CN104157826A - Preparation method of nano electrode negative electrode material - Google Patents
Preparation method of nano electrode negative electrode material Download PDFInfo
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- CN104157826A CN104157826A CN201410392193.XA CN201410392193A CN104157826A CN 104157826 A CN104157826 A CN 104157826A CN 201410392193 A CN201410392193 A CN 201410392193A CN 104157826 A CN104157826 A CN 104157826A
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- 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
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- 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
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- 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
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- 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 the field of electrochemistry, and discloses a preparation method of a nano electrode negative electrode material, and the preparation method comprises the following steps: step 1) preparation of a base material, step 2) preparation of a nano composite, step 3) preparation of modified diatomite, step 4) preparation of a polyvinylidene fluoride solution, step 5) mixing and stirring, and step 6) coating sintering. The preparation method is simple and feasible in process and low in raw material cost, overcomes the defects of negative electrode materials in the prior art, and has the advantages of high charge discharge efficiency and good cycle performance, and the like.
Description
Technical field
The invention belongs to electrochemical material field, disclose a kind of preparation method of nano-electrode negative material.
Background technology
Nanometer technology (nanotechnology) is with single atom, molecule, to manufacture the science and technology of material, character and the application of research structure size material in 1 to 100 nanometer range.Nanometer is the least unit of length metering, the length of 1 nanometer be 1 millimeter 1,000,000/, directly with the atom, atomic group, molecule, the micel that form various elements and material, assemble the high-quality precision and sophisticated technology that there is the material of specific function or there is special performance product.Successfully nanometer technology 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 is to be become to be grouped into by number of chemical, through science, prepare, unique physical and chemical reaction forms, if formula and technique are unreasonable, even if add some nanoscale raw materials, in quality, do not have too large raising yet, can cause on the contrary the raising of industrial cost.
Negative pole refers to the lower one end of current potential in power supply (electromotive force).In primary cell, referred to the electrode of oxidation, in cell reaction, write on the left side.From physical angle, it is the utmost point that in circuit, electronics flows out.And negative material refers to the raw material that forms negative pole in battery, common negative material has carbon negative pole material, tin base cathode material, lithium-containing transition metal nitride negative pole material, alloy type negative material and nanoscale negative material at present.
At present, the negative material of exploring has nitride, PAS, tin-based oxide, ashbury metal, nanometer anode material, and other some intermetallic compounds etc.But the new composite material of great majority is all in groping experimental stage, and wherein, silica-base material is paid attention to as another important non-carbon class negative material Ye Wei various countries scholar, and this class materials theory specific capacity is high, but cycle performance is poor; Tin-based oxide and various kamash alloy material are studied widely, and tin-based material theoretical specific capacity is high compared with material with carbon element, but in cyclic process often because larger change in volume causes material failure; Nanometer anode material is also in the Primary Study stage, and the product that is really applied to market is less.Chinese invention patent CN101167649A discloses a kind of preparation method of nano-electrode material, and electrode material prepared by the method exists the defect that efficiency for charge-discharge is lower.
Summary of the invention
The technical issues that need to address of the present invention are, overcome the deficiencies in the prior art part, a kind of preparation method of nano-electrode negative material is provided, this preparation method's technique simple possible, cost of material is cheap, overcome the defect of electrode anode material in prior art, possessed the advantages such as efficiency for charge-discharge is high, good cycle.
The object of the invention is to be achieved through the following technical solutions:
A preparation method for nano-electrode negative material, comprises the steps:
Step 1) prepare basis material, step 2) prepare nano composite material, step 3) prepare modification infusorial earth, step 4) preparation Kynoar solution, step 5) batch mixing stirs and step 6) coating sintering.
Preferably, above-mentioned preparation method specifically comprises:
Step 1) prepare basis material:
By ball grinder vent gas, and be filled with inert gas, quartz sand, manganese powder and copper powder are put in ball grinder successively according to the weight ratio of 10: 3: 1, the particle diameter that is milled to powder is 500 orders, stops ball milling, obtains basis material;
Step 2) prepare nano composite material:
Weight ratio by nanometer silicon carbide and nano titanium oxide according to 2: 1 mixes, and 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 use 5% (V/V) salt acid soak diatomite 10min, not have diatomite to be as the criterion, 500 leave the heart 3 minutes, collecting precipitation, after oven dry, grinding to form particle diameter is 500 object powder arts, obtains modification infusorial earth;
Step 4) preparation Kynoar solution: dimethylacetylamide is solvent, it is 18% Kynoar solution that Kynoar is configured to solid content;
Step 5) batch mixing stirs: basis material, nano composite material, modification infusorial earth and Kynoar solution are mixed according to the weight ratio of 20-30: 3-5: 1-2: 5-7, and 500 turn/min stir 4-5 minute, obtain mixed material,
Step 6) coating sintering: by step 5) gained mixed material is applied to and coats on round copper sheet; at 50-55 ℃, place 10-12 hour; then the water that is placed in 8-10 ℃ carries out cooling; take out; after drying at 100 ℃, carry out cutting; finally 650-700 ℃ of sintering 2-3 hour under argon shield atmosphere, obtains.
The invention also discloses the electrode material that utilizes above-mentioned preparation method to prepare.
The beneficial effect that the present invention obtains mainly comprises: the present invention has carried out reasonable compatibility to composite material, and part material has been carried out to modification, has changed raw-material microstructure; The present invention is by adding a certain amount of nano material, and its special molecular structure has improved battery performance together with can being closely fitted to each raw material; The preparation technology of cell negative electrode material prepared by the present invention is simple, and cost of material is cheap, has overcome the defect of composite material in prior art, possesses that efficiency for charge-discharge is high, good cycle and the advantage such as fail safe is good.
Embodiment
In order to make those skilled in the art person understand better the technical scheme in the application, below in conjunction with the application's specific embodiment, the present invention is described more clearly and completely, obviously, described embodiment is only the application's part embodiment, rather than whole embodiment.Embodiment based in the application, those of ordinary skills, not making the every other embodiment obtaining 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 basis material, step 2) prepare nano composite material, step 3) prepare modification infusorial earth, step 4) preparation Kynoar solution, step 5) batch mixing stirs and step 6) coating sintering;
Above-mentioned preparation method specifically comprises:
Step 1) prepare basis material:
By ball grinder vent gas, and be filled with inert gas, quartz sand, manganese powder and copper powder are put in ball grinder successively according to the weight ratio of 10: 3: 1, the particle diameter that is milled to powder is 500 orders, stops ball milling, obtains basis material;
Step 2) prepare nano composite material:
Weight ratio by nanometer silicon carbide and nano titanium oxide according to 2: 1 mixes, and is nano composite material; The particle diameter of nanometer silicon carbide or nano titanium oxide is 10nm.
Step 3) prepare modification infusorial earth: first use 5% (V/V) salt acid soak diatomite 10min, not have diatomite to be as the criterion, 500 leave the heart 3 minutes, collecting precipitation, after oven dry, grinding to form particle diameter is 500 object powder, obtains modification infusorial earth;
Step 4) preparation Kynoar solution: dimethylacetylamide is solvent, it is 18% Kynoar solution that Kynoar is configured to solid content;
Step 5) batch mixing stirs: by basis material, nano composite material, modification infusorial earth and Kynoar solution according to 20: 3: 1: 5 weight ratio is mixed, and 500 turn/min stir 4 minutes, obtain mixed material,
Step 6) coating sintering: by step 5) gained mixed material is applied to and coats on round copper sheet, places 10 hours at 50 ℃, and the water that is then placed in 8 ℃ carries out cooling; take out; after drying at 100 ℃, carry out cutting, finally 650 ℃ of sintering 3 hours under argon shield atmosphere, obtain.
Embodiment 2
A preparation method for nano-electrode negative material, comprises the steps:
Step 1) prepare basis material, step 2) prepare nano composite material, step 3) prepare modification infusorial earth, step 4) preparation Kynoar solution, step 5) batch mixing stirs and step 6) coating sintering.
Above-mentioned preparation method specifically comprises:
Step 1) prepare basis material:
By ball grinder vent gas, and be filled with inert gas, quartz sand, manganese powder and copper powder are put in ball grinder successively according to the weight ratio of 10: 3: 1, the particle diameter that is milled to powder is 500 orders, stops ball milling, obtains basis material;
Step 2) prepare nano composite material:
Weight ratio by nanometer silicon carbide and nano titanium oxide according to 2: 1 mixes, and is nano composite material; The particle diameter of nanometer silicon carbide or nano titanium oxide is 100nm;
Step 3) prepare modification infusorial earth: first use 5% (V/V) salt acid soak diatomite 10min, not have diatomite to be as the criterion, 500 leave the heart 3 minutes, collecting precipitation, after oven dry, grinding to form particle diameter is 500 object powder, obtains modification infusorial earth;
Step 4) preparation Kynoar solution: dimethylacetylamide is solvent, it is 18% Kynoar solution that Kynoar is configured to solid content;
Step 5) batch mixing stirs: by basis material, nano composite material, modification infusorial earth and Kynoar solution according to 30: 5: 2: 7 weight ratio is mixed, and 500 turn/min stir 5 minutes, obtain mixed material,
Step 6) coating sintering: by step 5) gained mixed material is applied to and coats on round copper sheet, places 12 hours at 55 ℃, and the water that is then placed in 10 ℃ carries out cooling; take out; after drying at 100 ℃, carry out cutting, finally 700 ℃ of sintering 2 hours under argon shield atmosphere, obtain.
Embodiment 3
The embodiment of the present invention 1 and 2 negative pole measured performance parameter:
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 anticathode material to carry out the test of constant current charge-discharge cycle performance, and charging and discharging currents density is 0.2mA/cm
2, voltage range is 0.01-2V (Li+/Li), concrete test result is in Table 1:
Table 1
Finally, it is also to be noted that, what more than enumerate is only several specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, can also have many distortion.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention, all should think protection scope of the present invention.
Claims (3)
1. a preparation method for nano-electrode negative material, is characterized in that, described preparation method comprises the steps:
Step 1) prepare basis material, step 2) prepare nano composite material, step 3) prepare modification infusorial earth, step 4) preparation Kynoar solution, step 5) batch mixing stirs and step 6) coating sintering.
2. preparation method as claimed in claim 1, is characterized in that, described preparation method comprises the steps:
Step 1) prepare basis material:
By ball grinder vent gas, and be filled with inert gas, quartz sand, manganese powder and copper powder are put in ball grinder successively according to the weight ratio of 10: 3: 1, the particle diameter that is milled to powder is 500 orders, stops ball milling, obtains basis material;
Step 2) prepare nano composite material:
Weight ratio by nanometer silicon carbide and nano titanium oxide according to 2: 1 mixes, and is nano composite material;
Step 3) prepare modification infusorial earth:
First use 5% salt acid soak diatomite 10min, not have diatomite to be as the criterion, 500 leave the heart 3 minutes, collecting precipitation, and after oven dry, grinding to form particle diameter is 500 object powder, obtains modification infusorial earth;
Step 4) preparation Kynoar solution:
Dimethylacetylamide is solvent, and it is 18% Kynoar solution that Kynoar is configured to solid content;
Step 5) batch mixing stirs:
Basis material, nano composite material, modification infusorial earth and Kynoar solution are mixed according to the weight ratio of 20-30: 3-5: 1-2: 5-7, and 500 turn/min stir 4-5 minute, obtain mixed material,
Step 6) coating sintering:
By step 5) gained mixed material is applied to and coats on round copper sheet, at 50-55 ℃, places 10-12 hour, and the water that is then placed in 8-10 ℃ carries out cooling; take out; after drying at 100 ℃, carry out cutting, finally 650-700 ℃ of sintering 2-3 hour under argon shield atmosphere, obtains.
3. preparation method as claimed in claim 2, is characterized 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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| CN104157826A true CN104157826A (en) | 2014-11-19 |
| CN104157826B CN104157826B (en) | 2016-06-08 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106058197A (en) * | 2016-07-26 | 2016-10-26 | 王攀 | Novel battery cathode material and preparation method thereof |
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 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106058197A (en) * | 2016-07-26 | 2016-10-26 | 王攀 | Novel battery cathode material and preparation method thereof |
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