CN103066276A - Preparation method of cobalt hydroxide-carbon composite cathode material of lithium ion battery - Google Patents
Preparation method of cobalt hydroxide-carbon composite cathode material of lithium ion battery Download PDFInfo
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Abstract
The invention provides a cobalt hydroxide-carbon composite cathode material of a lithium ion battery and a preparation method thereof. The method comprises weighing starch, concentrated sulfuric acid, water and a silica template, roasting to obtain porous carbon nanotube with hollow nanometer carbon tube inside; using the concentrated sulfuric acid for reflux, adding the above product into a glycol-water solution, adjusting a pH value by using cobalt oxalate, sodium bicarbonate and potassium borate, performing a hydrothermal reaction to obtain a cobalt hydroxide-porous carbon nanotube composite material; mixing the above product with acetylene black, carboxymethyl cellulose and water, and uniformly mixing by isopropanol to obtain the composite cathode material. The preparation method provided by the invention is relatively simple; and by uniformly distributing the cobalt hydroxide in and out of the porous carbon nanotube, the prepared cobalt hydroxide-porous carbon nanotube composite material is stable in structure and uniform in distribution, and thus has a high energy density and furthermore a stable cyclic performance; and when used as the cathode material of the lithium ion battery, is high in specific capacity and long in service life.
Description
Technical field
The present invention relates to a kind of preparation method of lithium ion battery, relate in particular to a kind of lithium ion battery cobalt hydroxide-carbon compound cathode materials and preparation method thereof.
Background technology
The trend of electronic apparatus miniaturization, energetic, portability, development and the exploitation of the development of space technology and the demand of defence equipment and electric automobile have higher requirement to the performance of lithium ion battery.
The improvement of performance of lithium ion battery depends primarily on the raising of embedding lithium electrode material energy density and cycle life, present commercial lithium ion battery mostly adopt lithium transition-metal oxide/graphite system as negative active core-shell material as lithium ion battery negative material, the theoretical specific capacity of CoO is about 2 times of graphitized carbon material up to 715mAh/g.
Although the CoO in the report has higher specific capacity, efficient and cycle performance are all relatively poor first for they.Cobalt hydroxide is used widely in Ni-MH battery, and its presoma as lithium ion battery electrode material also is widely studied and synthesizes, but all is oxide (CoO or the Co that it will be sintered into cobalt
3O
4), could use as lithium ion battery electrode material, employed process route complex steps, and power consumption is larger.
Summary of the invention
For overcoming the problems referred to above, the invention provides a kind of preparation method of lithium ion battery cobalt hydroxide-carbon compound cathode materials, when the anode material that uses the method to prepare is used for lithium ion battery, when having larger specific capacity, Stability Analysis of Structures, good cycle.
To achieve these goals, the preparation method of a kind of lithium ion battery cobalt hydroxide-carbon compound cathode materials provided by the invention comprises the steps:
Step 1, preparation porous carbon nanotube
According to weight ratio 1: (0.1-0.15): (1-10): (0.5-2) take by weighing starch, the concentrated sulfuric acid, water and template silicon dioxide, mix, mixture is dry, mixture is put into the pyroreaction still roasting of inert gas shielding, pyroreaction still heating rate is for per hour heating up 50-80 ℃, and temperature rises to 500-700 ℃, keeps 4-7 hour, remove template silicon dioxide, obtain the inner porous carbon nanotube of nano hollow carbon pipe that is;
Step 2, cobalt hydroxide-porous carbon nanometer tube composite materials
Above-mentioned porous carbon nanotube carbon is used concentrated sulfuric acid 60-80 ℃ of backflow 1-2 hour;
Then the porous carbon nanotube that 2-5 part was refluxed is added in the Glycol Mixture of 10-200 part, and the ethylene glycol in the Glycol Mixture and the volume ratio of water are 1: 10-1: 1, and then at room temperature ultrasonic dispersion is 3-6 hour; Then by weight, add 2-8 part cobalt oxalate, 0.5-1 part sodium acid carbonate and 0.2-0.5 part potassium borate, regulating the pH value is 10-13, stirs in the hot still of falling back sealing, and at 100-200 ℃ of lower hydro-thermal reaction 8-24 hour, obtain cobalt hydroxide-porous carbon nanometer tube composite materials;
Step 3, the preparation composite negative pole material
Described cobalt hydroxide-porous carbon nanometer tube composite materials, acetylene black, CMC (CMC) and water are mixed, wherein, the mixed proportion of described cobalt hydroxide-porous carbon nanometer tube composite materials, acetylene black, CMC and water is (10-20): (3-5): (2-3): (50-80), with isopropyl alcohol the described mixture that is mixed to get is mixed well, obtained composite negative pole material.
Wherein, stirred 3-6 hour before the mixture drying in the step 1.
Wherein, drying described in the step 1 is: heating rate is for per hour heating up 10-20 ℃, and temperature rises to 150-200 ℃, keeps 3-8 hour.
Wherein, in the step 1, the method for removing template silicon dioxide is: the mixture after the roasting is put into potassium hydroxide stirred 10-15 hour, make the silica template dissolving, then filter, wash, drying.
The present invention also provides a kind of lithium ion battery cobalt hydroxide-carbon compound cathode materials of said method preparation.
The cobalt hydroxide of the present invention's preparation-porous carbon nanometer tube composite materials, by cobalt hydroxide being evenly distributed on inside and outside the porous carbon nanotube, so that the Stability Analysis of Structures of composite material and being uniformly dispersed, therefore possessing outside the high energy density, also has stable cycle performance, during as lithium ion battery negative material, specific capacity is high, long service life.In addition, preparation method's technique of the present invention is relatively also comparatively simple.
Embodiment
Embodiment one
Preparation porous carbon nanotube
According to weight ratio 1: 0.15: 10: 2 took by weighing starch, the concentrated sulfuric acid and water and template silicon dioxide, uniform stirring is 6 hours after mixing, mixture is put into baking oven, the baking oven heating rate is for per hour heating up 20 ℃, temperature rises to 200 ℃, keeps 3 hours, after the solvent evaporation, mixture is put into the pyroreaction still roasting of inert gas shielding, pyroreaction still heating rate is for per hour heating up 80 ℃, and temperature rises to 700 ℃, keeps 4 hours, mixture after the roasting is put into potassium hydroxide to be stirred 15 hours, make the silica template dissolving, then filter, washing, drying obtains the inner porous carbon nanotube of nano hollow carbon pipe that is;
Cobalt hydroxide-porous carbon nanometer tube composite materials
Above-mentioned porous carbon nanotube carbon was refluxed 1 hour with 80 ℃ of the concentrated sulfuric acids; Then 5 parts of porous carbon nanotubes that refluxed are added in 200 parts the Glycol Mixture, ethylene glycol in the Glycol Mixture and the volume ratio of water are 1: 1, then at room temperature ultrasonic dispersion is 6 hours, then by weight, adds 8 parts of cobalt oxalates, 1 part of sodium acid carbonate and 0.5 part of potassium borate, regulating the pH value is 13, stirs in the hot still of falling back sealing, and after reacting 8 hours under 200 ℃, filter, wash, dry, obtain cobalt hydroxide-porous carbon nanometer tube composite materials.
The preparation composite negative pole material
Described cobalt hydroxide-porous carbon nanometer tube composite materials, acetylene black, CMC and water are mixed, wherein, the mixed proportion of described cobalt hydroxide-porous carbon nanometer tube composite materials, acetylene black, CMC and water can be 20: 5: 3: 80, with isopropyl alcohol the described mixture that is mixed to get is mixed well, obtained composite negative pole material.
Embodiment two
Preparation porous carbon nanotube
According to weight ratio 1: 0.1: 1: 0.5 took by weighing starch, the concentrated sulfuric acid and water and template silicon dioxide, uniform stirring is 3 hours after mixing, mixture is put into baking oven, the baking oven heating rate is for per hour heating up 10 ℃, temperature rises to 150 ℃, keeps 8 hours, after the solvent evaporation, mixture is put into the pyroreaction still roasting of inert gas shielding, pyroreaction still heating rate is for per hour heating up 50 ℃, and temperature rises to 500 ℃, keeps 7 hours, mixture after the roasting is put into potassium hydroxide to be stirred 10 hours, make the silica template dissolving, then filter, washing, drying obtains the inner porous carbon nanotube of nano hollow carbon pipe that is;
Cobalt hydroxide-porous carbon nanometer tube composite materials
Above-mentioned porous carbon nanotube carbon was refluxed 2 hours with 60 ℃ of the concentrated sulfuric acids; Then 2 parts of porous carbon nanotubes that refluxed are added in 10 parts the Glycol Mixture, ethylene glycol in the Glycol Mixture and the volume ratio of water are 1: 1, then at room temperature ultrasonic dispersion is 6 hours, then by weight, adds 2 parts of cobalt oxalates, 0.5 part sodium acid carbonate and 0.2 part of potassium borate, regulating the pH value is 10, stirs in the hot still of falling back sealing, and after reacting 8 hours under 100 ℃, filter, wash, dry, obtain cobalt hydroxide-porous carbon nanometer tube composite materials.
The preparation composite negative pole material
Described cobalt hydroxide-porous carbon nanometer tube composite materials, acetylene black, CMC and water are mixed, wherein, the mixed proportion of described cobalt hydroxide-porous carbon nanometer tube composite materials, acetylene black, CMC and water can be 10: 3: 2: 50, with isopropyl alcohol the described mixture that is mixed to get is mixed well, obtained composite negative pole material.
Comparative example
0.5 gram graphite oxide is dispersed in (volume ratio is 1: 10) in the 300ml isopropanol-water solution; stirred 6 hours under the room temperature; add 3.26 gram cabaltous nitrate hexahydrates; 15 milliliters of ammoniacal liquor; 0.08 gram sodium borohydride; stirring is fallen back in the hot still; sealing; and after reacting 5 hours under 120 degrees centigrade, filter, wash, dry; obtain graphite oxide-cobalt hydroxide composite material; with its under nitrogen protection 300 degrees centigrade processed 2 hours, obtain graphene nanometer sheet-cobaltous oxide composite negative electrode material.Described cobalt hydroxide-porous carbon nanometer tube composite materials, acetylene black, CMC and water are mixed, wherein, the mixed proportion of described cobalt hydroxide-porous carbon nanometer tube composite materials, acetylene black, CMC and water can be 10: 3: 2: 50, with isopropyl alcohol the described mixture that is mixed to get is mixed well, obtained composite negative pole material.
Take diameter as 18 millimeters, weight as the metal lithium sheet of 0.4 gram as positive active material, take the modified polypropene barrier film as barrier film, with the LiPF of 1 mol/L
6Solution (solvent is 1: 1 EC of volume ratio: the DMC mixed solvent) for electrolyte, respectively take 0.05 gram by above-described embodiment one, two and comparative example make product as negative material, be coated in equably and do negative pole on the copper mesh, make 2016 type button cells.Be to carry out electric performance test under 25 ℃ at probe temperature, after tested this embodiment one with two material compare with the material of comparative example, first discharge specific capacity has promoted more than the 35-45%, cycle life improves more than 2 times.
More than specific embodiments of the invention are described in detail, but it is just as example, the present invention is not restricted to specific embodiment described above.To those skilled in the art, any equivalent modifications that the present invention is carried out and substituting also all among category of the present invention.Therefore, not breaking away from impartial conversion and the modification of doing under the spirit and scope of the present invention, all should contain within the scope of the invention.
Claims (5)
1. the preparation method of a lithium ion battery cobalt hydroxide-carbon compound cathode materials is characterized in that, comprises the steps:
Step 1, preparation porous carbon nanotube
According to weight ratio 1: (0.1-0.15): (1-10): (0.5-2) take by weighing starch, the concentrated sulfuric acid, water and template silicon dioxide, mix, mixture is dry, mixture is put into the pyroreaction still roasting of inert gas shielding, pyroreaction still heating rate is for per hour heating up 50-80 ℃, and temperature rises to 500-700 ℃, keeps 4-7 hour, remove template silicon dioxide, obtain the inner porous carbon nanotube of nano hollow carbon pipe that is;
Step 2, cobalt hydroxide-porous carbon nanometer tube composite materials
Above-mentioned porous carbon nanotube carbon is used concentrated sulfuric acid 60-80 ℃ of backflow 1-2 hour;
Then the porous carbon nanotube that 2-5 part was refluxed is added in the Glycol Mixture of 10-200 part, and the ethylene glycol in the Glycol Mixture and the volume ratio of water are 1: 10-1: 1, and then at room temperature ultrasonic dispersion is 3-6 hour; Then by weight, add 2-8 part cobalt oxalate, 0.5-1 part sodium acid carbonate and 0.2-0.5 part potassium borate, regulating the pH value is 10-13, stirs in the hot still of falling back sealing, and at 100-200 ℃ of lower hydro-thermal reaction 8-24 hour, obtain cobalt hydroxide-porous carbon nanometer tube composite materials;
Step 3, the preparation composite negative pole material
Described cobalt hydroxide-porous carbon nanometer tube composite materials, acetylene black, CMC and water are mixed, wherein, the mixed proportion of described cobalt hydroxide-porous carbon nanometer tube composite materials, acetylene black, CMC and water is (10-20): (3-5): (2-3): (50-80), with isopropyl alcohol the described mixture that is mixed to get is mixed well, obtained composite negative pole material.
2. method according to claim 1 is characterized in that, stirs 3-6 hour before the mixture drying in the step 1.
3. method according to claim 1 and 2 is characterized in that, drying described in the step 1 is: heating rate is for per hour heating up 10-20 ℃, and temperature rises to 150-200 ℃, keeps 3-8 hour.
4. method according to claim 1 is characterized in that, in the step 1, the method for removing template silicon dioxide is: the mixture after the roasting is put into potassium hydroxide stirred 10-15 hour, make the silica template dissolving, then filter, wash, drying.
5. lithium ion battery cobalt hydroxide-carbon compound cathode materials of method preparation as claimed in claim 1.
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Cited By (7)
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| CN106129425A (en) * | 2016-09-21 | 2016-11-16 | 许昌学院 | A kind of porous carbon electrode material and its preparation method and application |
| CN106206060A (en) * | 2016-09-25 | 2016-12-07 | 桂林理工大学 | The preparation of cobalt hydroxide@carbon fiber nanometer composite material and electrode material for super capacitor application |
| CN109411732A (en) * | 2018-11-05 | 2019-03-01 | 桑顿新能源科技有限公司 | A kind of preparation method of the nucleocapsid cladding compound lithium sulfur battery anode material of sulphur-carbon nanotube |
| CN111200119A (en) * | 2018-11-19 | 2020-05-26 | 河南科技学院 | SiO (silicon dioxide)2/CoO/graphene composite negative electrode material and preparation method thereof |
| CN113663672A (en) * | 2020-05-15 | 2021-11-19 | 香港城市大学深圳研究院 | Cobaltous oxide photocatalytic material with high photoelectric catalytic activity and preparation method thereof |
| CN114272945A (en) * | 2020-10-13 | 2022-04-05 | 天津大学 | Cobalt hydroxide grown by metal organic framework derived carbon and preparation method thereof |
| CN116354351A (en) * | 2023-03-21 | 2023-06-30 | 中国丝绸博物馆 | Preparation method and application of energy-saving micro-environment humidity automatic regulating material |
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Cited By (10)
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| CN106129425A (en) * | 2016-09-21 | 2016-11-16 | 许昌学院 | A kind of porous carbon electrode material and its preparation method and application |
| CN106206060A (en) * | 2016-09-25 | 2016-12-07 | 桂林理工大学 | The preparation of cobalt hydroxide@carbon fiber nanometer composite material and electrode material for super capacitor application |
| CN109411732A (en) * | 2018-11-05 | 2019-03-01 | 桑顿新能源科技有限公司 | A kind of preparation method of the nucleocapsid cladding compound lithium sulfur battery anode material of sulphur-carbon nanotube |
| CN111200119A (en) * | 2018-11-19 | 2020-05-26 | 河南科技学院 | SiO (silicon dioxide)2/CoO/graphene composite negative electrode material and preparation method thereof |
| CN113663672A (en) * | 2020-05-15 | 2021-11-19 | 香港城市大学深圳研究院 | Cobaltous oxide photocatalytic material with high photoelectric catalytic activity and preparation method thereof |
| CN113663672B (en) * | 2020-05-15 | 2023-08-15 | 香港城市大学深圳研究院 | Cobalt oxide photocatalytic material with high photoelectrocatalytic activity and preparation method thereof |
| CN114272945A (en) * | 2020-10-13 | 2022-04-05 | 天津大学 | Cobalt hydroxide grown by metal organic framework derived carbon and preparation method thereof |
| CN114272945B (en) * | 2020-10-13 | 2023-07-18 | 天津大学 | Metal organic framework derived carbon grown cobalt hydroxide and preparation method thereof |
| CN116354351A (en) * | 2023-03-21 | 2023-06-30 | 中国丝绸博物馆 | Preparation method and application of energy-saving micro-environment humidity automatic regulating material |
| CN116354351B (en) * | 2023-03-21 | 2023-10-27 | 中国丝绸博物馆 | Preparation method and application of energy-saving micro-environment humidity automatic regulating material |
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