CN104157826B - The preparation method of a kind of nano-electrode negative material - Google Patents
The preparation method of a kind of nano-electrode negative material Download PDFInfo
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- CN104157826B CN104157826B CN201410392193.XA CN201410392193A CN104157826B CN 104157826 B CN104157826 B CN 104157826B CN 201410392193 A CN201410392193 A CN 201410392193A CN 104157826 B CN104157826 B CN 104157826B
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- 239000000463 material Substances 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims abstract description 40
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000012986 modification Methods 0.000 claims abstract description 17
- 230000004048 modification Effects 0.000 claims abstract description 17
- 239000002114 nanocomposite Substances 0.000 claims abstract description 16
- 238000005245 sintering Methods 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 239000011248 coating agent Substances 0.000 claims abstract description 8
- 238000000576 coating method Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims description 12
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 8
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 8
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 8
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 4
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 4
- 239000006004 Quartz sand Substances 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 239000012300 argon atmosphere Substances 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 4
- 239000012467 final product Substances 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000002994 raw material Substances 0.000 abstract description 7
- 230000007547 defect Effects 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 4
- 239000010405 anode material Substances 0.000 abstract description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000007772 electrode material Substances 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000000956 alloy Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000007773 negative electrode material Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910001128 Sn alloy Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 238000007600 charging Methods 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000006181 electrochemical material Substances 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000036647 reaction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000011366 tin-based material Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- -1 transition metal nitride Chemical class 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/364—Composites as mixtures
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention belongs to electrochemical field, the preparation method of a kind of nano-electrode negative material, comprise the steps: step 1) prepare body material, step 2) prepare nano composite material, step 3) prepare modification infusorial earth, step 4) preparation polyvinylidene difluoride (PVDF) solution, step 5) batch mixing stir and step 6) coating sintering. This preparation method's technique simple possible, low raw-material cost, overcomes the defect of electrode anode material in prior art, possesses the advantages such as efficiency for charge-discharge height, good cycle.
Description
Technical field
The invention belongs to electrochemical material field, disclose the preparation method of a kind of nano-electrode negative material.
Background technology
Nanotechnology (nanotechnology) is the science and technology manufacturing material with single atom, molecule, the character of research structure size material in 1 to 100 nanometer range and application. It nanometer it is the least unit of length metering, the length of 1 nanometer be 1 millimeter 1,000,000/, the various element of direct formation and the atom of material, atomic group, molecule, molecular grouping assembling have the material of specific function or have the high-quality precision and sophisticated technology of special performance products. Successful nanotechnology can be applicable to the every field such as electronics, chemical industry, military affairs, and countries in the world are all in research and development. Application of micron is in cell negative electrode material, as negative material, it becomes to be grouped into by number of chemical, prepare through science, unique physical and chemical reaction becomes, if formula and technique are unreasonable, even if adding some nano level raw materials, quality there will not be too big raising, the raising of industrial cost can be caused on the contrary.
Negative pole refers to one end that current potential in power supply (electromotive force) is lower. In galvanic cell, refer to the electrode of oxygenizement, cell reaction has been write on the left. From physical angle, it is the pole that in circuit, electronics flows out. And negative material, then referring in battery the raw material forming negative pole, negative material common at present has carbon negative pole material, tin base cathode material, lithium-containing transition metal nitride negative material, alloy type negative material and nano level negative material.
At present, the negative material explored has nitride, PAS, tin-based oxide, tin alloy, nanometer negative material, and other some intermetallic compounds etc. But the new matrix material of great majority is all in gropes experimental stage, wherein, the alternatively important non-carbon class negative material of silica-base material is also by various countries scholar is paid attention to, and this kind of materials theory specific storage is extremely high, but cycle performance is poor; Tin-based oxide and various tin-based alloy material are studied widely, tin-based material theoretical specific capacity relatively carbon material height, but often owing to bigger volume change causes material failure in working cycle; Nanometer negative material is also in the preliminary study stage, and the product being really applied to market is less. Chinese invention patent CN101167649A discloses the preparation method of a kind of nano-electrode material, and electrode materials prepared by the method exists the lower defect of efficiency for charge-discharge.
Summary of the invention
The technical issues that need to address of the present invention are, overcome the deficiencies in the prior art part, the preparation method of a kind of nano-electrode negative material is provided, this preparation method's technique simple possible, low raw-material cost, overcome the defect of electrode anode material in prior art, possess the advantages such as efficiency for charge-discharge height, good cycle.
It is an object of the invention to be achieved through the following technical solutions:
A preparation method for nano-electrode negative material, comprises the steps:
Step 1) prepare body material, step 2) prepare nano composite material, step 3) prepare modification infusorial earth, step 4) preparation polyvinylidene difluoride (PVDF) solution, step 5) batch mixing stir and step 6) coating sintering.
Preferably, above-mentioned preparation method specifically comprises:
Step 1) prepare body material:
By ball grinder vent gas, and being filled with rare gas element, quartz sand, manganese powder and copper powder are put into successively in ball grinder according to the weight ratio of 10: 3: 1, the particle diameter being milled to powder is 500 orders, stops ball milling, obtains body material;
Step 2) prepare nano composite material:
Nanometer silicon carbide and nano titanium oxide are mixed according to the weight ratio of 2: 1, is nano composite material; The particle diameter of nanometer silicon carbide or nano titanium oxide is 10-100nm.
Step 3) prepare modification infusorial earth: first with 5% (V/V) salt acid soak diatomite 10min, not have diatomite to be as the criterion, 500 turns are centrifugal 3 minutes, collecting precipitation, and after oven dry, grinding to form particle diameter is 500 object powder arts, obtains modification infusorial earth;
Step 4) preparation polyvinylidene difluoride (PVDF) solution: N,N-DIMETHYLACETAMIDE is solvent, and polyvinylidene difluoride (PVDF) is configured to the polyvinylidene difluoride (PVDF) solution that solid content is 18%;
Step 5) batch mixing stirring: body material, nano composite material, modification infusorial earth and polyvinylidene difluoride (PVDF) solution being mixed according to the weight ratio of 20-30: 3-5: 1-2: 5-7,500 turns/min stirs 4-5 minute, obtains mixture,
Step 6) coating sintering: by step 5) gained mixture is applied to and coats on round copper sheet; 10-12 hour is placed at 50-55 DEG C; then the water being placed in 8-10 DEG C cools; take out; cutting is carried out after drying at 100 DEG C; last under argon atmosphere 650-700 DEG C of sintering 2-3 hour, to obtain final product.
The invention also discloses the electrode materials utilizing above-mentioned preparation method to prepare.
The useful effect that the present invention obtains mainly comprises: matrix material has been carried out reasonable compatibility by the present invention, and part material has been carried out modification, changes raw-material microtexture; The present invention by adding a certain amount of nano material, together with its special molecular structure closely can be fitted to each raw material, it is to increase battery performance; The preparation technology of cell negative electrode material prepared by the present invention is simple, and low raw-material cost, overcomes the defect of matrix material in prior art, possesses the advantages such as efficiency for charge-discharge height, good cycle and security are good.
Embodiment
In order to make those skilled in the art understand the technical scheme in the application better, below in conjunction with the application's specific embodiment, the present invention is carried out clearly, intactly describes, it is clear that, described embodiment is only some embodiments of the present application, instead of whole embodiments. Based on the embodiment in the application, those of ordinary skill in the art, not making other embodiments all obtained under creative work prerequisite, should belong to the scope of protection of the invention.
Embodiment 1
A preparation method for nano-electrode negative material, comprises the steps:
Step 1) prepare body material, step 2) prepare nano composite material, step 3) prepare modification infusorial earth, step 4) preparation polyvinylidene difluoride (PVDF) solution, step 5) batch mixing stir and step 6) coating sintering;
Above-mentioned preparation method specifically comprises:
Step 1) prepare body material:
By ball grinder vent gas, and being filled with rare gas element, quartz sand, manganese powder and copper powder are put into successively in ball grinder according to the weight ratio of 10: 3: 1, the particle diameter being milled to powder is 500 orders, stops ball milling, obtains body material;
Step 2) prepare nano composite material:
Nanometer silicon carbide and nano titanium oxide are mixed according to the weight ratio of 2: 1, is nano composite material; The particle diameter of nanometer silicon carbide or nano titanium oxide is 10nm.
Step 3) prepare modification infusorial earth: first with 5% (V/V) salt acid soak diatomite 10min, not have diatomite to be as the criterion, 500 turns are centrifugal 3 minutes, collecting precipitation, and after oven dry, grinding to form particle diameter is 500 object powder, obtains modification infusorial earth;
Step 4) preparation polyvinylidene difluoride (PVDF) solution: N,N-DIMETHYLACETAMIDE is solvent, and polyvinylidene difluoride (PVDF) is configured to the polyvinylidene difluoride (PVDF) solution that solid content is 18%;
Step 5) batch mixing stirring: body material, nano composite material, modification infusorial earth and polyvinylidene difluoride (PVDF) solution being mixed according to the weight ratio of 20: 3: 1: 5,500 turns/min stirs 4 minutes, obtains mixture,
Step 6) coating sintering: by step 5) gained mixture is applied to and coats on round copper sheet, places 10 hours at 50 DEG C, the water being then placed in 8 DEG C cools; take out; at 100 DEG C dry after carry out cutting, finally under argon atmosphere 650 DEG C sintering 3 hours, to obtain final product.
Embodiment 2
A preparation method for nano-electrode negative material, comprises the steps:
Step 1) prepare body material, step 2) prepare nano composite material, step 3) prepare modification infusorial earth, step 4) preparation polyvinylidene difluoride (PVDF) solution, step 5) batch mixing stir and step 6) coating sintering.
Above-mentioned preparation method specifically comprises:
Step 1) prepare body material:
By ball grinder vent gas, and being filled with rare gas element, quartz sand, manganese powder and copper powder are put into successively in ball grinder according to the weight ratio of 10: 3: 1, the particle diameter being milled to powder is 500 orders, stops ball milling, obtains body material;
Step 2) prepare nano composite material:
Nanometer silicon carbide and nano titanium oxide are mixed according to the weight ratio of 2: 1, is nano composite material; The particle diameter of nanometer silicon carbide or nano titanium oxide is 100nm;
Step 3) prepare modification infusorial earth: first with 5% (V/V) salt acid soak diatomite 10min, not have diatomite to be as the criterion, 500 turns are centrifugal 3 minutes, collecting precipitation, and after oven dry, grinding to form particle diameter is 500 object powder, obtains modification infusorial earth;
Step 4) preparation polyvinylidene difluoride (PVDF) solution: N,N-DIMETHYLACETAMIDE is solvent, and polyvinylidene difluoride (PVDF) is configured to the polyvinylidene difluoride (PVDF) solution that solid content is 18%;
Step 5) batch mixing stirring: body material, nano composite material, modification infusorial earth and polyvinylidene difluoride (PVDF) solution being mixed according to the weight ratio of 30: 5: 2: 7,500 turns/min stirs 5 minutes, obtains mixture,
Step 6) coating sintering: by step 5) gained mixture is applied to and coats on round copper sheet, places 12 hours at 55 DEG C, the water being then placed in 10 DEG C cools; take out; at 100 DEG C dry after carry out cutting, finally under argon atmosphere 700 DEG C sintering 2 hours, to obtain final product.
Embodiment 3
The negative pole measured performance parameter of the embodiment of the present invention 1 and 2:
Control group, according to the preparation method of embodiment 1, does not add nano material, and all the other are with embodiment 1; Test adopts new prestige battery test system that negative material carries out constant current charge-discharge cycle performance test, and charging and discharging currents density is 0.2mA/cm2, voltage range is 0.01-2V (Li+/Li), and concrete test result is in table 1:
Table 1
Finally, in addition it is also necessary to it is to be noted that, what more than enumerate is only some the specific embodiments of the present invention. Obviously, the invention is not restricted to above embodiment, it is also possible to have many distortion. All distortion that the those of ordinary skill of this area can directly derive from content disclosed by the invention or associate, all should think protection scope of the present invention.
Claims (2)
1. the preparation method of a nano-electrode negative material, it is characterised in that, described preparation method comprises the steps:
Step 1) prepare body material:
By ball grinder vent gas, and being filled with rare gas element, quartz sand, manganese powder and copper powder are put into successively in ball grinder according to the weight ratio of 10: 3: 1, the particle diameter being milled to powder is 500 orders, stops ball milling, obtains body material;
Step 2) prepare nano composite material:
Nanometer silicon carbide and nano titanium oxide are mixed according to the weight ratio of 2: 1, is nano composite material;
Step 3) prepare modification infusorial earth:
Being first the salt acid soak diatomite 10min of 5% with volumn concentration, not have diatomite to be as the criterion, 500 turns centrifugal 3 minutes, collecting precipitation, and after oven dry, grinding to form particle diameter is 500 object powder, obtains modification infusorial earth;
Step 4) preparation polyvinylidene difluoride (PVDF) solution:
N,N-DIMETHYLACETAMIDE is solvent, and polyvinylidene difluoride (PVDF) is configured to the polyvinylidene difluoride (PVDF) solution that solid content is 18%;
Step 5) batch mixing stirring:
Body material, nano composite material, modification infusorial earth and polyvinylidene difluoride (PVDF) solution being mixed according to the weight ratio of 20-30: 3-5: 1-2: 5-7,500 turns/min stirs 4-5 minute, obtains mixture,
Step 6) coating sintering:
By step 5) gained mixture is applied to and coats on round copper sheet, places 10-12 hour at 50-55 DEG C, and the water being then placed in 8-10 DEG C cools; take out; at 100 DEG C dry after carry out cutting, finally under argon atmosphere 650-700 DEG C sintering 2-3 hour, to obtain final product.
2. preparation method as claimed in claim 1, it is characterised in that, the particle diameter of described nanometer silicon carbide or nano titanium oxide is 10-100nm.
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| CN201410392193.XA CN104157826B (en) | 2014-08-07 | 2014-08-07 | The preparation method of a kind of nano-electrode negative material |
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| CN201410392193.XA CN104157826B (en) | 2014-08-07 | 2014-08-07 | The preparation method of a kind of nano-electrode negative material |
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| CN104157826B true CN104157826B (en) | 2016-06-08 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102208636A (en) * | 2011-05-12 | 2011-10-05 | 北京科技大学 | Method for preparing porous silicon/carbon composite material by using diatomite as raw material and application |
| CN103531767A (en) * | 2013-10-30 | 2014-01-22 | 合肥恒能新能源科技有限公司 | Lithium battery special-purpose modified lithium titanate negative electrode material and preparation method thereof |
| CN103633305A (en) * | 2013-12-10 | 2014-03-12 | 苏州宇豪纳米材料有限公司 | Silicon composite anode material of lithium ion battery and preparation method of silicon composite anode material |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102208636A (en) * | 2011-05-12 | 2011-10-05 | 北京科技大学 | Method for preparing porous silicon/carbon composite material by using diatomite as raw material and application |
| CN103531767A (en) * | 2013-10-30 | 2014-01-22 | 合肥恒能新能源科技有限公司 | Lithium battery special-purpose modified lithium titanate negative electrode material and preparation method thereof |
| CN103633305A (en) * | 2013-12-10 | 2014-03-12 | 苏州宇豪纳米材料有限公司 | Silicon composite anode material of lithium ion battery and preparation method of silicon composite anode material |
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