CN109860601A - A kind of preparation method of the composite modified anode material of lithium battery of graphene/carbon nano-tube - Google Patents
A kind of preparation method of the composite modified anode material of lithium battery of graphene/carbon nano-tube Download PDFInfo
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Abstract
The present invention provides a kind of preparation method of composite modified anode material of lithium battery of graphene/carbon nano-tube, includes the following steps: the preparation of (1) graphene oxide；(2) preparation of graphene oxide suspension；(3) graphene oxide/carbon nano tube dispersion liquid preparation；(4) preparation of graphene/carbon nano-tube dispersion liquid；(5) preparation of aqueous solution；(6) preparation of mixed solution；(7) mixed solution for obtaining step 6 is added in water heating kettle, heating, then mixture is placed in drying box, it is dry, the mixture after drying is placed in tube furnace 350-600 DEG C of pre-burning 4-8h in a hydrogen atmosphere, then mixture is ground, finally 9-12h is sintered at 750-1000 DEG C, then cooling, grinding obtains the composite modified anode material of lithium battery of graphene, carbon nanotube.The present invention can effectively improve the height ratio capacity, high-rate discharge ability and cycle performance of active material.
Description
Technical field
The present invention relates to a kind of lithium battery materials, and in particular to a kind of composite modified lithium battery of graphene/carbon nano-tube is just
The preparation method of pole material.
Background technique
With the development of society, people are higher and higher to the performance requirement of lithium ion battery.Particularly with lithium ion power
Battery, it is desirable that cruising ability is strong, charge-discharge electric power is big, good cycle etc..Core key of the positive electrode as power battery
Material occupies 25% of battery manufacturing cost or more, and performance directly affects energy density, circulating density, the circulation of battery
The main performances such as service life, safety, in occupation of core status in lithium ion battery.But most of positive-active at present
Material is still difficult to meet the requirements due to the limitation of self structure, is that develop high-energy density, high circulation service life, high power forthright
The Pinch technology of energy, fast charging and discharging lithium ion battery.Therefore how to improve the electric conductivity of lithium electricity positive electrode, shorten Li+ and
The transmission path of electronics accelerates the transmission speed of Li+ and electronics, improves positive electrode and then meet the lithium electricity market demand having become
Research hotspot.
The representative of carbon nanotube and graphene as novel c-based nanomaterial has excellent electronic conduction characteristic, can
Effectively improve the height ratio capacity, high-rate discharge ability and cycle performance of active material.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation sides of the composite modified anode material of lithium battery of graphene/carbon nano-tube
Method can effectively improve the height ratio capacity, high-rate discharge ability and cycle performance of active material.
The technical solution adopted by the present invention to solve the technical problems is: a kind of composite modified lithium of graphene/carbon nano-tube
The preparation method of cell positive material, includes the following steps:
(1) preparation of graphene oxide: flaky graphite is added in the mixture of sodium nitrate and the concentrated sulfuric acid, in ice bath
Under the conditions of uniform magnetic agitation；Potassium permanganate is slowly added in mixed solution, control mixed solution temperature is lower than 20 DEG C and magnetic
Power stirs 1-3h, and it is 35-45 DEG C and magnetic agitation 1-2h that mixed solution temperature is then controlled under condition of ice bath；It is molten to mixing again
It is 70 DEG C of deionized waters that temperature is added in liquid, obtains bright orange color contamination liquid after being eventually adding the hydrogen peroxide that mass fraction concentration is 30%
Solution obtains graphene oxide after being 6-7 with deionized water centrifuge washing to pH；
(2) graphene oxide for obtaining step 1 is added in deionized water, and ultrasonic disperse 1-3h obtains graphene oxide
Suspension；
(3) carbon nanotube is added into the graphene oxide suspension that step 2 obtains, ultrasonic disperse 3-4h is aoxidized
Graphene/carbon nano-tube dispersion liquid；
(4) ethylenediamine is added into graphene oxide/carbon nano tube dispersion liquid that step 3 obtains, stirs 20-30min,
6-24h is sealed at 80-180 DEG C, obtains graphene/carbon nano-tube dispersion liquid；
(5) vanadic anhydride, oxalic acid are added in the graphene/carbon nano-tube dispersion liquid that step 4 obtains, at 20-90 DEG C
Stable aqueous solution is formed by 10-180min；
(6) phosphoric acid, lithium carbonate, ammonium dihydrogen phosphate are added into the aqueous solution that step 5 obtains, is mixed after being sufficiently mixed
Solution；
(7) mixed solution for obtaining step 6 is added in water heating kettle, and 8-12h is heated at 180-240 DEG C, will then be mixed
It closes object and is placed in drying box at 70-100 DEG C dry 40-50h, the mixture after drying is placed in tube furnace in hydrogen atmosphere
Lower 350-600 DEG C of pre-burning 4-8h, then grinds mixture, is finally sintered 9-12h at 750-1000 DEG C, then cold
But, it grinds, obtains the composite modified anode material of lithium battery of graphene, carbon nanotube.
Preferably, in step 1, flaky graphite, sodium nitrate, the concentrated sulfuric acid, potassium permanganate, 70 DEG C of deionized waters, quality point
The mass ratio for the hydrogen peroxide that Particle density is 30% is 1-5:3-6:100-180:1-4:150-200:1-4.
Preferably, in step 2, graphene oxide, deionized water mass ratio be 2-5:80-120.
Preferably, in step 3, the mass ratio that carbon nanotube is added in graphene oxide suspension is 100-120:2-6.
Preferably, in step 4, graphene oxide/carbon nano tube dispersion liquid, ethylenediamine mass ratio be 100-140:1-5.
Preferably, in step 5, graphene/carbon nano-tube dispersion liquid, vanadic anhydride, oxalic acid mass ratio be 130-
160:1-3:1-5。
Preferably, in step 6, aqueous solution, phosphoric acid, lithium carbonate, ammonium dihydrogen phosphate mass ratio be 150-200:2-6:1-
4:1-5。
The invention has the following advantages: the composite modified lithium battery anode of a kind of graphene/carbon nano-tube of the invention
The representative of the preparation method of material, carbon nanotube and graphene as novel c-based nanomaterial has excellent electronic conduction
Characteristic can effectively improve the height ratio capacity, high-rate discharge ability and cycle performance of active material；Vanadic anhydride is being formed
Valence state is just reduced when solution, reduces the pollution to environment.
Specific embodiment
Embodiment 1
A kind of preparation method of the composite modified anode material of lithium battery of graphene/carbon nano-tube, includes the following steps:
(1) preparation of graphene oxide: flaky graphite is added in the mixture of sodium nitrate and the concentrated sulfuric acid, in ice bath
Under the conditions of uniform magnetic agitation；Potassium permanganate is slowly added in mixed solution, control mixed solution temperature is lower than 20 DEG C and magnetic
Power stirs 1-3h, and it is 35-45 DEG C and magnetic agitation 1-2h that mixed solution temperature is then controlled under condition of ice bath；It is molten to mixing again
It is 70 DEG C of deionized waters that temperature is added in liquid, obtains bright orange color contamination liquid after being eventually adding the hydrogen peroxide that mass fraction concentration is 30%
Solution obtains graphene oxide after being 6-7 with deionized water centrifuge washing to pH；Flaky graphite, sodium nitrate, the concentrated sulfuric acid, height
The mass ratio for the hydrogen peroxide that potassium manganate, 70 DEG C of deionized waters, mass fraction concentration are 30% is 1:3:100:1:150:1；
(2) graphene oxide for obtaining step 1 is added in deionized water, ultrasonic disperse 1h, and it is outstanding to obtain graphene oxide
Supernatant liquid；Graphene oxide, deionized water mass ratio be 2:80；
(3) carbon nanotube is added into the graphene oxide suspension that step 2 obtains, ultrasonic disperse 3h obtains oxidation stone
Black alkene/carbon nano tube dispersion liquid；The mass ratio that carbon nanotube is added in graphene oxide suspension is 100:2；
(4) ethylenediamine is added into graphene oxide/carbon nano tube dispersion liquid that step 3 obtains, 20min is stirred, 80
6h is sealed at DEG C, obtains graphene/carbon nano-tube dispersion liquid；The mass ratio of graphene oxide/carbon nano tube dispersion liquid, ethylenediamine
For 100:1；
(5) vanadic anhydride, oxalic acid are added in the graphene/carbon nano-tube dispersion liquid that step 4 obtains, passes through at 20 DEG C
10min forms stable aqueous solution；Graphene/carbon nano-tube dispersion liquid, vanadic anhydride, oxalic acid mass ratio be 130:1:1；
(6) phosphoric acid, lithium carbonate, ammonium dihydrogen phosphate are added into the aqueous solution that step 5 obtains, is mixed after being sufficiently mixed
Solution；Aqueous solution, phosphoric acid, lithium carbonate, ammonium dihydrogen phosphate mass ratio be 150:2:1:1；
(7) the then mixed solution for obtaining step 6 is added in water heating kettle, 8h is heated at 180 DEG C, then by mixture
It is placed in drying box at 70 DEG C dry 40h, the mixture after drying is placed in tube furnace 350 DEG C of pre-burnings in a hydrogen atmosphere
Then 4h grinds mixture, be finally sintered 9h at 750 DEG C, then cooling, and grinding obtains graphene, carbon nanotube
Composite modified anode material of lithium battery.
Embodiment 2
A kind of preparation method of the composite modified anode material of lithium battery of graphene/carbon nano-tube, includes the following steps:
(1) preparation of graphene oxide: flaky graphite is added in the mixture of sodium nitrate and the concentrated sulfuric acid, in ice bath
Under the conditions of uniform magnetic agitation；Potassium permanganate is slowly added in mixed solution, control mixed solution temperature is lower than 20 DEG C and magnetic
Power stirs 1-3h, and it is 35-45 DEG C and magnetic agitation 1-2h that mixed solution temperature is then controlled under condition of ice bath；It is molten to mixing again
It is 70 DEG C of deionized waters that temperature is added in liquid, obtains bright orange color contamination liquid after being eventually adding the hydrogen peroxide that mass fraction concentration is 30%
Solution obtains graphene oxide after being 6-7 with deionized water centrifuge washing to pH；Flaky graphite, sodium nitrate, the concentrated sulfuric acid, height
The mass ratio for the hydrogen peroxide that potassium manganate, 70 DEG C of deionized waters, mass fraction concentration are 30% is 5:6:180:4:200:4；
(2) graphene oxide for obtaining step 1 is added in deionized water, ultrasonic disperse 3h, and it is outstanding to obtain graphene oxide
Supernatant liquid；Graphene oxide, deionized water mass ratio be 5:120；
(3) carbon nanotube is added into the graphene oxide suspension that step 2 obtains, ultrasonic disperse 4h obtains oxidation stone
Black alkene/carbon nano tube dispersion liquid；The mass ratio that carbon nanotube is added in graphene oxide suspension is 120:6；
(4) ethylenediamine is added into graphene oxide/carbon nano tube dispersion liquid that step 3 obtains, 30min is stirred, 180
It is sealed at DEG C for 24 hours, obtains graphene/carbon nano-tube dispersion liquid；The quality of graphene oxide/carbon nano tube dispersion liquid, ethylenediamine
Than for 140:5；
(5) vanadic anhydride, oxalic acid are added in the graphene/carbon nano-tube dispersion liquid that step 4 obtains, passes through at 90 DEG C
180min forms stable aqueous solution；Graphene/carbon nano-tube dispersion liquid, vanadic anhydride, oxalic acid mass ratio be 160:3:
5；
(6) phosphoric acid, lithium carbonate, ammonium dihydrogen phosphate are added into the aqueous solution that step 5 obtains, is mixed after being sufficiently mixed
Solution；Aqueous solution, phosphoric acid, lithium carbonate, ammonium dihydrogen phosphate mass ratio be 200:6:4:5.
(7) mixed solution for obtaining step 6 is added in water heating kettle, and 12h is heated at 240 DEG C, then sets mixture
50h is dried at 100 DEG C in drying box, the mixture after drying is placed in tube furnace 600 DEG C of pre-burnings in a hydrogen atmosphere
Then 8h grinds mixture, be finally sintered 12h at 1000 DEG C, then cooling, and grinding obtains graphene, carbon nanometer
Manage composite modified anode material of lithium battery；
Embodiment 3
A kind of preparation method of the composite modified anode material of lithium battery of graphene/carbon nano-tube, includes the following steps:
(1) preparation of graphene oxide: flaky graphite is added in the mixture of sodium nitrate and the concentrated sulfuric acid, in ice bath
Under the conditions of uniform magnetic agitation；Potassium permanganate is slowly added in mixed solution, control mixed solution temperature is lower than 20 DEG C and magnetic
Power stirs 1-3h, and it is 35-45 DEG C and magnetic agitation 1-2h that mixed solution temperature is then controlled under condition of ice bath；It is molten to mixing again
It is 70 DEG C of deionized waters that temperature is added in liquid, obtains bright orange color contamination liquid after being eventually adding the hydrogen peroxide that mass fraction concentration is 30%
Solution obtains graphene oxide after being 6-7 with deionized water centrifuge washing to pH；Flaky graphite, sodium nitrate, the concentrated sulfuric acid, height
The mass ratio for the hydrogen peroxide that potassium manganate, 70 DEG C of deionized waters, mass fraction concentration are 30% is 2:4:140:2:175:2；
(2) graphene oxide for obtaining step 1 is added in deionized water, ultrasonic disperse 2h, and it is outstanding to obtain graphene oxide
Supernatant liquid；Graphene oxide, deionized water mass ratio be 3:95；
(3) carbon nanotube is added into the graphene oxide suspension that step 2 obtains, ultrasonic disperse 3h obtains oxidation stone
Black alkene/carbon nano tube dispersion liquid；The mass ratio that carbon nanotube is added in graphene oxide suspension is 107:3；
(4) ethylenediamine is added into graphene oxide/carbon nano tube dispersion liquid that step 3 obtains, 24min is stirred, 110
12h is sealed at DEG C, obtains graphene/carbon nano-tube dispersion liquid；The quality of graphene oxide/carbon nano tube dispersion liquid, ethylenediamine
Than for 120:3；
(5) vanadic anhydride, oxalic acid are added in the graphene/carbon nano-tube dispersion liquid that step 4 obtains, passes through at 40 DEG C
40min forms stable aqueous solution；Graphene/carbon nano-tube dispersion liquid, vanadic anhydride, oxalic acid mass ratio be 140:2:3；
(6) phosphoric acid, lithium carbonate, ammonium dihydrogen phosphate are added into the aqueous solution that step 5 obtains, is mixed after being sufficiently mixed
Solution；Aqueous solution, phosphoric acid, lithium carbonate, ammonium dihydrogen phosphate mass ratio be 170:3:2:3；
(7) mixed solution for obtaining step 6 is added in water heating kettle, and 10h is heated at 200 DEG C, then sets mixture
44h is dried at 82 DEG C in drying box, the mixture after drying is placed in tube furnace 420 DEG C of pre-burnings in a hydrogen atmosphere
Then 5h grinds mixture, be finally sintered 10h at 900 DEG C, then cooling, and grinding obtains graphene, carbon nanometer
Manage composite modified anode material of lithium battery.
Embodiment 4
A kind of preparation method of the composite modified anode material of lithium battery of graphene/carbon nano-tube, includes the following steps:
(1) preparation of graphene oxide: flaky graphite is added in the mixture of sodium nitrate and the concentrated sulfuric acid, in ice bath
Under the conditions of uniform magnetic agitation；Potassium permanganate is slowly added in mixed solution, control mixed solution temperature is lower than 20 DEG C and magnetic
Power stirs 1-3h, and it is 35-45 DEG C and magnetic agitation 1-2h that mixed solution temperature is then controlled under condition of ice bath；It is molten to mixing again
It is 70 DEG C of deionized waters that temperature is added in liquid, obtains bright orange color contamination liquid after being eventually adding the hydrogen peroxide that mass fraction concentration is 30%
Solution obtains graphene oxide after being 6-7 with deionized water centrifuge washing to pH；Flaky graphite, sodium nitrate, the concentrated sulfuric acid, height
The mass ratio for the hydrogen peroxide that potassium manganate, 70 DEG C of deionized waters, mass fraction concentration are 30% is 4:5:160:3:180:3；
(2) graphene oxide for obtaining step 1 is added in deionized water, ultrasonic disperse 2h, and it is outstanding to obtain graphene oxide
Supernatant liquid；Graphene oxide, deionized water mass ratio be 4:100；
(3) carbon nanotube is added into the graphene oxide suspension that step 2 obtains, ultrasonic disperse 4h obtains oxidation stone
Black alkene/carbon nano tube dispersion liquid；The mass ratio that carbon nanotube is added in graphene oxide suspension is 114:5；
(4) ethylenediamine is added into graphene oxide/carbon nano tube dispersion liquid that step 3 obtains, 27min is stirred, 160
20h is sealed at DEG C, obtains graphene/carbon nano-tube dispersion liquid；The quality of graphene oxide/carbon nano tube dispersion liquid, ethylenediamine
Than for 130:4；
(5) vanadic anhydride, oxalic acid are added in the graphene/carbon nano-tube dispersion liquid that step 4 obtains, passes through at 75 DEG C
170min forms stable aqueous solution；Graphene/carbon nano-tube dispersion liquid, vanadic anhydride, oxalic acid mass ratio be 155:2:
4；
(6) phosphoric acid, lithium carbonate, ammonium dihydrogen phosphate are added into the aqueous solution that step 5 obtains, is mixed after being sufficiently mixed
Solution；Aqueous solution, phosphoric acid, lithium carbonate, ammonium dihydrogen phosphate mass ratio be 185:5:3:4；
(7) mixed solution for obtaining step 6 is added in water heating kettle, and 11h is heated at 230 DEG C, then sets mixture
47h is dried at 90 DEG C in drying box, the mixture after drying is placed in tube furnace 550 DEG C of pre-burnings in a hydrogen atmosphere
Then 7h grinds mixture, be finally sintered 11h at 900 DEG C, then cooling, and grinding obtains graphene, carbon nanometer
Manage composite modified anode material of lithium battery.
Claims (7)
1. a kind of preparation method of the composite modified anode material of lithium battery of graphene/carbon nano-tube, which is characterized in that including as follows
Step:
(1) preparation of graphene oxide: flaky graphite is added in the mixture of sodium nitrate and the concentrated sulfuric acid, in condition of ice bath
Uniform magnetic agitation down；Potassium permanganate is slowly added in mixed solution, control mixed solution temperature is lower than 20 DEG C and magnetic force stirs
1-3h is mixed, it is 35-45 DEG C and magnetic agitation 1-2h that mixed solution temperature is then controlled under condition of ice bath；Again into mixed solution
Addition temperature is 70 DEG C of deionized waters, and it is molten to obtain bright orange color contamination liquid after 30% hydrogen peroxide to be eventually adding mass fraction concentration
Liquid obtains graphene oxide after being 6-7 with deionized water centrifuge washing to pH；
(2) graphene oxide for obtaining step 1 is added in deionized water, ultrasonic disperse 1-3h, obtains graphene oxide suspension
Liquid；
(3) carbon nanotube is added into the graphene oxide suspension that step 2 obtains, ultrasonic disperse 3-4h obtains graphite oxide
Alkene/carbon nano tube dispersion liquid；
(4) ethylenediamine is added into graphene oxide/carbon nano tube dispersion liquid that step 3 obtains, 20-30min is stirred, in 80-
6-24h is sealed at 180 DEG C, obtains graphene/carbon nano-tube dispersion liquid；
(5) vanadic anhydride, oxalic acid are added in the graphene/carbon nano-tube dispersion liquid that step 4 obtains, passes through at 20-90 DEG C
10-180min forms stable aqueous solution；
(6) phosphoric acid, lithium carbonate, ammonium dihydrogen phosphate are added into the aqueous solution that step 5 obtains, obtains mixing after being sufficiently mixed molten
Liquid；
(7) mixed solution for obtaining step 6 is added in water heating kettle, 8-12h is heated at 180-240 DEG C, then by mixture
It is placed in drying box at 70-100 DEG C dry 40-50h, the mixture after drying is placed in tube furnace in a hydrogen atmosphere
350-600 DEG C of pre-burning 4-8h, then grinds mixture, is finally sintered 9-12h at 750-1000 DEG C, then cooling,
Grinding, obtains the composite modified anode material of lithium battery of graphene, carbon nanotube.
2. a kind of preparation method of the composite modified anode material of lithium battery of graphene/carbon nano-tube according to claim 1,
It is characterized in that, flaky graphite, sodium nitrate, the concentrated sulfuric acid, potassium permanganate, 70 DEG C of deionized waters, mass fractions are dense in step 1
Degree is 1-5:3-6:100-180:1-4:150-200:1-4 for the mass ratio of 30% hydrogen peroxide.
3. a kind of preparation method of the composite modified anode material of lithium battery of graphene/carbon nano-tube according to claim 1,
It is characterized in that, in step 2, graphene oxide, deionized water mass ratio be 2-5:80-120.
4. a kind of preparation method of the composite modified anode material of lithium battery of graphene/carbon nano-tube according to claim 1,
It is characterized in that, the mass ratio that carbon nanotube is added in graphene oxide suspension is 100-120:2-6 in step 3.
5. a kind of preparation method of the composite modified anode material of lithium battery of graphene/carbon nano-tube according to claim 1,
It is characterized in that, in step 4, graphene oxide/carbon nano tube dispersion liquid, ethylenediamine mass ratio be 100-140:1-5.
6. a kind of preparation method of the composite modified anode material of lithium battery of graphene/carbon nano-tube according to claim 1,
It is characterized in that, in step 5, graphene/carbon nano-tube dispersion liquid, vanadic anhydride, oxalic acid mass ratio be 130-160:1-
3:1-5。
7. a kind of preparation method of the composite modified anode material of lithium battery of graphene/carbon nano-tube according to claim 1,
It is characterized in that, in step 6, aqueous solution, phosphoric acid, lithium carbonate, ammonium dihydrogen phosphate mass ratio be 150-200:2-6:1-4:1-
5。
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| CN112054205A (en) * | 2020-09-28 | 2020-12-08 | 成都玉龙化工有限公司 | Conductive additive and preparation method thereof |
| CN115255355A (en) * | 2022-07-22 | 2022-11-01 | 株洲托普硬质合金材料有限公司 | Preparation method of high-wear-resistance thermal spraying powder |
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