SE547243C2 - A method for fabrication of nanostructured silicon and carbon composite - Google Patents

A method for fabrication of nanostructured silicon and carbon composite

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Publication number
SE547243C2
SE547243C2 SE2251361A SE2251361A SE547243C2 SE 547243 C2 SE547243 C2 SE 547243C2 SE 2251361 A SE2251361 A SE 2251361A SE 2251361 A SE2251361 A SE 2251361A SE 547243 C2 SE547243 C2 SE 547243C2
Authority
SE
Sweden
Prior art keywords
silicon
reaction chamber
organic compound
carbon material
inert gas
Prior art date
Application number
SE2251361A
Other languages
Swedish (sv)
Other versions
SE2251361A1 (en
Inventor
Mojtaba Gilzad Kohan
Rosa Maria Pineda Huitron
Original Assignee
Granode Mat Ab
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Granode Mat Ab filed Critical Granode Mat Ab
Priority to SE2251361A priority Critical patent/SE547243C2/en
Publication of SE2251361A1 publication Critical patent/SE2251361A1/en
Publication of SE547243C2 publication Critical patent/SE547243C2/en

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Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/13Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/133Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/24Deposition of silicon only
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/38Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H01M4/386Silicon or alloys based on silicon
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/182Graphene
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/20Graphite
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Electrochemistry (AREA)
  • Nanotechnology (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Composite Materials (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

There is provided a composite material comprising a carbon material, wherein the carbon material comprises at least one selected from the group consisting of graphite, graphene, few-layer graphene, and reduced graphene oxide, wherein particles comprising silicon are on the surface of the carbon material, wherein the particles have an average particle size in the interval 10 - 400 nm, wherein at least a part of the particles have partially diffused into the carbon material. There is also provided a method for manufacturing the material. An advantage is that homogeneous decoration of the particles comprising silicon on the carbon material, improves the processability of the consequent Siparticle/carbon composite, avoiding aggregations and agglomerations, which are commonly occurring in nanomaterials processing methods. Reducing the postprocessing routes such as ultra-sonication, and high shear mixing associated is an advantage for industrialapplications.

Claims (30)

1.A method for preparation of a composite material, Claims the method comprising the steps: a)providing
2.The method according to claim 1, i)solid silicon, wherein the silicon is provided in micronanostructure form with an average size in the interval 0.2 - 10 um, wherein the average size is calculated according to ISO 9276-2:2014 using the method of moments starting from a size distribution measured according to ISO 13320:2020 and ii) a carbon material comprising at least one selected from the group consisting of graphite, graphene, few-layer graphene, reduced graphene oxide, and carbon black, and, heating the silicon and the carbon material in a reaction chamber, wherein the reaction chamber comprises an inert gas and hydrogen gas, wherein the heating is to a temperature in the range 400 - 1000 °C, wherein the temperature is within the range during a total time in the interval 0.5 - 24 hours, wherein the pressure in the reaction chamber is from 0.02 to 1.0 atm, wherein the hydrogen reacts with the silicon to form at least one of SiH4 and Sifih, which at least partially react and form silicon nanostructures on the carbon material. wherein the hydrogen gas is added to the reaction chamber.
.The method according to any one of claims 1-2, wherein at least one organic compound is added to the reaction chamber, wherein the organic compound is selected so that it decomposes to form at least hydrogen gas at the temperature in the reaction chamber.
.The method according to any one of claims 1-3, wherein a catalytic metal is present during step b) and wherein the catalytic metal is at least one selected from the group consisting of Al and Fe.
.The method according to any one of claims 1-4, wherein the silicon comprises less than 10000 ppm Al calculated by weight.
.The method according to claim 3, wherein the organic compound decomposes to at least compound selected from the group consisting of CO, C02, CH4, OH, H20 in addition to hydrogen gas.
.The method according to any one of claims 1-6, wherein a reaction of hydrogen with the silicon to form at least one of SiH4 and Sififi, and a deposition as nanostructures on the carbon material, occurs at least partially simultaneously during step b).
The method according to any one of claims 1-7, wherein the content of silicon in the reaction chamber is in the interval 1 - 40 wt%.
.The method according to any one of claims 1-8, wherein the weight ratio of the silicon to the carbon material provided in step a) is from 1:20 to 20:
10. The method according to any one of claims 1-9, wherein the reaction chamber during step b) comprises less than 0.05 wt%
11. The method according to any one of claims 1-10, wherein the silicon is a recycling grade silicon slag from phosphoric acid manufacturing.
12. The method according to any one of claims 1-10, wherein the silicon is a commercial grade pure elemental silicon.
13. The method according to any one of claims 1-12, wherein the nanostructures deposited on the carbon material are particles with an average particle size in the interval 10 - 400 nm, wherein the average particle size is calculated according to ISO 9276-2:2014 using the method of moments starting from a particle size distribution measured from scanning electron microscope images according to ISO 19749:
14. The method according to any one of claims 1-13, wherein the reaction chamber is a tube furnace.
15. The method according to any one of claims 1-14, wherein the reaction chamber is flushed with at least one inert gas before the method is performed.
16. The method according to any one of claims 1-15, wherein the inert gas is at least one selected from the group consisting of Ng and Ar.
17. The method according to any one of claims 3 or 6, wherein the organic compound is liquid at room temperature and where the organic compound is fed into the container by bubbling the inert gas through the liquid organic compound so that the liquid organic compound at least partially evaporates and so that the inert gas carries the organic compound in gas phase into the reaction chamber.
18. The method according to any one of claims 3 or 6, wherein the organic compound is added in gas phase into the reaction chamber.
19. The method according to any one of claims 1-18, wherein a flow of the inert gas into the reaction chamber is from 100 to 1000 standard cubic centimeter per minute, wherein the standard cubic centimeter per minute is calculated for T = 0 °C and p = 1.01 bar.
20. The method according to any one of 1-19, wherein a flow of the at least one inert gas is into the reaction chamber from 400 to 600 standard cubic centimeter per minute for every 1 kg of the total weight of the silicon and the carbon material provided in step a), wherein the standard cubic centimeter per minute is calculated for T = 0 °C and p = 1.01 bar.
21. The method according to any one of 1-20, wherein the formed silicon nanostructures on the carbon material are in the form of particles and nano-islands.
22. The method according to any one of 1-21, wherein the carbon material provided in step a) is in powder form.
23. The method according to any one of claims 1-22, wherein the reaction chamber contains at least one selected from Cb). and CO during at least a part of step The method according to any one of claims 3, 6, 17 or 18, wherein the at least one organic compound is at least one compound selected from the group ketones, consisting of alcohols, and aromatic organic compounds. The method according to any one of claims 3, 6, 17, 18, and 24, wherein the at least one organic compound is at least one compound selected from the butanol, group consisting of ethanol, methanol, isobutanol, hexanol, acetone, styrene, and xylene. The method according to any one of claims 1-25, wherein the heating in step b) is performed with a heating rate in the interval 4-20 °C/min. The method according to any one of claims 1-26, wherein the composite material obtained after step b) is separated with centrifugation. The method according to any one of claims 1-27, wherein the composite material obtained after step b) is suspended in a solvent where after it is dried. The method according to any one of claims 1-28, wherein the silicon and the carbon provided in step a) are milled before introduction into the reaction chamber. The method according to any one of claims 3, 6, 17, and 18, wherein the organic compound is added during step b).
SE2251361A 2022-11-21 2022-11-21 A method for fabrication of nanostructured silicon and carbon composite SE547243C2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
SE2251361A SE547243C2 (en) 2022-11-21 2022-11-21 A method for fabrication of nanostructured silicon and carbon composite

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
SE2251361A SE547243C2 (en) 2022-11-21 2022-11-21 A method for fabrication of nanostructured silicon and carbon composite

Publications (2)

Publication Number Publication Date
SE2251361A1 SE2251361A1 (en) 2024-05-22
SE547243C2 true SE547243C2 (en) 2025-06-10

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SE (1) SE547243C2 (en)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018032975A1 (en) * 2016-08-15 2018-02-22 福建新峰二维材料科技有限公司 Manufacturing method of lithium-ion battery negative-electrode material effectively buffering volume change effect of silicon
WO2018032977A1 (en) * 2016-08-15 2018-02-22 福建新峰二维材料科技有限公司 Manufacturing method of negative-electrode material for lithium-ion battery
CN112028067A (en) * 2020-09-02 2020-12-04 南京同宁新材料研究院有限公司 Silicon-carbon negative electrode material and preparation method thereof
CN112635733B (en) * 2020-12-21 2021-12-31 江苏集芯半导体硅材料研究院有限公司 Negative electrode material of lithium ion battery, preparation method of negative electrode material and lithium ion battery

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018032975A1 (en) * 2016-08-15 2018-02-22 福建新峰二维材料科技有限公司 Manufacturing method of lithium-ion battery negative-electrode material effectively buffering volume change effect of silicon
WO2018032977A1 (en) * 2016-08-15 2018-02-22 福建新峰二维材料科技有限公司 Manufacturing method of negative-electrode material for lithium-ion battery
CN112028067A (en) * 2020-09-02 2020-12-04 南京同宁新材料研究院有限公司 Silicon-carbon negative electrode material and preparation method thereof
CN112635733B (en) * 2020-12-21 2021-12-31 江苏集芯半导体硅材料研究院有限公司 Negative electrode material of lithium ion battery, preparation method of negative electrode material and lithium ion battery

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
M.H. Parekh et al., "Encapsulation and networking of silicon nanoparticles using amorphous carbon and graphite for high performance Li-ion batteries", Carbon, vol. 148, 36 (2019); DOI: 10.1016/j.carbon.2019.03.037 *
Q. Man et al., "Interfacial design of silicon/carbon anodes for rechargeable batteries: A Review", Journal of Energy Chemistry, vol. 76, 576 (2023) [Available online 16 September 2022]; DOI: 10.1016/j.jechem.2022.09.020 *
Z.-L. Xu et al., "Electrospun carbon nanofiber anodes containing monodispersed Si nanoparticles and graphene oxide with exceptional high rate capacities", Nano Energy, vol. 6, 27 (2014); DOI: 10.1016/j.nanoen.2014.03.003 *

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