200 ⁇ m to 400 ⁇ m.
  • the high-speed mechanical milling apparatus may be a hammer mill, a jet mill, a bead mill, and a mixture thereof.
  • the microfluidizer according to an embodiment of the present invention may have a nozzle diameter of 50 to 400 ⁇ m.
  • the pressure for the use of the microfluidizer according to an embodiment of the present invention may be 1000 to 6000 bar.
  • the organic solvent according to an embodiment of the present invention may be alcohols, ketones, carbonates, ethers, dimethyl sulfoxide (DMSO), or the like, or a mixture thereof.
  • DMSO dimethyl sulfoxide
  • the amount of the silicon particles used in the mixture of the silicon particles and the organic solvent in step a) according to an embodiment of the present invention may be 0.01 to 25% by weight.
  • the method for manufacturing silicon nanoparticles according to the present invention has the advantage that it is possible to mass-produce silicon nanoparticles with an average particle diameter of 100 nm or less, in particular, due to low cost and ease of manufacture.
  • Example 1 is a SEM photograph of the silicon nanoparticles of Example 1 of the present invention.
  • Example 2 is a SEM photograph of the silicon nanoparticles of Example 2 of the present invention.
  • Example 3 is a SEM photograph of the silicon nanoparticles of Example 3 of the present invention.
  • Example 4 is a SEM photograph of the silicon nanoparticles of Example 4 of the present invention.
  • Example 5 is a SEM photograph of the silicon nanoparticles of Example 5 of the present invention.
  • Example 6 is a SEM photograph of the silicon nanoparticles of Example 6 of the present invention.
  • the present invention provides a method for producing silicon nanoparticles that are economically effective at low cost, and can be mass-produced because they are easy to manufacture.
  • step b) preparing silicon nanoparticles having an average particle diameter of 500 nm or less by using a microfluidizer at a constant pressure by using a mixture of the silicon particles and the organic solvent of step a).
  • step a-2 pulverizing the silicon particles of step a-1) into silicon particles having an average particle diameter of 5 ⁇ m to 10 ⁇ m using a jet mill
  • step b) mixing the silicon particles of step b) with an organic solvent, and pulverizing them into silicon particles having an average particle diameter of 1 ⁇ m to 3 ⁇ m using the bead mill 1.
  • step a-3 preparing silicon nanoparticles having an average particle diameter of 500 nm or less by using a microfluidizer at a constant pressure of the mixture of the silicon particles and the organic solvent in step a-3).
  • step (a-2) pulverizing the silicon particles of step (a-1) into silicon particles having an average particle diameter of 5 ⁇ m to 10 ⁇ m using a jet mill
  • step (a-3) mixing the silicon particles of step (a-2) with an organic solvent, and pulverizing them into silicon particles having an average particle diameter of 1 ⁇ m to 3 ⁇ m using a bead mill 1.
  • step (a-4) pulverizing the mixture of the silicon particles and the organic solvent of step (a-3) into silicon particles having an average particle diameter of 0.5 ⁇ m to 0.7 ⁇ m using a bead mill 2
  • step (a-4) preparing silicon nanoparticles having an average particle diameter of 500 nm or less by using a microfluidizer at a constant pressure by using a mixture of the silicon particles and the organic solvent in step (a-4).
  • step (a-2) pulverizing the silicon particles of step (a-1) into silicon particles having an average particle diameter of 5 ⁇ m to 10 ⁇ m using a jet mill
  • step (a-3) mixing the silicon particles of step (a-2) with an organic solvent, and pulverizing them into silicon particles having an average particle diameter of 1 ⁇ m to 3 ⁇ m using a bead mill 1.
  • step (a-4) pulverizing the mixture of the silicon particles and the organic solvent of step (a-3) into silicon particles having an average particle diameter of 0.5 ⁇ m to 0.7 ⁇ m using a bead mill 2
  • step (a-5) pulverizing the mixture of the silicon particles and the organic solvent of step (a-4) into silicon particles having an average particle diameter of 0.2 ⁇ m to 0.4 ⁇ m using a bead mill 3
  • step (a-5) preparing silicon nanoparticles having an average particle diameter of 500 nm or less by using a microfluidizer at a constant pressure by using a mixture of the silicon particles and the organic solvent in step (a-5).
  • step (a-2) pulverizing the silicon particles of step (a-1) into silicon particles having an average particle diameter of 5 ⁇ m to 10 ⁇ m using a jet mill
  • step (a-3) mixing the silicon particles of step (a-2) with an organic solvent, and pulverizing them into silicon particles having an average particle diameter of 1 ⁇ m to 3 ⁇ m using a bead mill 1.
  • step (a-4) pulverizing the mixture of the silicon particles and the organic solvent of step (a-3) into silicon particles having an average particle diameter of 0.5 ⁇ m to 0.7 ⁇ m using a bead mill 2
  • step (a-5) pulverizing the mixture of the silicon particles and the organic solvent of step (a-4) into silicon particles having an average particle diameter of 0.2 ⁇ m to 0.4 ⁇ m using a bead mill 3
  • step (a-6) pulverizing the mixture of the silicon particles and the organic solvent of step (a-5) into silicon particles having an average particle diameter of 0.1 ⁇ m to 0.15 ⁇ m using a bead mill 4
  • step (a-6) preparing silicon nanoparticles having an average particle diameter of 500 nm or less by using a microfluidizer at a constant pressure by using a mixture of the silicon particles and the organic solvent in step (a-6).
  • the silicon granules according to the methods for manufacturing silicon nanoparticles of the present invention may have an average particle diameter of 200 ⁇ m to 400 ⁇ m, and when it exceeds 400 ⁇ m, the overall manufacturing time increases, which is not economically preferable.
  • the high-speed mechanical milling apparatus may be a hammer mill, a jet mill, a bead mill, or a mixture thereof, preferably a mixture of a hammer mill, a jet mill and a bead mill. More preferably, it is used in the order of a hammer mill, a jet mill, and a bead mill.
  • the size of the bead for hammer mill, and the size of the bead for jet mill of (a-1) and (a-2) above use a conventional size used for manufacturing silicon particles of the desired size, and (a)
  • the bead sizes of bead mills 1, 2, 3, and 4 in steps -3) to (a-6) are the largest in bead mill 1 and the smallest in bead mill 4, respectively, '2 to 4 mm', ' 0.5 to 0.7 mm', '0.3 to 0.4 mm' and '0.1 to 0.2 mm'.
  • the time required for the pulverization of (a-3) to (a-6) is '1.5 hours to 2.5 hours', '3.0 hours to 4.5 hours', '6 hours to 10 hours', and '15 hours to, respectively. It may be 17 hours', and the above times may be the time when the mixture of silicon particles and organic solvent is 100 kg.
  • the microfluidizer according to the methods for producing silicon nanoparticles of the present invention may have a nozzle diameter of 50 ⁇ m to 400 ⁇ m, preferably 75 ⁇ m to 400 ⁇ m.
  • a phenomenon in which the manufactured silicon nanoparticles clog the nozzle occurs, which causes difficulties in the manufacturing process, and when the nozzle diameter is larger than 400 ⁇ m, it is difficult to obtain nano-sized particles of 500 nm or less.
  • the microfluidizer of step b) among the methods for producing silicon nanoparticles of the present invention can be applied in two steps using two different nozzle diameters, and the second step is a microfluidizer having a large nozzle diameter.
  • the fluidizer is applied (step b-1)
  • a microfluidizer with a small nozzle diameter is applied (step b-2).
  • the two different nozzle diameters may be two of the nozzle diameters of 50 ⁇ m to 400 ⁇ m, and preferably, two nozzle diameters selected from among 75 ⁇ m, 100 ⁇ m, 200 ⁇ m, and 400 ⁇ m.
  • the total application time of the microfluidizer in step b) is 1 to 2 hours, and the ratio of application time in step (b-1): step (b-2) may be 1:1.
  • the time may be when the mixture of the silicon particles and the organic solvent is 100 kg.
  • the pressure for the use of the microfluidizer according to the methods for producing silicon nanoparticles of the present invention may be 1000 to 6000 bar, preferably 1000 to 4000 bar, and when the pressure is less than 1000 bar, the silicon nanoparticles are the nozzles.
  • the pressure is greater than 6000 bar, there are economic disadvantages such as an increase in equipment maintenance cost.
  • the organic solvent according to the methods for producing silicon nanoparticles of the present invention may be alcohols, ketones, carbonates, ethers, or dimethyl sulfoxide (DMSO), or a mixture thereof.
  • DMSO dimethyl sulfoxide
  • the alcohols may be methanol, ethanol, isopropanol, n-butanol, isobutanol, ethylene glycol, cyclohexanol, etc.
  • the ketones may be cyclohexanone, methyl ethyl ketone, etc.
  • the carbonates may be diethyl carbonate, etc.
  • the ethers may be tetrahydrofuran, tetrahydropyran, or the like.
  • Preferred organic solvents are alcohols, and more preferably isopropanol.
  • the mixture of the silicon particles and the organic solvent in step a) is specifically made in step (a-1) of step a), and the amount of silicon particles in the mixture may be 0.01 to 25% by weight of the total mixture, preferably 5 to 15% by weight, and more preferably 7 to 12% by weight. If the amount of silicon used in the mixture is less than 0.01% by weight or greater than 25% by weight, processing by the bead mill is not performed.
  • Silicon granules which are silicon raw materials, are put into a hammer mill grinder and pulverized to an average particle diameter of 75 ⁇ m, which is pulverized into silicon particles having an average particle diameter of 5 ⁇ m using an air jet mill.
  • a mixture of 10 kg of the obtained silicon particles having an average particle diameter of 5 ⁇ m and 90 kg of IPA (isopropyl alcohol) is first processed for 2 hours with a bead mill 1 using 3 mm zirconia beads, and processed into silicon particles having an average particle diameter of 1 ⁇ m.
  • the obtained silicon particles having an average particle diameter of 0.1 ⁇ m were applied to a microfluidizer having a nozzle diameter of 200 ⁇ m, and primary processing was performed for 30 minutes at a pressure of 2500 bar to obtain silicon particles having an average particle diameter of 0.07 ⁇ m, which were obtained with a nozzle diameter of 75 ⁇ m. It was applied to a microfluidizer and secondary processing was performed for 30 minutes at a pressure of 2500 bar to make silicon nanoparticles with an average particle diameter of 0.03 ⁇ m.
  • the particle size of the silicon powder obtained by the pulverization as described above was confirmed through SEM analysis, and is shown in FIG. 1 .
  • Silicon granules which are silicon raw materials, are put into a hammer mill grinder and pulverized to an average particle diameter of 75 ⁇ m, which is pulverized into silicon particles having an average particle diameter of 5 ⁇ m using an air jet mill.
  • a mixture of 10 kg of the obtained silicon particles having an average particle diameter of 5 ⁇ m and 90 kg of IPA (isopropyl alcohol) is first processed for 2 hours in bead mill 1 using 3 mm zirconia beads, and processed into silicon particles having an average particle diameter of 1 ⁇ m.
  • the obtained silicon particles having an average particle diameter of 0.2 ⁇ m were applied to a microfluidizer having a nozzle diameter of 200 ⁇ m and subjected to primary processing at a pressure of 2500 bar for 30 minutes to obtain silicon nanoparticles having an average particle diameter of 0.15 ⁇ m, which were then subjected to a nozzle diameter of 75 ⁇ m. Silicon nanoparticles with an average particle diameter of 0.08 ⁇ m were made by second processing for 30 minutes at a pressure of 2500 bar by applying to a microfluidizer of .
  • the particle size of the silicon powder obtained by the pulverization as described above was confirmed through SEM analysis, and is shown in FIG. 2 .
  • Silicon granules which are silicon raw materials, are put into a hammer mill grinder and pulverized to an average particle diameter of 75 ⁇ m, which is pulverized into silicon particles having an average particle diameter of 5 ⁇ m using an air jet mill.
  • a mixture of 10 kg of the obtained silicon particles having an average particle diameter of 5 ⁇ m and 90 kg of IPA (isopropyl alcohol) is first processed for 2 hours in bead mill 1 using 3 mm zirconia beads, and processed into silicon particles having an average particle diameter of 1 ⁇ m.
  • the first-processed silicon particles having an average particle diameter of 1 ⁇ m were subjected to secondary processing for 4 hours with a bead mill 2 having a zirconia bead of 0.5 mm to obtain silicon particles having an average particle diameter of 0.5 ⁇ m.
  • the obtained silicon particles having an average particle diameter of 0.5 ⁇ m were applied to a microfluidizer having a nozzle diameter of 200 ⁇ m and subjected to primary processing at a pressure of 2500 bar for 30 minutes to obtain silicon nanoparticles having an average particle diameter of 0.45 ⁇ m, which were then subjected to a nozzle diameter of 75 ⁇ m.
  • Silicon nanoparticles with an average particle diameter of 0.13 ⁇ m were prepared by secondary processing for 30 minutes at a pressure of 2500 bar by applying to a microfluidizer of
  • the particle size of the silicon powder obtained by the pulverization as described above was confirmed through SEM analysis, and is shown in FIG. 3 .
  • Silicon granules which are raw materials for silicon, are put into a hammer mill grinder and pulverized to an average particle diameter of 75 ⁇ m, which is then pulverized into silicon particles having an average particle diameter of 5 ⁇ m using an air jet mill.
  • a mixture of 10 kg of the obtained silicon particles having an average particle diameter of 5 ⁇ m and 90 kg of IPA (isopropyl alcohol) was first processed with a bead mill 1 using 3 mm zirconia beads for 2 hours to obtain silicon particles having an average particle diameter of 1 ⁇ m.
  • the obtained silicon particles having an average particle diameter of 1 ⁇ m were applied to a microfluidizer having a nozzle diameter of 200 ⁇ m and subjected to primary processing at a pressure of 2500 bar for 40 minutes to obtain silicon nanoparticles having an average particle diameter of 0.48 ⁇ m, which were then subjected to a nozzle diameter of 75 ⁇ m. Silicon nanoparticles with an average particle diameter of 0.15 ⁇ m were prepared by applying secondary processing to a microfluidizer of 2500 bar for 40 minutes.
  • the particle size of the silicon powder obtained by the pulverization as described above was confirmed through a particle size analyzer and SEM analysis, and is shown in FIG. 4 .
  • Silicon granules which are raw materials for silicon, are put into a hammer mill grinder and pulverized to an average particle diameter of 75 ⁇ m, which is then pulverized into silicon particles having an average particle diameter of 5 ⁇ m using an air jet mill.
  • a mixture of 10 kg of the obtained silicon particles having an average particle diameter of 5 ⁇ m and 90 kg of IPA (isopropyl alcohol) was first processed with a bead mill 1 using 3 mm zirconia beads for 2 hours to obtain silicon particles having an average particle diameter of 1 ⁇ m.
  • the obtained silicon particles having an average particle diameter of 1 ⁇ m were applied to a microfluidizer having a nozzle diameter of 200 ⁇ m and subjected to primary processing at a pressure of 2000 bar for 40 minutes to obtain silicon nanoparticles having an average particle diameter of 0.85 ⁇ m, which were then subjected to a nozzle diameter of 75 ⁇ m. Silicon nanoparticles with an average particle diameter of 0.5 ⁇ m were made by applying secondary processing to a microfluidizer of 2000 bar pressure for 40 minutes.
  • the particle size of the silicon powder obtained by the pulverization as described above was confirmed through a particle size analyzer and SEM analysis, and is shown in FIG. 5 .
  • Silicon granules which are raw materials for silicon, are put into a hammer mill grinder and pulverized to an average particle diameter of 75 ⁇ m, which is then pulverized into silicon particles having an average particle diameter of 5 ⁇ m using an air jet mill.
  • a mixture of 10 kg of the obtained silicon particles having an average particle diameter of 5 ⁇ m and 90 kg of IPA (isopropyl alcohol) was first processed for 2 hours using a bead mill 1 using 3 mm zirconia beads to obtain silicon particles having an average particle diameter of 1 ⁇ m. .
  • the obtained silicon particles having an average particle diameter of 1 ⁇ m were applied to a microfluidizer having a nozzle diameter of 200 ⁇ m and subjected to primary processing for 40 minutes at a pressure of 3000 bar to obtain silicon nanoparticles having an average particle diameter of 0.4 ⁇ m, which were then subjected to a nozzle diameter of 75 ⁇ m. Silicon nanoparticles with an average particle diameter of 0.12 ⁇ m were made by second processing for 40 minutes at a pressure of 3000 bar by applying to a microfluidizer of
  • the particle size of the silicon powder obtained by the pulverization as described above was confirmed through a particle size analyzer and SEM analysis.
  • the particle size of the pulverized silicon powder was confirmed through a particle size analyzer and SEM analysis, and is shown in FIG. 6 .
  • Silicon granules which are raw materials for silicon, are put into a hammer mill grinder and pulverized to an average particle diameter of 75 ⁇ m, which is then pulverized into silicon particles having an average particle diameter of 5 ⁇ m using an air jet mill.
  • a mixture of 10 kg of the obtained silicon particles having an average particle diameter of 5 ⁇ m and 90 kg of IPA (isopropyl alcohol) is first processed for 2 hours with a bead mill 1 using 3 mm zirconia beads, and processed into silicon particles having an average particle diameter of 1 ⁇ m.
  • the average particle diameter of the silicon particles was processed to 0.5 ⁇ m, and then zirconia beads 0.3 mm beads It was processed into silicon with an average particle diameter of 0.2 ⁇ m by tertiary processing with mill 3 for 8 hours, and fourth processing was performed continuously for 16 hours with a bead mill 4 having an average particle diameter of 0.1 mm to produce silicon particles with an average particle diameter of 0.1 ⁇ m.
  • the silicon particles having an average particle diameter of 0.1 ⁇ m were subjected to a fifth processing with a bead mill 4 having an average particle diameter of 0.1 mm of zirconia beads for 55 to 60 hours to prepare silicon nanoparticles having an average particle diameter of 0.03 ⁇ m.
  • the particle size of the silicon powder obtained by the pulverization as described above was confirmed through a particle size analyzer and SEM analysis, and is shown in FIG. 7 .
  • Table 1 below shows the size of the silicon nanoparticles produced as a result of the process conditions and process duration of Examples 1 to 6 and Comparative Examples.
  • Example 1 Bead mill 1st, 2nd, 3rd, 4th - Microfluidizer 1st and 2nd (pressure 2500bar) 31 hours 30nm (0.03 ⁇ m)
  • Example 2 Bead mill 1st, 2nd, 3rd - Microfluidizer 1st, 2nd (pressure 2500bar) 15 hours 80nm (0.08 ⁇ m)
  • Example 3 - Bead Mill 1st and 2nd - Microfluidizer 1st and 2nd (Pressure 2500bar) 7 hours 130nm (0.13 ⁇ m)
  • Example 4 - Bead Mill 1st and 2nd - Microfluidizer 1st and 2nd Pressure 2500bar) 3 hours 20 minutes 150nm (0.15 ⁇ m)
  • Example 5 Bead Mill 1st and 2nd - Microfluidizer 1st and 2nd (Pressure 2000bar) 3 hours 20 minutes 500nm (0.5 ⁇ m)
  • Example 6 Bead Mill 1st and 2nd - Micro
  • the process conditions and total process time describe only the process conditions and process time for application of the bead mill and the microfluidizer, excluding the process conditions of the hammer mill and the jet mill among the process conditions of Examples 1 to 6 and Comparative Examples.
  • Example 1 relating to the production of silicon nanoparticles of 100 nm or less, compared to Comparative Example of producing silicon nanoparticles of the same size, the time required for the process is only about 1/3, so the method for producing silicon nanoparticles of the present invention Silver is advantageous for the production of silicon nanoparticles of 100 nm or less.
  • the method for manufacturing silicon nanoparticles of the present invention uses a mechanical milling device and a microfluidizer, and unlike conventional methods using plasma, high voltage electric energy, alkaline solution, etc., it is an economical and easy method to manufacture.
  • a mechanical milling device and a microfluidizer unlike conventional methods using plasma, high voltage electric energy, alkaline solution, etc., it is an economical and easy method to manufacture.

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Abstract

L'invention concerne un procédé de fabrication de nouvelles nanoparticules de silicium, comprenant les étapes consistant à : a) préparer des particules de silicium ayant un diamètre moyen de particule inférieur ou égal à 3 µm en utilisant un dispositif de broyage mécanique à grande vitesse pour des granules de silicium, qui sont des matières premières de silicium ; et b) préparer des nanoparticules de silicium ayant un diamètre moyen de particule inférieur ou égal à 500 nm à partir d'un mélange des particules de silicium de l'étape a) et d'un solvant organique en utilisant un microfluidiseur à pression constante.
PCT/KR2020/010577 2020-04-29 2020-08-11 Procédé de fabrication de nouvelles nanoparticules de silicium WO2021221234A1 (fr)

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WO2023128448A1 (fr) * 2021-12-30 2023-07-06 오씨아이 주식회사 Nanoparticules de silicium pour matériau actif d'anode de batterie secondaire et leur méthode de fabrication

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