WO2016176928A1 - Matériau d'électrode négative, son procédé de préparation, et pile rechargeable lithium-ion utilisant le matériau d'électrode négative - Google Patents

Matériau d'électrode négative, son procédé de préparation, et pile rechargeable lithium-ion utilisant le matériau d'électrode négative Download PDF

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WO2016176928A1
WO2016176928A1 PCT/CN2015/087882 CN2015087882W WO2016176928A1 WO 2016176928 A1 WO2016176928 A1 WO 2016176928A1 CN 2015087882 W CN2015087882 W CN 2015087882W WO 2016176928 A1 WO2016176928 A1 WO 2016176928A1
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ion secondary
secondary battery
lithium
soil
lithium ion
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PCT/CN2015/087882
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English (en)
Chinese (zh)
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陈军
胡小飞
程方益
张宁
丛亮
张凯
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南开大学
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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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • 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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
    • 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 a lithium ion secondary battery anode material and a preparation method thereof, and a lithium ion secondary battery using the anode material, in particular to a low cost and wide source soil as a negative electrode material for a lithium ion secondary battery and a preparation method thereof And a negative electrode made of the negative electrode material and lithium nickel cobalt aluminate (LiNi x Co y Al 1-xy O 2 , 0.8 ⁇ x ⁇ 0.92, 0.05 ⁇ y ⁇ 0.11, x+y ⁇ 1, abbreviated as NCA) cathode material
  • the lithium ion secondary battery is particularly characterized by room temperature chargeability, low cost, high rate and long life.
  • Still another object of the present invention is to provide a negative electrode material using a soil as a lithium ion secondary battery, which is assembled with a lithium nickel cobalt aluminate (NCA) positive electrode material into a lithium ion secondary battery, and the lithium ion secondary battery is particularly provided Room temperature can be charged, low cost, high rate and long life.
  • NCA lithium nickel cobalt aluminate
  • the mass percentage of the treated soil, the conductive agent and the binder is 40-10% of the conductive agent, 15-5% of the binder, and the remaining amount of the treated soil, and the current collector is foamed nickel or copper foil. Or foamed copper.
  • the mass percentage of the NCA, the conductive agent and the binder is 15-5% of the conductive agent, 10-5% of the binder, and the balance of the NCA, and the current collector is a foamed nickel or aluminum foil.
  • the binder and dispersant are polyvinylidene fluoride (PVdF) and N-methylpyrrolidone (NMP) or sodium carboxymethylcellulose (NaCMC) and water, respectively. 0.04 to 0.06 mL of dispersant is required for 1 mg of binder.
  • the invention provides a lithium ion secondary battery anode material, a preparation method thereof and a lithium ion secondary battery using the anode material, and the lithium ion secondary battery is particularly characterized by room temperature chargeability, low cost, high rate and long life.
  • the anode material of the present invention smooth treated soil
  • the anode material of the present invention is convenient to prepare, has a wide range of raw materials, and is relatively inexpensive, compared to the lithium ion battery that has been reported so far.
  • Fig. 3 is a Raman spectrum of the soil after the ball milling speed of 400 r min -1 of Example 1.
  • FIG. 4 is a graph showing charge and discharge curves of the button-type soil electrode A/lithium half-cell of Example 1 in the first two weeks at a current density of 0.2 Ag-1.
  • A is the soil after 400r min-1 ball milling treatment.
  • Fig. 5 is an X-ray diffraction diagram of soil after the ball milling speed of 650 rpm -1 of Example 2.
  • Fig. 6 is a scanning electron micrograph of the soil after the ball milling speed of 650 r min -1 of Example 2.
  • Figure 8 is a graph showing the charge and discharge curves of the button-type soil electrode B/lithium half-cell of Example 2 in the first two weeks at a current density of 0.2 Ag -1 .
  • B is the soil after 650r min-1 ball milling treatment.
  • Figure 9 is a graph showing the cycle performance of the button-type soil electrode B/lithium half-cell of Example 2 at a current density of 0.2 Ag -1 .
  • Fig. 10 is a graph showing the rate performance of the button-type soil electrode B/lithium half-cell of Example 2.
  • Figure 11 is a graph showing the charge and discharge curves of the button-type soil electrode C/lithium half-cell of Example 3 for the first two weeks at a current density of 0.2 Ag -1 .
  • C is the soil after 650r min-1 ball milling treatment.
  • Figure 12 is a graph showing the charge and discharge curves of the button-type soil electrode D/lithium half-cell of Example 4 in the first two weeks at a current density of 0.2 Ag -1 .
  • D is the soil after 650r min-1 ball milling treatment.
  • Figure 14 is a graph showing the cycle performance of a button-type NCA/soil electrode B full cell at a current density of 0.1 Ag -1 .
  • Figure 16 is a graph showing the cycle performance of Example 6, Model 18650 NCA/soil cell at 4 A current.
  • Figure 17 is a graph showing the charge and discharge curves for the first two weeks of a 0.1 N -1 current density of a comparative button NCA/KS6 full cell.
  • the soil load, soil electrode, soil anode, button soil or soil (whole) battery described in the description herein refers to the soil obtained by heating, calcination heat treatment and ball milling.
  • the lithium ion secondary battery anode material provided by the invention comprises: calcined and ball-milled soil, and the element distribution after calcination is: Si 30-40wt%, Al 3-4wt%, Fe 3-4wt%, Ca 1-2wt %, K 1-2 wt%, Na 0.1-0.5 wt%, O 52-60 wt%, and others are 0.01-0.05 wt% of trace elements (refer to other substances other than the above-mentioned elements contained in the soil, which are trace elements).
  • the steps of the soil pretreatment method are as follows:
  • the soil raw materials were collected from the campus of Nankai University, and the soil was heated to 750 ° C for 2 h in a muffle furnace.
  • the calcined soil was placed in a ball mill tank for ball milling, ball milling time 20 h, rotation speed 400 r min -1 .
  • ball mill tank volume is 98cm 3 , inner diameter 5cm, height 5cm, the soil mass is 6g each time, the total mass of zirconium balls is 30g, and the zirconium balls are 0.5cm and 1cm. the same).
  • the obtained product was subjected to XRD test to prove that the main component of the treated soil was SiO 2 (Fig. 1, ball mill speed 400 r min -1 ), wherein the diffraction peak of SiO 2 coincided with JCPDS card number 83-2466.
  • Scanning electron micrographs show a particle size of about 1.5 ⁇ m (Fig. 2, ball mill speed 400 r min -1 ), and a tap density of 0.9 g cm -3 .
  • the main element distribution of the soil obtained after the treatment O, 57.31 wt%; Si, 33.13 wt%; Al, 3.16 wt%; Fe, 3.07 wt%; Ca, 1.26 wt%; K, 1.90 wt%; Na, 0.16 wt%, other trace elements 0.01 wt%.
  • the treated soil, Vulcan XC-72, and PVdF were added to NMP in a mass ratio of 5:4:1 to prepare a slurry, uniformly coated on the foamed nickel, and subjected to a temperature of 100 ° C and a pressure of 0.1 MPa. Dry for 10h. Then, the baked electrode sheet was kneaded into a 12 mm wafer, and pressed at a pressure of 5 MPa for 10 s to obtain a soil electrode A having a soil loading of 1 mg cm -2 and a thickness of 0.5 mm.
  • the above soil electrode sheet and lithium sheet (diameter 14 mm, thickness 0.3 mm) were assembled into a CR2032 type button type half battery.
  • the diaphragm is a glass fiber filter paper (diameter 16mm, thickness 0.3mm, porosity 92-98%), the electrolyte is 1M LiPF 6 EC-DEC mixed solution (EC and DEC volume ratio is 1:1), the battery assembly process is in It is carried out in a glove box filled with Ar gas.
  • FIG. 4 is a graph showing the charge and discharge curves for the first week and the second week of a button-type soil electrode A/lithium half-cell at a current of 0.1 Ag -1 . It can be seen from the graph that a shorter discharge platform appears at around 0.8V in the first week, and the specific discharge capacity is 880mAh g -1 ; the second discharge shows a longer discharge platform at around 0.2V, and the specific discharge capacity is 432mAh g -1 , the large irreversible capacity is due to the formation of the SEI film.
  • the steps of the soil pretreatment method are as follows:
  • Soil materials were collected from the campus of Nankai University, and the soil was heated to 750 °C for 2 h in a muffle furnace. The calcined soil was placed in a ball mill jar for ball milling, ball milling time 20 h, and rotation speed 650 r min -1 .
  • Specific ball milling conditions ball mill tank volume is 98cm 3 , inner diameter 5cm, height 5cm, the soil mass is 6g each time, the total mass of zirconium balls is 30g, and the zirconium balls are 0.5cm and 1cm. the same).
  • the main element distribution of the soil obtained after the treatment O, 57.21 wt%; Si, 33.23 wt%; Al, 3.06 wt%; Fe, 3.17 wt%; Ca, 1.24 wt%; K, 1.92 wt%; Na, 0.16 wt%, other trace elements 0.01 wt%.
  • Figure 8 is a graph showing the charge and discharge curves of the first week and the second week of a button-type soil electrode B/lithium half-cell at a current of 0.1 Ag -1 . It can be seen from the graph that the discharge platform appears at 0.8 and 0.2V in the first week, and the specific discharge capacity is 1400 mAh g -1 ; the second discharge shows a longer discharge platform at 0.01 to 1 V, and the specific discharge capacity is 660 mAh g - 1. The large irreversible capacity is due to the formation of the SEI film. Fig.
  • FIG. 9 is a cycle performance diagram of a button-type soil electrode B/lithium half-cell at a current density of 0.1 Ag -1 , and the discharge specific capacity is stabilized at 500 mAh g -1 after a cycle of 50 weeks, and the capacity retention ratio is 91.5% (compared with On the fifth lap, the Coulomb efficiency was 98.6%.
  • Figure 10 is a graph showing the rate performance of a button-type soil electrode B/lithium half-cell, showing discharge specific capacities of 500-600, 400, and 350 mAh g -1 at current densities of 0.1, 0.2, and 0.3 A g -1 , respectively. .
  • the diaphragm is a glass fiber filter paper (diameter 16mm, thickness 0.3mm, porosity 92-98%), the electrolyte is 1M LiPF 6 EC-DEC mixed solution (EC and DEC volume ratio is 1:1), the battery assembly process is in It is carried out in a glove box filled with Ar gas.
  • FIG. 11 is a graph showing the charge and discharge curves of the first week and the second week of a button-type soil electrode C/lithium half-cell at a current of 0.1 Ag -1 . It can be seen from the graph that the discharge platform appears between 0.01 and 1.3V in the first week, the specific discharge capacity is 1200mAh g -1 ; the discharge platform appears between 0.01 and 1.2V in the second week, and the specific discharge capacity is 550mAh g. -1 , the large irreversible capacity is due to the formation of the SEI film.
  • the treated soil, KS6 and PVdF were added to NMP in a mass ratio of 5:4:1 to prepare a slurry, uniformly coated on the foamed nickel, and dried at a temperature of 100 ° C and a pressure of 0.1 MPa for 10 hours. . Then, the baked electrode sheet was kneaded into a 12 mm wafer, and pressed at a pressure of 5 MPa for 10 s to obtain a soil electrode D having a soil loading of 1 mg cm -2 and a thickness of 0.5 mm.
  • the above soil electrode sheet and lithium sheet (diameter 14 mm, thickness 0.3 mm) were assembled into a CR2032 type button type half battery.
  • the diaphragm is a glass fiber filter paper (diameter 16mm, thickness 0.3mm, porosity 92-98%), the electrolyte is 1M LiPF 6 EC-DEC mixed solution (EC and DEC volume ratio is 1:1), the battery assembly process is in It is carried out in a glove box filled with Ar gas.
  • FIG. 12 is a graph showing the charge and discharge curves for the first week and the second week of a button-type soil electrode D/lithium half-cell at a current of 0.1 Ag -1 . It can be seen from the graph that there are two discharge platforms between 0.01 and 1.3V in the first week, the specific discharge capacity is 1370mAh g -1 ; the second week is between 0.01 and 1.2V, a continuous discharge platform, discharge ratio The capacity is 620 mAh g -1 , and the large irreversible capacity is due to the formation of the SEI film.
  • the soil pretreatment method and the soil electrode preparation method are the same as those in the first embodiment.
  • the preparation method of LiNi 0.81 Co 0.1 Al 0.09 O 2 can be found in the literature: Jo, M., Noh, M., Oh, P., Kim, Y., Cho, J., A New High Power LiNi 0.81 Co 0.1 Al 0.09 O 2 Cathode Material for Lithium-Ion Batteries. Adv. Energy Mater., 2014, 4: 1301583.
  • the preparation method is as follows: The first step is the preparation of a Ni 0.89 Co 0.11 (OH) 2 precursor.
  • nickel sulfate hexahydrate and cobalt sulfate heptahydrate were placed in a 2M aqueous solution at a molar ratio of 9:1 and stirred in a 7 L reactor.
  • a 2M sodium hydroxide solution and an appropriate amount of ammonium hydroxide solution were separately added as a chelating agent to the above reactor and maintained at a pH of 50 ° C and pH 11.
  • the green coprecipitated powder was washed by centrifugation and dried under vacuum at 80 ° C overnight (14 h).
  • the second step is the preparation of the final product.
  • the above 2 mg precursor and aluminum acetate were dissolved in 30 mL of ethanol and stirred vigorously for 1 h.
  • FIG. 13 shows the charge-discharge curves of the first and second weeks of the button NCA/soil electrode B battery at 0.1Ag -1 current. It can be seen from the graph that the first week has a tilted discharge at around 2.5V.
  • the platform has a specific discharge capacity of ⁇ 160 mAh g -1 .
  • Figure 14 is a cycle performance diagram of a button-type NCA/soil electrode B full cell at a current density of 0.1 Ag -1 . After 200 cycles, the discharge specific capacity is stabilized at 140 mAh g -1 , and the capacity retention rate is 87.5%. Coulomb efficiency Is >95%.
  • the soil pretreatment method was the same as in Example 1.
  • the main element distribution of the soil obtained after the treatment O, 57.31 wt%; Si, 33.13 wt%; Al, 3.16 wt%; Fe, 3.07 wt%; Ca, 1.26 wt%; K, 1.90 wt%; Na, 0.16 wt%, other trace elements 0.01 wt%.
  • NCA The preparation method of NCA is the same as that of Example 5.
  • NCA LiNi 0.81 Co 0.1 Al 0.09 O 2 , lithium nickel cobalt aluminate, NCA
  • carbon black carbon black
  • PVdF PVdF
  • each battery was composed of two positive electrode sheets and three negative electrode sheets stacked together, and the electrolytic solution was the same as in Example 1, and the separator was Celgard 2340 (diameter: 16 mm, thickness: 30 mm).
  • the 18650 battery has a diameter of 18mm and a height of 65mm. The total mass of the battery is 50g, and the humidity in the battery assembly workshop is controlled below 3%.
  • Figure 15 shows the charge and discharge curves of the first and second weeks of the 18650 NCA/soil battery at 4A. From the graph, the first week discharge capacity is 3000mAh, the average voltage is 2.55V; the second week discharge The capacity is 3100 mAh g -1 and the average voltage is 2.55V.
  • Figure 16 is a cycle performance diagram of a 18650 NCA/soil cell at 4 A. The discharge capacity is stable at 3200 mAh g -1 after 100 cycles, the capacity retention is -100%, and the coulombic efficiency is 84-99%.
  • FIG. 17 shows the charge and discharge curves of the first week and the second week of the button NCA/KS6 full cell at a current density of 0.1A g -1 . It can be seen from the graph that the discharge platform appears at about 2.6V in the first week, and the discharge occurs. The specific capacity was 153.6 mAh g -1 ; a similar discharge platform appeared at around 2.6 V in the second week, and the specific discharge capacity was 155.8 mAh g -1 .
  • Figure 18 is a cycle performance diagram of the button-type NCA/KS6 full cell density at 0.1Ag -1 current. After 100 cycles, the discharge specific capacity is 108.3mAh g -1 , the capacity retention rate is 98.6%, and the coulombic efficiency is 88.7%.
  • Example 2 It can be seen from Table 1 that the button soil/Li half cell of Example 2 has a higher discharge specific capacity. Compared with Example 1, the higher ball milling speed converts the crystalline SiO 2 to amorphous SiO 2 , which is advantageous for the improvement of the lithium intercalation capacity. Compared with Example 3, a higher conductive carbon content favors a decrease in discharge potential and an increase in capacity. Conductive carbon Vulcan XC-72 has a similar effect as KS6 compared to Example 4.
  • the button type NCA/soil full battery of Example 5 has good cycle performance and high discharge specific capacity.
  • the batteries still have capacity retention rates of 107%, 106%, 102%, and 91% at 10, 50, 100, and 200 weeks, which is significantly higher than the button-type NCA/KS6 full battery in the comparative example.
  • having a soil anode facilitates the insertion and extraction of lithium ions, thereby improving the electrochemical performance of the battery as a whole.
  • the addition of conductive carbon and inactive substances in the soil (such as aluminosilicate) provide an effective buffer for the volume change generated during charging and discharging, and improve the life of the battery.
  • the invention provides a lithium ion secondary battery anode material, a preparation method thereof and a lithium ion secondary battery using the anode material, and the lithium ion secondary battery is particularly characterized by room temperature chargeability, low cost, high rate and long life. .
  • the pressing load at the time of electrode formation is small, the discharge capacity is large, the charge and discharge efficiency is high, and the load characteristics are excellent.
  • the anode material of the present invention smooth treated soil
  • the present invention can be widely used in various fields of application using lithium secondary batteries, for example, in the field of electronic devices.
  • the soil anode of the invention has the advantages of low cost, easy availability, wide source, simple synthesis and sex Can be excellent and so on. Therefore, in the industrial production field of lithium secondary batteries, it has great application value, and it is expected to become a commercial lithium ion battery negative electrode in the future.

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Abstract

La présente invention concerne un matériau d'électrode négative, son procédé de préparation, et une pile rechargeable lithium-ion utilisant le matériau d'électrode négative. La pile rechargeable lithium-ion est assemblée avec de la terre traitée et bon marché provenant d'un grand choix de sources et utilisée comme matériau d'électrode négative, et de l'aluminate de lithium-nickel-cobalt utilisé comme matériau d'électrode positive. Une membrane à trois couches constituée par du polyéthylène, du polypropylène et du polyéthylène, ou un papier de fibres de verre, sert de séparateur. Un électrolyte ester/sel contenant du lithium sert de solution électrolytique. Un ou plusieurs éléments parmi le noir d'acétylène, du Super P, du KS6, des nanotubes de carbone, du graphène et du Vulcan XC-72 sont mélangés pour servir d'agent conducteur. Un agent de liaison et un solvant utilisés respectivement sont du poly(fluorure de vinylidène) et de la N-méthylpyrrolidone ou de la carboxyméthylcellulose de sodium et de l'eau. Le présent matériau d'électrode négative pour pile rechargeable lithium-ion est peu coûteux, a un grand choix de sources, réduit efficacement les coûts pour une pile lithium-ion, et augmente sa sécurité et ses propriétés électrochimiques. La pile rechargeable lithium-ion est plus précisément caractérisée en ce qu'elle est rechargeable à température ambiante, peu coûteuse, de puissance élevée, et a une longue durée de vie.
PCT/CN2015/087882 2015-05-06 2015-08-24 Matériau d'électrode négative, son procédé de préparation, et pile rechargeable lithium-ion utilisant le matériau d'électrode négative WO2016176928A1 (fr)

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CN113471548A (zh) * 2021-07-05 2021-10-01 淮北享锂电子科技有限公司 一种锂离子电池加工方法
WO2022126858A1 (fr) * 2020-12-14 2022-06-23 鹏盛国能(深圳)新能源集团有限公司 Batterie au silicium-lithium et son procédé de fabrication
CN117154182A (zh) * 2023-10-30 2023-12-01 山东硅纳新材料科技有限公司 电解质成分渐变的固态硅-硫电池及其制备方法与应用
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CN109860564A (zh) * 2019-02-21 2019-06-07 三峡大学 一种无烟煤基锂硫电池正极材料的制备方法
CN112038618A (zh) * 2020-09-04 2020-12-04 中国有色桂林矿产地质研究院有限公司 一种具有空心结构的纳米硅粉聚合球复合负极材料及其制备方法与应用
CN112038618B (zh) * 2020-09-04 2022-12-30 中国有色桂林矿产地质研究院有限公司 一种具有空心结构的纳米硅粉聚合球复合负极材料及其制备方法与应用
WO2022126858A1 (fr) * 2020-12-14 2022-06-23 鹏盛国能(深圳)新能源集团有限公司 Batterie au silicium-lithium et son procédé de fabrication
CN113471548A (zh) * 2021-07-05 2021-10-01 淮北享锂电子科技有限公司 一种锂离子电池加工方法
CN117154182A (zh) * 2023-10-30 2023-12-01 山东硅纳新材料科技有限公司 电解质成分渐变的固态硅-硫电池及其制备方法与应用
CN117154182B (zh) * 2023-10-30 2024-01-16 山东硅纳新材料科技有限公司 电解质成分渐变的固态硅-硫电池及其制备方法与应用
CN117410437A (zh) * 2023-12-15 2024-01-16 中国科学院长春应用化学研究所 一种锑基电极及其制备方法和应用
CN117410437B (zh) * 2023-12-15 2024-03-12 中国科学院长春应用化学研究所 一种锑基电极及其制备方法和应用

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