CN105609744A - Battery positive electrode composite base material and preparation method therefor - Google Patents
Battery positive electrode composite base material and preparation method therefor Download PDFInfo
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- CN105609744A CN105609744A CN201610162759.9A CN201610162759A CN105609744A CN 105609744 A CN105609744 A CN 105609744A CN 201610162759 A CN201610162759 A CN 201610162759A CN 105609744 A CN105609744 A CN 105609744A
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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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- 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
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- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention provides a battery positive electrode composite base material and a preparation method therefor. The battery positive electrode composite base material is prepared from the following components: lithium hydroxide, saccharose, vanadium pentoxide, magnesium acetate, magnesium hydrate, magnesium nitrate hexahydrate, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, ferric phosphate, ferric hydroxide, solid paraffin, ethylene bis-stearamide, calcium oxide and absolute ethyl alcohol; the preparation method comprises the following steps of mixing and stirring all the components; then putting the components into a planet ball mill to be subjected to ball milling; then putting the components into an oven to be dried; taking the components out and putting the components into a dispersion machine to be dispersed; then loading the components into a tubular furnace to be sintered; taking the components out, and grinding the components in a mortar; and finally loading the components into the tubular furnace to be sintered, and cooling the components to obtain the battery positive electrode composite base material. The battery positive electrode composite base material is quite high in specific discharge capacity, good in electrochemical performance, relatively high in tap density, stable in performance and high in circulation utilization ratio.
Description
Technical field
The present invention relates to field of electronic materials, be specifically related to a kind of anode compound matrix material and preparation method thereof.
Background technology
Be accompanied by China's economy, science and technology and social fast development; the environment of China has suffered destruction without restraint; the energy of China is faced with huge crisis, and wherein, the shortage of energy PetroChina Company Limited. and the air pollution being caused by automobile and chemical industry are difficult problems that continues to be resolved. For this reason, constantly research and develop countries in the world, in the hope of solve the problem of oil by electric power, at present, the appearance of the electric hybrid vehicle of first item oil of producing along with Lexus under group of Japanese Toyota, individual automobile industry also exploitation energetically with improve better oily electric hybrid vehicle to solve oil shortage problem. In the electric hybrid technology of oil, key technology is exactly battery, can say that power battery technology is exactly the bottleneck of hybrid vehicle development. In numerous batteries, the research of lithium battery is comparatively popular at present, and it has advantages of, and specific energy is high, operating voltage long, the life-span is long and it is little to pollute, still, and for for the tool space that has greatly improved also on electric automobile. Therefore, research and develop and improve the long term growth of lithium battery material for automobile industry, solving energy problem and protection of the environment and all have great importance.
Summary of the invention
The technical problem solving:The object of this invention is to provide a kind of anode compound matrix material, have very high specific discharge capacity, good chemical property, meanwhile, also has larger tap density, and stable performance, recycles rate high.
Technical scheme:A kind of anode compound matrix material, is prepared from by following composition: lithium hydroxide 30-50 part, sucrose 30-50 part, vanadic anhydride 20-40 part, magnesium acetate 1-2 part, magnesium hydroxide 1-2 part, magnesium nitrate hexahydrate 1-3 part, ammonium dihydrogen phosphate (ADP) 10-20 part, diammonium hydrogen phosphate 10-15 part, ferric phosphate 5-10 part, iron hydroxide 2-5 part, solid paraffin 1-2 part, the two stearic hard acid amides 1-3 parts of ethylene, calcium oxide 0.5-1 part, absolute ethyl alcohol 30-40 part.
Further preferred, described a kind of anode compound matrix material, is prepared from by following composition: lithium hydroxide 35-45 part, sucrose 35-45 part, vanadic anhydride 25-35 part, magnesium acetate 1.2-1.8 part, magnesium hydroxide 1.2-1.6 part, magnesium nitrate hexahydrate 1.5-2.5 part, ammonium dihydrogen phosphate (ADP) 12-17 part, diammonium hydrogen phosphate 11-14 part, ferric phosphate 6-9 part, iron hydroxide 3-4 part, solid paraffin 1.2-1.7 part, the two stearic hard acid amides 1.5-2.5 parts of ethylene, calcium oxide 0.6-0.9 part, absolute ethyl alcohol 33-37 part.
The preparation method of above-mentioned anode compound matrix material comprises the following steps:
Step 1: all components are mixed, stir 10-20 minute;
Step 2: put into planetary ball mill, at revolution 50-70r/min, carry out ball milling 7-8 hour under rotation 500-700r/min;
Step 3: put into baking oven dry at temperature 40-70 DEG C;
Step 4: put into dispersion machine and disperse under rotating speed 800-1200r/min;
Step 5: pack in tube furnace sintering 3-5 hour at temperature 250-350 DEG C into;
Step 6: grind in mortar after taking-up;
Step 7: pack in tube furnace, sintering 12-13 hour at temperature 750-850 DEG C, cooling and get final product.
Further preferred, in step 1, mixing time is 15 minutes.
Further preferred, in step 2, revolution speed is 55-65r/min, and rotational velocity is 550-650r/min, and Ball-milling Time is 7.5 hours.
Further preferred, in step 3, temperature is 50-60 DEG C.
Further preferred, step 4 medium speed is 900-1100r/min.
Further preferred, in step 5, temperature is 300 DEG C, and the time is 3.5-4.5 hour.
Further preferred, in step 7, temperature is 800 DEG C, and the time is 12.5 hours.
Beneficial effect:Anode compound matrix material of the present invention has very high specific discharge capacity, reaches as high as 115mAh/g, has good chemical property, and meanwhile, this material also has larger tap density, and stable performance recycles rate high.
Detailed description of the invention
Embodiment 1
A kind of anode compound matrix material, is prepared from by following composition: 30 parts of lithium hydroxides, 30 parts of sucrose, 20 parts of vanadic anhydrides, 1 part of magnesium acetate, 1 part of magnesium hydroxide, 1 part of magnesium nitrate hexahydrate, 10 parts of ammonium dihydrogen phosphate (ADP)s, 10 parts of diammonium hydrogen phosphates, ferric phosphate 5-10 part, 2 parts of iron hydroxides, 1 part of solid paraffin, 1 part of the two stearic hard acid amides of ethylene, 0.5 part, calcium oxide, 30 parts of absolute ethyl alcohols.
The preparation method of above-mentioned anode compound matrix material is: first all components are mixed, stir 10 minutes, then put into planetary ball mill, at revolution 50r/min, under rotation 500r/min, carry out ball milling 7 hours, then put into baking oven dry at 40 DEG C of temperature; Put into dispersion machine disperses under rotating speed 800r/min; Pack in tube furnace, at 250 DEG C of temperature, sintering 3 hours grinds after taking-up in mortar, finally pack in tube furnace, and sintering 12 hours at 750 DEG C of temperature, cooling and get final product.
Embodiment 2
A kind of anode compound matrix material, is prepared from by following composition: 35 parts of lithium hydroxides, 35 parts of sucrose, 25 parts of vanadic anhydrides, 1.2 parts of magnesium acetates, 1.2 parts of magnesium hydroxides, 1.5 parts of magnesium nitrate hexahydrates, 12 parts of ammonium dihydrogen phosphate (ADP)s, 11 parts of diammonium hydrogen phosphates, 6 parts of ferric phosphates, 3 parts of iron hydroxides, 1.2 parts of solid paraffins, 1.5 parts of the two stearic hard acid amides of ethylene, 0.6 part, calcium oxide, 33 parts of absolute ethyl alcohols.
The preparation method of above-mentioned anode compound matrix material is: first all components are mixed, stir 15 minutes, then put into planetary ball mill, at revolution 55r/min, under rotation 550r/min, carry out ball milling 7.5 hours, then put into baking oven dry under temperature 50 C; Put into dispersion machine disperses under rotating speed 900r/min; Pack in tube furnace, at 300 DEG C of temperature, sintering 3.5 hours grinds after taking-up in mortar, finally pack in tube furnace, and sintering 12.5 hours at 800 DEG C of temperature, cooling and get final product.
Embodiment 3
A kind of anode compound matrix material, is prepared from by following composition: 40 parts of lithium hydroxides, 40 parts of sucrose, 30 parts of vanadic anhydrides, 1.5 parts of magnesium acetates, 1.5 parts of magnesium hydroxides, 2 parts of magnesium nitrate hexahydrates, 15 parts of ammonium dihydrogen phosphate (ADP)s, 12.5 parts of diammonium hydrogen phosphates, ferric phosphate 5-10 part, 3.5 parts of iron hydroxides, 1.5 parts of solid paraffins, 2 parts of the two stearic hard acid amides of ethylene, 0.75 part, calcium oxide, 35 parts of absolute ethyl alcohols.
The preparation method of above-mentioned anode compound matrix material is: first all components are mixed, stir 15 minutes, then put into planetary ball mill, at revolution 60r/min, under rotation 600r/min, carry out ball milling 7.5 hours, then put into baking oven dry at 55 DEG C of temperature; Put into dispersion machine disperses under rotating speed 1000r/min; Pack in tube furnace, at 300 DEG C of temperature, sintering 4 hours grinds after taking-up in mortar, finally pack in tube furnace, and sintering 12.5 hours at 800 DEG C of temperature, cooling and get final product.
Embodiment 4
A kind of anode compound matrix material, is prepared from by following composition: 45 parts of lithium hydroxides, 45 parts of sucrose, 35 parts of vanadic anhydrides, 1.8 parts of magnesium acetates, 1.6 parts of magnesium hydroxides, 2.5 parts of magnesium nitrate hexahydrates, 17 parts of ammonium dihydrogen phosphate (ADP)s, 14 parts of diammonium hydrogen phosphates, 9 parts of ferric phosphates, 4 parts of iron hydroxides, 1.7 parts of solid paraffins, 2.5 parts of the two stearic hard acid amides of ethylene, 0.9 part, calcium oxide, 37 parts of absolute ethyl alcohols.
The preparation method of above-mentioned anode compound matrix material is: first all components are mixed, stir 15 minutes, then put into planetary ball mill, at revolution 65r/min, under rotation 650r/min, carry out ball milling 7.5 hours, then put into baking oven dry under temperature 60 C; Put into dispersion machine disperses under rotating speed 1100r/min; Pack in tube furnace, at 300 DEG C of temperature, sintering 4.5 hours grinds after taking-up in mortar, finally pack in tube furnace, and sintering 12.5 hours at 800 DEG C of temperature, cooling and get final product.
Embodiment 5
A kind of anode compound matrix material, is prepared from by following composition: 50 parts of lithium hydroxides, 50 parts of sucrose, 40 parts of vanadic anhydrides, 2 parts of magnesium acetates, 2 parts of magnesium hydroxides, 3 parts of magnesium nitrate hexahydrates, 20 parts of ammonium dihydrogen phosphate (ADP)s, 15 parts of diammonium hydrogen phosphates, 10 parts of ferric phosphates, 5 parts of iron hydroxides, 2 parts of solid paraffins, 3 parts of the two stearic hard acid amides of ethylene, 1 part, calcium oxide, 40 parts of absolute ethyl alcohols.
The preparation method of above-mentioned anode compound matrix material is: first all components are mixed, stir 20 minutes, then put into planetary ball mill, at revolution 70r/min, under rotation 700r/min, carry out ball milling 8 hours, then put into baking oven dry under temperature 70 C; Put into dispersion machine disperses under rotating speed 1200r/min; Pack in tube furnace, at 350 DEG C of temperature, sintering 5 hours grinds after taking-up in mortar, finally pack in tube furnace, and sintering 13 hours at 850 DEG C of temperature, cooling and get final product.
Comparative example 1
The difference of the present embodiment and embodiment 5 is not contain magnesium acetate, magnesium hydroxide and magnesium nitrate hexahydrate. Specifically:
A kind of anode compound matrix material, is prepared from by following composition: 50 parts of lithium hydroxides, 50 parts of sucrose, 40 parts of vanadic anhydrides, 20 parts of ammonium dihydrogen phosphate (ADP)s, 15 parts of diammonium hydrogen phosphates, 10 parts of ferric phosphates, 5 parts of iron hydroxides, 2 parts of solid paraffins, 3 parts of the two stearic hard acid amides of ethylene, 1 part, calcium oxide, 40 parts of absolute ethyl alcohols.
The preparation method of above-mentioned anode compound matrix material is: first all components are mixed, stir 20 minutes, then put into planetary ball mill, at revolution 70r/min, under rotation 700r/min, carry out ball milling 8 hours, then put into baking oven dry under temperature 70 C; Put into dispersion machine disperses under rotating speed 1200r/min; Pack in tube furnace, at 350 DEG C of temperature, sintering 5 hours grinds after taking-up in mortar, finally pack in tube furnace, and sintering 13 hours at 850 DEG C of temperature, cooling and get final product.
Comparative example 2
The difference of the present embodiment and embodiment 5 is not contain solid paraffin and the two stearic hard acid amides of ethylene. Specifically:
A kind of anode compound matrix material, is prepared from by following composition: 50 parts of lithium hydroxides, 50 parts of sucrose, 40 parts of vanadic anhydrides, 2 parts of magnesium acetates, 2 parts of magnesium hydroxides, 3 parts of magnesium nitrate hexahydrates, 20 parts of ammonium dihydrogen phosphate (ADP)s, 15 parts of diammonium hydrogen phosphates, 10 parts of ferric phosphates, 5 parts of iron hydroxides, 1 part, calcium oxide, 40 parts of absolute ethyl alcohols.
The preparation method of above-mentioned anode compound matrix material is: first all components are mixed, stir 20 minutes, then put into planetary ball mill, at revolution 70r/min, under rotation 700r/min, carry out ball milling 8 hours, then put into baking oven dry under temperature 70 C; Put into dispersion machine disperses under rotating speed 1200r/min; Pack in tube furnace, at 350 DEG C of temperature, sintering 5 hours grinds after taking-up in mortar, finally pack in tube furnace, and sintering 13 hours at 850 DEG C of temperature, cooling and get final product.
Following table is the partial properties index of material of the present invention, and we can see, material of the present invention has very high specific discharge capacity, reach as high as 115mAh/g, there is good chemical property, simultaneously, this material also has larger tap density, and stable performance recycles rate high.
The partial properties index of table 1 anode compound matrix material
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Comparative example 1 | Comparative example 2 | |
| Specific discharge capacity (mAh/g) | 112 | 112 | 114 | 115 | 114 | 102 | 112 |
| Tap density (g/cm3） | 1.03 | 1.05 | 1.06 | 1.06 | 1.05 | 1.01 | 0.97 |
Note: being determined as under the charging and discharging currents density of 1500mA/g of specific discharge capacity carried out.
Claims (9)
1. an anode compound matrix material, is characterized in that: be prepared from by following composition: lithium hydroxide 30-50 part, sucrose 30-50 part, vanadic anhydride 20-40 part, magnesium acetate 1-2 part, magnesium hydroxide 1-2 part, magnesium nitrate hexahydrate 1-3 part, ammonium dihydrogen phosphate (ADP) 10-20 part, diammonium hydrogen phosphate 10-15 part, ferric phosphate 5-10 part, iron hydroxide 2-5 part, solid paraffin 1-2 part, the two stearic hard acid amides 1-3 parts of ethylene, calcium oxide 0.5-1 part, absolute ethyl alcohol 30-40 part.
2. a kind of anode compound matrix material according to claim 1, is characterized in that: be prepared from weight portion by following composition: lithium hydroxide 35-45 part, sucrose 35-45 part, vanadic anhydride 25-35 part, magnesium acetate 1.2-1.8 part, magnesium hydroxide 1.2-1.6 part, magnesium nitrate hexahydrate 1.5-2.5 part, ammonium dihydrogen phosphate (ADP) 12-17 part, diammonium hydrogen phosphate 11-14 part, ferric phosphate 6-9 part, iron hydroxide 3-4 part, solid paraffin 1.2-1.7 part, the two stearic hard acid amides 1.5-2.5 parts of ethylene, calcium oxide 0.6-0.9 part, absolute ethyl alcohol 33-37 part.
3. the preparation method of a kind of anode compound matrix material described in claim 1 to 2 any one, is characterized in that: comprise the following steps:
Step 1: all components are mixed, stir 10-20 minute;
Step 2: put into planetary ball mill, at revolution 50-70r/min, carry out ball milling 7-8 hour under rotation 500-700r/min;
Step 3: put into baking oven dry at temperature 40-70 DEG C;
Step 4: put into dispersion machine and disperse under rotating speed 800-1200r/min;
Step 5: pack in tube furnace sintering 3-5 hour at temperature 250-350 DEG C into;
Step 6: grind in mortar after taking-up;
Step 7: pack in tube furnace, sintering 12-13 hour at temperature 750-850 DEG C, cooling and get final product.
4. the preparation method of a kind of anode compound matrix material according to claim 3, is characterized in that: in described step 1, mixing time is 15 minutes.
5. the preparation method of a kind of anode compound matrix material according to claim 3, is characterized in that: in described step 2, revolution speed is 55-65r/min, and rotational velocity is 550-650r/min, and Ball-milling Time is 7.5 hours.
6. the preparation method of a kind of anode compound matrix material according to claim 3, is characterized in that: in described step 3, temperature is 50-60 DEG C.
7. the preparation method of a kind of anode compound matrix material according to claim 3, is characterized in that: described step 4 medium speed is 900-1100r/min.
8. the preparation method of a kind of anode compound matrix material according to claim 3, is characterized in that: in described step 5, temperature is 300 DEG C, and the time is 3.5-4.5 hour.
9. the preparation method of a kind of anode compound matrix material according to claim 3, is characterized in that: in described step 7, temperature is 800 DEG C, and the time is 12.5 hours.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1349266A (en) * | 2000-10-06 | 2002-05-15 | 索尼株式会社 | Non-aqueous electrolyte secondary cell |
| CN101162776A (en) * | 2007-10-26 | 2008-04-16 | 深圳市贝特瑞新能源材料股份有限公司 | Lithium iron phosphate suitable for high multiplying power electrokinetic cell and method for producing the same |
| CN101393982A (en) * | 2008-10-28 | 2009-03-25 | 南京海泰纳米材料有限公司 | Method for producing carbon coated nano stage lithium iron phosphate by precipitation |
| CN102034958A (en) * | 2009-09-25 | 2011-04-27 | 中国科学院物理研究所 | Mesoporous phosphate anode material with olivine structure and preparation method and use thereof |
| CN103265001A (en) * | 2013-05-02 | 2013-08-28 | 杭州电子科技大学 | Method for preparing carbon-coated lithium iron phosphate from basic lithium iron phosphate |
-
2016
- 2016-03-22 CN CN201610162759.9A patent/CN105609744B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1349266A (en) * | 2000-10-06 | 2002-05-15 | 索尼株式会社 | Non-aqueous electrolyte secondary cell |
| CN101162776A (en) * | 2007-10-26 | 2008-04-16 | 深圳市贝特瑞新能源材料股份有限公司 | Lithium iron phosphate suitable for high multiplying power electrokinetic cell and method for producing the same |
| CN101393982A (en) * | 2008-10-28 | 2009-03-25 | 南京海泰纳米材料有限公司 | Method for producing carbon coated nano stage lithium iron phosphate by precipitation |
| CN102034958A (en) * | 2009-09-25 | 2011-04-27 | 中国科学院物理研究所 | Mesoporous phosphate anode material with olivine structure and preparation method and use thereof |
| CN103265001A (en) * | 2013-05-02 | 2013-08-28 | 杭州电子科技大学 | Method for preparing carbon-coated lithium iron phosphate from basic lithium iron phosphate |
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