Improved preparation method of large single crystal layered positive electrode material for lithium ion battery

A technology for lithium-ion batteries and positive electrode materials, applied in battery electrodes, positive electrodes, secondary batteries, etc., can solve problems such as low volume energy density, achieve high phase purity, meet high volume energy density, high tap density and compaction The effect of solid density

Active Publication Date: 2017-11-03
UNIV OF JINAN
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  • Description
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  • Application Information

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Problems solved by technology

[0007] In order to solve the above-mentioned layered cathode material Li 1+z [Ni 1-x-y co x mn y ] 1-z o 2 The relatively low volumetric energy density meets the needs of lithium-ion batteries with high volumetric energy density in the market. The applicant proposes to prepare micron-sized large single crystal layered

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  • Improved preparation method of large single crystal layered positive electrode material for lithium ion battery
  • Improved preparation method of large single crystal layered positive electrode material for lithium ion battery
  • Improved preparation method of large single crystal layered positive electrode material for lithium ion battery

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preparation example Construction

[0031] The preparation method comprises the following steps:

[0032] The first step: preparing a Co-Mn precursor according to the molar ratio of the transition metal element shown in the general formula of the large single crystal layered positive electrode material;

[0033] There are many methods for preparing Co-Mn precursors in the prior art. From the perspective of synthesis effect, the present invention adopts the co-precipitation method to synthesize Co-Mn precursors. The types of the precursors include [Co 1-x mn x ](OH) 2 、[Co 1-x mn x ]CO 3 、[Co 1-x mn x ]C 2 o 4 or [Co 1-x mn x ]O y , can be prepared by conventional methods in the prior art, for example, by one or more of hydroxide, carbonate or oxalate co-precipitation methods.

[0034] The second step: Mix the Co-Mn precursor obtained in the above step with the lithium source evenly, wherein the molar ratio of lithium element to transition metal element is set to 0

    • Embodiment 1

    [0049] Embodiment 1 prepares precursor [Co1 / 2 mn 1 / 2 ](OH) 2

    [0050] Weigh 11.246Kg CoSO 4 ·7H 2 O and 6.76Kg MnSO 4 ·H 2 O preparation concentration is 20L of 2M salt solution. Add the above salt solution to 1L h -1 Add it dropwise into the continuously stirring reactor at a speed of 200rpm, and at the same time control the pH value in the kettle at about 11.0 with a mixed solution of 10M NaOH solution and 1M ammonia solution, until the salt solution is completely consumed, centrifuge, wash, and Dry to obtain the precursor [Co 1 / 2 mn 1 / 2 ](OH) 2 ,Such as figure 1 shown.

    Embodiment 2

    [0052] Take the precursor prepared by 90.94g embodiment 1 [Co 1 / 2 mn 1 / 2 ](OH) 2 with 18.47g battery-grade Li 2 CO 3 (Li / Co-Mn=0.5) was evenly mixed, and the mixture was placed in a muffle furnace and sintered in an air atmosphere at 950°C for 8h. Since the molar ratio Li / Co-Mn4 , since the spinel phase is easier to grow than the layered phase, micron-sized grains are obtained, and 46.35g of nano-sized Ni(OH) is further added to the micron-sized grains 2 and 38.61g battery-grade Li 2 CO 3 , so that Li / Ni-Co-Mn = 1.03, it was placed in a muffle furnace and sintered in an air atmosphere at 900°C for 12 hours to obtain a large single-crystal layered cathode material Li[Ni 1 / 3 co 1 / 3 mn 1 / 3 ]O 2 , its SEM and XRD such as figure 2 (b) and image 3 As shown in (b), the first-cycle charge-discharge curves and cycle stability of the electrodes prepared with large single-crystal layered cathode materials are as follows: Figure 4 shown.

    [0053] From figure 2 In (a), it ...

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    Abstract

    The invention discloses an improved preparation method of a large single crystal layered positive electrode material for a lithium ion battery. The method comprises the following steps of firstly mixing Co-Mn precursors with a lithium source, wherein the mol ratio of the lithium element to the transition metal element is between 0 and 1; high-temperature calcination is performed; at the moment, a spinel phase is formed due to insufficiency of the lithium element; the spinel phase is favorable for the fusion and the growth of the primary crystal grains; micrometer stage large-dimension composite phase primary crystal grains or pure phase primary crystal grains are obtained; then, a lithium source and a nickel source at the chemical metering ratio are supplemented into the prepared primary crystal grains, so that the mol ratio of the nickel element to the cobalt element to the manganese element Ni/Co/Mn is (1-x-y)/x/y; the mol ratio of the lithium element to the transition metal element Li/Ni-Co-Mn is (1+z)/(1-z) to (1+z)/(1-z)+0.05; in the high-temperature calcination, the solid phase reaction is initiated by the diffusion of lithium ions and nickel ions; the large single crystal layered positive material for the lithium ion battery is obtained.

    Description

    technical field [0001] The invention belongs to the technical field of lithium-ion batteries, and in particular relates to a micron-sized large single crystal layered lithium-ion battery cathode material and a preparation method thereof. Background technique [0002] As a high-energy-density energy storage technology, lithium-ion batteries have been widely used in "3C" portable electronic devices, and are gradually expanding to large-capacity, high-power systems such as electric tools and automobiles, high-efficiency energy storage and military systems. Compared with carbon negative electrodes with excellent comprehensive performance, high cost and low capacity cathode materials limit the performance improvement of lithium ion batteries and their wide application in large capacity and high power systems. Therefore, the development of low cost, high performance cathode materials is of great importance It is of great significance to promote the development of lithium-ion batte...

    Claims

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    Application Information

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    IPC IPC(8): C01G53/00H01M4/505H01M4/525H01M10/0525
    CPCC01G53/44C01G53/50C01P2002/72C01P2004/03C01P2004/30C01P2004/61C01P2006/11C01P2006/40H01M4/505H01M4/525H01M10/0525H01M2004/021H01M2004/028Y02E60/10
    Inventor 侯配玉李凤
    Owner UNIV OF JINAN
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