CN108695514A - A kind of anode material for lithium-ion batteries of good cycle and preparation method thereof - Google Patents
A kind of anode material for lithium-ion batteries of good cycle and preparation method thereof Download PDFInfo
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- CN108695514A CN108695514A CN201810636243.2A CN201810636243A CN108695514A CN 108695514 A CN108695514 A CN 108695514A CN 201810636243 A CN201810636243 A CN 201810636243A CN 108695514 A CN108695514 A CN 108695514A
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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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
Abstract
The invention discloses a kind of anode material for lithium-ion batteries of good cycle and preparation method thereof, include the raw material of following parts by weight:12-18 parts of molysite, 15-18 parts of phosphate, 10-15 parts of lithium salts, 4-7 parts of vanadic anhydride, 4.5-6.6 parts of tartaric acid, 2.4-4 parts of pear tannin, 4-5.5 parts of 1.8-2.7 parts of 3-4.5 parts of 3-6 parts of 8-14 parts of ammonium hydroxide, gelatine, polyaniline, glycine, the glucose and 5-7 parts of blueberry that mass fraction is 8-15%.Raw material sources of the present invention are extensive, by carrying out different preparation processes to different raw materials, under the synergistic effect of various raw materials, element doping ratio can be adjusted, the impedance of material internal is reduced, electric conductivity, hoist capacity are improved, the finished product of drying, once sintered and double sintering, preparation has good capacitance and cycle performance.
Description
Technical field
The present invention relates to field of lithium ion battery, the anode material for lithium-ion batteries of specifically a kind of good cycle.
Background technology
Due to the continuous consumption of the fossil fuel based on oil and coal, and for the continuous exacerbation of environmental pollution, such as
Current haze weather and vehicle exhaust has become the number one killer etc. of human health, seriously affected human health and
Living environment.More and more people turn one's attention to new energy technology, tap a new source of energy as the energy strategy weight of numerous countries
Point, lithium battery are one of important directions, and lithium ion battery just becomes most potential power source with its excellent performance
One of.
It by lithium metal or lithium alloy is negative material, using the battery of non-aqueous electrolytic solution that lithium battery, which is a kind of, with lead
Traditional secondary cell such as acid, ni-Cd, ni-mh is compared, and lithium ion battery has high operating voltage, small, light weight, capacity
Density height, memory-less effect, pollution-free and self discharge is small, the advantages that having extended cycle life, and has gradually replaced traditional plumbic acid electricity
The electrochmical power sources such as pond.In particular with the increasingly prominent of energy and environment problem, lithium ion battery has obtained more and more weights
Depending on.
The research of anode material for lithium-ion batteries is one of most active direction.Commercial Li-ion battery is used at present
Positive electrode be mainly embedding lithium transition-metal oxide, including cobalt acid lithium, LiMn2O4, nickle cobalt lithium manganate ternary system etc..It is existing
The problems such as in common cobalt acid lithium material because expensive, chemical stability and thermal stability are poor, inhibits it in large capacity
Application on battery.Cheap lithium manganate material capacity is relatively low, and high temperature circulation is poor, and there is no obtain at home extensively
Popularization.Although ternary material has higher energy density, safety relatively poor.Lithium iron phosphate positive material has
The advantages that cost of material is low, environmental-friendly, platform voltage is steady, thermal stability is good, safety is good, but iron phosphate lithium positive pole material
The specific capacity of material is low, poor circulation, this improves with regard to being badly in need of people.
Invention content
The purpose of the present invention is to provide a kind of anode material for lithium-ion batteries of good cycle, to solve above-mentioned background
The problem of being proposed in technology.
To achieve the above object, the present invention provides the following technical solutions:
A kind of anode material for lithium-ion batteries of good cycle, includes the raw material of following parts by weight:12-18 parts of molysite,
15-18 parts of phosphate, 10-15 parts of lithium salts, 4-7 parts of vanadic anhydride, 4.5-6.6 parts of tartaric acid, 2.4-4 parts of pear tannin, matter
Measure 1.8-2.7 parts of 3-4.5 parts of 3-6 parts of 8-14 parts of ammonium hydroxide, gelatine, polyaniline, glycine, the glucose 4- that score is 8-15%
5.5 parts and 5-7 parts of blueberry.
As a further solution of the present invention:Molysite and lithium salts are all made of sulphate, phosphate cpd and acetic acid
At least one of object is closed, phosphate includes one or several kinds of mixing of potassium phosphate, magnesium phosphate, sodium phosphate and aluminum phosphate
Object.
As a further solution of the present invention:The grain size of vanadic anhydride is 36-75um.
The preparation method of the anode material for lithium-ion batteries of the good cycle, is as follows:
Blueberry is crushed and is extracted in the mixed solution that pH value is 5-6, temperature is 50-75 degrees Celsius by step 1
1.5-2.5 hours, mixed solution included that mass ratio is 3-5.6:2-3.3:1 trimethylamine oxide, lentinan and water, filtering,
Centrifugation and isolated blueberry extracting solution;
Molysite, phosphate, lithium salts, tartaric acid, polyaniline and glucose are mixed and its total weight are added by step 2
2.4-3.8 times of deionized water stirs 20-35 minutes under 40-48 degrees Celsius and 750-960rpm of rotating speed, then in 60-
It is stirred 45-60 minutes under 65 degrees Celsius and 1500-1800rpm of rotating speed, obtains the first mixture;
Step 3, it is 60-72 that ratio of grinding media to material, which is added, in vanadic anhydride, glycine, glucose and blueberry extracting solution:1 ball
In grinding machine, ball milling product is added in ammonium hydroxide and supersonic oscillations are uniform, obtains the second mixture;
Step 4, the rotating speed by gelatine, the first mixture and the second mixture at 35-44 degrees Celsius and 180-270rpm
Under stir evenly, while stirring be added pear tannin, continue after being added completely into stirring 30-50 minute, obtain third mix
Object;
Third mixture is dried to obtain powder by step 5, and powder is sintered under inert atmosphere and 360-480 degrees Celsius
8-12 hours, then be warming up to 960-1050 degrees Celsius with the speed of 10-18 degrees celsius/minutes and be sintered 15-22 hours, it is natural
The dizzy processing of plasma electric is carried out after being cooled to room temperature to get to finished product.
As a further solution of the present invention:The power of supersonic oscillations is 180-220W, supersonic oscillations in step 3
Frequency be 30-40KHz.
As a further solution of the present invention:The temperature of ball milling is 55-66 degrees Celsius in step 3, and the speed of ball milling is
600-750rpm。
As a further solution of the present invention:The environment of plasma sided corona treatment is air environment.
Compared with prior art, the beneficial effects of the invention are as follows:Raw material sources of the present invention are extensive, by different raw materials
Different preparation processes is carried out, under the synergistic effect of various raw materials, element doping ratio can be adjusted, reduce material internal
Impedance, improves electric conductivity, and the finished product of hoist capacity, drying, once sintered and double sintering, preparation has good electricity
Capacity and cycle performance meet the use demand as anode material for lithium-ion batteries.
Specific implementation mode
The technical solution of this patent is described in more detail With reference to embodiment.
Embodiment 1
A kind of anode material for lithium-ion batteries of good cycle, includes the raw material of following parts by weight:12 parts of molysite, phosphoric acid
15 parts of salt, 10 parts of lithium salts, 4 parts of vanadic anhydride, 4.5 parts of tartaric acid, 2.4 parts of pear tannin, the ammonium hydroxide 8 that mass fraction is 12%
Part, 3 parts of gelatine, 3 parts of polyaniline, 1.8 parts of glycine, 4 parts of glucose and 5 parts of blueberry.Molysite and lithium salts are all made of acetic acid chemical combination
Object, phosphate include the mixture of potassium phosphate, magnesium phosphate and aluminum phosphate.
The preparation method of the anode material for lithium-ion batteries of the good cycle, is as follows:
Step 1, blueberry is crushed and in the mixed solution that pH value is 5.4, temperature is 58 degrees Celsius extraction it is 1.8 small
When, mixed solution includes that mass ratio is 3.8:2.5:1 trimethylamine oxide, lentinan and water, filtering, centrifugation and it is isolated
Blueberry extracting solution;
Molysite, phosphate, lithium salts, tartaric acid, polyaniline and glucose are mixed and its total weight are added by step 2
2.6 times of deionized water stirs 28 minutes under 44 degrees Celsius and 840rpm of rotating speed, then in 63 degrees Celsius and 1650rpm
Rotating speed under stir 50 minutes, obtain the first mixture;
Step 3, it is 66 that ratio of grinding media to material, which is added, in vanadic anhydride, glycine, glucose and blueberry extracting solution:1 ball mill
In, ball milling product is added in ammonium hydroxide and supersonic oscillations are uniform, the power of supersonic oscillations is 200W, supersonic oscillations
Frequency is 35KHz, obtains the second mixture;
Step 4 stirs gelatine, the first mixture and the second mixture under 38 degrees Celsius and 210rpm of rotating speed
Uniformly, pear tannin is added while stirring, continues stirring 45 minutes after being added completely into, obtains third mixture;
Third mixture is dried to obtain powder by step 5, and it is small that powder is sintered under inert atmosphere and 450 degrees Celsius to 11
When, then be warming up to 980 degrees Celsius with the speed of 16 degrees celsius/minutes and be sintered 18 hours, it is carried out after cooled to room temperature
Plasma sided corona treatment is to get to finished product.
Embodiment 2
A kind of anode material for lithium-ion batteries of good cycle, includes the raw material of following parts by weight:14.5 parts of molysite, phosphorus
16.6 parts of hydrochlorate, 12 parts of lithium salts, 5.5 parts of vanadic anhydride, 5.4 parts of tartaric acid, 3 parts of pear tannin, mass fraction are 15%
6.2 parts of 11 parts of ammonium hydroxide, 4.6 parts of gelatine, 3.8 parts of polyaniline, 2.2 parts of glycine, 4.7 parts of glucose and blueberry.Molysite and lithium salts
It is all made of the mixture of sulphate and phosphate cpd, phosphate uses sodium phosphate.The grain size of vanadic anhydride is 55um.
The preparation method of the anode material for lithium-ion batteries of the good cycle, is as follows:
Step 1, blueberry is crushed and in the mixed solution that pH value is 5.8, temperature is 68 degrees Celsius extraction it is 2.2 small
When, mixed solution includes that mass ratio is 5.2:3.1:1 trimethylamine oxide, lentinan and water, filtering, centrifugation and it is isolated
Blueberry extracting solution;
Molysite, phosphate, lithium salts, tartaric acid, polyaniline and glucose are mixed and its total weight are added by step 2
3.5 times of deionized water stirs 33 minutes under 48 degrees Celsius and 960rpm of rotating speed, then in 64 degrees Celsius and 1800rpm
Rotating speed under stir 48 minutes, obtain the first mixture;
Step 3, it is 68 that ratio of grinding media to material, which is added, in vanadic anhydride, glycine, glucose and blueberry extracting solution:1 ball mill
In, the temperature of ball milling is 62 degrees Celsius, and the speed of ball milling is 660rpm, and ball milling product is added in ammonium hydroxide and supersonic oscillations
Uniformly, the second mixture is obtained;
Step 4 stirs gelatine, the first mixture and the second mixture under 40 degrees Celsius and 240rpm of rotating speed
Uniformly, pear tannin is added while stirring, continues stirring 45 minutes after being added completely into, obtains third mixture;
Third mixture is dried to obtain powder by step 5, and it is small that powder is sintered under inert atmosphere and 440 degrees Celsius to 10
When, then be warming up to 1020 degrees Celsius with the speed of 12 degrees celsius/minutes and be sintered 20 hours, in sky after cooled to room temperature
Plasma sided corona treatment is carried out under compression ring border to get to finished product.
Embodiment 3
A kind of anode material for lithium-ion batteries of good cycle, includes the raw material of following parts by weight:17 parts of molysite, phosphoric acid
17.5 parts of salt, 14.2 parts of lithium salts, 6.6 parts of vanadic anhydride, 6 parts of tartaric acid, 3.5 parts of pear tannin, mass fraction are 15%
6.4 parts of 13 parts of ammonium hydroxide, 5.5 parts of gelatine, 4.2 parts of polyaniline, 2.5 parts of glycine, 5.2 parts of glucose and blueberry.Molysite uses sulphur
Acid compound, lithium salts using sulphate, phosphate cpd and acetic acid compound mixture, phosphate include sodium phosphate and
The mixture of aluminum phosphate.
The preparation method of the anode material for lithium-ion batteries of the good cycle, is as follows:
Blueberry is crushed and is extracted 2.5 hours in the mixed solution that pH value is 6, temperature is 60 degrees Celsius by step 1,
Mixed solution includes that mass ratio is 5.4:3.3:1 trimethylamine oxide, lentinan and water, filtering, centrifugation and isolated indigo plant
Certain kind of berries extracting solution;
Molysite, phosphate, lithium salts, tartaric acid, polyaniline and glucose are mixed and its total weight are added by step 2
3.6 times of deionized water stirs 28 minutes under 45 degrees Celsius and 750rpm of rotating speed, then in 64 degrees Celsius and 1800rpm
Rotating speed under stir 55 minutes, obtain the first mixture;
Step 3, it is 68 that ratio of grinding media to material, which is added, in vanadic anhydride, glycine, glucose and blueberry extracting solution:1 ball mill
In, the temperature of ball milling is 64 degrees Celsius, and the speed of ball milling is 720rpm, and ball milling product is added in ammonium hydroxide and supersonic oscillations
Uniformly, the power of supersonic oscillations is 190W, and the frequency of supersonic oscillations is 36KHz, obtains the second mixture;
Step 4 stirs gelatine, the first mixture and the second mixture under 40 degrees Celsius and 240rpm of rotating speed
Uniformly, pear tannin is added while stirring, continues stirring 46 minutes after being added completely into, obtains third mixture;
Third mixture is dried to obtain powder by step 5, and it is small that powder is sintered under inert atmosphere and 450 degrees Celsius to 9
When, then be warming up to 1000 degrees Celsius with the speed of 14 degrees celsius/minutes and be sintered 20 hours, it is carried out after cooled to room temperature
Plasma sided corona treatment is to get to finished product.
Embodiment 4
A kind of anode material for lithium-ion batteries of good cycle, includes the raw material of following parts by weight:18 parts of molysite, phosphoric acid
18 parts of salt, 15 parts of lithium salts, 7 parts of vanadic anhydride, 6.6 parts of tartaric acid, 4 parts of pear tannin, the ammonium hydroxide 14 that mass fraction is 10%
Part, 6 parts of gelatine, 4.5 parts of polyaniline, 2.7 parts of glycine, 5.5 parts of glucose and 7 parts of blueberry.Molysite and lithium salts are all made of sulfuric acid
The mixture of compound, phosphate cpd and acetic acid compound, phosphate include potassium phosphate, magnesium phosphate, sodium phosphate and aluminum phosphate
Mixture.The grain size of vanadic anhydride is 66um.
The preparation method of the anode material for lithium-ion batteries of the good cycle, is as follows:
Step 1, blueberry is crushed and in the mixed solution that pH value is 5.6, temperature is 70 degrees Celsius extraction it is 1.8 small
When, mixed solution includes that mass ratio is 5:2.8:1 trimethylamine oxide, lentinan and water, filtering, centrifugation and isolated indigo plant
Certain kind of berries extracting solution;
Molysite, phosphate, lithium salts, tartaric acid, polyaniline and glucose are mixed and its total weight are added by step 2
3.6 times of deionized water stirs 28 minutes under 45 degrees Celsius and 840rpm of rotating speed, then in 64 degrees Celsius and 1740rpm
Rotating speed under stir 56 minutes, obtain the first mixture;
Step 3, it is 70 that ratio of grinding media to material, which is added, in vanadic anhydride, glycine, glucose and blueberry extracting solution:1 ball mill
In, the temperature of ball milling is 64 degrees Celsius, and the speed of ball milling is 690rpm, and ball milling product is added in ammonium hydroxide and supersonic oscillations
Uniformly, the power of supersonic oscillations is 210W, and the frequency of supersonic oscillations is 38KHz, obtains the second mixture;
Step 4 stirs gelatine, the first mixture and the second mixture under 42 degrees Celsius and 240rpm of rotating speed
Uniformly, pear tannin is added while stirring, continues stirring 44 minutes after being added completely into, obtains third mixture;
Third mixture is dried to obtain powder by step 5, and it is small that powder is sintered under inert atmosphere and 450 degrees Celsius to 10
When, then be warming up to 1030 degrees Celsius with the speed of 17 degrees celsius/minutes and be sintered 20 hours, in sky after cooled to room temperature
Plasma sided corona treatment is carried out under compression ring border to get to finished product.
Comparative example 1
Except without containing blueberry, remaining raw material and preparation method are same as Example 2.
Comparative example 2
Except without containing pear tannin, remaining raw material and preparation method are same as Example 1.
Comparative example 3
Except without containing blueberry and pear tannin, remaining raw material and preparation method are same as Example 4.
Comparative example 4
Using existing LiFePO 4 material as a comparison case 4.
The product of the product of embodiment 1-4 and comparative example 1-4 as anode and are assembled into lithium ion battery, at 1C
Electric performance test is carried out, test result is shown in Table 1.
Table 1
From table 1 it follows that the cycle performance after the capacitance of comparative example 1-3 products and 300 times is superior to comparative example 4
Product, the cycle performance after the capacitance of embodiment 1-4 products and 300 times is far superior to the product of comparative example 1-3, shows
Finished product prepared by the present invention has good specific capacity and cycle performance as the positive electrode of lithium ion battery.
The present invention extracts blueberry, and part material is stirred to obtain the first mixture, and blueberry extracting solution is sweet
It the ball milling mixings such as propylhomoserin and is dispersed in ammonium hydroxide, glucose, vanadic anhydride etc. is modified, then gelatine, first are mixed
It closes object and the second mixture mix and pear tannin is added while stirring, gelatine and pear tannin are used cooperatively, not only
Various raw materials can be bonded, element doping ratio can also be adjusted, reduce the impedance of material internal, improve electric conductivity,
The finished product of hoist capacity, drying, once sintered and double sintering, preparation has good capacitance and cycle performance.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case of without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Profit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent requirements of the claims
Variation is included within the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiment being appreciated that.
Claims (7)
1. a kind of anode material for lithium-ion batteries of good cycle, which is characterized in that include the raw material of following parts by weight:Molysite
12-18 parts, 15-18 parts of phosphate, 10-15 parts of lithium salts, 4-7 parts of vanadic anhydride, 4.5-6.6 parts of tartaric acid, pear tannin
2.4-4 parts, mass fraction be 8-15% 1.8-2.7 parts of 3-4.5 parts of 3-6 parts of 8-14 parts of ammonium hydroxide, gelatine, polyaniline, glycine,
5-7 parts of 4-5.5 parts of glucose and blueberry.
2. the anode material for lithium-ion batteries of good cycle according to claim 1, which is characterized in that the molysite and
Lithium salts is all made of at least one of sulphate, phosphate cpd and acetic acid compound, and phosphate includes potassium phosphate, phosphoric acid
One or several kinds of mixtures of magnesium, sodium phosphate and aluminum phosphate.
3. the anode material for lithium-ion batteries of good cycle according to claim 1, which is characterized in that five oxidation
The grain size of two vanadium is 36-75um.
4. a kind of preparation method of the anode material for lithium-ion batteries of good cycle as described in any one of claims 1-3,
It is characterized in that, is as follows:
Blueberry is crushed and extracts 1.5-2.5 in the mixed solution that pH value is 5-6, temperature is 50-75 degrees Celsius by step 1
Hour, mixed solution includes that mass ratio is 3-5.6:2-3.3:1 trimethylamine oxide, lentinan and water, filtering centrifuge and divide
From obtaining blueberry extracting solution;
Molysite, phosphate, lithium salts, tartaric acid, polyaniline and glucose are mixed and its total weight 2.4- are added by step 2
3.8 times of deionized water is stirred 20-35 minutes under 40-48 degrees Celsius and 750-960rpm of rotating speed, is then taken the photograph in 60-65
It is stirred 45-60 minutes under the rotating speed of family name's degree and 1500-1800rpm, obtains the first mixture;
Step 3, it is 60-72 that ratio of grinding media to material, which is added, in vanadic anhydride, glycine, glucose and blueberry extracting solution:1 ball mill
In, ball milling product is added in ammonium hydroxide and supersonic oscillations are uniform, obtains the second mixture;
Step 4 stirs gelatine, the first mixture and the second mixture under 35-44 degrees Celsius and 180-270rpm of rotating speed
It mixes uniformly, pear tannin is added while stirring, continue stirring 30-50 minutes after being added completely into, obtain third mixture;
Third mixture is dried to obtain powder by step 5, and powder is sintered 8-12 under inert atmosphere and 360-480 degrees Celsius
Hour, then be warming up to 960-1050 degrees Celsius with the speed of 10-18 degrees celsius/minutes and be sintered 15-22 hours, natural cooling
The dizzy processing of plasma electric is carried out after to room temperature to get to finished product.
5. the preparation method of the anode material for lithium-ion batteries of good cycle according to claim 4, which is characterized in that
The power of supersonic oscillations is 180-220W in the step 3, and the frequency of supersonic oscillations is 30-40KHz.
6. the preparation method of the anode material for lithium-ion batteries of good cycle according to claim 4 or 5, feature exist
In the temperature of ball milling is 55-66 degrees Celsius in the step 3, and the speed of ball milling is 600-750rpm.
7. the preparation method of the anode material for lithium-ion batteries of good cycle according to claim 6, which is characterized in that
The environment of the plasma sided corona treatment is air environment.
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| CN116344776A (en) * | 2023-04-21 | 2023-06-27 | 湖北万润新能源科技股份有限公司 | Lithium iron phosphate-based composite positive electrode material and preparation method thereof |
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