WO2023123658A1 - 碳纳米管包覆硅负极材料的方法 - Google Patents

碳纳米管包覆硅负极材料的方法 Download PDF

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WO2023123658A1
WO2023123658A1 PCT/CN2022/079205 CN2022079205W WO2023123658A1 WO 2023123658 A1 WO2023123658 A1 WO 2023123658A1 CN 2022079205 W CN2022079205 W CN 2022079205W WO 2023123658 A1 WO2023123658 A1 WO 2023123658A1
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negative electrode
carbon nanotubes
electrode material
silicon negative
silicon
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French (fr)
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郜天宇
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深圳市纳米港有限公司
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • 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

Definitions

  • the invention relates to the technical field of preparation of negative electrode materials for lithium batteries, in particular to a method for coating silicon negative electrode materials with carbon nanotubes.
  • lithium-ion batteries generally use graphite carbon materials as negative electrodes, and the theoretical capacity of graphite is 372mAh/g. This low capacity limits the energy density of lithium-ion batteries.
  • the theoretical capacity of the silicon negative electrode material is 4200mAh/g, and the theoretical capacity of silicon oxide is 2000mAh/g, which is the first choice for the new generation of battery negative electrode materials.
  • the volume of silicon oxide will expand violently, which will easily cause the capacity of lithium-ion batteries to decrease or even short circuit.
  • one of the solutions is to make a catalyst solution with a catalyst and a solvent, add the silicon material into the catalyst solution so that the catalyst is supported on the surface of the silicon material, and then add it to the carbon source solution so that the carbon source is supported on its surface .
  • the catalyst cannot be evenly loaded on the surface of the silicon material, and the obtained battery has a low gram capacity, and needs to be cleaned with hydrochloric acid, nitric acid, and hydrofluoric acid in the later stage.
  • the silicon material is prone to agglomeration during the drying process after cleaning, which affects the composite use with graphite anode materials.
  • Another solution involves silicon in-situ coating of carbon nanotubes and amorphous carbon, but the obtained carbon tubes are thick and short, the length of the carbon nanotubes is about 3-4 microns, the diameter is about 500 nanometers, and the aspect ratio is 6- 8.
  • the conductivity of the obtained lithium ion negative electrode is not good, so the performance of the obtained product is also limited, the specific capacity is about 1000-1360mAh/g, and the commercial value is also low.
  • silicon or its oxides are used to grow carbon tubes in situ, and coated carbon nanotubes are prepared by attaching metal catalysts to the surface of silicon or its oxides and generating carbon nanotubes on the surface by chemical vapor deposition. tubes of silicon or its silicon oxide. , but this solution cannot remove the metal catalyst impurities, which will aggravate the self-discharge of the battery and affect the storage performance. Moreover, the output is limited, mass production is difficult, and the cost is relatively high.
  • the present invention aims to solve the above problems, and provides a carbon nanotube-coated silicon with uniform coating, good electrical conductivity, small volume expansion, high capacity, no other metal impurities, low manufacturing cost and strong practicability. methods for negative electrode materials.
  • the present invention provides a method for carbon nanotube-coated silicon negative electrode material, the method comprising the following steps:
  • the obtained nanotube-coated silicon negative electrode material is a powder composed of micron-sized particles, and the particle size of the particles is 2 microns to 10 microns.
  • the carbon nanotubes are single-walled carbon nanotubes, double-walled carbon nanotubes, multi-walled carbon nanotubes or a mixture of any two.
  • the carbon nanotube is a fibrous aggregate with a tube diameter of 2-100 nanometers, a length of 5-50 microns, and a bulk density of 0.01-0.1 g/cubic centimeter.
  • the silicon negative electrode material is silicon oxide.
  • the silicon oxide is a particle with a particle diameter of 2-10 microns and a density of 1.1 g/cm3.
  • the thickness of the cladding layer is 2 nanometers to 500 nanometers.
  • the method includes the following steps:
  • the obtained nanotube-coated silicon negative electrode material is a powder composed of micron-sized particles, and the particle size of the particles is 2-10 microns.
  • the contribution of the present invention is that it effectively solves the problems existing in the prior art.
  • the invention realizes the carbon nanotube coating of the silicon negative electrode material through a physical method, and the obtained product has uniform carbon nanotube coating, good electrical conductivity, small volume expansion, and does not bring in other metal impurities.
  • the method can significantly reduce the manufacturing cost, thus having high commercial value and practicability.
  • Multi-walled carbon nanotubes are fibrous aggregates with a diameter of 50 nanometers, a length of 25 microns, and a bulk density of 0.1 g/cm3. During the operation of the coating equipment, the multi-walled carbon nanotubes are dispersed into a network.
  • the carbon nanotubes are embedded in the surface of the silicon oxide. carbon black layer.
  • a carbon nanotube coating layer is formed on the surface of the silicon oxide, and the thickness of the coating layer is 100 nanometers to obtain a silicon negative electrode material coated with carbon nanotubes.
  • the coating equipment is NOBILTA powder processing equipment, which can mix or accurately mix the above two different types of materials in a short time.
  • the nanotube-coated silicon negative electrode material obtained by the coating equipment is a powder composed of micron-sized particles with a particle size of about 5-10 microns, which can be used as a lithium-ion battery negative electrode material.
  • a carbon nanotube coating layer is formed on the surface of the silicon oxide, and the thickness of the coating layer is 100 nanometers to obtain a silicon negative electrode material coated with carbon nanotubes.
  • Described cladding equipment is with embodiment 1.
  • the nanotube-coated silicon negative electrode material obtained by the coating equipment is a powder composed of micron-sized particles, and the particle size of the particles is about 5-10 microns, which can be used as a lithium-ion battery negative electrode material.
  • the nanotube-coated silicon negative electrode material obtained by the coating equipment is a powder composed of micron-sized particles, and the particle size of the particles is about 5-10 microns, which can be used as a lithium-ion battery negative electrode material.
  • a carbon nanotube coating layer is formed on the surface of the silicon oxide, and the thickness of the coating layer is 80 nanometers to obtain a silicon negative electrode material coated with carbon nanotubes.
  • Such coating equipment is commercially available.
  • the nanotube-coated silicon negative electrode material obtained by the coating equipment is a powder composed of micron-sized particles, and the particle size of the particles is about 5-10 microns, which can be used as a lithium-ion battery negative electrode material.
  • the double-walled carbon nanotubes have a diameter of 4 nanometers, a length of 50 microns, and a bulk density of 0.02 grams per cubic centimeter of fibrous aggregates.
  • the composition and morphology of the silicon oxide are the same as in Example 1. Start the cladding equipment and run for 5 minutes at a line speed of 25m/s. During the operation of the coating equipment, the double-walled carbon nanotubes are dispersed into a network. Due to the high linear velocity and shear force, and the surface of the silicon oxide is covered with a layer of carbon black, the carbon nanotubes are embedded in the surface of the silicon oxide.
  • the carbon black layer forms a carbon nanotube coating layer on the surface of silicon oxide, and the thickness of the coating layer is 50 nanometers, so as to obtain a silicon negative electrode material coated with carbon nanotubes.
  • Such coating equipment is commercially available.
  • the nanotube-coated silicon negative electrode material obtained by the coating equipment is a powder composed of micron-sized particles, and the particle size of the particles is about 5-10 microns, which can be used as a lithium-ion battery negative electrode material.
  • the carbon black layer forms a carbon nanotube coating layer on the surface of silicon oxide, and the thickness of the coating layer is 500 nanometers, so as to obtain a silicon negative electrode material coated with carbon nanotubes.
  • Such coating equipment is commercially available.
  • the nanotube-coated silicon negative electrode material obtained by the coating equipment is a powder composed of micron-sized particles with a particle size of about 2-10 microns, which can be used as a negative electrode material for lithium ion batteries.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

一种碳纳米管包覆硅负极材料的方法，该方法包括下列步骤：a、取重量比为0.1～2：99.9～98的碳纳米管粉料和硅负极材料粉料投入包覆设备；b、启动包覆设备，以3～40m/s的转速运转1～20分钟，使碳纳米管在硅负极材料表面形成包覆层，获得碳纳米管包覆的硅负极材料；c、所获得的纳米管包覆的硅负极材料为微米级微粒构成的粉体，其微粒的粒径为5微米～10微米。本发明具有包覆均匀，导电性好，体积膨胀小，高容量，且不会带入其它金属杂质，制造成本低，实用性强等特点。

Description

碳纳米管包覆硅负极材料的方法 【技术领域】
本发明涉及锂电池负极材料制备技术领域，特别是涉及一种碳纳米管包覆硅负极材料的方法。
【背景技术】
目前商业化的锂离子电池普遍以石墨碳材料为负极，而石墨的理论容量为372mAh/g，这种较低的容量限制了锂离子电池的能量密度。而硅负极材料的理论容量为4200mAh/g,氧化亚硅的理论容量为2000mAh/g，其为新一代电池负极材料的首选。然而，由于在锂离子的嵌入与脱出过程中，氧化亚硅体积会发生剧烈的膨胀，极易造成锂离子电池容量下降、甚至短路。
为改善硅与氧化亚硅电化学稳定性，人们做了很多工作。由于碳纳米管有较大的长径比，能够增加硅材料的导电性与力学性能，缓解硅材料体积膨胀的不利影响。但目前大部分的硅材料团聚体与碳纳米管是在电池制备中混浆，或者原位生长方法，不仅过程复杂，成本高，而且工艺繁琐，均一性差。
现有技术中，解决方案之一是将催化剂与溶剂制成催化剂溶液，将硅材料加入催化剂溶液中使催化剂负载在硅材料表面，再将其加入碳源溶液中，使碳源负载在其表面。该方法中，催化剂不能均匀的负载在硅材料表面，得到的电池克容量较低，且后期需要采用盐酸、硝 酸、及氢氟酸清洗。此外，清洗后烘干过程硅材料极易发生团聚，影响与石墨负极材料的复配使用。另外的方案涉及硅原位包覆碳纳米管与无定形碳的方法，但得到的碳管粗而短，其碳纳米管的长度大约3-4微米，直径大约500纳米，长径比6-8，得到的锂离子负极导电性不好，因此得到产品性能也有限，比容量大约1000-1360mAh/g，同样商业价值较低。其它方案中采用硅或其氧化物原位生长碳管的方法，利用将金属催化剂附着在硅或其氧化物表面，通过化学气相沉积法在其表面生成碳纳米管的方式制备出包覆碳纳米管的硅或其硅氧化物。，但该方案不能将金属催化剂杂质去除，将会加剧电池的自放电，影响储存性能。而且产量受限，批量生产困难，成本较高。
【发明内容】
本发明旨在解决上述问题，而提供一种包覆均匀，导电性好，体积膨胀小，高容量，且不会带入其它金属杂质，制造成本低，实用性强的碳纳米管包覆硅负极材料的方法。
为实现上述目的，本发明提供一种碳纳米管包覆硅负极材料的方法，该方法包括下列步骤：
a、取重量比为0.1～2：99.9～98的碳纳米管粉料和硅负极材料粉料投入包覆设备；
b、启动包覆设备，以3～40m/s的转速运转1～20分钟，使碳纳米管在硅负极材料表面形成包覆层，获得碳纳米管包覆的硅负极材料；
c、所获得的纳米管包覆的硅负极材料为微米级微粒构成的粉体， 其微粒的粒径为2微米～10微米。
所述碳纳米管为单壁碳纳米管、双壁碳纳米管、多壁碳纳米管或者任二者的混合物。
所述碳纳米管是管径为2～100纳米，长度为5～50微米，堆密度为0.01～0.1克/立方厘米的纤维状团聚体。
所述硅负极材料为氧化亚硅。
所述氧化亚硅是粒径为2～10微米，密度为1.1克/立方厘米的颗粒。
所述包覆层的厚度为2纳米～500纳米。
在具体实施例中，该方法包括下列步骤：
a、取重量比为2:98的碳纳米管粉料和硅负极材料粉料投入包覆设备；
b、启动包覆设备，以20m/s的转速运转10分钟，使碳纳米管在硅负极材料表面形成包覆层，获得碳纳米管包覆的硅负极材料；
c、所获得的纳米管包覆的硅负极材料为微米级微粒构成的粉体，其微粒的粒径为2微米～10微米。
本发明的贡献在于，其有效解决了现有技术中存在的问题。本发明通过物理方法实现了硅负极材料的碳纳米管包覆，所获得的产物具有碳纳米管包覆均匀，导电性好，体积膨胀小，且不会带入其它金属杂质。该方法可显著降低制造成本，因而具有较高的商业价值高和实用性。
【具体实施方式】
下列实施例是对本发明的进一步解释和说明，对本发明不构成任何限制。
实施例1
取氧化亚硅粉料500克,多壁碳纳米管粉料4克投入包覆设备中，启动该包覆设备，以15m/s的线速度运行5分钟。本实施例中，所述氧化亚硅颗粒的粒径为5～10微米，密度为1.1克/立方厘米。多壁碳纳米管是管径为50纳米，长度为25微米，堆密度为0.1克/立方厘米的纤维状团聚体。包覆设备运行过程中，多壁碳纳米管被分散成网状，由于线速度和剪切力都较大，且氧化亚硅表面有一层碳黑包裹，使得碳纳米管嵌入氧化亚硅表面的炭黑层。包覆完成后，在氧化亚硅表面形成碳纳米管包覆层，该包覆层的厚度为100纳米，获得碳纳米管包覆的硅负极材料。所述包覆设备可商购获得。本实施例中，所述包覆设备为NOBILTA粉体处理设备，其可在短时间内对上述两种不同类别的物料进行混合或精确混合。经该包覆设备所获得的纳米管包覆的硅负极材料为微米级微粒构成的粉体，其微粒的粒径约为5～10微米，其可用作锂离子电池负极材料。
实施例2
取氧化亚硅粉料500克,多壁碳纳米管粉料4克投入包覆设备中，其中，氧化亚硅和多壁碳纳米管的构成及形态同实施例1。启动该包覆设备，以10m/s的线速度运行5分钟。包覆设备运行过程中，多壁碳纳米管被分散成网状，由于线速度和剪切力都较大，且氧化亚硅表 面有一层碳黑包裹，使得碳纳米管嵌入氧化亚硅表面的炭黑层。包覆完成后，在氧化亚硅表面形成碳纳米管包覆层，该包覆层的厚度为100纳米，获得碳纳米管包覆的硅负极材料。所述包覆设备同实施例1。经该包覆设备所获得的纳米管包覆的硅负极材料为微米级微粒构成的粉体，其微粒的粒径约为5～10微米，其可用作锂离子电池负极材料。
实施例3
取氧化亚硅粉料500克,8012单壁碳纳米管0.5克，多壁碳纳米管2克投入包覆设备中，其中，单壁碳纳米管是管径为2纳米，长度为50微米，堆密度为0.01克/立方厘米的纤维状团聚体。所述氧化亚硅、多壁碳纳米管的构成及形态同实施例1。启动该包覆设备，以15m/s的线速度运行5分钟。包覆设备运行过程中，单壁碳纳米管和多壁碳纳米管被分散成网状，由于线速度和剪切力都较大，且氧化亚硅表面有一层碳黑包裹，使得碳纳米管嵌入氧化亚硅表面的炭黑层。包覆完成后，在氧化亚硅表面形成碳纳米管包覆层，该包覆层的厚度为80纳米，获得碳纳米管包覆的硅负极材料。所述包覆设备同实施例1。经该包覆设备所获得的纳米管包覆的硅负极材料为微米级微粒构成的粉体，其微粒的粒径约为5～10微米，其可用作锂离子电池负极材料。
实施例4
取氧化亚硅粉料500克,8012单壁碳纳米管0.5克，NTP3003多壁碳纳米管2克投入包覆设备中，其中，氧化亚硅和单壁碳纳米管、 多壁碳纳米管的构成及形态同实施例3。启动该包覆设备，以15m/s的线速度运行10分钟。包覆设备运行过程中，单壁碳纳米管和多壁碳纳米管被分散成网状，由于线速度和剪切力都较大，且氧化亚硅表面有一层碳黑包裹，使得碳纳米管嵌入氧化亚硅表面的炭黑层。包覆完成后，在氧化亚硅表面形成碳纳米管包覆层，该包覆层的厚度为80纳米，获得碳纳米管包覆的硅负极材料。所述包覆设备可商购获得。经该包覆设备所获得的纳米管包覆的硅负极材料为微米级微粒构成的粉体，其微粒的粒径约为5～10微米，其可用作锂离子电池负极材料。
实施例5
取氧化亚硅粉料500克,9012双壁碳纳米管1克投入包覆设备中，其中，双壁碳纳米管是管径为4纳米，长度为50微米，堆密度为0.02克/立方厘米的纤维状团聚体。所述氧化亚硅构成及形态同实施例1。启动该包覆设备，以25m/s的线速度运行5分钟。包覆设备运行过程中，双壁碳纳米管被分散成网状，由于线速度和剪切力都较大，且氧化亚硅表面有一层碳黑包裹，使得碳纳米管嵌入氧化亚硅表面的炭黑层，在氧化亚硅表面形成碳纳米管包覆层，该包覆层的厚度为50纳米，获得碳纳米管包覆的硅负极材料。所述包覆设备可商购获得。经该包覆设备所获得的纳米管包覆的硅负极材料为微米级微粒构成的粉体，其微粒的粒径约为5～10微米，其可用作锂离子电池负极材料。
实施例6
取氧化亚硅粉料500克,NTP3023多壁碳纳米管10.2克投入包覆设备中，其中，氧化亚硅和多壁碳纳米管的构成及形态同实施例1。启动该包覆设备，以25m/s的线速度运行20分钟。包覆设备运行过程中，多壁碳纳米管被分散成网状，由于线速度和剪切力都较大，且氧化亚硅表面有一层碳黑包裹，使得碳纳米管嵌入氧化亚硅表面的炭黑层，在氧化亚硅表面形成碳纳米管包覆层，该包覆层的厚度为500纳米，获得碳纳米管包覆的硅负极材料。所述包覆设备可商购获得。经该包覆设备所获得的纳米管包覆的硅负极材料为微米级微粒构成的粉体，其微粒的粒径约为2～10微米，其可用作锂离子电池负极材料。
尽管通过以上实施例对本发明进行了揭示，但本发明的保护范围并不局限于此，在不偏离本发明构思的条件下，对以上各构件所做的变形、替换等均将落入本发明的权利要求范围内。

Claims (7)

  1. 一种碳纳米管包覆硅负极材料的方法，其特征在于，该方法包括下列步骤：
    a、取重量比为0.1～2：99.9～98的碳纳米管粉料和硅负极材料粉料投入包覆设备；
    b、启动包覆设备，以3～40m/s的转速运转1～20分钟，使碳纳米管在硅负极材料表面形成包覆层，获得碳纳米管包覆的硅负极材料；
    c、所获得的纳米管包覆的硅负极材料为微米级微粒构成的粉体，其微粒的粒径为2微米～10微米。
  2. 如权利要求1所述的方法，其特征在于，所述碳纳米管为单壁碳纳米管、双壁碳纳米管、多壁碳纳米管或者任二者的混合物。
  3. 如权利要求2所述的方法，其特征在于，所述碳纳米管是管径为2～100纳米，长度为5～50微米，堆密度为0.01～0.1克/立方厘米的纤维状团聚体。
  4. 如权利要求1所述的方法，其特征在于，所述硅负极材料为氧化亚硅。
  5. 如权利要求4所述的方法，其特征在于，所述氧化亚硅是粒径为2～10微米，密度为1.1克/立方厘米的颗粒。
  6. 如权利要求1所述的方法，其特征在于，所述包覆层的厚度为2纳米～500纳米。
  7. 如权利要求1所述的方法，其特征在于，该方法包括下列步 骤：
    a、取重量比为2:98的碳纳米管粉料和硅负极材料粉料投入包覆设备；
    b、启动包覆设备，以20m/s的转速运转10分钟，使碳纳米管在硅负极材料表面形成包覆层，获得碳纳米管包覆的硅负极材料；
    c、所获得的纳米管包覆的硅负极材料为微米级微粒构成的粉体，其微粒的粒径为2微米～10微米。
PCT/CN2022/079205 2021-12-28 2022-03-04 碳纳米管包覆硅负极材料的方法 WO2023123658A1 (zh)

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