CN112645322A - Carbon soaking method for super capacitor - Google Patents
Carbon soaking method for super capacitor Download PDFInfo
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- CN112645322A CN112645322A CN202011378102.9A CN202011378102A CN112645322A CN 112645322 A CN112645322 A CN 112645322A CN 202011378102 A CN202011378102 A CN 202011378102A CN 112645322 A CN112645322 A CN 112645322A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 239000003990 capacitor Substances 0.000 title claims abstract description 31
- 238000002791 soaking Methods 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 26
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 13
- 239000000243 solution Substances 0.000 claims abstract description 22
- 238000003763 carbonization Methods 0.000 claims abstract description 19
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 18
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims abstract description 18
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002243 precursor Substances 0.000 claims abstract description 16
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 239000011259 mixed solution Substances 0.000 claims abstract description 11
- 239000007787 solid Substances 0.000 claims abstract description 11
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 9
- 229960000583 acetic acid Drugs 0.000 claims abstract description 6
- 239000000654 additive Substances 0.000 claims abstract description 6
- 230000000996 additive effect Effects 0.000 claims abstract description 6
- 150000001721 carbon Chemical class 0.000 claims abstract description 6
- 239000011248 coating agent Substances 0.000 claims abstract description 6
- 238000000576 coating method Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 6
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 6
- 238000010992 reflux Methods 0.000 claims abstract description 6
- 239000012528 membrane Substances 0.000 claims description 32
- 238000001035 drying Methods 0.000 claims description 30
- 239000000463 material Substances 0.000 claims description 17
- 238000005266 casting Methods 0.000 claims description 10
- 239000012153 distilled water Substances 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- -1 nitric acid modified carbon Chemical class 0.000 claims description 5
- 238000005470 impregnation Methods 0.000 claims 1
- 238000004146 energy storage Methods 0.000 abstract description 6
- 239000003792 electrolyte Substances 0.000 description 3
- 230000008595 infiltration Effects 0.000 description 3
- 238000001764 infiltration Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 230000004913 activation Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/354—After-treatment
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/354—After-treatment
- C01B32/372—Coating; Grafting; Microencapsulation
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/44—Raw materials therefor, e.g. resins or coal
-
- 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
- Y02E60/13—Energy storage using capacitors
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Power Engineering (AREA)
- Inorganic Chemistry (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to a super-capacitor carbon soaking method, which comprises the following specific steps: 1) preparing activated carbon: adding 9-10 parts of acrylonitrile, 10-15 parts of dimethylformamide and 0.5-1 part of azobisisobutyro into a container, and stirring for 4-6 hours at the temperature of 60-75 ℃ in a water bath; secondly, extracting the mixed solution obtained in the first step by using ethanol to obtain acrylonitrile solid; thirdly, using 10 wt% of PAN and 0.3 wt% of additive to stir for 2h at the temperature of 65 ℃ water bath by controlling the concentration of PAN; and fourthly, performing heat treatment on the prepared precursor film in a muffle furnace. 2) Putting the porous activated carbon in the step 1) to the concentration65-70% of HNO3Cooling and refluxing; 3) preparing 3-5 parts of modified carbon obtained in the step 2), 30-50 parts of glacial acetic acid and 4-7 parts of potassium iodide into a soaking solution by using a polymerization carbonization method; 4) and uniformly coating the soaking solution on the outer side of the super capacitor. The super-capacitor carbon soaking method is simple and can change the dynamics of the electrode in the energy storage process.
Description
Technical Field
The invention relates to a super capacitor, in particular to a super capacitor carbon soaking method.
Background
Super capacitors are electrochemical elements developed from the seventh and eighties of the last century that store energy through polarized electrolytes. It is different from traditional chemical power source, and is a power source with special performance between traditional capacitor and battery, and mainly depends on electric double layer and redox pseudo-capacitor charge to store electric energy. But no chemical reaction occurs in the process of energy storage, and the energy storage process is reversible, and the super capacitor can be repeatedly charged and discharged for tens of thousands of times. The basic principle of the method is the same as that of other kinds of double-layer capacitors, and the extra-large capacity is obtained by using an electric double-layer structure consisting of an activated carbon porous electrode and an electrolyte. The super capacitor needs to be activated by activated carbon in the preparation process, but the current activation property does not meet the requirement.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a super-capacitor carbon infiltration method which is simple, can change the dynamics of an electrode in the energy storage process and has a good infiltration effect.
In order to solve the technical problem, the technical scheme of the invention is a super-capacitor carbon soaking method, which comprises the following specific steps:
1)
preparing activated carbon: adding 9-10 parts of acrylonitrile, 10-15 parts of dimethylformamide and 0.5-1 part of azobisisobutyro into a container, and stirring for 4-6 hours at the temperature of 60-75 ℃ in a water bath to obtain a mixed solution;
secondly, extracting the mixed solution obtained in the first step by using ethanol to obtain acrylonitrile solid, and then drying the acrylonitrile solid by hot air at the temperature of 60-80 ℃;
thirdly, using 10 wt% of PAN, controlling the concentration of PAN to change the dosage of the additive to be 0.3 wt% and stirring for 2 hours at the water bath temperature of 65 ℃ to obtain uniform membrane casting solution, removing bubbles from the obtained membrane casting solution, preparing a membrane forming material by using a spin coater, soaking the prepared membrane material in distilled water for 20-24 hours, then placing the membrane forming material in a drying box, and drying at the temperature of 45-55 ℃ to prepare a precursor membrane;
fourthly, the prepared precursor film is subjected to heat treatment in a muffle furnace, and then the precursor film after the heat treatment is subjected to carbonization treatment in a vacuum furnace, wherein the carbonization treatment temperature is 65-70 ℃ and the time is 1.5-2.5 hours, so that the porous activated carbon is obtained;
2) putting the porous activated carbon in the step 1) into 65-70% HNO3Cooling and refluxing for 10-12 hours, adjusting the pH value of the obtained activated carbon to be neutral, and then drying to obtain nitric acid modified carbon;
3) preparing 3-5 parts of modified carbon obtained in the step 2), 30-50 parts of glacial acetic acid and 4-7 parts of potassium iodide into a soaking solution by using a polymerization carbonization method;
4) uniformly coating the soaking solution on the outer side of the super capacitor, and then putting the super capacitor into an oven for drying at the temperature of 45-55 ℃.
In the third step, the drying temperature of the membrane material is 45-50 ℃.
After the technical scheme is adopted, the method is simple, the dynamics of the electrode in the energy storage process can be changed, the infiltration effect is good, the effective utilization rate of the specific surface in the energy storage process is improved, and the influence that the electrolyte cannot enter the pore channel structure due to the capillary condensation phenomenon and the surface tension is reduced. Thereby obviously improving the performance of the super capacitor of the carbon electrode material.
Detailed Description
Example one
A super-capacitor carbon soaking method comprises the following specific steps:
1)
preparing activated carbon: adding 9 parts of acrylonitrile, 10 parts of dimethylformamide and 0.5 part of azobisisobutyro into a container, and stirring for 4 hours under the condition of a water bath at 60 ℃ to obtain a mixed solution;
secondly, extracting the mixed solution obtained in the first step by using ethanol to obtain an acrylonitrile solid, and then drying the acrylonitrile solid by hot air at 60 ℃;
thirdly, using 10 wt% of PAN, controlling the concentration of PAN to change the dosage of the additive to be 0.3 wt% and stirring for 2 hours at the water bath temperature of 65 ℃ to obtain uniform membrane casting solution, removing bubbles from the obtained membrane casting solution, preparing a membrane forming material by using a spin coater, soaking the prepared membrane material in distilled water for 20 hours, then placing the membrane forming material in a drying box, and drying at the temperature of 45 ℃ to prepare a precursor membrane;
fourthly, the prepared precursor film is subjected to heat treatment in a muffle furnace, and then the precursor film after the heat treatment is subjected to carbonization treatment in a vacuum furnace, wherein the carbonization treatment temperature is 650 ℃ and the carbonization treatment time is 1.5 hours, so that porous activated carbon is obtained;
2) putting the porous activated carbon in the step 1) into 65 percent of HNO3Cooling and refluxing for 10 hours, adjusting the pH value of the obtained activated carbon to be neutral, and then drying to obtain nitric acid modified carbon;
3) preparing 3 parts of modified carbon obtained in the step 2), 30 parts of glacial acetic acid and 4 parts of potassium iodide into a soaking solution by using a polymerization carbonization method;
4) and uniformly coating the soaking solution on the outer side of the super capacitor, and then putting the super capacitor into an oven for drying, wherein the drying temperature is 45 ℃.
Example two
A super-capacitor carbon soaking method comprises the following specific steps:
1)
preparing activated carbon: adding 10 parts of acrylonitrile, 15 parts of dimethylformamide and 1 part of azobisisobutyro into a container, and stirring for 6 hours at 75 ℃ in a water bath to obtain a mixed solution;
secondly, extracting the mixed solution obtained in the first step by using ethanol to obtain an acrylonitrile solid, and then drying the acrylonitrile solid by using hot air at the temperature of 80 ℃;
thirdly, using 10 wt% of PAN, controlling the concentration of PAN to change the dosage of the additive to be 0.3 wt% and stirring for 2 hours at the water bath temperature of 65 ℃ to obtain uniform membrane casting solution, removing bubbles from the obtained membrane casting solution, preparing a membrane forming material by using a spin coater, soaking the prepared membrane material in distilled water for 24 hours, then placing the membrane forming material in a drying box, and drying at the temperature of 48 ℃ to prepare a precursor membrane;
fourthly, the prepared precursor film is subjected to heat treatment in a muffle furnace, and then the precursor film after the heat treatment is subjected to carbonization treatment in a vacuum furnace, wherein the carbonization treatment temperature is 70 ℃ and the carbonization treatment time is 2.5 hours, so that porous activated carbon is obtained;
2) putting the porous activated carbon in the step 1) into HNO with the concentration of 70 percent3Cooling and refluxing for 12 hours, adjusting the pH value of the obtained activated carbon to be neutral, and then drying to obtain nitric acid modified carbon;
3) preparing 5 parts of modified carbon obtained in the step 2), 50 parts of glacial acetic acid and 7 parts of potassium iodide into a soaking solution by using a polymerization carbonization method;
4) and uniformly coating the soaking solution on the outer side of the super capacitor, and then putting the super capacitor into an oven for drying, wherein the drying temperature is 55 ℃.
EXAMPLE III
1. A super-capacitor carbon soaking method is characterized by comprising the following specific steps:
1)
preparing activated carbon: adding 9.5 parts of acrylonitrile, 12 parts of dimethylformamide and 0.8 part of azobisisobutyro into a container, and stirring for 5 hours under the condition of a water bath at 70 ℃ to obtain a mixed solution;
secondly, extracting the mixed solution obtained in the first step by using ethanol to obtain an acrylonitrile solid, and then drying the acrylonitrile solid by using hot air at 70 ℃;
thirdly, using 10 wt% of PAN, controlling the concentration of PAN to change the dosage of the additive to be 0.3 wt% and stirring for 2 hours at the water bath temperature of 65 ℃ to obtain uniform membrane casting solution, removing bubbles from the obtained membrane casting solution, preparing a membrane forming material by using a spin coater, soaking the prepared membrane material in distilled water for 22 hours, then placing the membrane forming material in a drying box, and drying at the temperature of 48 ℃ to prepare a precursor membrane;
fourthly, the prepared precursor film is subjected to heat treatment in a muffle furnace, and then the precursor film after the heat treatment is subjected to carbonization treatment in a vacuum furnace, wherein the carbonization treatment temperature is 68 ℃ and the carbonization treatment time is 2 hours, so that porous activated carbon is obtained;
2) putting the porous activated carbon in the step 1) into HNO with the concentration of 68 percent3Cooling and refluxing for 11 hours, adjusting the pH value of the obtained activated carbon to be neutral, and then drying to obtain nitric acid modified carbon;
3) preparing 4 parts of modified carbon obtained in the step 2), 40 parts of glacial acetic acid and 5 parts of potassium iodide into a soaking solution by using a polymerization carbonization method;
4) and uniformly coating the soaking solution on the outer side of the super capacitor, and then putting the super capacitor into an oven for drying at the drying temperature of 50 ℃.
Claims (2)
1. A super-capacitor carbon soaking method is characterized by comprising the following specific steps:
1)
preparing activated carbon: adding 9-10 parts of acrylonitrile, 10-15 parts of dimethylformamide and 0.5-1 part of azobisisobutyro into a container, and stirring for 4-6 hours at the temperature of 60-75 ℃ in a water bath to obtain a mixed solution;
secondly, extracting the mixed solution obtained in the first step by using ethanol to obtain acrylonitrile solid, and then drying the acrylonitrile solid by hot air at the temperature of 60-80 ℃;
thirdly, using 10 wt% of PAN, controlling the concentration of PAN to change the dosage of the additive to be 0.3 wt% and stirring for 2 hours at the water bath temperature of 65 ℃ to obtain uniform membrane casting solution, removing bubbles from the obtained membrane casting solution, preparing a membrane forming material by using a spin coater, soaking the prepared membrane material in distilled water for 20-24 hours, then placing the membrane forming material in a drying box, and drying at the temperature of 45-55 ℃ to prepare a precursor membrane;
fourthly, the prepared precursor film is subjected to heat treatment in a muffle furnace, and then the precursor film after the heat treatment is subjected to carbonization treatment in a vacuum furnace, wherein the carbonization treatment temperature is 65-70 ℃ and the time is 1.5-2.5 hours, so that the porous activated carbon is obtained;
2) putting the porous activated carbon in the step 1) into 65-70% HNO3Cooling and refluxing for 10-12 hours, adjusting the pH value of the obtained activated carbon to be neutral, and then drying to obtain nitric acid modified carbon;
3) preparing 3-5 parts of modified carbon obtained in the step 2), 30-50 parts of glacial acetic acid and 4-7 parts of potassium iodide into a soaking solution by using a polymerization carbonization method;
4) uniformly coating the soaking solution on the outer side of the super capacitor, and then putting the super capacitor into an oven for drying at the temperature of 45-55 ℃.
2. The method for carbon impregnation of a super capacitor according to claim 1, wherein: in the third step, the drying temperature of the membrane material is 45-50 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011378102.9A CN112645322A (en) | 2020-11-30 | 2020-11-30 | Carbon soaking method for super capacitor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011378102.9A CN112645322A (en) | 2020-11-30 | 2020-11-30 | Carbon soaking method for super capacitor |
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| Publication Number | Publication Date |
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| CN112645322A true CN112645322A (en) | 2021-04-13 |
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| CN202011378102.9A Pending CN112645322A (en) | 2020-11-30 | 2020-11-30 | Carbon soaking method for super capacitor |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1837035A (en) * | 2005-12-28 | 2006-09-27 | 大连理工大学 | Process for preparing nano hybrid carbon film |
| CN102806022A (en) * | 2012-09-06 | 2012-12-05 | 天津工业大学 | Method for preparing polyacrylonitrile (PAN)-base microporous membrane |
| CN106847532A (en) * | 2017-04-07 | 2017-06-13 | 苏州海凌达电子科技有限公司 | A kind of preparation method of the high performance material for ultracapacitor |
| CN107217482A (en) * | 2017-07-10 | 2017-09-29 | 西安科技大学 | A kind of polyaniline hybridized electrode materials of nitrogen-phosphor codoping porous carbon membrane@with interface covalent linkage and preparation method thereof |
| CN108439405A (en) * | 2018-04-19 | 2018-08-24 | 句容市盛达环保净化材料有限公司 | A kind of preparation method of modified activated carbon |
-
2020
- 2020-11-30 CN CN202011378102.9A patent/CN112645322A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1837035A (en) * | 2005-12-28 | 2006-09-27 | 大连理工大学 | Process for preparing nano hybrid carbon film |
| CN102806022A (en) * | 2012-09-06 | 2012-12-05 | 天津工业大学 | Method for preparing polyacrylonitrile (PAN)-base microporous membrane |
| CN106847532A (en) * | 2017-04-07 | 2017-06-13 | 苏州海凌达电子科技有限公司 | A kind of preparation method of the high performance material for ultracapacitor |
| CN107217482A (en) * | 2017-07-10 | 2017-09-29 | 西安科技大学 | A kind of polyaniline hybridized electrode materials of nitrogen-phosphor codoping porous carbon membrane@with interface covalent linkage and preparation method thereof |
| CN108439405A (en) * | 2018-04-19 | 2018-08-24 | 句容市盛达环保净化材料有限公司 | A kind of preparation method of modified activated carbon |
Non-Patent Citations (1)
| Title |
|---|
| 王湛等, 化学工业出版社 * |
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