WO2021212481A1 - 负极活性材料及使用其的电化学装置和电子装置 - Google Patents
负极活性材料及使用其的电化学装置和电子装置 Download PDFInfo
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- WO2021212481A1 WO2021212481A1 PCT/CN2020/086741 CN2020086741W WO2021212481A1 WO 2021212481 A1 WO2021212481 A1 WO 2021212481A1 CN 2020086741 W CN2020086741 W CN 2020086741W WO 2021212481 A1 WO2021212481 A1 WO 2021212481A1
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- active material
- negative electrode
- carbon material
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Images
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- Y02E60/10—Energy storage using batteries
Definitions
- This application relates to the field of energy storage, in particular to a negative electrode active material and an electrochemical device and an electronic device using the same.
- Electrochemical devices for example, lithium-ion batteries
- Small-sized lithium-ion batteries are generally used as power sources for driving portable electronic communication devices (for example, camcorders, mobile phones, or notebook computers, etc.), especially high-performance portable devices.
- portable electronic communication devices for example, camcorders, mobile phones, or notebook computers, etc.
- Examples of medium-sized and large-sized lithium batteries with high output characteristics have been developed for use in electric vehicles (EV) and large-scale energy storage systems (ESS).
- EV electric vehicles
- ESS large-scale energy storage systems
- the present application attempts to solve at least one problem existing in related fields at least to some extent by providing a negative electrode active material, an electrochemical device and an electronic device using the same.
- the present application provides an anode active material, the anode active material comprises a carbon material, wherein the graphitization degree Gr of the carbon material measured by X-ray diffraction analysis method is 0.82 to 0.92, And based on the total number of particles of the carbon material, the proportion of particles with an aspect ratio of 3.3 or more in the carbon material is 10% or less.
- the graphitization degree Gr of the carbon material measured by X-ray diffraction analysis method is 0.85 to 0.90. In some embodiments, the graphitization degree Gr of the carbon material measured by X-ray diffraction analysis is 0.82, 0.83, 0.84, 0.85, 0.86, 0.87, 0.88, 0.89, 0.90, 0.91, 0.92 or any of the above. Within the range of two values.
- the proportion of particles with an aspect ratio of 3.3 or more in the carbon material is 8% or less. In some embodiments, based on the total number of particles of the carbon material, the proportion of particles with an aspect ratio of 3.3 or more in the carbon material is 6% or less. In some embodiments, based on the total number of particles of the carbon material, the proportion of particles with an aspect ratio of 3.3 or more in the carbon material is 1% or more. In some embodiments, based on the total number of particles of the carbon material, the proportion of particles with an aspect ratio of 3.3 or more in the carbon material is 3% or more.
- the proportion of particles with an aspect ratio of 3.3 or more in the carbon material is more than 5%. In some embodiments, based on the total number of particles of the carbon material, the proportion of particles with an aspect ratio of 3.3 or more in the carbon material is within a range composed of any two endpoints above.
- the proportion of particles with an aspect ratio of 2 or more in the carbon material is less than 50%, and the carbon material has an aspect ratio of 1.5 or more.
- the proportion of particles is less than 80%.
- the proportion of particles with an aspect ratio of 2 or more in the carbon material is 45% or less. In some embodiments, based on the total number of particles of the carbon material, the proportion of particles with an aspect ratio of 2 or more in the carbon material is less than 40%. In some embodiments, based on the total number of particles of the carbon material, the proportion of particles with an aspect ratio of 2 or more in the carbon material is 30% or more. In some embodiments, based on the total number of particles of the carbon material, the proportion of particles with an aspect ratio of 2 or more in the carbon material is 35% or more. In some embodiments, based on the total number of particles of the carbon material, the proportion of particles with an aspect ratio of 2 or more in the carbon material is within a range composed of any two endpoints above.
- the proportion of particles with an aspect ratio of 1.5 or more in the carbon material is 75% or less. In some embodiments, based on the total number of particles of the carbon material, the proportion of particles with an aspect ratio of 1.5 or more in the carbon material is 70% or less. In some embodiments, based on the total number of particles of the carbon material, the proportion of particles with an aspect ratio of 1.5 or more in the carbon material is more than 50%. In some embodiments, based on the total number of particles of the carbon material, the proportion of particles with an aspect ratio of 1.5 or more in the carbon material is 55% or more.
- the proportion of particles with an aspect ratio of 1.5 or more in the carbon material is 60% or more. In some embodiments, based on the total number of particles of the carbon material, the proportion of particles with an aspect ratio of 1.5 or more in the carbon material is more than 65%. In some embodiments, based on the total number of particles of the carbon material, the proportion of particles with an aspect ratio of 1.5 or more in the carbon material is within a range composed of any two endpoints described above.
- the crystal grain size La of the crystal grains of the carbon material along the horizontal axis determined by X-ray diffraction analysis is different from the crystal grain size of the carbon material along the vertical axis determined by X-ray diffraction analysis.
- the ratio of the grain size Lc is K, and Gr and K satisfy the following relationship: 4.0 ⁇ K ⁇ Gr ⁇ 5.2.
- Gr and K satisfy the following relationship: 4.2 ⁇ K ⁇ Gr ⁇ 5.0.
- Gr and K satisfy the following relationship: 4.5 ⁇ K ⁇ Gr ⁇ 4.8.
- the particle size of the negative active material satisfies the following relationship: 35 ⁇ m ⁇ Dv99-Dv10 ⁇ 50 ⁇ m. In some embodiments, the particle size of the negative active material satisfies the following relationship: 42 ⁇ m ⁇ Dv99-Dv10 ⁇ 48 ⁇ m. In some embodiments, the particle size of the negative active material satisfies the following relationship: 43 ⁇ m ⁇ Dv99-Dv10 ⁇ 45 ⁇ m.
- the interplanar spacing d002 of the negative electrode active material measured by X-ray diffraction analysis method is ⁇ 0.3365 nm. In some embodiments, the interplanar spacing d002 of the negative active material determined by X-ray diffraction analysis method is ⁇ 0.3370 nm. In some embodiments, the interplanar spacing d002 of the negative active material determined by X-ray diffraction analysis method is ⁇ 0.3375 nm.
- the interplanar spacing d002 of the negative electrode active material determined by X-ray diffraction analysis is 0.3365nm, 0.3368nm, 0.3370nm, 0.3372nm, 0.3375 or within a range composed of any two of the above values. .
- the ratio of the peak area C004 of the (004) crystal plane and the peak area C110 of the (110) crystal plane of the negative electrode active material C004/C110 ⁇ 8 is determined by X-ray diffraction analysis.
- C004/C110 of the negative electrode active material determined by X-ray diffraction analysis method is ⁇ 7.5.
- C004/C110 of the negative electrode active material determined by X-ray diffraction analysis method is less than or equal to 7.
- C004/C110 of the negative electrode active material determined by X-ray diffraction analysis method is ⁇ 6.5.
- C004/C110 of the negative electrode active material determined by X-ray diffraction analysis method is less than or equal to 6. In some implementations, C004/C110 of the negative electrode active material determined by X-ray diffraction analysis method is less than or equal to 5.5. In some implementations, C004/C110 of the negative electrode active material determined by X-ray diffraction analysis method is less than or equal to 5. In some implementations, C004/C110 ⁇ 3 of the negative electrode active material determined by X-ray diffraction analysis. In some implementations, C004/C110 of the negative electrode active material determined by X-ray diffraction analysis method is ⁇ 3.5.
- C004/C110 ⁇ 4 of the negative electrode active material determined by X-ray diffraction analysis is ⁇ 4.5. In some implementations, the C004/C110 of the negative electrode active material measured by X-ray diffraction analysis is within the range composed of any two endpoints.
- the gram capacity C mAh/g of the negative electrode active material and the graphitization degree Gr of the carbon material satisfy the following relationship: 390Gr-C ⁇ 20, C ⁇ 350.
- C and Gr satisfy the following relationship: 390Gr-C ⁇ 18. In some embodiments, C and Gr satisfy the following relationship: 390Gr-C ⁇ 15. In some embodiments, C and Gr satisfy the following relationship: 390Gr-C ⁇ 12. In some embodiments, C and Gr satisfy the following relationship: 390Gr-C ⁇ 15. In some embodiments, C and Gr satisfy the following relationship: 390Gr-C ⁇ 10. In some embodiments, C and Gr satisfy the following relationship: 390Gr-C ⁇ 8. In some embodiments, C and Gr satisfy the following relationship: 390Gr-C ⁇ 5. In some embodiments, C and Gr satisfy the following relationship: 390Gr-C ⁇ 1. In some embodiments, C and Gr satisfy the following relationship: 390Gr-C ⁇ 3. In some embodiments, the value of 390Gr-C is within the range composed of any two endpoint values described above.
- the present application provides an electrochemical device, which includes a positive electrode, an electrolyte, and a negative electrode, wherein the negative electrode includes a negative electrode active material layer and a negative electrode current collector, and the negative electrode active material layer includes the The negative active material described in the application.
- the compacted density PD g/cm 3 of the negative active material layer and the graphitization degree Gr of the carbon material satisfy the following relationship: PD ⁇ 2.5Gr-0.45 ⁇ 1.85.
- PD and Gr satisfy the following relationship: PD ⁇ 2.5Gr-0.45 ⁇ 1.80.
- PD and Gr satisfy the following relationship: PD ⁇ 2.5Gr-0.45 ⁇ 1.75.
- PD and Gr satisfy the following relationship: PD ⁇ 2.5Gr-0.45 ⁇ 1.70.
- PD and Gr satisfy the following relationship: PD ⁇ 2.5Gr-0.45 ⁇ 1.65.
- PD and Gr satisfy the following relationship: PD ⁇ 2.5Gr-0.45 ⁇ 1.60.
- the compacted density of the negative active material layer is 1.45 g/cm 3 to 1.75 g/cm 3 . In some embodiments, the compacted density of the negative active material layer is 1.50 g/cm 3 to 1.70 g/cm 3 . In some embodiments, the compacted density of the negative active material layer is 1.55 g/cm 3 to 1.65 g/cm 3 .
- the compacted density of the negative active material layer is 1.45 g/cm 3 , 1.50 g/cm 3 , 1.55 g/cm 3 , 1.60 g/cm 3 , 1.65 g/cm 3 , 1.70 g/cm 3 cm 3 , 1.75g/cm 3 or within the range composed of any two of the above values.
- the ratio C004'/C110' of the peak area C004' of the (004) plane and the peak area C110' of the (110) plane of the negative electrode active material layer measured by X-ray diffraction analysis method is 7 to 18.
- the C004'/C110' of the negative electrode active material layer measured by X-ray diffraction analysis is 10-16.
- the C004'/C110' of the negative active material layer measured by X-ray diffraction analysis is 12-15.
- the C004'/C110' of the negative electrode active material layer measured by X-ray diffraction analysis is 7, 10, 12, 14, 16, 18 or in the range composed of any two of the foregoing values.
- the ratio of Ig Id/Ig is 0.2 to 0.5.
- the Id/Ig of the negative active material layer measured by Raman spectroscopy is 0.25 to 0.45.
- the Id/Ig of the negative active material layer measured by Raman spectroscopy is 0.3 to 0.4.
- the Id/Ig of the negative electrode active material layer measured by Raman spectroscopy is 0.2, 0.25, 0.3, 0.35, 0.4, 0.45, 0.5 or within a range composed of any two of the foregoing values.
- the present application provides an electronic device, which includes the electrochemical device according to the present application.
- FIG. 1 shows a scanning electron microscope (SEM) image of the negative electrode active material used in Example 3 of the present application.
- Fig. 2 shows the SEM morphology of particles with an aspect ratio of about 5.0 in the carbon material used in Example 3 of the present application.
- FIG. 3 shows the SEM morphology of particles with an aspect ratio of about 2.5 in the carbon material used in Example 3 of the present application.
- FIG. 4 shows the SEM morphology of particles with an aspect ratio of about 1.5 in the carbon material used in Example 3 of the present application.
- FIG. 5 shows the SEM morphology of particles with an aspect ratio of about 1.0 in the carbon material used in Example 3 of the present application.
- Fig. 6 shows a curve diagram of the cycle capacity retention rate with the number of cycles in Comparative Example 2 and Example 1 according to the present application.
- Fig. 7 shows a graph of the thickness rebound rate with the number of cycles in Comparative Example 2 and Example 1 according to the present application.
- a list of items connected by the term "at least one of” can mean any combination of the listed items. For example, if items A and B are listed, then the phrase "at least one of A and B" means only A; only B; or A and B. In another example, if items A, B, and C are listed, then the phrase "at least one of A, B, and C" means only A; or only B; only C; A and B (excluding C); A and C (exclude B); B and C (exclude A); or all of A, B, and C.
- Project A can contain a single element or multiple elements.
- Project B can contain a single element or multiple elements.
- Project C can contain a single element or multiple elements.
- Cycle performance is an important indicator for evaluating the performance of lithium-ion batteries.
- Methods such as selecting raw materials, controlling the granulation process, and performing surface coating to improve the active materials in the pole pieces can improve the cycle performance of lithium-ion batteries, but the improvement effect is limited and cannot meet the growing market demand.
- the present application solves the above-mentioned problems by adjusting the graphitization degree of the negative electrode active material and the aspect ratio of the particles and their distribution.
- the present application provides a negative electrode active material, the negative electrode active material comprises a carbon material, wherein the graphitization degree Gr of the carbon material measured by X-ray diffraction analysis method is 0.82 to 0.92, and is based on For the total number of particles of the carbon material, the proportion of particles with an aspect ratio of 3.3 or more in the carbon material is 10% or less.
- the “aspect ratio" of a carbon material refers to the ratio of the longest diameter passing through the inside of the carbon material particle and the longest diameter perpendicular to it (ie, width).
- the aspect ratio of the carbon material can be obtained by dynamic particle image analysis (for example, using the Sinpatec QICPIC dynamic particle image analyzer).
- the aspect ratio of the carbon material can be controlled in a graded manner.
- the long diameter of the carbon material is relatively small, and the carbon material particles have a slender shape.
- Example 1 shows a scanning electron microscope (SEM) image of the carbon material used in Example 3 of the present application, in which particles with an aspect ratio of about 5.0 are elongated, and their morphology is shown in FIG. 2.
- the spherical carbon material particles have a small specific surface area, consume less electrolyte, and have a low orientation in the negative electrode, which is beneficial to the infiltration of the electrolyte, thereby improving the cycle performance of the electrochemical device.
- the "graphitization degree" of a carbon material refers to the degree to which non-graphitic carbon is transformed into graphite-like carbon at high temperature or during secondary heating.
- the carbon material has a higher graphitization degree (for example, greater than 0.92)
- the interplanar spacing d002 of the carbon material is reduced, which is not conducive to the deintercalation of lithium ions from the carbon material.
- the carbon material has a low degree of graphitization (for example, less than 0.92)
- there are more SP 3 bonds in the carbon material which makes the layers of the carbon material constrain each other, thereby making the structure of the carbon material more stable.
- the graphitization degree Gr of the carbon material measured by X-ray diffraction analysis method is 0.85 to 0.90. In some embodiments, the graphitization degree Gr of the carbon material measured by X-ray diffraction analysis is 0.82, 0.83, 0.84, 0.85, 0.86, 0.87, 0.88, 0.89, 0.90, 0.91, 0.92 or any of the above. Within the range of two values.
- the proportion of particles with an aspect ratio of 3.3 or more in the carbon material is 8% or less. In some embodiments, based on the total number of particles of the carbon material, the proportion of particles with an aspect ratio of 3.3 or more in the carbon material is 6% or less. In some embodiments, based on the total number of particles of the carbon material, the proportion of particles with an aspect ratio of 3.3 or more in the carbon material is 1% or more. In some embodiments, based on the total number of particles of the carbon material, the proportion of particles with an aspect ratio of 3.3 or more in the carbon material is 3% or more.
- the proportion of particles with an aspect ratio of 3.3 or more in the carbon material is more than 5%. In some embodiments, based on the total number of particles of the carbon material, the proportion of particles with an aspect ratio of 3.3 or more in the carbon material is within a range composed of any two endpoints above.
- the cycle performance of the electrochemical device can be significantly improved, and the service life of the electrochemical device can be prolonged.
- the proportion of particles with an aspect ratio of 2 or more in the carbon material is less than 50%, and the carbon material has an aspect ratio of 1.5 or more.
- the proportion of particles is less than 80%.
- particles with an aspect ratio of about 2.5 are ellipsoidal.
- particles having an aspect ratio of about 1.5 and about 1.0 are approximately spherical.
- the proportion of particles with an aspect ratio of 2 or more in the carbon material is 45% or less. In some embodiments, based on the total number of particles of the carbon material, the proportion of particles with an aspect ratio of 2 or more in the carbon material is less than 40%. In some embodiments, based on the total number of particles of the carbon material, the proportion of particles with an aspect ratio of 2 or more in the carbon material is 30% or more. In some embodiments, based on the total number of particles of the carbon material, the proportion of particles with an aspect ratio of 2 or more in the carbon material is 35% or more. In some embodiments, based on the total number of particles of the carbon material, the proportion of particles with an aspect ratio of 2 or more in the carbon material is within a range composed of any two endpoints above.
- the proportion of particles with an aspect ratio of 1.5 or more in the carbon material is 75% or less. In some embodiments, based on the total number of particles of the carbon material, the proportion of particles with an aspect ratio of 1.5 or more in the carbon material is 70% or less. In some embodiments, based on the total number of particles of the carbon material, the proportion of particles with an aspect ratio of 1.5 or more in the carbon material is more than 50%. In some embodiments, based on the total number of particles of the carbon material, the proportion of particles with an aspect ratio of 1.5 or more in the carbon material is 55% or more.
- the proportion of particles with an aspect ratio of 1.5 or more in the carbon material is 60% or more. In some embodiments, based on the total number of particles of the carbon material, the proportion of particles with an aspect ratio of 1.5 or more in the carbon material is more than 65%. In some embodiments, based on the total number of particles of the carbon material, the proportion of particles with an aspect ratio of 1.5 or more in the carbon material is within a range composed of any two endpoints above.
- the crystal grain size La of the crystal grains of the carbon material along the horizontal axis determined by X-ray diffraction analysis is different from the crystal grain size of the carbon material along the vertical axis determined by X-ray diffraction analysis.
- the ratio of the grain size Lc is K, and Gr and K satisfy the following relationship: 4.0 ⁇ K ⁇ Gr ⁇ 5.2.
- Gr and K satisfy the following relationship: 4.2 ⁇ K ⁇ Gr ⁇ 5.0.
- Gr and K satisfy the following relationship: 4.5 ⁇ K ⁇ Gr ⁇ 4.8.
- the particle size of the negative active material satisfies the following relationship: 35 ⁇ m ⁇ Dv99-Dv10 ⁇ 50 ⁇ m. In some embodiments, the particle size of the negative active material satisfies the following relationship: 42 ⁇ m ⁇ Dv99-Dv10 ⁇ 48 ⁇ m. In some embodiments, the particle size of the negative active material satisfies the following relationship: 43 ⁇ m ⁇ Dv99-Dv10 ⁇ 45 ⁇ m.
- the interplanar spacing d002 of the negative electrode active material measured by X-ray diffraction analysis method is ⁇ 0.3365 nm. In some embodiments, the interplanar spacing d002 of the negative active material determined by X-ray diffraction analysis method is ⁇ 0.3370 nm. In some embodiments, the interplanar spacing d002 of the negative active material determined by X-ray diffraction analysis method is ⁇ 0.3375 nm.
- the interplanar spacing d002 of the negative electrode active material determined by X-ray diffraction analysis is 0.3365nm, 0.3368nm, 0.3370nm, 0.3372nm, 0.3375 or within a range composed of any two of the above values. .
- the interplanar spacing d002 of the negative electrode active material is within the above range, it is helpful for the rapid deintercalation of lithium ions, can reduce the damage of the sheet layer of the negative electrode active material, and can further improve the cycle performance of the electrochemical device.
- the ratio of the peak area C004 of the (004) crystal plane and the peak area C110 of the (110) crystal plane of the negative electrode active material C004/C110 ⁇ 8 is determined by X-ray diffraction analysis.
- C004/C110 of the negative electrode active material determined by X-ray diffraction analysis method is ⁇ 7.5.
- C004/C110 of the negative electrode active material determined by X-ray diffraction analysis method is less than or equal to 7.
- C004/C110 of the negative electrode active material determined by X-ray diffraction analysis method is ⁇ 6.5.
- C004/C110 of the negative electrode active material determined by X-ray diffraction analysis method is less than or equal to 6. In some implementations, C004/C110 of the negative electrode active material determined by X-ray diffraction analysis method is less than or equal to 5.5. In some implementations, C004/C110 of the negative electrode active material determined by X-ray diffraction analysis method is less than or equal to 5. In some implementations, C004/C110 ⁇ 3 of the negative electrode active material determined by X-ray diffraction analysis. In some implementations, C004/C110 of the negative electrode active material determined by X-ray diffraction analysis method is ⁇ 3.5.
- C004/C110 ⁇ 4 of the negative electrode active material determined by X-ray diffraction analysis is ⁇ 4.5. In some implementations, the C004/C110 of the negative electrode active material measured by X-ray diffraction analysis is within the range composed of any two endpoints.
- the C004/C110 value can reflect the orientation of the material.
- the C004/C110 value of the negative electrode active material is large, the lithium ion extraction direction in the negative electrode active material is single, resulting in a longer lithium ion extraction path, which is not conducive to the rapid extraction of lithium ions, which will affect the electrochemistry The cycle performance of the device is adversely affected.
- lithium ions can be intercalated or deintercalated in all directions, reducing the diffusion path of lithium ions and the loss of active lithium ions, thus Further improve the cycle performance of the electrochemical device.
- the gram capacity C mAh/g of the negative electrode active material and the graphitization degree Gr of the carbon material satisfy the following relationship: 390Gr-C ⁇ 20, C ⁇ 350.
- C and Gr satisfy the following relationship: 390Gr-C ⁇ 18. In some embodiments, C and Gr satisfy the following relationship: 390Gr-C ⁇ 15. In some embodiments, C and Gr satisfy the following relationship: 390Gr-C ⁇ 12. In some embodiments, C and Gr satisfy the following relationship: 390Gr-C ⁇ 15. In some embodiments, C and Gr satisfy the following relationship: 390Gr-C ⁇ 10. In some embodiments, C and Gr satisfy the following relationship: 390Gr-C ⁇ 8. In some embodiments, C and Gr satisfy the following relationship: 390Gr-C ⁇ 5. In some embodiments, C and Gr satisfy the following relationship: 390Gr-C ⁇ 1. In some embodiments, C and Gr satisfy the following relationship: 390Gr-C ⁇ 3. In some embodiments, the value of 390Gr-C is within the range composed of any two endpoint values described above.
- the negative electrode active material can have a balanced performance, thereby further improving the cycle performance of the electrochemical device.
- the application also provides an electrochemical device, which includes a positive electrode, a negative electrode, a separator, and an electrolyte.
- a positive electrode a negative electrode
- a separator a separator
- electrolyte an electrolyte
- the negative electrode used in the electrochemical device of the present application includes a negative electrode current collector and a negative electrode active material layer, and the negative electrode active material layer includes the negative electrode active material according to the present application.
- the compacted density PD g/cm 3 of the negative active material layer and the graphitization degree Gr of the carbon material satisfy the following relationship: PD ⁇ 2.5Gr-0.45 ⁇ 1.85.
- PD and Gr satisfy the following relationship: PD ⁇ 2.5Gr-0.45 ⁇ 1.80.
- PD and Gr satisfy the following relationship: PD ⁇ 2.5Gr-0.45 ⁇ 1.75.
- PD and Gr satisfy the following relationship: PD ⁇ 2.5Gr-0.45 ⁇ 1.70.
- PD and Gr satisfy the following relationship: PD ⁇ 2.5Gr-0.45 ⁇ 1.65.
- PD and Gr satisfy the following relationship: PD ⁇ 2.5Gr-0.45 ⁇ 1.60.
- the compacted density of the negative active material layer is 1.45 g/cm 3 to 1.75 g/cm 3 . In some embodiments, the compacted density of the negative active material layer is 1.50 g/cm 3 to 1.70 g/cm 3 . In some embodiments, the compacted density of the negative active material layer is 1.55 g/cm 3 to 1.65 g/cm 3 .
- the compacted density of the negative active material layer is 1.45 g/cm 3 , 1.50 g/cm 3 , 1.55 g/cm 3 , 1.60 g/cm 3 , 1.65 g/cm 3 , 1.70 g/cm 3 cm 3 , 1.75g/cm 3 or within the range composed of any two of the above values.
- the compaction density of the negative electrode active material layer is too high, the electrolyte is not easy to infiltrate the negative electrode active material, which is not conducive to the rapid participation of lithium ions in the electrochemical reaction, thereby adversely affecting the cycle performance of the lithium ion battery.
- the compacted density of the negative active material layer and the graphitization degree of the carbon material satisfy the above relationship or the compacted density of the negative active material is within the above range, the cycle performance of the electrochemical device can be further improved.
- the ratio C004'/C110' of the peak area C004' of the (004) plane and the peak area C110' of the (110) plane of the negative electrode active material layer measured by X-ray diffraction analysis is in In the range of 7 to 18. In some embodiments, the C004'/C110' of the negative active material layer measured by X-ray diffraction analysis is in the range of 10-16. In some embodiments, the C004'/C110' of the negative active material layer measured by X-ray diffraction analysis is in the range of 12-15.
- the C004'/C110' of the negative electrode active material layer measured by X-ray diffraction analysis is 7, 10, 12, 14, 16, 18 or in the range composed of any two of the foregoing values. Inside. When the C004'/C110' of the negative active material layer is within the above range, the cycle performance of the electrochemical device can be improved.
- the measurement by Raman spectroscopy in the negative active material layer Id 1340cm -1 to peak intensity at 1380cm -1 and the peak intensity of the negative electrode active material layer of 1560cm -1 to 1600cm -1
- the ratio of Ig Id/Ig is 0.2 to 0.5.
- the Id/Ig of the negative active material layer measured by Raman spectroscopy is 0.25 to 0.45.
- the Id/Ig of the negative active material layer measured by Raman spectroscopy is 0.3 to 0.4.
- the Id/Ig of the negative electrode active material layer measured by Raman spectroscopy is 0.2, 0.25, 0.3, 0.35, 0.4, 0.45, 0.5 or within a range composed of any two of the foregoing values.
- the Id/Ig of the negative electrode active material layer can characterize the surface defect degree of the negative electrode active material layer. When the Id/Ig is too small, the negative electrode active material layer has fewer surface defects, and the graphite flakes are arranged tightly and regularly; when the Id/Ig is too large, the negative electrode active material layer has more surface defects, which will affect the solid electrolyte membrane (SEI Film) stability.
- the negative electrode active material layer has an appropriate amount of surface defects, which can ensure the insertion/extraction of lithium ions and the stability of the SEI film, which helps to improve Cycle performance of electrochemical devices.
- the negative electrode current collector used in the present application may be selected from copper foil, nickel foil, stainless steel foil, titanium foil, foamed nickel, foamed copper, polymer substrates coated with conductive metals, and combinations thereof.
- the negative electrode further includes a conductive layer.
- the conductive material of the conductive layer may include any conductive material as long as it does not cause a chemical change.
- conductive materials include carbon-based materials (e.g., natural graphite, artificial graphite, carbon black, acetylene black, Ketjen black, carbon fibers, carbon nanotubes, graphene, etc.), metal-based materials (e.g., metal Powder, metal fibers, etc., such as copper, nickel, aluminum, silver, etc.), conductive polymers (e.g., polyphenylene derivatives), and mixtures thereof.
- the negative electrode further includes a binder, and the binder is selected from at least one of the following: polyvinyl alcohol, carboxymethyl cellulose, hydroxypropyl cellulose, and diacetyl cellulose , Polyvinyl chloride, carboxylated polyvinyl chloride, polyvinyl fluoride, ethylene oxide-containing polymers, polyvinylpyrrolidone, polyurethane, polytetrafluoroethylene, polyvinylidene fluoride, polyethylene, poly Propylene, styrene butadiene rubber, acrylic (ester) styrene butadiene rubber, epoxy resin or nylon, etc.
- the binder is selected from at least one of the following: polyvinyl alcohol, carboxymethyl cellulose, hydroxypropyl cellulose, and diacetyl cellulose , Polyvinyl chloride, carboxylated polyvinyl chloride, polyvinyl fluoride, ethylene oxide-containing polymers, polyvinylpyrrolidone
- the positive electrode includes a positive electrode current collector and a positive electrode active material provided on the positive electrode current collector.
- the specific types of positive electrode active materials are not subject to specific restrictions, and can be selected according to requirements.
- the positive electrode active material includes a positive electrode material capable of absorbing and releasing lithium (Li).
- positive electrode materials capable of absorbing/releasing lithium (Li) may include lithium cobalt oxide, lithium nickel cobalt manganate, lithium nickel cobalt aluminate, lithium manganate, lithium iron manganese phosphate, lithium vanadium phosphate, lithium vanadyl phosphate, and phosphoric acid. Lithium iron, lithium titanate and lithium-rich manganese-based materials.
- the chemical formula of lithium cobalt oxide can be as chemical formula 1:
- M1 represents selected from nickel (Ni), manganese (Mn), magnesium (Mg), aluminum (Al), boron (B), titanium (Ti), vanadium (V), chromium (Cr), iron (Fe), Copper (Cu), zinc (Zn), molybdenum (Mo), tin (Sn), calcium (Ca), strontium (Sr), tungsten (W), yttrium (Y), lanthanum (La), zirconium (Zr) and For at least one of silicon (Si), the values of x, a, b, and c are within the following ranges: 0.8 ⁇ x ⁇ 1.2, 0.8 ⁇ a ⁇ 1, 0 ⁇ b ⁇ 0.2, -0.1 ⁇ c ⁇ 0.2.
- the chemical formula of lithium nickel cobalt manganate or lithium nickel cobalt aluminate can be as chemical formula 2:
- M2 represents selected from cobalt (Co), manganese (Mn), magnesium (Mg), aluminum (Al), boron (B), titanium (Ti), vanadium (V), chromium (Cr), iron (Fe), At least one of copper (Cu), zinc (Zn), molybdenum (Mo), tin (Sn), calcium (Ca), strontium (Sr), tungsten (W), zirconium (Zr), and silicon (Si),
- the values of y, d, e, and f are in the following ranges: 0.8 ⁇ y ⁇ 1.2, 0.3 ⁇ d ⁇ 0.98, 0.02 ⁇ e ⁇ 0.7, -0.1 ⁇ f ⁇ 0.2.
- the chemical formula of lithium manganate can be as chemical formula 3:
- M3 represents selected from cobalt (Co), nickel (Ni), magnesium (Mg), aluminum (Al), boron (B), titanium (Ti), vanadium (V), chromium (Cr), iron (Fe), At least one of copper (Cu), zinc (Zn), molybdenum (Mo), tin (Sn), calcium (Ca), strontium (Sr) and tungsten (W), with z, g and h values in the following ranges respectively Inner: 0.8 ⁇ z ⁇ 1.2, 0 ⁇ g ⁇ 1.0 and -0.2 ⁇ h ⁇ 0.2.
- the weight of the positive electrode active material layer is 1.5 to 15 times the weight of the negative electrode active material layer. In some embodiments, the weight of the positive active material layer is 3 to 10 times the weight of the negative active material layer. In some embodiments, the weight of the positive active material layer is 5 to 8 times the weight of the negative active material layer. In some embodiments, the weight of the positive active material layer is 1.5 times, 2 times, 3 times, 4 times, 5 times, 6 times, 7 times, 8 times, 9 times the weight of the negative active material layer. , 10 times, 11 times, 12 times, 13 times, 14 times or 15 times.
- the positive active material layer may have a coating on the surface, or may be mixed with another compound having a coating.
- the coating may include oxides of coating elements, hydroxides of coating elements, oxyhydroxides of coating elements, oxycarbonates of coating elements, and hydroxycarbonates of coating elements ( At least one coating element compound selected from hydroxycarbonate).
- the compound used for the coating may be amorphous or crystalline.
- the coating element contained in the coating may include Mg, Al, Co, K, Na, Ca, Si, Ti, V, Sn, Ge, Ga, B, As, Zr, F, or a mixture thereof.
- the coating can be applied by any method as long as the method does not adversely affect the performance of the positive electrode active material.
- the method may include any coating method well-known to those of ordinary skill in the art, such as spraying, dipping, and the like.
- the positive active material layer further includes a binder, and optionally further includes a positive conductive material.
- the binder can improve the binding of the positive electrode active material particles to each other, and also improve the binding of the positive electrode active material to the current collector.
- binders include polyvinyl alcohol, hydroxypropyl cellulose, diacetyl cellulose, polyvinyl chloride, carboxylated polyvinyl chloride, polyvinyl fluoride, ethylene oxide-containing polymers, polyvinyl chloride Vinylpyrrolidone, polyurethane, polytetrafluoroethylene, polyvinylidene fluoride, polyethylene, polypropylene, styrene butadiene rubber, acrylic (ester) styrene butadiene rubber, epoxy resin, nylon, etc.
- the positive electrode active material layer includes a positive electrode conductive material, thereby imparting conductivity to the electrode.
- the positive electrode conductive material may include any conductive material as long as it does not cause a chemical change.
- Non-limiting examples of positive electrode conductive materials include carbon-based materials (e.g., natural graphite, artificial graphite, carbon black, acetylene black, Ketjen black, carbon fiber, etc.), metal-based materials (e.g., metal powder, metal fiber, etc., Including, for example, copper, nickel, aluminum, silver, etc.), conductive polymers (for example, polyphenylene derivatives), and mixtures thereof.
- the positive electrode current collector used in the electrochemical device according to the present application may be aluminum (Al), but is not limited thereto.
- the electrolyte that can be used in the embodiments of the present application may be an electrolyte known in the prior art.
- the electrolyte that can be used in the electrolyte in the embodiments of the present application includes, but is not limited to: inorganic lithium salts, such as LiClO 4 , LiAsF 6 , LiPF 6 , LiBF 4 , LiSbF 6 , LiSO 3 F, LiN(FSO 2 ) 2, etc.; Fluorine-containing organic lithium salts, such as LiCF 3 SO 3 , LiN(FSO 2 )(CF 3 SO 2 ), LiN(CF 3 SO 2 ) 2 , LiN(C 2 F 5 SO 2 ) 2 , cyclic 1,3- Lithium hexafluoropropane disulfonimide, lithium cyclic 1,2-tetrafluoroethane disulfonimide, LiN (CF 3 SO 2 ) (C 4 F 9 SO 2 ), LiC (CF 3 SO 2 ) 3.
- inorganic lithium salts such as LiClO 4 , LiAsF 6 , LiPF 6 , Li
- Lithium salt containing dicarboxylic acid complex such as bis(oxalato) lithium borate, difluorooxalic acid Lithium borate, tris(oxalato) lithium phosphate, diflu
- the electrolyte includes a combination of LiPF 6 and LiBF 4.
- the electrolyte includes a combination of an inorganic lithium salt such as LiPF 6 or LiBF 4 and a fluorine-containing organic lithium salt such as LiCF 3 SO 3 , LiN(CF 3 SO 2 ) 2 , and LiN(C 2 F 5 SO 2 ) 2 .
- the electrolyte includes LiPF 6 .
- the concentration of the electrolyte is in the range of 0.8-3 mol/L, for example, in the range of 0.8-2.5 mol/L, in the range of 0.8-2 mol/L, in the range of 1-2 mol/L, for example It is 1mol/L, 1.15mol/L, 1.2mol/L, 1.5mol/L, 2mol/L or 2.5mol/L.
- Solvents that can be used in the electrolyte of the embodiments of the present application include, but are not limited to, cyclic carbonate, chain carbonate, cyclic carboxylic acid ester, chain carboxylic acid ester, cyclic ether, chain ether, phosphorus-containing Organic solvents, sulfur-containing organic solvents and aromatic fluorine-containing solvents.
- the cyclic carbonate includes, but is not limited to, ethylene carbonate (EC), propylene carbonate (PC), and butylene carbonate.
- the cyclic carbonate has 3-6 carbon atoms.
- the chain carbonate includes, but is not limited to: dimethyl carbonate, ethyl methyl carbonate, diethyl carbonate (DEC), methyl n-propyl carbonate, ethyl n-propyl carbonate Carbonic acid esters, di-n-propyl carbonate and other chain carbonates, as chain carbonates substituted by fluorine, such as bis(fluoromethyl)carbonate, bis(difluoromethyl)carbonate, bis(trifluoromethyl) ) Carbonate, bis(2-fluoroethyl)carbonate, bis(2,2-difluoroethyl)carbonate, bis(2,2,2-trifluoroethyl)carbonate, 2-fluoroethyl Methyl carbonate, 2,2-difluoroethyl methyl carbonate and 2,2,2-trifluoroethyl methyl carbonate.
- fluorine such as bis(fluoromethyl)carbonate, bis(difluoromethyl)carbonate,
- cyclic carboxylic acid esters include, but are not limited to, ⁇ -butyrolactone and ⁇ -valerolactone.
- part of the hydrogen atoms of the cyclic carboxylic acid ester may be substituted by fluorine.
- the chain carboxylic acid esters include, but are not limited to: methyl acetate, ethyl acetate, propyl acetate, isopropyl acetate, butyl acetate, sec-butyl acetate, isobutyl acetate, tertiary acetate Butyl ester, methyl propionate, ethyl propionate, propyl propionate, isopropyl propionate, methyl butyrate, ethyl butyrate, propyl butyrate, methyl isobutyrate, ethyl isobutyrate , Methyl valerate, ethyl valerate, methyl pivalate and ethyl pivalate.
- part of the hydrogen atoms of the chain carboxylic acid ester may be replaced by fluorine.
- fluorine-substituted chain carboxylic acid esters include, but are not limited to: methyl trifluoroacetate, ethyl trifluoroacetate, propyl trifluoroacetate, butyl trifluoroacetate, and trifluoroacetic acid 2,2 ,2-Trifluoroethyl ester.
- cyclic ethers include, but are not limited to, tetrahydrofuran, 2-methyltetrahydrofuran, 1,3-dioxolane, 2-methyl 1,3-dioxolane, 4-methyl 1 ,3-dioxolane, 1,3-dioxane, 1,4-dioxane and dimethoxypropane.
- chain ethers include, but are not limited to, dimethoxymethane, 1,1-dimethoxyethane, 1,2-dimethoxyethane, diethoxymethane, 1 ,1-diethoxyethane, 1,2-diethoxyethane, ethoxymethoxymethane, 1,1-ethoxymethoxyethane and 1,2-ethoxymethane Oxyethane.
- the phosphorus-containing organic solvent includes, but is not limited to, trimethyl phosphate, triethyl phosphate, dimethyl ethyl phosphate, methyl diethyl phosphate, ethylene methyl phosphate, ethylene phosphate Ethyl ester, triphenyl phosphate, trimethyl phosphite, triethyl phosphite, triphenyl phosphite, tris(2,2,2-trifluoroethyl) phosphate and tris(2,2, 3,3,3-pentafluoropropyl) ester.
- sulfur-containing organic solvents include, but are not limited to, sulfolane, 2-methyl sulfolane, 3-methyl sulfolane, dimethyl sulfone, diethyl sulfone, ethyl methyl sulfone, methyl propyl sulfone Sulfone, dimethyl sulfoxide, methyl methanesulfonate, ethyl methanesulfonate, methyl ethanesulfonate, ethyl ethanesulfonate, dimethyl sulfate, diethyl sulfate, and dibutyl sulfate.
- part of the hydrogen atoms of the sulfur-containing organic solvent may be replaced by fluorine.
- the aromatic fluorine-containing solvent includes, but is not limited to, fluorobenzene, difluorobenzene, trifluorobenzene, tetrafluorobenzene, pentafluorobenzene, hexafluorobenzene, and trifluoromethylbenzene.
- the solvent used in the electrolyte of the present application includes one or more of the above.
- the solvent used in the electrolyte of the present application includes cyclic carbonate, chain carbonate, cyclic carboxylic acid ester, chain carboxylic acid ester, and combinations thereof.
- the solvent used in the electrolyte of the present application includes an organic solvent selected from the group consisting of: ethylene carbonate, propylene carbonate, diethyl carbonate, ethyl propionate, propionic acid Propyl ester, n-propyl acetate, ethyl acetate and combinations thereof.
- the solvent used in the electrolyte of the present application includes: ethylene carbonate, propylene carbonate, diethyl carbonate, ethyl propionate, propyl propionate, ⁇ -butyrolactone or a combination thereof .
- the additives that can be used in the electrolyte of the embodiments of the present application include, but are not limited to, compounds with 2-3 cyano groups, cyclic carbonates containing carbon-carbon double bonds, compounds containing sulfur-oxygen double bonds, difluorophosphoric acid lithium.
- the compound having 2-3 cyano groups may include selected from succinonitrile (SN), adiponitrile (ADN), ethylene glycol bis(propionitrile) ether (EDN), 1,3, 5-pentanetricarbonitrile, 1,2,3-propanetricarbonitrile, 1,3,6-hexamethylenetricarbonitrile (HTCN), 1,2,6-hexamethylenetricarbonitrile, 1,2,3-tris(2-cyanide At least one of ethoxy)propane (TCEP) or 1,2,4-tris(2-cyanoethoxy)butane.
- SN succinonitrile
- ADN adiponitrile
- EDN ethylene glycol bis(propionitrile) ether
- HTCN 1,3,6-hexamethylenetricarbonitrile
- TCEP ethoxypropane
- 1,2,4-tris(2-cyanoethoxy)butane 1,2,4-tris(2-cyanoethoxy)butane.
- the cyclic carbonate having a carbon-carbon double bond specifically includes, but is not limited to: vinylene carbonate, methyl vinylene carbonate, ethyl vinylene carbonate, vinyl ethylene ethylene carbonate Or at least one of carbonic acid-1,2-dimethyl vinylene ester.
- compounds containing sulfur and oxygen double bonds include, but are not limited to: vinyl sulfate, 1,2-propanediol sulfate, 1,3-propane sultone, 1-fluoro-1,3-propane At least one of sultone, 2-fluoro-1,3-propane sultone or 3-fluoro-1,3-propane sultone.
- a separator is provided between the positive electrode and the negative electrode to prevent short circuits.
- the material and shape of the isolation film that can be used in the embodiments of the present application are not particularly limited, and they can be any technology disclosed in the prior art.
- the isolation membrane includes a polymer or an inorganic substance formed of a material that is stable to the electrolyte of the present application, or the like.
- the isolation film may include a substrate layer and a surface treatment layer.
- the substrate layer is a non-woven fabric, film or composite film with a porous structure, and the material of the substrate layer is selected from at least one of polyethylene, polypropylene, polyethylene terephthalate and polyimide.
- a polypropylene porous film, a polyethylene porous film, a polypropylene non-woven fabric, a polyethylene non-woven fabric, or a polypropylene-polyethylene-polypropylene porous composite film can be selected.
- the porous structure can improve the heat resistance, oxidation resistance and electrolyte infiltration performance of the isolation membrane, and enhance the adhesion between the isolation membrane and the pole piece.
- a surface treatment layer is provided on at least one surface of the substrate layer.
- the surface treatment layer may be a polymer layer or an inorganic substance layer, or a layer formed by a mixed polymer and an inorganic substance.
- the inorganic layer includes inorganic particles and a binder.
- the inorganic particles are selected from alumina, silica, magnesium oxide, titanium oxide, hafnium dioxide, tin oxide, ceria, nickel oxide, zinc oxide, calcium oxide, zirconium oxide, One or a combination of yttrium oxide, silicon carbide, boehmite, aluminum hydroxide, magnesium hydroxide, calcium hydroxide, and barium sulfate.
- the binder is selected from polyvinylidene fluoride, vinylidene fluoride-hexafluoropropylene copolymer, polyamide, polyacrylonitrile, polyacrylate, polyacrylic acid, polyacrylate, polyvinylpyrrolidone, polyvinyl ether, One or a combination of polymethyl methacrylate, polytetrafluoroethylene and polyhexafluoropropylene.
- the polymer layer contains a polymer, and the material of the polymer is selected from polyamide, polyacrylonitrile, acrylate polymer, polyacrylic acid, polyacrylate, polyvinylpyrrolidone, polyvinyl ether, polyvinylidene fluoride, poly At least one of (vinylidene fluoride-hexafluoropropylene).
- the present application also provides an electrochemical device, which includes a positive electrode, an electrolyte, and a negative electrode.
- the positive electrode includes a positive electrode active material layer and a positive electrode current collector.
- the negative electrode includes a negative electrode active material layer and a negative electrode current collector.
- the material layer includes the negative active material according to the present application.
- the electrochemical device of the present application includes any device that undergoes an electrochemical reaction, and specific examples thereof include all kinds of primary batteries, secondary batteries, fuel cells, solar cells, or capacitors.
- the electrochemical device is a lithium secondary battery, including a lithium metal secondary battery, a lithium ion secondary battery, a lithium polymer secondary battery, or a lithium ion polymer secondary battery.
- the application also provides an electronic device, which includes the electrochemical device according to the application.
- the use of the electrochemical device of the present application is not particularly limited, and it can be used in any electronic device known in the prior art.
- the electrochemical device of the present application can be used in, but not limited to, notebook computers, pen-input computers, mobile computers, e-book players, portable phones, portable fax machines, portable copiers, portable printers, and headsets.
- Stereo headsets video recorders, LCD TVs, portable cleaners, portable CD players, mini discs, transceivers, electronic notebooks, calculators, memory cards, portable recorders, radios, backup power supplies, motors, cars, motorcycles, power assistance Bicycles, bicycles, lighting equipment, toys, game consoles, clocks, power tools, flashlights, cameras, large household storage batteries and lithium-ion capacitors, etc.
- Graphite, styrene-butadiene rubber (SBR) and sodium carboxymethyl cellulose (CMC) are mixed thoroughly in an appropriate amount of deionized water at a weight ratio of 97.2:1.8:1 to form a uniform negative electrode slurry.
- the graphitization degree of graphite is obtained by controlling the graphitization temperature and holding time.
- the heating time is in the range of 12-17 hours, and the temperature is raised to the range of 2600°C-3000°C, and then the temperature is kept.
- the holding time is in the range of 85h-100h, and the temperature is naturally lowered.
- the aspect ratio is controlled by the shaping and screening process.
- LiFePO 4 lithium iron phosphate
- PVDF conductive agent acetylene black
- NMP N-methylpyrrolidone
- ethylene carbonate abbreviated as EC
- DEC diethyl carbonate
- PC propylene carbonate
- a polyethylene (PE) porous polymer film is used as the isolation membrane.
- the positive electrode, separator, and negative electrode in order, so that the separator is between the positive electrode and the negative electrode for isolation, and then wind to obtain a bare cell; after welding the tabs, place the bare cell on the outer packaging foil aluminum plastic
- the electrolyte prepared above is injected into the dried bare cell, and the process of vacuum packaging, standing, forming, shaping, and capacity testing is carried out to obtain a lithium ion battery.
- Simpatec QICPIC dynamic particle image analyzer was used to test the aspect ratio distribution of the negative electrode active material.
- Id/Ig is the calculated ratio of D peak intensity Id to G peak intensity Ig.
- the compaction density of the active material layer was tested in accordance with the National Standard of the People's Republic of China GB/T 24533-2009 "Graphite Anode Materials for Lithium Ion Batteries".
- the compact density of the obtained active material layer is the density after decompression of 5T.
- the testing instrument is Malvern Master Size 3000, the anode material is dispersed in the dispersant (ethanol), ultrasonic After 30 minutes, the sample was added to the Malvern particle size tester to start the test.
- the particle size that reaches 10% of the cumulative volume from the small particle size side is the Dv10 of the negative electrode material; at the same time, the negative electrode material is in the volume-based particle size distribution, starting from the small particle size.
- the particle size from the radial side up to 99% of the cumulative volume is the Dv99 of the negative electrode material.
- the electrolyte prepared above is added, and the lithium metal sheet is used as the counter electrode to assemble a button battery.
- the test temperature is 23-26°C
- the test process is 0.05C discharge to 5mV, then 0.05mA discharge to 5mV, 0.02mA discharge to 5mV, 0.1C charge to 2.0V, and record the discharge capacity.
- the value of the gram capacity of the negative active material C (mAh/g) discharge capacity/weight of the negative active material.
- the lithium-ion battery was charged to 3.6V at 1C direct current, then charged to 0.05C at a constant voltage of 3.6V, allowed to stand for 10 minutes, and then discharged to 2.5V at 1C direct current. This is a cycle, and the discharge capacity of the first cycle is recorded. Repeat the above steps 1000 times, and record the discharge capacity after the cycle. Calculate the cycle capacity retention rate of lithium-ion batteries by the following formula:
- Cycle capacity retention rate (discharge capacity after cycle/discharge capacity at first cycle) ⁇ 100%.
- the lithium-ion battery was charged to 3.6V at 1C DC, then charged at a constant voltage of 3.6V to 0.05C, allowed to stand for 10 minutes, and then discharged to 2.5V at 1C DC. This is a cycle, and the thickness H0 of the lithium-ion battery after being charged at a constant voltage of 3.6V to 0.05C during the cycle stage and standing for 10 minutes is recorded. Repeat the above steps 1000 times, and record the thickness H1 of the lithium-ion battery after charging at a constant voltage of 3.6V to 0.05C during the 1000th cycle and standing for 10 minutes. Calculate the thickness rebound rate of lithium-ion batteries by the following formula:
- Thickness rebound rate (H1-H0)/H0 ⁇ 100%.
- Table 1 shows the influence of the graphitization degree and aspect ratio of the carbon material in the negative active material on the cycle performance of the lithium ion battery.
- Table 2 shows the influence of the aspect ratio of the carbon material in the negative active material on the cycle performance of the lithium ion battery. Examples 7-12 are based on the improvement of Example 3, and the difference lies only in the parameters listed in Table 2.
- Table 3 shows the influence of the grain size and graphitization degree of the carbon material and the compaction density of the negative electrode active material layer on the cycle performance of the lithium ion battery. Examples 13-22 are improvements based on Example 8, and the difference lies only in the parameters listed in Table 3.
- Table 4 shows the influence of the particle size, interplanar spacing and orientation of the negative active material on the performance of the lithium ion battery. Examples 23-29 are improvements based on Example 16, and the difference lies only in the parameters listed in Table 4.
- the cycle capacity retention rate and thickness rebound rate of the lithium ion battery can be further improved.
- Table 5 shows the influence of the gram capacity of the negative active material on the cycle performance of the lithium ion battery. Examples 30-36 are improvements based on Example 24, and the difference lies only in the parameters listed in Table 5.
- the C004'/C110' of the negative electrode active material layer in the lithium ion battery of Example 33 was 8.63, and the Id/Ig was 0.25; the C004/C110 of the negative electrode active material was 5.78.
- the lithium ion battery of Example 36 was cycled 3000 times using the cycle procedure in "Testing Method for Cycle Capacity Retention Rate of Lithium Ion Battery". Then disassemble the fully charged lithium-ion battery, take out the negative electrode, wash and dry it. The negative electrode active material layer and the negative electrode active material are extracted.
- the C004'/C110' of the negative active material layer after cycling was 8.51, and the Id/Ig was 0.37; the C004/C110 of the negative active material after cycling was 5.76.
- the C004'/C110' of the negative active material layer is still in the range of 7 to 18, and the Id/Ig is still in the range of 0.2 to 0.5. That is, the orientation of the negative electrode active material layer of the lithium ion battery of the present application does not change significantly after cycling, and the active material has good structural stability.
- Fig. 6 shows a curve diagram of the cycle capacity retention rate with the number of cycles in Comparative Example 2 and Example 1 according to the present application. The results show that the lithium ion battery of Example 1 has a cycle capacity retention rate significantly higher than that of the lithium ion battery of Comparative Example 2.
- Fig. 7 shows a graph of the thickness rebound rate with the number of cycles in Comparative Example 2 and Example 1 according to the present application. The results show that the lithium ion battery of Example 1 has a thickness rebound rate significantly lower than that of the lithium ion battery of Comparative Example 2.
- references to “embodiments”, “parts of embodiments”, “one embodiment”, “another example”, “examples”, “specific examples” or “partial examples” throughout the specification mean that At least one embodiment or example in this application includes the specific feature, structure, material, or characteristic described in the embodiment or example. Therefore, descriptions appearing in various places throughout the specification, such as: “in some embodiments”, “in an embodiment”, “in one example”, “in another example”, “in an example “In”, “in a specific example” or “exemplary”, which are not necessarily quoting the same embodiment or example in this application.
- the specific features, structures, materials or characteristics herein can be combined in one or more embodiments or examples in any suitable manner.
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Abstract
一种负极活性材料及使用其的电化学装置和电子装置,所述负极活性材料包含碳材料,其中所述碳材料具有特定的石墨化度以及长径比分布,所述负极活性材料有助于改善电化学装置的循环性能。
Description
本申请涉及储能领域,具体涉及一种负极活性材料及使用其的电化学装置和电子装置。
电化学装置(例如,锂离子电池)由于具有环境友好、工作电压高、比容量大和循环寿命长等优点而被广泛应用,已成为当今世界最具发展潜力的新型绿色化学电源。小尺寸锂离子电池通常用作驱动便携式电子通讯设备(例如,便携式摄像机、移动电话或者笔记本电脑等)的电源,特别是高性能便携式设备的电源。具有高输出特性的中等尺寸和大尺寸锂例子电池被发展应用于电动汽车(EV)和大规模储能系统(ESS)。随着锂离子电池的广泛应用,其循环性能已成为亟待解决的关键技术问题。改进极片中的活性材料是解决上述问题的研究方向之一。
有鉴于此,确有必要提供一种改进的负极活性材料及使用其的电化学装置和电子装置。
发明内容
本申请通过提供一种负极活性材料及使用其的电化学装置和电子装置以试图在至少某种程度上解决至少一种存在于相关领域中的问题。
根据本申请的一个方面,本申请提供了一种负极活性材料,所述负极活性材料包含碳材料,其中由X射线衍射分析法测定得到的所述碳材料的石墨化度Gr为0.82至0.92,且基于所述碳材料的总颗粒数量,所述碳材料中长径比为3.3以上的颗粒的占比为10%以下。
在一些实施例中,由X射线衍射分析法测定得到的所述碳材料的石墨化度Gr为0.85至0.90。在一些实施例中,由X射线衍射分析法测定得到的所述碳材料的石墨化度Gr为0.82、0.83、0.84、0.85、0.86、0.87、0.88、0.89、0.90、0.91、0.92或在以上任意两个数值所组成的范围内。
在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为3.3以上的颗粒的占比为8%以下。在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材 料中长径比为3.3以上的颗粒的占比为6%以下。在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为3.3以上的颗粒的占比为1%以上。在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为3.3以上的颗粒的占比为3%以上。在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为3.3以上的颗粒的占比为5%以上。在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为3.3以上的颗粒的占比在上述任意两个端点值所组成的范围内。
根据本申请的实施例,基于所述碳材料的总颗粒数量,所述碳材料中长径比为2以上的颗粒的占比为50%以下,所述碳材料中长径比为1.5以上的颗粒的占比为80%以下。
在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为2以上的颗粒的占比为45%以下。在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为2以上的颗粒的占比为40%以下。在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为2以上的颗粒的占比为30%以上。在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为2以上的颗粒的占比为35%以上。在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为2以上的颗粒的占比在上述任意两个端点值所组成的范围内。
在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为1.5以上的颗粒的占比为75%以下。在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为1.5以上的颗粒的占比为70%以下。在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为1.5以上的颗粒的占比为50%以上。在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为1.5以上的颗粒的占比为55%以上。在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为1.5以上的颗粒的占比为60%以上。在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为1.5以上的颗粒的占比为65%以上。在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为1.5以上的颗粒的占比在上述任意两个端点值所组成的范围内。
根据本申请的实施例,由X射线衍射分析法测定的所述碳材料的晶粒沿水平轴的晶粒尺寸La与由X射线衍射分析法测定的所述碳材料的晶粒沿垂直轴的晶粒尺寸Lc的比值为K,Gr与K满足以下关系:4.0≤K×Gr≤5.2。在一些实施例中,Gr与K满足以下关系:4.2≤K×Gr≤5.0。在一些实施例中,Gr与K满足以下关系:4.5≤K×Gr ≤4.8。
根据本申请的实施例,所述负极活性材料的颗粒尺寸满足以下关系:35μm<Dv99-Dv10<50μm。在一些实施例中,所述负极活性材料的颗粒尺寸满足以下关系:42μm<Dv99-Dv10<48μm。在一些实施例中,所述负极活性材料的颗粒尺寸满足以下关系:43μm<Dv99-Dv10<45μm。
根据本申请的实施例,由X射线衍射分析法测定的所述负极活性材料的晶面间距d002≥0.3365nm。在一些实施例中,由X射线衍射分析法测定的所述负极活性材料的晶面间距d002≥0.3370nm。在一些实施例中,由X射线衍射分析法测定的所述负极活性材料的晶面间距d002≥0.3375nm。在一些实施例中,由X射线衍射分析法测定的所述负极活性材料的晶面间距d002为0.3365nm、0.3368nm、0.3370nm、0.3372nm、0.3375或在以上任意两个数值所组成的范围内。
根据本申请的实施例,由X射线衍射分析法测定得到的所述负极活性材料的(004)晶面的峰面积C004和(110)晶面的峰面积C110的比值C004/C110≤8。在一些实施中,由X射线衍射分析法测定得到的所述负极活性材料的C004/C110≤7.5。在一些实施中,由X射线衍射分析法测定得到的所述负极活性材料的C004/C110≤7。在一些实施中,由X射线衍射分析法测定得到的所述负极活性材料的C004/C110≤6.5。在一些实施中,由X射线衍射分析法测定得到的所述负极活性材料的C004/C110≤6。在一些实施中,由X射线衍射分析法测定得到的所述负极活性材料的C004/C110≤5.5。在一些实施中,由X射线衍射分析法测定得到的所述负极活性材料的C004/C110≤5。在一些实施中,由X射线衍射分析法测定得到的所述负极活性材料的C004/C110≥3。在一些实施中,由X射线衍射分析法测定得到的所述负极活性材料的C004/C110≥3.5。在一些实施中,由X射线衍射分析法测定得到的所述负极活性材料的C004/C110≥4。在一些实施中,由X射线衍射分析法测定得到的所述负极活性材料的C004/C110≥4.5。在一些实施中,由X射线衍射分析法测定得到的所述负极活性材料的C004/C110在上述任意两个端点值所组成的范围内。
根据本申请的实施例,所述负极活性材料的克容量C mAh/g与所述碳材料的石墨化度Gr满足以下关系:390Gr-C≤20,C≤350。
在一些实施例中,C与Gr满足以下关系:390Gr-C≤18。在一些实施例中,C与Gr满足以下关系:390Gr-C≤15。在一些实施例中,C与Gr满足以下关系:390Gr-C≤12。在一些实施例中,C与Gr满足以下关系:390Gr-C≤15。在一些实施例中,C与 Gr满足以下关系:390Gr-C≤10。在一些实施例中,C与Gr满足以下关系:390Gr-C≤8。在一些实施例中,C与Gr满足以下关系:390Gr-C≤5。在一些实施例中,C与Gr满足以下关系:390Gr-C≥1。在一些实施例中,C与Gr满足以下关系:390Gr-C≥3。在一些实施例中,390Gr-C的值在上述任意两个端点值所组成的范围内。
在一些实施例中,C≤340。在一些实施例中,C≤330。在一些实施例中,C≤320。在一些实施例中,C≤310。在一些实施例中,C≤300。在一些实施例中,C≥250。在一些实施例中,C≥280。在一些实施例中,C≥290。在一些实施例中,所述负极活性材料的克容量的值C在上述任意两个端点值所组成的范围内。
根据本申请的另一个方面,本申请提供了一种电化学装置,其包括正极、电解液和负极,其中所述负极包括负极活性材料层和负极集流体,所述负极活性材料层包含根据本申请所述的负极活性材料。
根据本申请的实施例,所述负极活性材料层的压实密度PD g/cm
3和所述碳材料的石墨化度Gr满足以下关系:PD≤2.5Gr-0.45≤1.85。在一些实施例中,PD和Gr满足以下关系:PD≤2.5Gr-0.45≤1.80。在一些实施例中,PD和Gr满足以下关系:PD≤2.5Gr-0.45≤1.75。在一些实施例中,PD和Gr满足以下关系:PD≤2.5Gr-0.45≤1.70。在一些实施例中,PD和Gr满足以下关系:PD≤2.5Gr-0.45≤1.65。在一些实施例中,PD和Gr满足以下关系:PD≤2.5Gr-0.45≤1.60。
根据本申请的实施例,所述负极活性材料层的压实密度为1.45g/cm
3至1.75g/cm
3。在一些实施例中,所述负极活性材料层的压实密度为1.50g/cm
3至1.70g/cm
3。在一些实施例中,所述负极活性材料层的压实密度为1.55g/cm
3至1.65g/cm
3。在一些实施例中,所述负极活性材料层的压实密度为1.45g/cm
3、1.50g/cm
3、1.55g/cm
3、1.60g/cm
3、1.65g/cm
3、1.70g/cm
3、1.75g/cm
3或在上述任意两个数值所组成的范围内。
根据本申请的实施例,由X射线衍射分析法测定得到的所述负极活性材料层的(004)面的峰面积C004'和(110)面的峰面积C110'的比值C004'/C110'为7至18。在一些实施例中,由X射线衍射分析法测定得到的所述负极活性材料层的C004'/C110'为10至16。在一些实施例中,由X射线衍射分析法测定得到的所述负极活性材料层的C004'/C110'为12至15。在一些实施例中,由X射线衍射分析法测定得到的所述负极活性材料层的C004'/C110'为7、10、12、14、16、18或在上述任意两个数值所组成的范围内。
根据本申请的实施例,由拉曼光谱法测定的所述负极活性材料层在1340cm
-1至 1380cm
-1的峰强度Id与所述负极活性材料层在1560cm
-1至1600cm
-1的峰强度Ig的比值Id/Ig为0.2至0.5。在一些实施例中,由拉曼光谱法测定的所述负极活性材料层的Id/Ig为0.25至0.45。在一些实施例中,由拉曼光谱法测定的所述负极活性材料层的Id/Ig为0.3至0.4。在一些实施例中,由拉曼光谱法测定的所述负极活性材料层的Id/Ig为0.2、0.25、0.3、0.35、0.4、0.45、0.5或在上述任意两个数值所组成的范围内。
根据本申请的又一个方面,本申请提供了一种电子装置,其包括根据本申请所述的电化学装置。
本申请的额外层面及优点将部分地在后续说明中描述、显示、或是经由本申请实施例的实施而阐释。
在下文中将简要地说明为了描述本申请实施例或现有技术所必要的附图以便于描述本申请的实施例。显而易见地,下文描述中的附图仅只是本申请中的部分实施例。对本领域技术人员而言,在不需要创造性劳动的前提下,依然可以根据这些附图中所例示的结构来获得其他实施例的附图。
图1展示了本申请实施例3中使用的负极活性材料的扫描电子显微镜(SEM)图。
图2展示了本申请实施例3中使用的碳材料中长径比为约5.0的颗粒的SEM形貌。
图3展示了本申请实施例3中使用的碳材料中长径比为约2.5的颗粒的SEM形貌。
图4展示了本申请实施例3中使用的碳材料中长径比为约1.5的颗粒的SEM形貌。
图5展示了本申请实施例3中使用的碳材料中长径比为约1.0的颗粒的SEM形貌。
图6展示了对比例2和根据本申请实施例1随循环次数的循环容量保持率曲线图。
图7展示了对比例2和根据本申请实施例1随循环次数的厚度反弹率的曲线图。
本申请的实施例将会被详细的描示在下文中。在本申请说明书中,将相同或相似的组件以及具有相同或相似的功能的组件通过类似附图标记来表示。在此所描述的有关附图的实施例为说明性质的、图解性质的且用于提供对本申请的基本理解。本申请的实施例不应该被解释为对本申请的限制。
在具体实施方式及权利要求书中,由术语“中的至少一种”连接的项目的列表可意味着所列项目的任何组合。例如,如果列出项目A及B,那么短语“A及B中的至少一种”意味着仅A;仅B;或A及B。在另一实例中,如果列出项目A、B及C,那么短语“A、B及C中的至少一种”意味着仅A;或仅B;仅C;A及B(排除C);A及C (排除B);B及C(排除A);或A、B及C的全部。项目A可包含单个元件或多个元件。项目B可包含单个元件或多个元件。项目C可包含单个元件或多个元件。
随着电化学装置(例如,锂离子电池)的广泛应用,对其性能的要求不断提升。循环性能是评价锂离子电池性能的一个重要指标。筛选原料、控制造粒过程、进行表面包覆等手段来改进极片中的活性材料可提高锂离子电池的循环性能,但提升效果有限,已无法满足日益增长的市场需求。
本申请通过调整负极活性材料的石墨化度和颗粒的长径比及其分布以解决上述问题。具体来说,本申请提供了一种负极活性材料,所述负极活性材料包含碳材料,其中由X射线衍射分析法测定得到的所述碳材料的石墨化度Gr为0.82至0.92,且基于所述碳材料的总颗粒数量,所述碳材料中长径比为3.3以上的颗粒的占比为10%以下。
如本文中所使用,碳材料的“长径比”指的是经过碳材料颗粒内部的最长径和与它相垂直的最长径(即,宽经)之比。碳材料的长径比可通过动态颗粒图像分析(例如,使用新帕泰克QICPIC动态颗粒图像分析仪)获得。在负极活性材料的制备过程中,可通过分级的方式控制碳材料的长径比。碳材料的长径比较小时,碳材料颗粒呈细长形状。碳材料的宽长比越接近1,表明碳材料颗粒的长径与宽经越相近,即,碳材料颗粒越接近正方形或圆形。图1展示了本申请实施例3中使用的碳材料的扫描电子显微镜(SEM)图,其中长径比为约5.0的颗粒呈细长形,其形貌如图2所示。球形的碳材料颗粒比表面积较小,消耗电解液少,而且在负极中的排布取向度低,有利于电解液的浸润,从而可提高了电化学装置的循环性能。
如本文中所使用,碳材料的“石墨化度”是指碳材料在高温下或二次加热过程中非石墨炭转变为类石墨炭的程度。当碳材料具有较高的石墨化度(例如,大于0.92)时,碳材料的晶面间距d002减小,不利于锂离子从碳材料中脱嵌。当碳材料具有较低的石墨化度(例如,小于0.92)时,碳材料中的SP
3键较多,使碳材料的各层之间相互牵制,从而使碳材料的结构更稳定。
在一些实施例中,由X射线衍射分析法测定得到的所述碳材料的石墨化度Gr为0.85至0.90。在一些实施例中,由X射线衍射分析法测定得到的所述碳材料的石墨化度Gr为0.82、0.83、0.84、0.85、0.86、0.87、0.88、0.89、0.90、0.91、0.92或在以上任意两个数值所组成的范围内。
在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为3.3以上的颗粒的占比为8%以下。在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材 料中长径比为3.3以上的颗粒的占比为6%以下。在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为3.3以上的颗粒的占比为1%以上。在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为3.3以上的颗粒的占比为3%以上。在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为3.3以上的颗粒的占比为5%以上。在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为3.3以上的颗粒的占比在上述任意两个端点值所组成的范围内。
当负极活性材料中的碳材料同时满足上述石墨化度和具有特定长径比的颗粒占比时,可显著改电化学装置的循环性能,延长电化学装置的使用寿命。
根据本申请的实施例,基于所述碳材料的总颗粒数量,所述碳材料中长径比为2以上的颗粒的占比为50%以下,所述碳材料中长径比为1.5以上的颗粒的占比为80%以下。如图3所示,长径比为约2.5的颗粒呈椭球形。如图4和5所示,长径比为约1.5和约1.0的颗粒近似球形。当碳材料的长径比较小时,碳材料颗粒的接触面积分布更均匀,有利于电解液浸润负极活性材料层。搭配使用不同形状的颗粒可进一步改善电化学装置的循环性能。
在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为2以上的颗粒的占比为45%以下。在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为2以上的颗粒的占比为40%以下。在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为2以上的颗粒的占比为30%以上。在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为2以上的颗粒的占比为35%以上。在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为2以上的颗粒的占比在上述任意两个端点值所组成的范围内。
在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为1.5以上的颗粒的占比为75%以下。在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为1.5以上的颗粒的占比为70%以下。在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为1.5以上的颗粒的占比为50%以上。在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为1.5以上的颗粒的占比为55%以上。在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为1.5以上的颗粒的占比为60%以上。在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为1.5以上的颗粒的占比为65%以上。在一些实施例中,基于所述碳材料的总颗粒数量,所述碳材料中长径比为1.5以上的颗粒的占比在上述任意两个端点值所 组成的范围内。
根据本申请的实施例,由X射线衍射分析法测定的所述碳材料的晶粒沿水平轴的晶粒尺寸La与由X射线衍射分析法测定的所述碳材料的晶粒沿垂直轴的晶粒尺寸Lc的比值为K,Gr与K满足以下关系:4.0≤K×Gr≤5.2。在一些实施例中,Gr与K满足以下关系:4.2≤K×Gr≤5.0。在一些实施例中,Gr与K满足以下关系:4.5≤K×Gr≤4.8。当碳材料的晶粒尺寸La和Lc的比值K与石墨化度Gr满足上述关系时,可以进一步改善电化学装置的循环性能。
根据本申请的实施例,所述负极活性材料的颗粒尺寸满足以下关系:35μm<Dv99-Dv10<50μm。在一些实施例中,所述负极活性材料的颗粒尺寸满足以下关系:42μm<Dv99-Dv10<48μm。在一些实施例中,所述负极活性材料的颗粒尺寸满足以下关系:43μm<Dv99-Dv10<45μm。控制负极活性材料的颗粒尺寸使其Dv99和Dv10满足上述关系时,可以进一步改善电化学装置的循环性能。
根据本申请的实施例,由X射线衍射分析法测定的所述负极活性材料的晶面间距d002≥0.3365nm。在一些实施例中,由X射线衍射分析法测定的所述负极活性材料的晶面间距d002≥0.3370nm。在一些实施例中,由X射线衍射分析法测定的所述负极活性材料的晶面间距d002≥0.3375nm。在一些实施例中,由X射线衍射分析法测定的所述负极活性材料的晶面间距d002为0.3365nm、0.3368nm、0.3370nm、0.3372nm、0.3375或在以上任意两个数值所组成的范围内。当负极活性材料的晶面间距d002在上述范围内时,有助于锂离子的快速脱嵌,可减少负极活性材料的片层的破坏,从而可进一步改善电化学装置的循环性能。
根据本申请的实施例,由X射线衍射分析法测定得到的所述负极活性材料的(004)晶面的峰面积C004和(110)晶面的峰面积C110的比值C004/C110≤8。在一些实施中,由X射线衍射分析法测定得到的所述负极活性材料的C004/C110≤7.5。在一些实施中,由X射线衍射分析法测定得到的所述负极活性材料的C004/C110≤7。在一些实施中,由X射线衍射分析法测定得到的所述负极活性材料的C004/C110≤6.5。在一些实施中,由X射线衍射分析法测定得到的所述负极活性材料的C004/C110≤6。在一些实施中,由X射线衍射分析法测定得到的所述负极活性材料的C004/C110≤5.5。在一些实施中,由X射线衍射分析法测定得到的所述负极活性材料的C004/C110≤5。在一些实施中,由X射线衍射分析法测定得到的所述负极活性材料的C004/C110≥3。在一些实施中,由X射线衍射分析法测定得到的所述负极活性材料的C004/C110≥3.5。在一些实施中, 由X射线衍射分析法测定得到的所述负极活性材料的C004/C110≥4。在一些实施中,由X射线衍射分析法测定得到的所述负极活性材料的C004/C110≥4.5。在一些实施中,由X射线衍射分析法测定得到的所述负极活性材料的C004/C110在上述任意两个端点值所组成的范围内。
C004/C110值可反映出材料的取向性。C004/C110越小,材料的各向同性越大;C004/C110越大,材料的各向异性越大。当负极活性材料的C004/C110值较大时,锂离子在负极活性材料中的脱嵌方向单一,导致锂离子的脱嵌路径变长,不利于锂离子的快速脱嵌,从而会对电化学装置的循环性能产生不利影响。当负极活性材料的C004/C110值在上述范围内时,在循环过程中,锂离子可在各个方向上嵌入或脱嵌,减小了锂离子的扩散路径以及活性锂离子的损失,由此可进一步改善电化学装置的循环性能。
根据本申请的实施例,所述负极活性材料的克容量C mAh/g与所述碳材料的石墨化度Gr满足以下关系:390Gr-C≤20,C≤350。
在一些实施例中,C与Gr满足以下关系:390Gr-C≤18。在一些实施例中,C与Gr满足以下关系:390Gr-C≤15。在一些实施例中,C与Gr满足以下关系:390Gr-C≤12。在一些实施例中,C与Gr满足以下关系:390Gr-C≤15。在一些实施例中,C与Gr满足以下关系:390Gr-C≤10。在一些实施例中,C与Gr满足以下关系:390Gr-C≤8。在一些实施例中,C与Gr满足以下关系:390Gr-C≤5。在一些实施例中,C与Gr满足以下关系:390Gr-C≥1。在一些实施例中,C与Gr满足以下关系:390Gr-C≥3。在一些实施例中,390Gr-C的值在上述任意两个端点值所组成的范围内。
在一些实施例中,C≤340。在一些实施例中,C≤330。在一些实施例中,C≤320。在一些实施例中,C≤310。在一些实施例中,C≤300。在一些实施例中,C≥250。在一些实施例中,C≥280。在一些实施例中,C≥290。在一些实施例中,所述负极活性材料的克容量的值C在上述任意两个端点值所组成的范围内。
当负极活性材料的克容量的值C与碳材料的石墨化度Gr满足上述关系时,可使负极活性材料具有平衡的性能,从而可进一步改善电化学装置的循环性能。
本申请还提供了一种电化学装置,其包括正极、负极、隔离膜和电解液。以下说明可用于本申请中正极、负极、隔离膜和电解液。
负极
本申请的电化学装置所使用的负极包括负极集流体和负极活性材料层,所述负极活性材料层包含根据本申请所述的负极活性材料。
根据本申请的实施例,所述负极活性材料层的压实密度PD g/cm
3和所述碳材料的石墨化度Gr满足以下关系:PD≤2.5Gr-0.45≤1.85。在一些实施例中,PD和Gr满足以下关系:PD≤2.5Gr-0.45≤1.80。在一些实施例中,PD和Gr满足以下关系:PD≤2.5Gr-0.45≤1.75。在一些实施例中,PD和Gr满足以下关系:PD≤2.5Gr-0.45≤1.70。在一些实施例中,PD和Gr满足以下关系:PD≤2.5Gr-0.45≤1.65。在一些实施例中,PD和Gr满足以下关系:PD≤2.5Gr-0.45≤1.60。
根据本申请的实施例,所述负极活性材料层的压实密度为1.45g/cm
3至1.75g/cm
3。在一些实施例中,所述负极活性材料层的压实密度为1.50g/cm
3至1.70g/cm
3。在一些实施例中,所述负极活性材料层的压实密度为1.55g/cm
3至1.65g/cm
3。在一些实施例中,所述负极活性材料层的压实密度为1.45g/cm
3、1.50g/cm
3、1.55g/cm
3、1.60g/cm
3、1.65g/cm
3、1.70g/cm
3、1.75g/cm
3或在上述任意两个数值所组成的范围内。
当负极活性材料层的压实密度过高时,电解液不易浸润负极活性材料,不利于锂离子快速参与电化学反应,从而对锂离子电池的循环性能产生不利影响。当负极活性材料层的压实密度和碳材料的石墨化度满足上述关系或负极活性材料的压实密度在上述范围内时,可进一步改善电化学装置的循环性能。
根据本申请的实施例,由X射线衍射分析法测定得到的所述负极活性材料层的(004)面的峰面积C004'和(110)面的峰面积C110'的比值C004'/C110'在7至18的范围内。在一些实施例中,由X射线衍射分析法测定得到的所述负极活性材料层的C004'/C110'在10至16的范围内。在一些实施例中,由X射线衍射分析法测定得到的所述负极活性材料层的C004'/C110'在12至15的范围内。在一些实施例中,由X射线衍射分析法测定得到的所述负极活性材料层的C004'/C110'为7、10、12、14、16、18或在上述任意两个数值所组成的范围内。当负极活性材料层的C004'/C110'在上述范围内时,可一进步改善电化学装置的循环性能。
根据本申请的实施例,由拉曼光谱法测定的所述负极活性材料层在1340cm
-1至1380cm
-1的峰强度Id与所述负极活性材料层在1560cm
-1至1600cm
-1的峰强度Ig的比值Id/Ig为0.2至0.5。在一些实施例中,由拉曼光谱法测定的所述负极活性材料层的Id/Ig为0.25至0.45。在一些实施例中,由拉曼光谱法测定的所述负极活性材料层的Id/Ig为0.3至0.4。在一些实施例中,由拉曼光谱法测定的所述负极活性材料层的Id/Ig为0.2、0.25、0.3、0.35、0.4、0.45、0.5或在上述任意两个数值所组成的范围内。负极活性材料层的Id/Ig可表征负极活性材料层的表面缺陷度。当Id/Ig过小时,负极活性材料层的 表面缺陷比较少,石墨片层排布紧密规整;当Id/Ig过大时,负极活性材料层的表面缺陷比较多,会影响固体电解质膜(SEI膜)的稳定性。Id/Ig当负极活性材料层的表面缺陷度Id/Ig在上述范围内时,负极活性材料层具有适量的表面缺陷,可保证锂离子的嵌入/脱出以及SEI膜的稳定性,有助于改善电化学装置的循环性能。
用于本申请所述的负极集流体可以选自铜箔、镍箔、不锈钢箔、钛箔、泡沫镍、泡沫铜、覆有导电金属的聚合物基底和它们的组合。
根据本申请的实施例,所述负极进一步包括导电层。在一些实施方案中,所述导电层的导电材料可以包括任何导电材料,只要它不引起化学变化。导电材料的非限制性示例包括基于碳的材料(例如,天然石墨、人造石墨、碳黑、乙炔黑、科琴黑、碳纤维、碳纳米管、石墨烯等)、基于金属的材料(例如,金属粉、金属纤维等,例如铜、镍、铝、银等)、导电聚合物(例如,聚亚苯基衍生物)和它们的混合物。
根据本申请的实施例,所述负极进一步包括粘结剂,所述粘结剂选自以下的至少一种:聚乙烯醇、羧甲基纤维素、羟丙基纤维素、二乙酰基纤维素、聚氯乙烯、羧化的聚氯乙烯、聚氟乙烯、含亚乙基氧的聚合物、聚乙烯吡咯烷酮、聚氨酯、聚四氟乙烯、聚偏1,1-二氟乙烯、聚乙烯、聚丙烯、丁苯橡胶、丙烯酸(酯)化的丁苯橡胶、环氧树脂或尼龙等。
正极
正极包括正极集流体和设置在所述正极集流体上的正极活性材料。正极活性材料的具体种类均不受到具体的限制,可根据需求进行选择。
在一些实施方案中,正极活性材料包括够吸收和释放锂(Li)的正极材料。能够吸收/释放锂(Li)的正极材料的例子可以包括钴酸锂、镍钴锰酸锂、镍钴铝酸锂、锰酸锂、磷酸锰铁锂、磷酸钒锂、磷酸钒氧锂、磷酸铁锂、钛酸锂和富锂锰基材料。
具体的,钴酸锂的化学式可以如化学式1:
Li
xCo
aM1
bO
2-c 化学式1
其中M1表示选自镍(Ni)、锰(Mn)、镁(Mg)、铝(Al)、硼(B)、钛(Ti)、钒(V)、铬(Cr)、铁(Fe)、铜(Cu)、锌(Zn)、钼(Mo)、锡(Sn)、钙(Ca)、锶(Sr)、钨(W)、钇(Y)、镧(La)、锆(Zr)和硅(Si)中的至少一种,x、a、b和c值分别在以下范围内:0.8≤x≤1.2、0.8≤a≤1、0≤b≤0.2、-0.1≤c≤0.2。
镍钴锰酸锂或镍钴铝酸锂的化学式可以如化学式2:
Li
yNi
dM2
eO
2-f 化学式2
其中M2表示选自钴(Co)、锰(Mn)、镁(Mg)、铝(Al)、硼(B)、钛(Ti)、钒(V)、铬(Cr)、铁(Fe)、铜(Cu)、锌(Zn)、钼(Mo)、锡(Sn)、钙(Ca)、锶(Sr)、钨(W)、锆(Zr)和硅(Si)中的至少一种,y、d、e和f值分别在以下范围内:0.8≤y≤1.2、0.3≤d≤0.98、0.02≤e≤0.7、-0.1≤f≤0.2。
锰酸锂的化学式可以如化学式3:
Li
zMn
2-gM3
gO
4-h 化学式3
其中M3表示选自钴(Co)、镍(Ni)、镁(Mg)、铝(Al)、硼(B)、钛(Ti)、钒(V)、铬(Cr)、铁(Fe)、铜(Cu)、锌(Zn)、钼(Mo)、锡(Sn)、钙(Ca)、锶(Sr)和钨(W)中的至少一种,z、g和h值分别在以下范围内:0.8≤z≤1.2、0≤g<1.0和-0.2≤h≤0.2。
在一些实施例中,所述正极活性材料层的重量是所述负极活性材料层的重量的1.5至15倍。在一些实施例中,所述正极活性材料层的重量是所述负极活性材料层的重量的3至10倍。在一些实施例中,所述正极活性材料层的重量是所述负极活性材料层的重量的5至8倍。在一些实施例中,所述正极活性材料层的重量是所述负极活性材料层的重量的1.5倍、2倍、3倍、4倍、5倍、6倍、7倍、8倍、9倍、10倍、11倍、12倍、13倍、14倍或15倍。
在一些实施例中,正极活性材料层可以在表面上具有涂层,或者可以与具有涂层的另一化合物混合。所述涂层可以包括从涂覆元素的氧化物、涂覆元素的氢氧化物、涂覆元素的羟基氧化物、涂覆元素的碳酸氧盐(oxycarbonate)和涂覆元素的羟基碳酸盐(hydroxycarbonate)中选择的至少一种涂覆元素化合物。用于涂层的化合物可以是非晶的或结晶的。在涂层中含有的涂覆元素可以包括Mg、Al、Co、K、Na、Ca、Si、Ti、V、Sn、Ge、Ga、B、As、Zr、F或它们的混合物。可以通过任何方法来施加涂层,只要所述方法不对正极活性材料的性能产生不利影响即可。例如,所述方法可以包括对本领域普通技术人员来说众所周知的任何涂覆方法,例如喷涂、浸渍等。
在一些实施方案中,正极活性材料层还包含粘合剂,并且可选地还包括正极导电材料。
粘合剂可提高正极活性材料颗粒彼此间的结合,并且还提高正极活性材料与集流体的结合。粘合剂的非限制性示例包括聚乙烯醇、羟丙基纤维素、二乙酰基纤维素、聚氯乙烯、羧化的聚氯乙烯、聚氟乙烯、含亚乙基氧的聚合物、聚乙烯吡咯烷酮、聚氨酯、聚四氟乙烯、聚偏1,1-二氟乙烯、聚乙烯、聚丙烯、丁苯橡胶、丙烯酸(酯)化的丁苯橡 胶、环氧树脂、尼龙等。
正极活性材料层包括正极导电材料,从而赋予电极导电性。所述正极导电材料可以包括任何导电材料,只要它不引起化学变化。正极导电材料的非限制性示例包括基于碳的材料(例如,天然石墨、人造石墨、碳黑、乙炔黑、科琴黑、碳纤维等)、基于金属的材料(例如,金属粉、金属纤维等,包括例如铜、镍、铝、银等)、导电聚合物(例如,聚亚苯基衍生物)和它们的混合物。
用于根据本申请的电化学装置的正极集流体可以是铝(Al),但不限于此。
电解液
可用于本申请实施例的电解液可以为现有技术中已知的电解液。
可用于本申请实施例的电解液中的电解质包括,但不限于:无机锂盐,例如LiClO
4、LiAsF
6、LiPF
6、LiBF
4、LiSbF
6、LiSO
3F、LiN(FSO
2)
2等;含氟有机锂盐,例如LiCF
3SO
3、LiN(FSO
2)(CF
3SO
2)、LiN(CF
3SO
2)
2、LiN(C
2F
5SO
2)
2、环状1,3-六氟丙烷二磺酰亚胺锂、环状1,2-四氟乙烷二磺酰亚胺锂、LiN(CF
3SO
2)(C
4F
9SO
2)、LiC(CF
3SO
2)
3、LiPF
4(CF
3)
2、LiPF
4(C
2F
5)
2、LiPF
4(CF
3SO
2)
2、LiPF
4(C
2F
5SO
2)
2、LiBF
2(CF
3)
2、LiBF2(C2F5)2、LiBF
2(CF
3SO
2)
2、LiBF
2(C
2F
5SO
2)
2;含二羧酸配合物锂盐,例如双(草酸根合)硼酸锂、二氟草酸根合硼酸锂、三(草酸根合)磷酸锂、二氟双(草酸根合)磷酸锂、四氟(草酸根合)磷酸锂等。另外,上述电解质可以单独使用一种,也可以同时使用两种或两种以上。在一些实施例中,电解质包括LiPF
6和LiBF
4的组合。在一些实施例中,电解质包括LiPF
6或LiBF
4等无机锂盐与LiCF
3SO
3、LiN(CF
3SO
2)
2、LiN(C
2F
5SO
2)
2等含氟有机锂盐的组合。在一些实施例中,电解质包括LiPF
6。
在一些实施例中,电解质的浓度在0.8-3mol/L的范围内,例如0.8-2.5mol/L的范围内、0.8-2mol/L的范围内、1-2mol/L的范围内、又例如为1mol/L、1.15mol/L、1.2mol/L、1.5mol/L、2mol/L或2.5mol/L。
可用于本申请实施例的电解液中的溶剂包括,但不限于,环状碳酸酯、链状碳酸酯、环状羧酸酯、链状羧酸酯、环状醚、链状醚、含磷有机溶剂、含硫有机溶剂和芳香族含氟溶剂。
在一些实施例中,环状碳酸酯包括,但不限于,碳酸亚乙酯(ethylene carbonate,EC)、碳酸亚丙酯(propylene carbonate,PC)和碳酸亚丁酯。
在一些实施例中,环状碳酸酯具有3-6个碳原子。
在一些实施例中,链状碳酸酯包括,但不限于:碳酸二甲酯、碳酸甲乙酯、碳酸二 乙酯(diethyl carbonate,DEC)、碳酸甲基正丙基酯、碳酸乙基正丙基酯、碳酸二正丙酯等链状碳酸酯,作为被氟取代的链状碳酸酯,例如双(氟甲基)碳酸酯、双(二氟甲基)碳酸酯、双(三氟甲基)碳酸酯、双(2-氟乙基)碳酸酯、双(2,2-二氟乙基)碳酸酯、双(2,2,2-三氟乙基)碳酸酯、2-氟乙基甲基碳酸酯、2,2-二氟乙基甲基碳酸酯和2,2,2-三氟乙基甲基碳酸酯。
在一些实施例中,环状羧酸酯包括,但不限于,γ-丁内酯和γ-戊内酯。在一些实施例中,环状羧酸酯的部分氢原子可被氟取代。
在一些实施例中,链状羧酸酯包括,但不限于:乙酸甲酯、乙酸乙酯、乙酸丙酯、乙酸异丙酯、乙酸丁酯、乙酸仲丁酯、乙酸异丁酯、乙酸叔丁酯、丙酸甲酯、丙酸乙酯、丙酸丙酯、丙酸异丙酯、丁酸甲酯、丁酸乙酯、丁酸丙酯、异丁酸甲酯、异丁酸乙酯、戊酸甲酯、戊酸乙酯、特戊酸甲酯和特戊酸乙酯。在一些实施例中,链状羧酸酯的部分氢原子可被氟取代。在一些实施例中,氟取代的链状羧酸酯包括,但不限于:三氟乙酸甲酯、三氟乙酸乙酯、三氟乙酸丙酯、三氟乙酸丁酯和三氟乙酸2,2,2-三氟乙酯。
在一些实施例中,环状醚包括,但不限于,四氢呋喃、2-甲基四氢呋喃、1,3-二氧戊环、2-甲基1,3-二氧戊环、4-甲基1,3-二氧戊环、1,3-二氧六环、1,4-二氧六环和二甲氧基丙烷。
在一些实施例中,链状醚包括,但不限于,二甲氧基甲烷、1,1-二甲氧基乙烷、1,2-二甲氧基乙烷、二乙氧基甲烷、1,1-二乙氧基乙烷、1,2-二乙氧基乙烷、乙氧基甲氧基甲烷、1,1-乙氧基甲氧基乙烷和1,2-乙氧基甲氧基乙烷。
在一些实施例中,含磷有机溶剂包括,但不限于,磷酸三甲酯、磷酸三乙酯、磷酸二甲基乙酯、磷酸甲基二乙酯、磷酸亚乙基甲酯、磷酸亚乙基乙酯、磷酸三苯酯、亚磷酸三甲酯、亚磷酸三乙酯、亚磷酸三苯酯、磷酸三(2,2,2-三氟乙基)酯和磷酸三(2,2,3,3,3-五氟丙基)酯。
在一些实施例中,含硫有机溶剂包括,但不限于,环丁砜、2-甲基环丁砜、3-甲基环丁砜、二甲基砜、二乙基砜、乙基甲基砜、甲基丙基砜、二甲基亚砜、甲磺酸甲酯、甲磺酸乙酯、乙磺酸甲酯、乙磺酸乙酯、硫酸二甲酯、硫酸二乙酯和硫酸二丁酯。在一些实施例中,含硫有机溶剂的部分氢原子可被氟取代。
在一些实施例中,芳香族含氟溶剂包括,但不限于,氟苯、二氟苯、三氟苯、四氟苯、五氟苯、六氟苯和三氟甲基苯。
在一些实施例中,本申请的电解液中使用的溶剂包括如上所述的一种或多种。在一 些实施例中,本申请的电解液中使用的溶剂包括环状碳酸酯、链状碳酸酯、环状羧酸酯、链状羧酸酯及其组合。在一些实施例中,本申请的电解液中使用的溶剂包含选自由下列物质组成的群组的有机溶剂:碳酸亚乙酯、碳酸亚丙酯、碳酸二乙酯、丙酸乙酯、丙酸丙酯、乙酸正丙酯、乙酸乙酯及其组合。在一些实施例中,本申请的电解液中使用的溶剂包含:碳酸亚乙酯、碳酸亚丙酯、碳酸二乙酯、丙酸乙酯、丙酸丙酯、γ-丁内酯或其组合。
可用于本申请实施例的电解液中的添加剂包括,但不限于,具有2-3个氰基的化合物、含碳碳双键的环状碳酸酯、含硫氧双键的化合物、二氟磷酸锂。
在一些实施例中,具有2-3个氰基的化合物可以包括选自丁二腈(SN)、己二腈(ADN)、乙二醇双(丙腈)醚(EDN)、1,3,5-戊三甲腈、1,2,3-丙三甲腈、1,3,6-己三甲腈(HTCN)、1,2,6-己三甲腈、1,2,3-三(2-氰基乙氧基)丙烷(TCEP)或1,2,4-三(2-氰基乙氧基)丁烷中的至少一种。
在一些实施例中,具有碳-碳双键的环状碳酸酯具体包括,但不限于:碳酸亚乙烯酯、碳酸甲基亚乙烯酯、碳酸乙基亚乙烯酯、乙烯基碳酸乙烯亚乙酯或碳酸-1,2-二甲基亚乙烯酯中的至少一种。
在一些实施例中,含硫氧双键的化合物包括,但不限于:硫酸乙烯酯、1,2-丙二醇硫酸酯、1,3-丙磺酸内酯、1-氟-1,3-丙磺酸内酯、2-氟-1,3-丙磺酸内酯或3-氟-1,3-丙磺酸内酯中的至少一种。
隔离膜
在一些实施方案中,正极与负极之间设有隔离膜以防止短路。可用于本申请的实施例中使用的隔离膜的材料和形状没有特别限制,其可为任何现有技术中公开的技术。在一些实施方案中,隔离膜包括由对本申请的电解液稳定的材料形成的聚合物或无机物等。
例如,隔离膜可包括基材层和表面处理层。基材层为具有多孔结构的无纺布、膜或复合膜,基材层的材料选自聚乙烯、聚丙烯、聚对苯二甲酸乙二醇酯和聚酰亚胺中的至少一种。具体的,可选用聚丙烯多孔膜、聚乙烯多孔膜、聚丙烯无纺布、聚乙烯无纺布或聚丙烯-聚乙烯-聚丙烯多孔复合膜。多孔结构可以提升隔离膜的耐热性能、抗氧化性能和电解质浸润性能,增强隔离膜与极片之间的粘接性。
基材层的至少一个表面上设置有表面处理层,表面处理层可以是聚合物层或无机物层,也可以是混合聚合物与无机物所形成的层。
无机物层包括无机颗粒和粘结剂,无机颗粒选自氧化铝、氧化硅、氧化镁、氧化钛、二氧化铪、氧化锡、二氧化铈、氧化镍、氧化锌、氧化钙、氧化锆、氧化钇、碳化硅、勃姆石、氢氧化铝、氢氧化镁、氢氧化钙和硫酸钡中的一种或几种的组合。粘结剂选自聚偏氟乙烯、偏氟乙烯-六氟丙烯的共聚物、聚酰胺、聚丙烯腈、聚丙烯酸酯、聚丙烯酸、聚丙烯酸盐、聚乙烯呲咯烷酮、聚乙烯醚、聚甲基丙烯酸甲酯、聚四氟乙烯和聚六氟丙烯中的一种或几种的组合。
聚合物层中包含聚合物,聚合物的材料选自聚酰胺、聚丙烯腈、丙烯酸酯聚合物、聚丙烯酸、聚丙烯酸盐、聚乙烯呲咯烷酮、聚乙烯醚、聚偏氟乙烯、聚(偏氟乙烯-六氟丙烯)中的至少一种。
电化学装置
本申请还提供了一种电化学装置,其包括正极、电解液和负极,所述正极包括正极活性材料层和正极集流体,所述负极包括负极活性材料层和负极集流体,所述负极活性材料层包括根据本申请所述的负极活性材料。
本申请的电化学装置包括发生电化学反应的任何装置,它的具体实例包括所有种类的一次电池、二次电池、燃料电池、太阳能电池或电容器。特别地,该电化学装置是锂二次电池,包括锂金属二次电池、锂离子二次电池、锂聚合物二次电池或锂离子聚合物二次电池。
电子装置
本申请另提供了一种电子装置,其包括根据本申请的电化学装置。
本申请的电化学装置的用途没有特别限定,其可用于现有技术中已知的任何电子装置。在一些实施方案中,本申请的电化学装置可用于,但不限于,笔记本电脑、笔输入型计算机、移动电脑、电子书播放器、便携式电话、便携式传真机、便携式复印机、便携式打印机、头戴式立体声耳机、录像机、液晶电视、手提式清洁器、便携CD机、迷你光盘、收发机、电子记事本、计算器、存储卡、便携式录音机、收音机、备用电源、电机、汽车、摩托车、助力自行车、自行车、照明器具、玩具、游戏机、钟表、电动工具、闪光灯、照相机、家庭用大型蓄电池和锂离子电容器等。
下面以锂离子电池为例并且结合具体的实施例说明锂离子电池的制备,本领域的技术人员将理解,本申请中描述的制备方法仅是实例,其他任何合适的制备方法均在本申请的范围内。
实施例
以下说明根据本申请的锂离子电池的实施例和对比例进行性能评估。
一、锂离子电池的制备
1、负极的制备
将石墨、丁苯橡胶(SBR)和羧甲基纤维素钠(CMC)按照重量比97.2:1.8:1在适量的去离子水中充分搅拌混合,使其形成均匀的负极浆料。将负极浆料涂覆重量涂覆于负极集流体(铜箔)上,烘干、冷压、裁片、分切后,得到负极。石墨的石墨化度通过控制石墨化温度与保温时间得到,升温时间在12-17小时的范围,升温到2600℃-3000℃的范围,然后保温,保温时间在85h-100h的范围,自然降温。长径比通过整形与筛分工序控制。
2、正极的制备
将磷酸铁锂(LiFePO
4)、导电剂乙炔黑和粘结剂聚偏二氟乙烯(PVDF)按重量比96.3:2.2:1.5在适量的N-甲基吡咯烷酮(NMP)溶剂中充分搅拌混合,使其形成均匀的正极浆料。将此浆料涂覆于正极集流体铝箔上,烘干、冷压、裁片、分切后,得到正极。
3、电解液的制备
在干燥的氩气气氛手套箱中,将碳酸乙烯酯(简写为EC)、碳酸二乙酯(简写为DEC)和碳酸丙烯酯(简写为PC)按照2:6:2的质量比混合均匀,接着加入3%的氟代碳酸乙烯酯,3%的丁二腈,溶解并充分搅拌后加入锂盐LiPF
6,混合均匀后获得电解液,其中LiPF
6的浓度为1mol/L。
4、隔离膜的制备
以聚乙烯(PE)多孔聚合物薄膜作为隔离膜。
5、锂离子电池的制备
将正极、隔离膜、负极按顺序叠好,使隔离膜处于正极和负极之间起到隔离的作用,然后卷绕得到裸电芯;焊接极耳后将裸电芯置于外包装箔铝塑膜中,将上述制备好的电解液注入到干燥后的裸电芯中,经过真空封装、静置、化成、整形、容量测试等工序,获得锂离子电池。
二、测试方法
1、负极活性材料的长径比分布的测试方法
使用新帕泰克QICPIC动态颗粒图像分析仪测试负极活性材料的长径比分布。
2、负极活性材料的石墨化度的测试方法
按照JJS K 0131-1996《X射线衍射分析法通则》来测试晶面间距d
002,仪器为布鲁 克Bruker-X射线单晶衍射仪(XRD)。通过衍射峰确定衍射角θ,通过布拉格方程2dsinθ=λ计算出晶面间距d
002,然后用石墨化度计算公式G=(0.3440–d
002)/(0.3440–0.3354)×100%得到石墨化度,式中G为石墨化度%,d
002为炭材料(002)晶面的层间距nm。
3、负极活性材料层的C004/C110的测试方法
按照中华人民共和国机械行业标准JB/T 4220-2011《人造石墨的点阵参数测定方法》测试负极活性材料层的X射线衍射图谱中的(004)面衍射线图形和(110)面衍射线图形。在记录004衍射线图形时,衍射角2θ的扫描范围为53°-57°。在记录110衍射线图形时,衍射角2θ的扫描范围为75°-79°。由(004)面衍射线图形得到的峰面积记为C004。由(110)面衍射线图形得到的峰面积记为C110。计算负极活性材料层的C004/C110的比值。
4、负极活性材料层的Id/Ig的测试方法
采用拉曼光谱法测定的负极活性材料层在1340cm
-1至1380cm
-1的峰强度Id和在1560cm
-1至1600cm
-1的峰强度Ig。Id/Ig为D峰强度Id与G峰强度Ig的计算比值。
5、负极活性材料层的压实密度的测试方法
按照中华人民共和国国家标准GB/T 24533-2009《锂离子电池石墨类负极材料》测试活性材料层的压实密度。得到的活性材料层的压实密度为5T泄压后的密度。
6、负极活性材料的粒径的测试方法
按照中华人民共和国国家标准GB/T 19077-2016粒度分析-激光衍射法测试活性材料的粒度,测试仪器为马尔文粒度测试仪Malvern Master Size 3000,将负极材料分散在分散剂中(乙醇),超声30min后,将样品加入到马尔文粒度测试仪内,开始测试。所述负极材料在体积基准的粒度分布中,从小粒径侧起、达到体积累积10%的粒径即为所述负极材料的Dv10;同时所述负极材料在体积基准的粒度分布中,从小粒径侧起、达到体积累积99%的粒径即为所述负极材料的Dv99。
7、负极活性材料的晶面间距的测试方法
按照JJS K 0131-1996《X射线衍射分析法通则》来测试晶面间距d
002,仪器为布鲁克Bruker-X射线单晶衍射仪(XRD)。通过衍射峰确定衍射角θ,通过布拉格方程2dsinθ=λ计算出晶面间距d
002。
8、锂离子电池的克容量的测试方法
以蓝电测试仪来测试活性材料的克容量,首先组装扣式电池,扣式电池型号:CR2430。将满放的锂离子电池拆解得到负极,选择负极集流体双面均有负极活性材料层区域(也可以选择双面活性材料层区,清洗掉其中一个面的活性材料层),取直径为 14mm的圆片,称重,记为m
0g,清洗掉其中一个面的活性材料层,称重,记为m
1g,单面活性材料层重量m
2(g)=m
0-m
1。加入上述制备的电解液,以锂金属片做对应电极,组装成扣式电池。测试温度为23-26℃,测试流程为0.05C放电至5mV,之后再以0.05mA放电至5mV,0.02mA放电至5mV,0.1C充电至2.0V,记录放电容量。负极活性材料的重量可以按照此公式计算:m(g)=m
2×0.972。负极活性材料的克容量的值C(mAh/g)=放电容量/负极活性材料重量。
9、锂离子电池的循环容量保持率的测试方法
在25℃下,将锂离子电池以1C直流充电至3.6V,然后以3.6V恒压充电至0.05C,静置10分钟,随后以1C直流放电至2.5V。此为一个循环,记录首次循环的放电容量。重复上述步骤1000次,记录循环后放电容量。通过下式计算锂离子电池的循环容量保持率:
循环容量保持率=(循环后放电容量/首次循环的放电容量)×100%。
10、锂离子电池的厚度反弹率的测试方法
在45℃下,将锂离子电池以1C直流充电至3.6V,然后以3.6V恒压充电至0.05C,静置10分钟,随后以1C直流放电至2.5V。此为一个循环,记录锂离子电池在该循环阶段内3.6V恒压充电至0.05C,静置10分钟后的厚度H0。重复上述步骤1000次,记录锂离子电池在第1000次循环阶段内3.6V恒压充电至0.05C,静置10分钟后的厚度H1。通过下式计算锂离子电池的厚度反弹率:
厚度反弹率=(H1-H0)/H0×100%。
三、测试结果
表1展示了负极活性材料中的碳材料的石墨化度和长径比占比对锂离子电池的循环性能的影响。
表1
如对比例1所示,当碳材料中长径比≥3.3的颗粒小于总颗粒数量的10%但碳材料的石墨化度小于0.82时,锂离子电池的循环容量保持率较低,厚度反弹率较高。
如对比例2和3所示,当碳材料中长径比≥3.3的颗粒小于总颗粒数量的10%但碳材料的石墨化度大于0.92时,锂离子电池的循环容量保持率较低,厚度反弹率较高。
如对比例4-7所示,当碳材料的石墨化度在0.82至0.92的范围内但碳材料中长径比≥3.3的颗粒大于总颗粒数量的10%时,锂离子电池的循环容量保持率较低,厚度反弹率较高。
如对比例8所示,当碳材料的石墨化度小于0.82且碳材料中长径比≥3.3的颗粒大于总颗粒数量的10%时,锂离子电池的循环容量保持率较低,厚度反弹率较高。
如对比例9-12所示,当碳材料的石墨化度大于0.92且碳材料中长径比≥3.3的颗粒大于总颗粒数量的10%时,锂离子电池的循环容量保持率较低,厚度反弹率较高。
如实施例1-6所示,当碳材料的石墨化度在0.82至0.92的范围内且碳材料中长径比≥3.3的颗粒小于总颗粒数量的10%时,锂离子电池的循环容量保持率显著升高,厚度反弹率显著降低,即,锂离子电池具有显著改善的循环性能。
表2展示了负极活性材料中的碳材料的长径比占比对锂离子电池的循环性能的影响。实施例7-12是基于实施例3的改进,其区别仅在于表2中所列参数。
表2
结果表明,当碳材料中长径≥2的颗粒的占比为50%以下且长径比≥1.5的颗粒的占比为80%以下时,可进一步提升锂离子电池的循环容量保持率并进一步降低其厚度反弹率。
表3展示了碳材料的晶粒尺寸和石墨化度以及负极活性材料层的压实密度对锂离子电池的循环性能的影响。实施例13-22是基于实施例8的改进,其区别仅在于表3中所列参数。
表3
K×Gr | 2.5Gr-0.45 | PD(g/cm 3) | 循环保持率 | 厚度反弹率 | |
实施例8 | 3.8 | 1.725 | 1.80 | 93.6% | 2.98% |
实施例13 | 4.0 | 1.725 | 1.58 | 94.2% | 2.89% |
实施例14 | 4.83 | 1.725 | 1.63 | 94.2% | 2.88% |
实施例15 | 5.18 | 1.725 | 1.66 | 94.1% | 2.85% |
实施例16 | 5.2 | 1.725 | 1.66 | 94.2% | 2.85% |
实施例17 | 4.75 | 1.725 | 1.74 | 94.3% | 2.85% |
实施例18 | 4.6 | 1.725 | 1.77 | 94.2% | 2.85% |
实施例19 | 3.79 | 1.725 | 1.52 | 93.6% | 2.90% |
实施例20 | 3.85 | 1.725 | 1.61 | 93.7% | 2.88% |
实施例21 | 5.25 | 1.725 | 1.65 | 93.8% | 2.91% |
实施例22 | 5.4 | 1.725 | 1.65 | 93.8% | 2.92% |
结果表明,当碳材料的晶粒尺寸La与Lc的比值为K和石墨化度Gr满足4.0≤K×Gr≤5.2时和/或当负极活性材料层的压实密度的值PD和碳材料的石墨化度Gr满足PD≤2.5Gr-0.45≤1.85且PD为1.45至1.75时,可以进一步改善锂离子电池的循环容量保持率和厚度反弹率。
表4展示了负极活性材料的颗粒尺寸、晶面间距和取向性对锂离子电池的性能的影响。实施例23-29是基于实施例16的改进,其区别仅在于表4中所列参数。
表4
当负极活性材料的颗粒尺寸满足35μm<Dv99-Dv10<50μm、晶面间距d002≥0.3365nm和/或C004/C110≤8时,可进一步改善锂离子电池的循环容量保持率和厚度反弹率。
表5展示了负极活性材料的克容量对锂离子电池的循环性能的影响。实施例30-36是基于实施例24的改进,其区别仅在于表5中所列参数。
表5
结果表明,当负极活性材料的克容量的值C与石墨化度Gr满足390Gr-C≤20且C≤350时,可进一步改善锂离子电池的循环容量保持率和厚度反弹率。
此外,实施例33的锂离子电池中的负极活性材料层的C004'/C110'为8.63,Id/Ig为0.25;负极活性材料的C004/C110为5.78。采用“锂离子电池的循环容量保持率的测试方法”中的循环步骤使实施例36的锂离子电池循环3000次。然后将满充后的锂离子电池拆解,取出负极,清洗,烘干。提取负极活性材料层和负极活性材料。经测试,循环 后的负极活性材料层的C004'/C110'为8.51,Id/Ig为0.37;循环后的负极活性材料的C004/C110为5.76。循环后的负极活性材料层的C004'/C110'仍在7至18的范围内,Id/Ig仍在0.2至0.5范围内。即,本申请的锂离子电池的负极活性材料层的取向性在循环后未发生明显变化,活性材料结构稳定性好。
图6展示了对比例2和根据本申请实施例1随循环次数的循环容量保持率曲线图。结果表明,实施例1的锂离子电池具有显著高于对比例2的锂离子电池的循环容量保持率。
图7展示了对比例2和根据本申请实施例1随循环次数的厚度反弹率的曲线图。结果表明,实施例1的锂离子电池具有显著低于对比例2的锂离子电池的厚度反弹率。
整个说明书中对“实施例”、“部分实施例”、“一个实施例”、“另一举例”、“举例”、“具体举例”或“部分举例”的引用,其所代表的意思是在本申请中的至少一个实施例或举例包含了该实施例或举例中所描述的特定特征、结构、材料或特性。因此,在整个说明书中的各处所出现的描述,例如:“在一些实施方案中”、“在实施例中”、“在一个实施例中”、“在另一个举例中”,“在一个举例中”、“在特定举例中”或“举例”,其不必然是引用本申请中的相同的实施例或示例。此外,本文中的特定特征、结构、材料或特性可以以任何合适的方式在一个或多个实施例或举例中结合。
尽管已经演示和描述了说明性实施例,本领域技术人员应该理解上述实施例不能被解释为对本申请的限制,并且可以在不脱离本申请的精神、原理及范围的情况下对实施例进行改变,替代和修改。
Claims (12)
- 一种负极活性材料,所述负极活性材料包含碳材料,其中由X射线衍射分析法测定得到的所述碳材料的石墨化度Gr为0.82至0.92,且基于所述碳材料的总颗粒数量,所述碳材料中长径比为3.3以上的颗粒的占比为10%以下。
- 根据权利要求1所述的负极活性材料,其中基于所述碳材料的总颗粒数量,所述碳材料中长径比为2以上的颗粒的占比为50%以下,所述碳材料中长径比为1.5以上的颗粒的占比为80%以下。
- 根据权利要求1所述的负极活性材料,其中由X射线衍射分析法测定的所述碳材料的晶粒沿水平轴的晶粒尺寸La与由X射线衍射分析法测定的所述碳材料的晶粒沿垂直轴的晶粒尺寸Lc的比值为K,Gr与K满足以下关系:4.0≤K×Gr≤5.2。
- 根据权利要求1所述的负极活性材料,其中所述负极活性材料的颗粒尺寸满足以下关系:35μm<Dv99-Dv10<50μm。
- 根据权利要求1所述的负极活性材料,其中由X射线衍射分析法测定的所述负极活性材料的晶面间距d002≥0.3365nm。
- 根据权利要求1所述的负极活性材料,其中由X射线衍射分析法测定得到的所述负极活性材料的(004)晶面的峰面积C004和(110)晶面的峰面积C110的比值C004/C110≤8。
- 根据权利要求1所述的负极活性材料,其中所述负极活性材料的克容量CmAh/g与所述碳材料的石墨化度Gr满足以下关系:390Gr-C≤20,且C≤350。
- 一种电化学装置,其包括正极、电解液和负极,其中所述负极包括负极活性材料层和负极集流体,所述负极活性材料层包含根据权利要求1-7中任一权利 要求所述的负极活性材料。
- 根据权利要求8所述的电化学装置,其中所述负极活性材料层的压实密度PD g/cm 3和所述碳材料的石墨化度Gr满足以下关系:PD≤2.5Gr-0.45≤1.85,PD为1.45至1.75。
- 根据权利要求8所述的电化学装置,其中由X射线衍射分析法测定得到的所述负极活性材料层的(004)面的峰面积C004'和(110)面的峰面积C110'的比值C004'/C110'为7至18。
- 根据权利要求8所述的电化学装置,其中由拉曼光谱法测定的所述负极活性材料层在1340cm -1至1380cm -1的峰强度Id与所述负极活性材料层在1560cm -1至1600cm -1的峰强度Ig的比值Id/Ig为0.2至0.5。
- 一种电子装置,其包括根据权利要求8-11中任一权利要求所述的电化学装置。
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