Preparation method of lithium ion battery negative electrode material high-entropy oxide

Abstract

The invention discloses a preparation method of a lithium ion battery negative electrode material high-entropy oxide. The preparation method comprises the following steps: S1, carrying out oil removal, polishing and rust removal, distilled water washing, alcohol solution secondary washing and vacuum drying on a high-entropy alloy Cr<0.2>Fe<0.2>Mn<0.2>Ni<0.2>Co<0.2> solid; S2, conducting melting, carrying out gas atomization granulation, and conducting cooling and sieving; and S3, taking the high-entropy alloy powder, and conducting oxidation treatment under flowing oxygen, so as to obtain the required (Cr<0.2>Fe<0.2>Mn<0.2>Ni<0.2>Co<0.2>)<3>O<4> high-entropy oxide lithium ion electrode material. The lithium battery negative electrode material (Cr<0.2>Fe<0.2>Mn<0.2>Ni<0.2>Co<0.2>)<3>O<4> high-entropy oxide obtained through the method is a pure phase, the particle morphology is uniform, the particle size is 0.1-2 microns, namely, the material performance is more stable, a battery assembled by the lithium battery negative electrode material high-entropy oxide has very high specific capacity and very good cycle stability and has remarkable economic value, and the method is short in process, easy to operate, low in cost and suitable for industrial production. The method is high in controllability, good in repeatability, wide in applicability and suitable for industrial production.

Description

technical field

[0001] The invention relates to a method for preparing a negative electrode material of a battery, in particular to a method for preparing a high-entropy oxide for a negative electrode material of a lithium ion battery, and belongs to the field of battery preparation. Background technique

[0002] With the increasing demand for lithium-ion batteries, it is imminent to develop a low-cost, high-capacity secondary battery system. As a member of secondary batteries, lithium-ion batteries, as a conversion and storage device with long life, high safety, high energy density, high power density and no memory effect, have been widely used in mobile electronic fields such as automotive and aerospace. Nowadays, the anode materials of commercial lithium-ion batteries mainly use carbon materials. However, their specific capacity is low and the rate performance is poor, which seriously restricts the further development of lithium-ion batteries. In recent years, high-entr...

Examples

Embodiment 1

[0022] (1) Take 10 g Cr 0.2 Fe 0.2 mn 0.2 Ni 0.2 co 0.2 High-entropy alloy ingots are degreased, polished and derusted, washed with distilled water, washed twice with alcohol solution, and dried in vacuum at 60°C for 20 hours;

[0023] (2) For high entropy alloy Cr 0.2 Fe 0.2 mn 0.2 Ni 0.2 co 0.2 Melting, gas atomization granulation under argon atmosphere, and then sieving to select alloy powder with a particle size of <53 μm;

[0024] (3) Weigh 200 mg of high-entropy alloy powder, heat it up to 1000 °C at a rate of 5 °C / min, keep it for 24 h, and its oxygen partial pressure is 80 kPa. After cooling, (Cr 0.2 Fe 0.2 mn 0.2 Ni 0.2 co 0.2 ) 3 o 4 High entropy oxides.

[0025] Such as figure 1 As shown, the lithium battery negative electrode material (Cr 0.2 Fe 0.2 mn 0.2 Ni 0.2 co 0.2 )3 o 4 The peak of the high-entropy oxide on XRD is basically consistent with the peak of the standard product, and there is no impurity peak, so it can be determined that the...

Embodiment 2

[0032] (1) Take 8 g Cr 0.2 Fe 0.2 mn 0.2 Ni 0.2 co 0.2 High-entropy alloy ingots are degreased, polished and derusted, washed with distilled water, washed twice with alcohol solution, and dried in vacuum at 40°C for 72 hours;

[0033] (2) For high entropy alloy Cr 0.2 Fe 0.2 mn 0.2 Ni 0.2 co 0.2 Melting, gas atomization granulation under argon atmosphere, and then sieving to select alloy powder with a particle size of <30 μm;

[0034] (3) Weigh 2000 mg of high-entropy alloy powder, raise the temperature to 800 °C at a rate of 10 °C / min, keep it for 48 h, and its oxygen partial pressure is 80 kPa. After cooling, (Cr 0.2 Fe 0.2 mn 0.2 Ni 0.2 co 0.2 ) 3 o 4 High entropy oxides.

[0035] The obtained lithium battery negative electrode material (Cr 0.2 Fe 0.2 mn 0.2 Ni 0.2 co 0.2 ) 3 o 4 The peaks of high-entropy oxides on XRD are basically the same as those of standard products, and there are no impurity peaks. It can be determined that the obtained material...

Embodiment 3

[0042] (1) Take 15 g Cr 0.2 Fe 0.2 mn 0.2 Ni 0.2 co 0.2 High-entropy alloy ingots are degreased, polished and derusted, washed with distilled water, washed twice with alcohol solution, and dried in vacuum at 90°C for 12 hours;

[0043] (2) For high entropy alloy Cr 0.2 Fe 0.2 mn 0.2 Ni 0.2 co 0.2 Carry out melting, carry out gas atomization granulation under the mixed gas atmosphere of argon and nitrogen, and then sieve, select the alloy powder with particle size <230 μm;

[0044] (3) Weigh 1000 mg of high-entropy alloy powder, raise the temperature to 1100 ℃ at a rate of 0.1 ℃ / min, keep it for 8 hours, and its oxygen partial pressure is 21.278 kPa. After cooling, (Cr 0.2 Fe 0.2 mn 0.2 Ni 0.2 co 0.2 ) 3 o 4 High entropy oxides.

[0045] The obtained lithium battery negative electrode material (Cr 0.2 Fe 0.2 mn 0.2 Ni 0.2 co 0.2 ) 3 o 4 The peaks of high-entropy oxides on XRD are basically the same as those of standard products, and there are no impurity ...

technical field

[0001] The invention relates to a method for preparing a negative electrode material of a battery, in particular to a method for preparing a high-entropy oxide for a negative electrode material of a lithium ion battery, and belongs to the field of battery preparation. Background technique

[0002] With the increasing demand for lithium-ion batteries, it is imminent to develop a low-cost, high-capacity secondary battery system. As a member of secondary batteries, lithium-ion batteries, as a conversion and storage device with long life, high safety, high energy density, high power density and no memory effect, have been widely used in mobile electronic fields such as automotive and aerospace. Nowadays, the anode materials of commercial lithium-ion batteries mainly use carbon materials. However, their specific capacity is low and the rate performance is poor, which seriously restricts the further development of lithium-ion batteries. In recent years, high-entr...

Examples

Embodiment 1

[0022] (1) Take 10 g Cr 0.2 Fe 0.2 mn 0.2 Ni 0.2 co 0.2 High-entropy alloy ingots are degreased, polished and derusted, washed with distilled water, washed twice with alcohol solution, and dried in vacuum at 60°C for 20 hours;

[0023] (2) For high entropy alloy Cr 0.2 Fe 0.2 mn 0.2 Ni 0.2 co 0.2 Melting, gas atomization granulation under argon atmosphere, and then sieving to select alloy powder with a particle size of <53 μm;

[0024] (3) Weigh 200 mg of high-entropy alloy powder, heat it up to 1000 °C at a rate of 5 °C / min, keep it for 24 h, and its oxygen partial pressure is 80 kPa. After cooling, (Cr 0.2 Fe 0.2 mn 0.2 Ni 0.2 co 0.2 ) 3 o 4 High entropy oxides.

[0025] Such as figure 1 As shown, the lithium battery negative electrode material (Cr 0.2 Fe 0.2 mn 0.2 Ni 0.2 co 0.2 )3 o 4 The peak of the high-entropy oxide on XRD is basically consistent with the peak of the standard product, and there is no impurity peak, so it can be determined that the...

Embodiment 2

[0032] (1) Take 8 g Cr 0.2 Fe 0.2 mn 0.2 Ni 0.2 co 0.2 High-entropy alloy ingots are degreased, polished and derusted, washed with distilled water, washed twice with alcohol solution, and dried in vacuum at 40°C for 72 hours;

[0033] (2) For high entropy alloy Cr 0.2 Fe 0.2 mn 0.2 Ni 0.2 co 0.2 Melting, gas atomization granulation under argon atmosphere, and then sieving to select alloy powder with a particle size of <30 μm;

[0034] (3) Weigh 2000 mg of high-entropy alloy powder, raise the temperature to 800 °C at a rate of 10 °C / min, keep it for 48 h, and its oxygen partial pressure is 80 kPa. After cooling, (Cr 0.2 Fe 0.2 mn 0.2 Ni 0.2 co 0.2 ) 3 o 4 High entropy oxides.

[0035] The obtained lithium battery negative electrode material (Cr 0.2 Fe 0.2 mn 0.2 Ni 0.2 co 0.2 ) 3 o 4 The peaks of high-entropy oxides on XRD are basically the same as those of standard products, and there are no impurity peaks. It can be determined that the obtained material...

Embodiment 3

[0042] (1) Take 15 g Cr 0.2 Fe 0.2 mn 0.2 Ni 0.2 co 0.2 High-entropy alloy ingots are degreased, polished and derusted, washed with distilled water, washed twice with alcohol solution, and dried in vacuum at 90°C for 12 hours;

[0043] (2) For high entropy alloy Cr 0.2 Fe 0.2 mn 0.2 Ni 0.2 co 0.2 Carry out melting, carry out gas atomization granulation under the mixed gas atmosphere of argon and nitrogen, and then sieve, select the alloy powder with particle size <230 μm;

[0044] (3) Weigh 1000 mg of high-entropy alloy powder, raise the temperature to 1100 ℃ at a rate of 0.1 ℃ / min, keep it for 8 hours, and its oxygen partial pressure is 21.278 kPa. After cooling, (Cr 0.2 Fe 0.2 mn 0.2 Ni 0.2 co 0.2 ) 3 o 4 High entropy oxides.

[0045] The obtained lithium battery negative electrode material (Cr 0.2 Fe 0.2 mn 0.2 Ni 0.2 co 0.2 ) 3 o 4 The peaks of high-entropy oxides on XRD are basically the same as those of standard products, and there are no impurity ...

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