WO2022007402A1 - Poudre contenant du silicium pour matériau d'électrode négative de batterie au lithium-ion et son procédé de préparation - Google Patents

Poudre contenant du silicium pour matériau d'électrode négative de batterie au lithium-ion et son procédé de préparation Download PDF

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WO2022007402A1
WO2022007402A1 PCT/CN2021/075669 CN2021075669W WO2022007402A1 WO 2022007402 A1 WO2022007402 A1 WO 2022007402A1 CN 2021075669 W CN2021075669 W CN 2021075669W WO 2022007402 A1 WO2022007402 A1 WO 2022007402A1
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silicon
containing powder
negative electrode
powder
lithium ion
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PCT/CN2021/075669
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Chinese (zh)
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胡亮
张少波
方伟
曹德福
夏永生
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马鞍山科达普锐能源科技有限公司
安徽科达铂锐能源科技有限公司
安徽科达新材料有限公司
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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
    • H01M4/362—Composites
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • H01M4/386—Silicon or alloys based on silicon
    • 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
    • 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
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • 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 belongs to the technical field of lithium ion batteries, and in particular relates to a silicon-containing powder for a negative electrode material of a lithium ion battery and a preparation method thereof.
  • the conventional lithium ion anode materials are mainly graphite anodes, but the theoretical specific capacity of graphite anodes is only 372mAh/g, which can no longer meet the urgent needs of users.
  • the theoretical capacity of silicon is as high as 4200mAh/g, which is more than 10 times that of the graphite anode material.
  • the coulombic efficiency of the silicon-carbon composite product is also close to that of the graphite anode, and it is cheap, environmentally friendly, and rich in earth reserves. It is a new generation of high-capacity products. The best choice for negative electrode materials.
  • silicon carbon material has many advantages as the negative electrode material of battery, silicon carbon material inevitably has a certain volume expansion effect during the charging and discharging process, which affects the initial efficiency and cycle performance of the battery. Therefore, there is still a need to find a silicon-containing powder for lithium-ion battery negative electrode materials that can alleviate the volume expansion during charging and discharging, and at the same time achieve the effect of improving electrochemical performance.
  • silicon carbon anode material The most important component of silicon carbon anode material is silicon. Silicon is not only related to the volume expansion coefficient of the anode material during the charge and discharge process, but also greatly affects the electrochemical performance of the anode material. In order to optimize the performance of the anode material, this paper The invention provides a silicon-containing powder for a negative electrode material of a lithium ion battery.
  • the silicon-containing powder contains 50-90 wt.% silicon, 5-30 wt.% oxygen and 5-20 wt.% zirconium.
  • the grain size is below 12nm.
  • the silicon-containing powder is detected by a field emission scanning electron microscope, and it can be observed that the silicon particles and zirconium particles in the silicon-containing powder are irregular in shape, and some zirconium particles have sharp edges and corners and are uniformly dispersed in the silicon particles.
  • the silicon-containing powder contains 55-85 wt.% silicon, and more preferably, the silicon-containing powder contains 65-75 wt.% silicon.
  • the silicon-containing powder is detected by an oxygen, nitrogen and hydrogen analyzer, and the oxygen content can be obtained to be 5-30 wt.%, preferably 10-25 wt.%, more preferably 15-20%.
  • part of the oxygen element exists on the surface of the silicon particles.
  • the part of the oxygen element forms silicon oxide on the surface of the silicon particles.
  • the silicon-containing powder is detected by an inductively coupled plasma emission spectrometer, and it is obtained that the zirconium content is 5-20 wt.%, preferably 10-15 wt.%.
  • the zirconium particles are in the form of zirconium oxide.
  • the silicon-containing powder has a true density of 1.2-2.6 g/cm 3 and a specific surface area of 2-300 m 2 /g.
  • the present invention also relates to a method for preparing the silicon-containing powder for lithium ion battery negative electrode material described in any one of the above, characterized in that:
  • micron silicon powder to the mixing tank matched with the sand mill.
  • the median particle size D50 of the micron silicon powder is 1-1000 ⁇ m, and the purity of the micron silicon powder is ⁇ 99%.
  • solvent to the mixing tank for wet grinding to control the stirring.
  • the solid content of the mixed solution in the tank is 5-40%, start slow stirring, fill the sand mill with 0.05-0.5mm zirconia balls, and control the mass ratio of zirconia beads to silicon powder to be 15:1 ⁇ 20:1, the main engine speed of the sand mill is 900-1000rpm, the grinding time is 10-90h, preferably 35-60h, and the obtained silicon slurry is heated and dried to obtain silicon-containing powder;
  • the structure and shape of the sand mill stirring shaft is a disc type, a rod type or a rod disc type;
  • the grinding solvent is pure water, methanol, toluene, benzyl alcohol, ethanol, ethylene glycol, chlorinated ethanol, propanol, isopropanol, propylene glycol, butanol, n-butanol, isobutanol, amyl alcohol, neopentyl alcohol One or more of alcohol, octanol, acetone or cyclohexanone.
  • the viscosity of the slurry after wet grinding is 0-100 Pa ⁇ s.
  • the solid content of the wet-milled slurry is 5-40%, preferably 10-25%.
  • the present invention also relates to a negative electrode material for a lithium ion battery, which is characterized in that it comprises the silicon-containing powder described in any one of the above in combination with a carbon-based material, wherein the carbon-based material is artificial graphite, natural graphite, porous One or more of layered graphite sheets, soft carbon, hard carbon, graphene, carbon nanotubes, carbon nanofibers, porous carbon, and cracked carbon.
  • the silicon-containing powder prepared by wet grinding of the present invention can significantly reduce its absolute volume expansion during charging and discharging due to the large reduction in macroscopic and microscopic dimensions;
  • the silicon-containing powder prepared by wet grinding of the present invention contains 5-30 wt.% oxygen, which partially exists on the surface of nano-silicon to form silicon oxide, which can reduce the surface activation energy of nano-silicon and form
  • the protective layer on the one hand, can reduce the risk of spontaneous combustion of nanoparticles in the production process and improve the safety factor; on the other hand, silicon oxide can inhibit the volume expansion of nano-silicon during the charging and discharging process, and improve the cycle performance of the negative electrode material;
  • the silicon-containing powder prepared by wet grinding in the present invention contains 5-20 wt.% zirconium.
  • Zirconium is an electrochemically inert component, which will not intercalate and delithiate, and can stabilize the powder structure and further inhibit nano The expansion effect of silicon;
  • the silicon-containing powder prepared by the present invention when used in a negative electrode material, it can provide high specific capacity and excellent cycle performance.
  • Example 1 is a field emission scanning electron microscope image of the silicon-containing powder prepared in Example 1 of the present invention.
  • Example 3 is the XRD data of the silicon-containing powder prepared in Example 1 of the present invention.
  • FIG. 4 is a buckling charge-discharge curve of the negative electrode material prepared in Example 1 of the present invention.
  • a preparation method of a lithium ion battery negative electrode material containing silicon powder comprising the following steps:
  • Preparation of silicon-containing powder Add 1000 g of silicon powder with a median particle size of 1 ⁇ m to the stirring tank equipped with the sand mill, and the purity of the silicon powder is 99.92%, and then add methanol into the stirring tank to control the stirring tank.
  • the solid content of the mixed solution is 10%, start slow stirring, fill the sand mill with 0.3mm zirconia beads, control the mass ratio of zirconia beads to silicon powder to be 15:1, and the speed of the main machine of the sand mill is 1000rpm, grinding for 60h, the obtained silicon slurry, and then the silicon slurry is heated and dried to obtain a silicon-containing powder.
  • the median particle size D50 of the silicon-containing powder is 56nm, and the grain size of silicon is 7.9nm.
  • the silicon powder contained 65.6 wt.% silicon, 26.3 wt.% oxygen and 8.1 wt.% zirconium.
  • Step (2) Preparation of negative electrode material for lithium ion battery:
  • the silicon-containing powder obtained in step (1) is mixed with artificial graphite in a mass ratio of 7:3 to obtain the negative electrode material.
  • a preparation method of a lithium ion battery negative electrode material containing silicon powder comprising the following steps:
  • Preparation of silicon-containing powder Add 1000 g of silicon powder with a median particle size of 50 ⁇ m to the stirring tank matched with the sand mill, and the purity of the silicon powder is 99.53%. Then add propanol to the stirring tank to control the stirring tank. The solid content of the mixed solution is 15%, start slow stirring, fill the sand mill with 0.05mm zirconia beads, control the mass ratio of zirconia beads to silicon powder to be 18:1, and the main engine speed of the sand mill.
  • the median particle size D50 of the silicon-containing powder is 71 nm
  • the grain size of silicon is 8.5 nm
  • the silicon-containing powder is contains 74.4 wt.% silicon, 19.4 wt.% oxygen and 6.2 wt.% zirconium;
  • Step (2) Preparation of negative electrode material for lithium ion battery:
  • the silicon-containing powder obtained in step (1) is mixed with natural graphite and graphene in a ratio of 7:2:1 to obtain the negative electrode material.
  • a preparation method of a lithium ion battery negative electrode material containing silicon powder comprising the following steps:
  • Preparation of silicon-containing powder Add 1000 g of silicon powder with a median particle size of 500 ⁇ m to the stirring tank matched with the sand mill, and the purity of the silicon powder is 99.67%. Then add butanol to the stirring tank to control the stirring tank.
  • the solid content of the mixed solution is 10%, start slow stirring, fill the sand mill with 0.2mm zirconia beads, control the mass ratio of zirconia beads to silicon powder to be 20:1, and the speed of the main machine of the sand mill.
  • the median particle size D50 of the silicon-containing powder is 86 nm
  • the grain size of silicon is 10.3 nm
  • the silicon-containing powder is contains 57.6 wt.% silicon, 24.1 wt.% oxygen and 18.3 wt.% zirconium;
  • Step (2) Preparation of negative electrode material for lithium ion battery:
  • the silicon-containing powder obtained in step (1) is mixed with soft carbon at a ratio of 7:3 to obtain the negative electrode material.
  • a preparation method of a lithium ion battery negative electrode material containing silicon powder comprising the following steps:
  • Preparation of silicon-containing powder Add 1000 g of silicon powder with a median particle size of 1000 ⁇ m to the stirring tank equipped with the sand mill, and the purity of the silicon powder is 99.29%, and then add absolute ethanol to the stirring tank to control the stirring.
  • the solid content of the mixed solution in the tank is 25%, start slow stirring, fill the sand mill with 0.5mm zirconia beads, control the mass ratio of zirconia beads and silicon powder to 20:1, and the host of the sand mill
  • the rotating speed is 950 rpm, grinding is performed for 60 hours, and the obtained silicon slurry is heated and dried to obtain silicon-containing powder.
  • the silicon-containing powder has a median particle size D50 of 102 nm, a grain size of silicon of 11.6 nm, and the silicon-containing powder contains 83.5 wt. % silicon, 5.3 wt. % oxygen and 11.2 wt. % zirconium;
  • step (1) Preparation of negative electrode material for lithium ion battery:
  • the silicon-containing powder obtained in step (1) is mixed with hard carbon and carbon nanometers at a ratio of 7:2:1 to obtain the negative electrode material.
  • step (2) the silicon-containing powder obtained in step (1) is mixed with natural graphite in a mass ratio of 7:3, and the rest are the same as in Example 1, and will not be repeated here.
  • step (2) the silicon-containing powder obtained in step (1) is mixed with soft carbon in a mass ratio of 7:3, and the rest are the same as in Example 1, and are not repeated here.
  • step (2) the silicon-containing powder obtained in step (1) and carbon nanotubes are mixed at a mass ratio of 7:3, and the rest are the same as those in Example 1, which will not be repeated here.
  • Example 1 The difference from Example 1 is that the silicon powder raw material is not nano-sized, and the rest are the same as in Example 1, and will not be repeated here.
  • Example 1 The difference from Example 1 is that the grinding time is adjusted to 10h, and the rest are the same as those in Example 1, which will not be repeated here.
  • Example 1 The difference from Example 1 is that the grinding time is adjusted to 30h, and the rest are the same as those in Example 1, which will not be repeated here.
  • Example 1 The difference from Example 1 is that the grinding time is adjusted to 90h, and the rest are the same as those in Example 1, which will not be repeated here.
  • Example 1 The difference from Example 1 is that zirconia beads are not used, but cemented carbide beads of the same size are used, so that there is no zirconium element in the obtained silicon-containing powder.
  • Example 1 The difference from Example 1 is that dry grinding is performed without adding a grinding solvent, and the rest are the same as in Example 1, and will not be repeated here.
  • the particle size range of the material was tested with a Malvern Mastersizer 3000.
  • the morphology and patterning of the materials were analyzed by field emission scanning electron microscopy (SEM) (JSM-7160).
  • the oxygen, nitrogen and hydrogen analyzer (ONH) is used to accurately and quickly determine the oxygen content in materials.
  • XRD diffractometer (X'Pert3 Powder) was used to analyze the phase of the material to determine the grain size of the material.
  • the true density of the powder was tested by the American Mack true density tester (AccuPyc II 1340).
  • the viscosity of the slurry was measured using a digital display viscometer (NDJ-5S type).
  • the silicon-containing powders described in Examples 1-7 all had a true density of 1.2-2.6 g/cm 3 and a specific surface area of 2-300 m 2 /g; The viscosity is 0 to 100 Pa ⁇ s.
  • the field emission scanning electron microscope image of the silicon-containing powder prepared in Example 1 is shown in Figure 1; the particle size detection data of the silicon-containing powder is shown in Figure 2; the XRD data of the silicon-containing powder is shown in Figure 3; the negative electrode prepared in Example 1 is shown in Figure 2.
  • the charge-discharge curve of the material is shown in Figure 4.
  • the silicon-containing negative electrode materials obtained in Examples 1 to 7 and Comparative Examples 1 to 6 were mixed with negative electrode material, conductive agent carbon black (Super P), carbon nanotubes and LA133 glue in a mass ratio of 91:2:2:5. Solvent pure water, homogenize, control the solid content at 45%, coat on copper foil current collector, vacuum dry to prepare negative pole piece.
  • a button cell was assembled in an argon atmosphere glove box.
  • the charge and discharge test of the button battery is carried out, the voltage range is 5mV ⁇ 1.5V, and the current density is 80mA/g.
  • the first reversible capacity and efficiency of the silicon-containing anode materials in Examples and Comparative Examples were measured.
  • the test equipment of the button battery adopts the LAND battery test system of Wuhan Jinnuo Electronics Co., Ltd.
  • Table 1 is the performance test results of the silicon carbon anode materials in Examples 1-7 and Comparative Examples 1-6
  • the median particle size, silicon grain size, oxygen content and zirconium content of the silicon-containing powder can be adjusted to obtain the negative electrode material with the best comprehensive performance.
  • the first 50-week cycle capacity retention rate of the battery prepared with silicon-containing powder in Example 1 is the best, which is 91.7%, but due to the high oxygen content, the first Coulomb efficiency has a certain loss, which is only 80.4%; in Examples 2-4
  • the oxygen content of the silicon-containing powder gradually decreases, and the first coulombic efficiency of the prepared battery is high, ranging from 81.2 to 84.7%, but its cycle performance has a decreasing trend.
  • the zirconium content of the silicon-containing powder in Example 3 is high, it is beneficial to improve the cycle performance, and the cycle capacity retention rate for the first 50 weeks is 90.2%.
  • the obtained silicon-containing powder when the obtained silicon-containing powder was mixed with natural graphite, soft carbon and carbon nanotubes at a mass ratio of 7:3, respectively, the obtained silicon-carbon negative electrode material had the first capacity and the first Coulomb efficiency.
  • the cycle performance is basically the same as the first 50 weeks. It can be seen that the performance of the silicon carbon anode material is mainly affected by the performance indicators of nano-silicon.
  • Comparative Example 6 when dry grinding was performed without adding an organic solvent, the temperature of the material was too high, and there was agglomeration. The grinding was carried out for only 1 hour, and the material was taken out. The performance of the test was close to that of the silicon powder raw material.
  • the present invention illustrates the detailed process equipment and process flow of the present invention through the above-mentioned embodiments, but the present invention is not limited to the above-mentioned detailed process equipment and process flow, that is, it does not mean that the present invention must rely on the above-mentioned detailed process equipment and process flow. Process flow can be implemented. Those skilled in the art should understand that any improvement of the present invention, the equivalent replacement of each raw material of the product of the present invention, the addition of auxiliary components, the selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

Abstract

La présente invention concerne le domaine technique des batteries au lithium-ion, et concerne spécifiquement une poudre contenant du silicium pour un matériau d'électrode négative de batterie au lithium-ion et un procédé de préparation associé. La poudre contenant du silicium contient de 50 à 90 % en poids de silicium, de 5 à 30 % en poids d'oxygène et de 5 à 20 % en poids de zirconium. La taille moyenne des particules D50 de la poudre contenant du silicium est inférieure ou égale à 110 nm. La poudre contenant du silicium est analysée au moyen de motifs de diffraction des rayons X en fonction de la largeur de demi-pic des pics de diffraction attribués à Si (111) proche de 2θ = 28,4°, et la taille de grain du silicium calculée par la formule de Scherrer est inférieure à 12 nm. Par rapport à la technologie existante, la poudre contenant du silicium préparée par la présente invention peut fournir une capacité spécifique élevée et une excellente performance cyclique lorsqu'elle est utilisée dans un matériau d'électrode négative.
PCT/CN2021/075669 2020-07-06 2021-02-06 Poudre contenant du silicium pour matériau d'électrode négative de batterie au lithium-ion et son procédé de préparation WO2022007402A1 (fr)

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CN104737336A (zh) * 2012-10-26 2015-06-24 日立化成株式会社 锂离子二次电池用负极材料、锂离子二次电池用负极和锂离子二次电池
CN106415897A (zh) * 2014-06-11 2017-02-15 小林光 锂离子电池的负极材料、锂离子电池、锂离子电池的负极或负极材料的制造方法及制造装置
CN111180719A (zh) * 2020-01-07 2020-05-19 马鞍山科达普锐能源科技有限公司 一种三级研磨制备纳米硅的方法
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CN111755679A (zh) * 2020-07-06 2020-10-09 马鞍山科达普锐能源科技有限公司 一种锂离子电池负极材料用含硅粉末及其制备方法
CN111755681A (zh) * 2020-07-06 2020-10-09 马鞍山科达普锐能源科技有限公司 一种锂离子电池用硅碳负极材料及其制备方法

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