CN119265528A - Methods for enhancing the electrochemical properties of battery electrodes - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 37
- 230000002708 enhancing effect Effects 0.000 title abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 71
- 238000004544 sputter deposition Methods 0.000 claims abstract description 66
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 50
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 50
- 239000010703 silicon Substances 0.000 claims abstract description 50
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 20
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 15
- 230000007704 transition Effects 0.000 claims abstract description 12
- 229910002804 graphite Inorganic materials 0.000 claims description 62
- 239000010439 graphite Substances 0.000 claims description 62
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 40
- 239000010949 copper Substances 0.000 claims description 29
- 238000000137 annealing Methods 0.000 claims description 28
- 229910052786 argon Inorganic materials 0.000 claims description 20
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 18
- 229910052802 copper Inorganic materials 0.000 claims description 18
- 238000000151 deposition Methods 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 3
- 239000010410 layer Substances 0.000 abstract description 52
- 230000008569 process Effects 0.000 abstract description 7
- 125000004122 cyclic group Chemical group 0.000 abstract description 6
- 230000007547 defect Effects 0.000 abstract description 5
- 238000005336 cracking Methods 0.000 abstract description 2
- 239000011229 interlayer Substances 0.000 abstract description 2
- 239000007769 metal material Substances 0.000 abstract description 2
- 238000007747 plating Methods 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 12
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 9
- 229910001416 lithium ion Inorganic materials 0.000 description 9
- 238000001035 drying Methods 0.000 description 8
- 238000005406 washing Methods 0.000 description 8
- 239000007773 negative electrode material Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000007774 positive electrode material Substances 0.000 description 5
- 230000007613 environmental effect Effects 0.000 description 4
- 239000010405 anode material Substances 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000002210 silicon-based material Substances 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910013870 LiPF 6 Inorganic materials 0.000 description 1
- 229910018487 Ni—Cr Inorganic materials 0.000 description 1
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical class [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- VNNRSPGTAMTISX-UHFFFAOYSA-N chromium nickel Chemical compound [Cr].[Ni] VNNRSPGTAMTISX-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
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- 238000005265 energy consumption Methods 0.000 description 1
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- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000012982 microporous membrane Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011870 silicon-carbon composite anode material Substances 0.000 description 1
- 239000002153 silicon-carbon composite material Substances 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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- Physical Vapour Deposition (AREA)
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Abstract
The invention relates to the field of metal material plating, in particular to a method for electrochemically enhancing a battery electrode. According to the method, the electrode structure is prepared by adopting a magnetron sputtering process, the alternating structure of graphene and silicon is obtained, the graphene has a large surface area, the bonding property with a current collector and a silicon layer is better, the conductivity and the cyclic stability of the electrode can be improved, and the graphene molecular structure is a three-dimensional hollow structure and has a large elastic modulus, so that the cyclic stress deformation generated by the silicon layer in the cyclic charge and discharge process can be absorbed, the sputtering power is gradually changed when the multilayer structure is prepared, and the tendency of interlayer cracking can be avoided while the deformation is further relieved by adopting a transition gradient mode. When the Si layer is prepared, cu is doped, cu atoms cause lattice distortion in the Si silicon layer, enough defects such as dislocation and vacancy are generated, a buffer space is provided for subsequent deformation, and the conductivity of the electrode is further improved.
Description
Technical Field
The invention relates to the field of metal material plating, in particular to a method for enhancing electrochemical property of a battery electrode.
Background
New energy is paid attention to because of its clean, renewable and environmental protection properties, but there are problems of power stability and cost effectiveness, etc., which limits the large-scale application of new energy. The secondary battery is the best choice capable of realizing continuous and stable power supply energy storage equipment at present, is the energy storage equipment with the highest application range at present, can effectively store energy and convert energy, can meet the increasing energy demands of people, and plays an important role in production and life and other aspects. There are various types of secondary batteries, and lithium ion batteries, secondary batteries, nickel-chromium batteries, and the like are common secondary batteries. Among these secondary batteries, lithium ion batteries have been distinguished from the advantages of environmental friendliness and excellent electrochemical performance, and the good energy density and long cycle life enable the lithium ion batteries to cope with various application scenarios, thereby achieving wide applications.
The key materials of the internal structure of the lithium ion battery consist of a positive electrode material, a negative electrode material, an electrolyte material and a diaphragm material. The positive electrode material mainly aims at providing active lithium ions (Li +), the negative electrode material mainly aims at storing and releasing energy, the electrolyte mainly aims at conducting lithium ions (Li +) between the positive electrode and the negative electrode, and the diaphragm mainly aims at preventing the positive electrode material and the negative electrode material from contacting to cause the battery to short out the lithium ion battery, wherein Li + is taken out of the positive electrode material when the battery is charged, and is inserted into the negative electrode material after passing through the electrolyte medium. At the same time, electrons are transferred from the positive electrode to the negative electrode through an external circuit, converting electrical energy into storable chemical energy. When the battery discharges, lithium ions spontaneously escape from the negative electrode material and return to be embedded into the positive electrode material due to the potential difference between the positive electrode and the negative electrode. Meanwhile, the negative electrons migrate back to the positive electrode through an external circuit, converting the stored chemical energy into electrical energy.
The lithium ion battery anode material has the following conditions of low electrochemical reaction potential, strong lithium storage capacity, small change of a voltage platform, higher ionic electronic conductivity, stable solid electrolyte interface film, low cost, simple preparation process, environmental friendliness and the like. Commonly used anode materials can be classified into carbon-based and non-carbon-based materials. Silicon-based materials have a theoretical specific capacity 4200 mAh g -1 far higher than that of graphite, and have obvious advantages of environmental friendliness, high earth element abundance, easiness in processing and the like, and are considered as one of the most promising negative electrode material candidates, and have attracted extensive attention. However, since the silicon material is easily expanded in volume, the expansion deformation rate is even more than 300%, so that the silicon negative electrode is severely cracked due to expansion and contraction stress generated in the charge and discharge process, and the battery is accelerated to fail. The commercialization of silicon anodes is multiple hampered. The best way to alleviate the above problems is to prepare silicon-carbon composites using high specific capacity silicon materials and high stability carbon materials.
The silicon-carbon composite anode material has a plurality of preparation methods, such as a chemical vapor deposition method, a mechanical ball milling method, a spray method, a magnesia-thermal reduction method, a sol-gel method, a pyrolysis method and the like. The spray method has the defects of high energy consumption and high instrument requirement, the magnesian reduction method has the defects of lower discharge specific capacity, the sol-gel method has the defects of high cost, poor dispersion performance and serious agglomeration phenomenon, the mechanical ball milling method has the advantages that the service life of the anode material is first, and raw materials adopted by chemical vapor deposition are toxic and flammable.
On the basis, the application adopts the magnetron sputtering technology to alternately prepare the silicon-graphene gradient electrode and dope Cu, thereby improving the electrochemical performance of the electrode on the basis of overcoming the disadvantages of the preparation method in the prior art.
Disclosure of Invention
A method for enhancing electrochemical property of battery electrode adopts magnetron sputtering to prepare silicon-graphene gradient composite electrode and is doped with metal Cu.
The current collector is firstly cleaned and dried, and then the current collector is put into a vacuum magnetron sputtering cavity. The background vacuum degree of the sputtering cavity is better than 2.0X10 -4 Pa, the working gas is high-purity argon with the purity of 99.999 percent, and the flow rate of the argon is 8-12sccm. The current collector is PET, PP, PI or PC.
And then preparing the Si-graphene gradient alternating structure. The targets used are a silicon target with purity of 99.999%, a graphite target with purity of 99.99% and a Cu target with purity of 99.999%, wherein the sputtering power of the silicon target is 80-100W, the sputtering power of the graphite target is 80-100W, and the sputtering power of the copper target is 20-30W. Starting a graphite target at the initial stage of sputtering, sputtering a graphite layer with the thickness of 15-25nm, gradually reducing the power of the graphite target to 0W, gradually increasing the sputtering power of a silicon target and a copper target to a preset value, sputtering a Si layer with the thickness of 15-25nm, alternately depositing a graphite layer and a silicon layer multilayer structure according to the mode, and realizing gradient transition.
And finally, annealing the electrode with the alternating multilayer structure to convert graphite into graphene, further reducing internal stress generated in the sputtering process, further improving diffusion transition between the graphene and the Si layer, and carrying out annealing for 20-30 minutes at the background vacuum degree of 3.0X10 -4 pa and 300-400 ℃ while maintaining vacuum and naturally cooling to room temperature after annealing to finally obtain the battery electrode with enhanced electrochemistry.
According to the invention, an electrode structure is prepared by a magnetron sputtering process, so that an alternating structure of graphene and silicon is obtained, the graphene has a large surface area, better combination property with a current collector and a silicon layer, the conductivity and the cyclic stability of the electrode can be improved, and the graphene molecular structure is a three-dimensional hollow structure and has a large elastic modulus, so that cyclic stress deformation generated by the silicon layer in the cyclic charge and discharge process can be absorbed, the sputtering power is gradually changed when a multilayer structure is prepared, and the tendency of interlayer cracking can be avoided while the deformation is further relieved by adopting a transitional gradient mode. When the Si layer is prepared, cu is doped, cu atoms cause lattice distortion in the Si silicon layer, enough defects such as dislocation and vacancy are generated, a buffer space is provided for subsequent deformation, and the conductivity of the electrode is further improved.
Detailed Description
Example 1:
A method for enhancing electrochemical performance of battery electrode includes washing and drying current collector, and putting current collector into vacuum magnetron sputtering cavity. The background vacuum degree of the sputtering cavity is better than 2.0X10 -4 Pa, the working gas is high-purity argon with the purity of 99.999 percent, and the flow rate of the argon is 10sccm. And then preparing the Si-graphene gradient alternating structure. The targets used were a silicon target with a purity of 99.999%, a graphite target with a purity of 99.99% and a Cu target with a purity of 99.999%, the silicon target sputtering power was 100W, the graphite target sputtering power was 100W, and the copper target sputtering power was 30W. Starting a graphite target at the initial stage of sputtering, sputtering a graphite layer with the thickness of 25nm, gradually reducing the power of the graphite target to 0W, gradually increasing the sputtering power of a silicon target and a copper target to 100W and 30W, sputtering a Si layer with the thickness of 25nm, alternately depositing a multi-layer structure of the graphite layer and the silicon layer according to the mode, and realizing gradient transition. And finally, annealing the electrode with the alternating multilayer structure, wherein the background vacuum degree is 3.0 multiplied by 10 -4 Pa, and the annealing is carried out for 25 minutes at 350 ℃, and the vacuum is kept to be naturally cooled to the room temperature after the annealing, so that the electrochemical enhanced battery electrode is finally obtained.
The battery cathode is obtained through the process, a lithium sheet is adopted as the anode, a three-component mixed solvent EC:DMC:EMC=1:1:1 of 1mol/L LiPF 6 is used as the anode, a v/v solution is used as an electrolyte, a polypropylene microporous membrane is used as a diaphragm, and the CR2016 simulated battery is assembled for subsequent testing. The constant current charge and discharge test of button cell was carried out by using the company test system of Xinwei, the cycle performance test comprises the steps of activating one circle with 0.05C current, then circulating 400 circles of charge and discharge under 0.5C current, measuring the electrode size change condition and the discharge specific capacity, and the test results are shown in Table 1.
Example 2:
A method for enhancing electrochemical performance of battery electrode includes washing and drying current collector, and putting current collector into vacuum magnetron sputtering cavity. The background vacuum degree of the sputtering cavity is better than 2.0X10 -4 Pa, the working gas is high-purity argon with the purity of 99.999 percent, and the flow rate of the argon is 10sccm. And then preparing the Si-graphene gradient alternating structure. The targets used were a silicon target with a purity of 99.999%, a graphite target with a purity of 99.99% and a Cu target with a purity of 99.999%, the silicon target sputter power was 80W, the graphite target sputter power was 80W, and the copper target sputter power was 20W. Starting a graphite target at the initial stage of sputtering, sputtering a graphite layer with the thickness of 20nm, gradually reducing the power of the graphite target to 0W, gradually increasing the sputtering power of a silicon target and a copper target to 80W and 20W, sputtering a Si layer with the thickness of 20nm, alternately depositing a multi-layer structure of the graphite layer and the silicon layer according to the mode, and realizing gradient transition. And finally, annealing the electrode with the alternating multilayer structure, wherein the background vacuum degree is 3.0 multiplied by 10 -4 Pa, and the annealing is carried out for 25 minutes at 350 ℃, and the vacuum is kept to be naturally cooled to the room temperature after the annealing, so that the electrochemical enhanced battery electrode is finally obtained. Battery assembly and test mode reference is made to example 1.
Example 3:
A method for enhancing electrochemical performance of battery electrode includes washing and drying current collector, and putting current collector into vacuum magnetron sputtering cavity. The background vacuum degree of the sputtering cavity is better than 2.0X10 -4 Pa, the working gas is high-purity argon with the purity of 99.999 percent, and the flow rate of the argon is 10sccm. And then preparing the Si-graphene gradient alternating structure. The targets used were a silicon target with a purity of 99.999%, a graphite target with a purity of 99.99% and a Cu target with a purity of 99.999%, the silicon target sputtering power was 90W, the graphite target sputtering power was 90W, and the copper target sputtering power was 25W. Starting a graphite target at the initial stage of sputtering, sputtering a graphite layer with the thickness of 20nm, gradually reducing the power of the graphite target to 0W, gradually increasing the sputtering power of a silicon target and a copper target to 90W and 25W, sputtering a Si layer with the thickness of 20nm, alternately depositing a multi-layer structure of the graphite layer and the silicon layer according to the mode, and realizing gradient transition. And finally, annealing the electrode with the alternating multilayer structure, wherein the background vacuum degree is 3.0 multiplied by 10 -4 Pa, and the annealing is carried out for 25 minutes at 350 ℃, and the vacuum is kept to be naturally cooled to the room temperature after the annealing, so that the electrochemical enhanced battery electrode is finally obtained. Battery assembly and test mode reference is made to example 1.
Comparative example 1:
A method for enhancing electrochemical performance of battery electrode includes washing and drying current collector, and putting current collector into vacuum magnetron sputtering cavity. The background vacuum degree of the sputtering cavity is better than 2.0X10 -4 Pa, the working gas is high-purity argon with the purity of 99.999 percent, and the flow rate of the argon is 10sccm. And then preparing the Si-graphene gradient alternating structure. The targets used were a silicon target with a purity of 99.999% and a graphite target with a purity of 99.99%, the silicon target sputter power was 80W, and the graphite target sputter power was 80W. Starting a graphite target at the initial stage of sputtering, sputtering a graphite layer with the thickness of 20nm, gradually reducing the power of the graphite target to 0W, gradually increasing the sputtering power of a silicon target to 80W, sputtering a Si layer with the thickness of 20nm, alternately depositing a graphite layer and a silicon layer multilayer structure according to the mode, and realizing gradient transition. And finally, annealing the electrode with the alternating multilayer structure, wherein the background vacuum degree is 3.0 multiplied by 10 -4 Pa, and the annealing is carried out for 25 minutes at 350 ℃, and the vacuum is kept to be naturally cooled to the room temperature after the annealing, so that the electrochemical enhanced battery electrode is finally obtained. Battery assembly and test mode reference is made to example 1.
Comparative example 2:
A method for enhancing electrochemical performance of battery electrode includes washing and drying current collector, and putting current collector into vacuum magnetron sputtering cavity. The background vacuum degree of the sputtering cavity is better than 2.0X10 -4 Pa, the working gas is high-purity argon with the purity of 99.999 percent, and the flow rate of the argon is 10sccm. And then preparing the Si-graphene gradient alternating structure. The targets used were a silicon target with a purity of 99.999%, a graphite target with a purity of 99.99% and a Cu target with a purity of 99.999%, the silicon target sputter power was 80W, the graphite target sputter power was 80W, and the copper target sputter power was 20W. Starting a graphite target at the initial stage of sputtering, sputtering a graphite layer with the thickness of 20nm, gradually reducing the power of the graphite target to 0W, gradually increasing the sputtering power of a silicon target and a copper target to 80W and 20W, sputtering a Si layer with the thickness of 20nm, alternately depositing a multi-layer structure of the graphite layer and the silicon layer according to the mode, realizing gradient transition, and finally obtaining the electrochemical enhanced battery electrode. Battery assembly and test mode reference is made to example 1.
Comparative example 3:
a method for enhancing electrochemical performance of battery electrode includes washing and drying current collector, and putting current collector into vacuum magnetron sputtering cavity. The background vacuum degree of the sputtering cavity is better than 2.0X10 -4 Pa, the working gas is high-purity argon with the purity of 99.999 percent, and the flow rate of the argon is 10sccm. And then preparing the Si-graphene gradient alternating structure. The targets used were a silicon target with a purity of 99.999%, a graphite target with a purity of 99.99% and a Cu target with a purity of 99.999%, the silicon target sputter power was 80W, the graphite target sputter power was 80W, and the copper target sputter power was 20W. Starting a graphite target at the initial stage of sputtering, sputtering a graphite layer with the thickness of 20nm, starting a silicon target and a copper target along with the closing of the graphite target, sputtering power of 80W and 20W, sputtering a Si layer with the thickness of 20nm, alternately depositing a multi-layer structure of the graphite layer and the silicon layer according to the mode, and realizing gradient transition. And finally, annealing the electrode with the alternating multilayer structure, wherein the background vacuum degree is 3.0 multiplied by 10 -4 Pa, and the annealing is carried out for 25 minutes at 350 ℃, and the vacuum is kept to be naturally cooled to the room temperature after the annealing, so that the electrochemical enhanced battery electrode is finally obtained. Battery assembly and test mode reference is made to example 1.
Comparative example 4:
A method for enhancing electrochemical performance of battery electrode includes washing and drying current collector, and putting current collector into vacuum magnetron sputtering cavity. The background vacuum degree of the sputtering cavity is better than 2.0X10 -4 Pa, the working gas is high-purity argon with the purity of 99.999 percent, and the flow rate of the argon is 10sccm. And then preparing the Si-graphene gradient alternating structure. The targets used were a silicon target with a purity of 99.999%, a graphite target with a purity of 99.99% and a Cu target with a purity of 99.999%, the silicon target sputter power was 80W, the graphite target sputter power was 80W, and the copper target sputter power was 10W. Starting a graphite target at the initial stage of sputtering, sputtering a graphite layer with the thickness of 20nm, gradually reducing the power of the graphite target to 0W, gradually increasing the sputtering power of a silicon target and a copper target to 80W and 10W, sputtering a Si layer with the thickness of 20nm, alternately depositing a multi-layer structure of the graphite layer and the silicon layer according to the mode, and realizing gradient transition. And finally, annealing the electrode with the alternating multilayer structure, wherein the background vacuum degree is 3.0 multiplied by 10 -4 Pa, and the annealing is carried out for 25 minutes at 350 ℃, and the vacuum is kept to be naturally cooled to the room temperature after the annealing, so that the electrochemical enhanced battery electrode is finally obtained. Battery assembly and test mode reference is made to example 1.
Comparative example 5:
A method for enhancing electrochemical performance of battery electrode includes washing and drying current collector, and putting current collector into vacuum magnetron sputtering cavity. The background vacuum degree of the sputtering cavity is better than 2.0X10 -4 Pa, the working gas is high-purity argon with the purity of 99.999 percent, and the flow rate of the argon is 10sccm. And then preparing the Si-graphene gradient alternating structure. The targets used were a silicon target with a purity of 99.999%, a graphite target with a purity of 99.99% and a Cu target with a purity of 99.999%, the silicon target sputter power was 80W, the graphite target sputter power was 80W, and the copper target sputter power was 40W. Starting a graphite target at the initial stage of sputtering, sputtering a graphite layer with the thickness of 20nm, gradually reducing the power of the graphite target to 0W, gradually increasing the sputtering power of a silicon target and a copper target to 80W and 40W, sputtering a Si layer with the thickness of 20nm, alternately depositing a multi-layer structure of the graphite layer and the silicon layer according to the mode, and realizing gradient transition. And finally, annealing the electrode with the alternating multilayer structure, wherein the background vacuum degree is 3.0 multiplied by 10 -4 Pa, and the annealing is carried out for 25 minutes at 350 ℃, and the vacuum is kept to be naturally cooled to the room temperature after the annealing, so that the electrochemical enhanced battery electrode is finally obtained. Battery assembly and test mode reference is made to example 1.
Table 1 test results
。
Claims (10)
1. The electrochemical enhancement method of the battery electrode is characterized in that a current collector is firstly placed in a vacuum magnetron sputtering cavity, the background vacuum degree of the sputtering cavity is better than 2.0X10-4 Pa, the working gas is high-purity argon with the purity of 99.999%, and the flow rate of the argon is 8-12sccm;
Then preparing a Si-graphene gradient alternating structure, wherein the sputtering power of a silicon target is 80-100W, the sputtering power of a graphite target is 80-100W, the sputtering power of a copper target is 20-30W, starting the graphite target at the initial stage of sputtering, sputtering a graphite layer with the thickness of 15-25nm, then gradually reducing the power of the graphite target to 0W, gradually increasing the sputtering power of the silicon target and the sputtering power of the copper target to a preset value, sputtering a Si layer with the thickness of 15-25nm, alternately depositing a graphite layer and a silicon layer multilayer structure according to the mode, and realizing gradient transition;
and finally, annealing the electrode with the alternating multilayer structure for 20-30 minutes at 300-400 ℃, and naturally cooling to room temperature after annealing.
2. The method of claim 1, wherein the silicon target used has a purity of 99.999%.
3. The method of claim 1, wherein the graphite target used has a purity of 99.99%.
4. The method of claim 1, wherein the Cu target used has a purity of 99.999%.
5. The method of claim 1, wherein the current collector is PET, PP, PI or PC.
6. The method of claim 1, wherein the vacuum is maintained during natural cooling to room temperature after annealing.
7. The method of claim 1, wherein the background vacuum level upon annealing is 3.0 x 10 -4 pa.
8. The method of claim 1, wherein the current collector is cleaned and dried prior to being placed in the vacuum magnetron sputtering chamber.
9. The improved battery electrode of claim 1.
10. The battery electrode of claim 9 wherein the current collector is PET, PP, PI or PC.
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Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101414674A (en) * | 2008-08-05 | 2009-04-22 | 华南师范大学 | Cathode material for lithium ion battery tin/carbon nanometer multilayer film, and preparation method and application thereof |
| CN101444985A (en) * | 2007-12-19 | 2009-06-03 | 中国人民解放军装甲兵工程学院 | Amorphous carbon coating and preparation method and application thereof |
| CN101913598A (en) * | 2010-08-06 | 2010-12-15 | 浙江大学 | A kind of graphene film preparation method |
| EP2720809A1 (en) * | 2011-06-17 | 2014-04-23 | University of North Texas | Direct graphene growth on mgo (111) by physical vapor deposition: interfacial chemistry and band gap formation |
| CN107742746A (en) * | 2017-09-18 | 2018-02-27 | 深圳市烯谷能源控股有限公司 | A kind of manufacture method of composite graphite alkene lithium ion battery and composite graphite alkene electrode |
| CN108251808A (en) * | 2018-06-05 | 2018-07-06 | 昆明物理研究所 | The preparation method of Copper-cladding Aluminum Bar multi-layer graphene |
| CN108807883A (en) * | 2018-05-28 | 2018-11-13 | 云南大学 | Silicon carbon film negative material and preparation method thereof |
| CN111850484A (en) * | 2020-07-24 | 2020-10-30 | 太原理工大学 | A device and method for preparing toughened amorphous carbon-based multiphase hybrid film |
| CN116344750A (en) * | 2023-03-08 | 2023-06-27 | 昆明理工大学 | A kind of lithium-ion battery silicon carbon thin film negative electrode material and preparation method thereof |
| WO2024099027A1 (en) * | 2023-07-21 | 2024-05-16 | 广东省科学院新材料研究所 | High-temperature super-lubrication silicon-doped diamond-like carbon film, and preparation method therefor and use thereof |
| US20240178371A1 (en) * | 2022-11-30 | 2024-05-30 | Lanzhou Institute Of Chemical Physics, Cas | Silicon-based anode material with high stability and conductivity for lithium-ion batteries and preparation method thereof |
-
2024
- 2024-12-10 CN CN202411803767.8A patent/CN119265528B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101444985A (en) * | 2007-12-19 | 2009-06-03 | 中国人民解放军装甲兵工程学院 | Amorphous carbon coating and preparation method and application thereof |
| CN101414674A (en) * | 2008-08-05 | 2009-04-22 | 华南师范大学 | Cathode material for lithium ion battery tin/carbon nanometer multilayer film, and preparation method and application thereof |
| CN101913598A (en) * | 2010-08-06 | 2010-12-15 | 浙江大学 | A kind of graphene film preparation method |
| EP2720809A1 (en) * | 2011-06-17 | 2014-04-23 | University of North Texas | Direct graphene growth on mgo (111) by physical vapor deposition: interfacial chemistry and band gap formation |
| CN107742746A (en) * | 2017-09-18 | 2018-02-27 | 深圳市烯谷能源控股有限公司 | A kind of manufacture method of composite graphite alkene lithium ion battery and composite graphite alkene electrode |
| CN108807883A (en) * | 2018-05-28 | 2018-11-13 | 云南大学 | Silicon carbon film negative material and preparation method thereof |
| CN108251808A (en) * | 2018-06-05 | 2018-07-06 | 昆明物理研究所 | The preparation method of Copper-cladding Aluminum Bar multi-layer graphene |
| CN111850484A (en) * | 2020-07-24 | 2020-10-30 | 太原理工大学 | A device and method for preparing toughened amorphous carbon-based multiphase hybrid film |
| US20240178371A1 (en) * | 2022-11-30 | 2024-05-30 | Lanzhou Institute Of Chemical Physics, Cas | Silicon-based anode material with high stability and conductivity for lithium-ion batteries and preparation method thereof |
| CN116344750A (en) * | 2023-03-08 | 2023-06-27 | 昆明理工大学 | A kind of lithium-ion battery silicon carbon thin film negative electrode material and preparation method thereof |
| WO2024099027A1 (en) * | 2023-07-21 | 2024-05-16 | 广东省科学院新材料研究所 | High-temperature super-lubrication silicon-doped diamond-like carbon film, and preparation method therefor and use thereof |
Non-Patent Citations (1)
| Title |
|---|
| 马天慧等: "功能材料制备技术", 31 May 2023, 哈尔滨工业大学出版社, pages: 172 - 176 * |
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