CN108866603B - Preparation method of electrochemical capacitor electrode - Google Patents
Preparation method of electrochemical capacitor electrode Download PDFInfo
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- CN108866603B CN108866603B CN201810696895.5A CN201810696895A CN108866603B CN 108866603 B CN108866603 B CN 108866603B CN 201810696895 A CN201810696895 A CN 201810696895A CN 108866603 B CN108866603 B CN 108866603B
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- 239000003990 capacitor Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 76
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 37
- 239000006260 foam Substances 0.000 claims abstract description 28
- 239000000243 solution Substances 0.000 claims abstract description 25
- 238000009713 electroplating Methods 0.000 claims abstract description 23
- 239000000843 powder Substances 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052809 inorganic oxide Inorganic materials 0.000 claims abstract description 13
- 239000000758 substrate Substances 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 9
- 239000011159 matrix material Substances 0.000 claims abstract description 8
- 150000002815 nickel Chemical class 0.000 claims abstract description 8
- 238000004519 manufacturing process Methods 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims abstract description 4
- 238000011282 treatment Methods 0.000 claims abstract description 4
- 239000002184 metal Substances 0.000 claims abstract description 3
- 229910052751 metal Inorganic materials 0.000 claims abstract description 3
- 239000012266 salt solution Substances 0.000 claims abstract description 3
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical group [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 17
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 17
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 10
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 10
- 229910002412 SrMoO4 Inorganic materials 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 238000012545 processing Methods 0.000 claims description 8
- 238000007747 plating Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- KERTUBUCQCSNJU-UHFFFAOYSA-L nickel(2+);disulfamate Chemical compound [Ni+2].NS([O-])(=O)=O.NS([O-])(=O)=O KERTUBUCQCSNJU-UHFFFAOYSA-L 0.000 claims description 3
- 230000003213 activating effect Effects 0.000 claims description 2
- 238000005238 degreasing Methods 0.000 claims 1
- 239000002131 composite material Substances 0.000 abstract description 11
- 238000010438 heat treatment Methods 0.000 abstract description 8
- 230000004913 activation Effects 0.000 abstract description 7
- 238000005520 cutting process Methods 0.000 abstract description 7
- 238000002791 soaking Methods 0.000 abstract 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 14
- 239000004327 boric acid Substances 0.000 description 14
- 238000004140 cleaning Methods 0.000 description 7
- 238000004090 dissolution Methods 0.000 description 7
- 239000012153 distilled water Substances 0.000 description 7
- 238000001035 drying Methods 0.000 description 7
- 238000007599 discharging Methods 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000007600 charging Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010277 constant-current charging Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/0029—Processes of manufacture
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/004—Details
- H01G9/04—Electrodes or formation of dielectric layers thereon
-
- 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
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electroplating Methods And Accessories (AREA)
- Electroplating And Plating Baths Therefor (AREA)
Abstract
The invention discloses a preparation method of an electrochemical capacitor electrode, which directly deposits a powder material and metallic nickel on a foam nickel substrate by using a composite electroplating mode: preparing nickel salt and water into a certain solution, heating, adding inorganic oxide powder, continuously stirring, cutting into a foamed nickel matrix with required size, carrying out oil removal, water washing, activation and other treatments, or cutting the foamed nickel subjected to the oil removal, water washing, activation and other treatments into the required size, then soaking the foamed nickel matrix into the nickel salt solution dispersed with the inorganic oxide powder as a cathode, taking a metal nickel plate as an anode, and electrifying for a certain time to obtain the electrode. The invention has wide application range, simple electrode manufacturing process, convenient operation and good combination of inorganic oxide and a matrix.
Description
Technical Field
The invention relates to the manufacture of an electrochemical capacitor electrode, in particular to a preparation method of the electrochemical capacitor electrode.
Background
In recent years, electrochemical capacitors are increasingly receiving attention from people in the fields of mobile communication, information technology, aerospace and the like. The preparation of the electrode is very critical, but in the charge storage and conversion process of the electrochemical capacitor, the inorganic oxide is used as an electrode active material, and the conductivity of the inorganic oxide is difficult to ensure the rapid transmission and transfer of electrons, so that the capacitance performance and the service life of the electrochemical capacitor are limited. The invention uses the composite electroplating technology to improve the combination performance of the inorganic oxide and the electrode matrix and the conductivity of the electrochemical capacitor electrode, thereby improving the capacitance performance and the service life of the electrochemical capacitor.
At present, the preparation of electrochemical capacitor electrodes is generally carried out by a method of mixing active powder with various carbon materials and then coating the mixture on an electrode substrate. The carbon material has a certain charge storage function and can improve the conductivity of the electrode.
Disclosure of Invention
In order to solve the technical problem, the invention provides a preparation method of an electrochemical capacitor electrode.
The invention directly utilizes a composite electroplating mode to directly deposit a powder material and metallic nickel on a foam nickel matrix, and comprises the following steps:
firstly, preparing a powder material and preparing an electroplating solution;
dispersing the powder in an electroplating solution, specifically adding inorganic oxide powder into the electroplating solution and continuously stirring;
and thirdly, placing the electrode substrate in an electroplating solution and electroplating under certain conditions, wherein the method comprises the specific steps of immersing the electrode substrate into a nickel salt solution dispersed with inorganic oxide powder to be used as a cathode, taking a metal nickel plate as an anode, and electrifying for a certain time to prepare the electrode.
The plating times are one or more.
The electroplating solution is nickel salt and water, and the nickel salt is nickel sulfate, nickel chloride, nickel sulfamate or a mixture of the nickel sulfate, the nickel chloride and the nickel sulfamate.
The electrode substrate is a foam nickel substrate, and the foam nickel substrate is subjected to oil removal, water washing and activation treatment before electroplating.
The nickel foam substrate may be cut to the desired size before or after processing.
The invention has the advantages that: compared with the prior art, the invention has the following advantages:
1. the application range is wide: can be suitable for most inorganic oxide powder, and any substrate with surface conductivity meeting the requirement of nickel electroplating;
2. the electrode manufacturing process is simple, the operation is convenient, and complex equipment is not needed;
3. the inorganic oxide is well combined with the matrix;
4. the specific capacitance performance of the electrode can be regulated and controlled to a certain degree by changing the composite plating time and/or the current density of the electrode to be plated.
Drawings
Fig. 1 is a schematic structural view of the present invention.
Detailed Description
The preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings so that the advantages and features of the present invention can be more easily understood by those skilled in the art, and the scope of the present invention will be more clearly and clearly defined.
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto. The specific capacitance test method is a constant current charging and discharging method, the electrode prepared by the invention in the measurement is a working electrode, Pt is used as an auxiliary electrode, Hg/HgO is used as a reference electrode, and the charging and discharging current density is 1A/g in 5M KOH electrolyte. The method comprises the following steps:
example 1
Firstly, 260g of nickel sulfate is dissolved in distilled water, and 30g of nickel chloride is added and stirred for dissolution after the nickel sulfate is completely dissolved;
adding 30g of boric acid, and heating to 40 ℃;
③ after the boric acid is completely dissolved, 1.6g of SrMoO4Dispersing the powder particles in the solution and uniformly stirring;
cutting the foam nickel with the thickness of 5mm to obtain the foam nickel with the surface size of 1cm multiplied by 2cm, removing oil from the cut foam nickel, washing with water, putting the foam nickel into the solution after activation to keep the cathode current density at 0.3A/dm2And taking out after 30s, and cleaning and drying to finish the preparation. The specific capacitance of the electrode after composite electroplating processing is 1050 F.g under the condition that the charge-discharge current density is 1A/g-1。
Example 2
Firstly, 260g of nickel sulfate is dissolved in distilled water, and 30g of nickel chloride is added and stirred for dissolution after the nickel sulfate is completely dissolved;
adding 30g of boric acid, and heating to 40 ℃;
③ after the boric acid is completely dissolved, 1.6g of SrMoO4Dispersing the powder particles in the solution and uniformly stirring;
cutting the foam nickel with the thickness of 5mm to obtain the foam nickel with the surface size of 1cm multiplied by 2cm, removing oil from the cut foam nickel, washing with water, putting the foam nickel into the solution after activation to keep the cathode current density at 0.3A/dm2And taking out after 60s, and cleaning and drying to finish the preparation. The specific capacitance of the electrode after composite electroplating processing is 750 F.g under the condition that the charge-discharge current density is 1A/g-1。
Example 3
Firstly, 260g of nickel sulfate is dissolved in distilled water, and 30g of nickel chloride is added and stirred for dissolution after the nickel sulfate is completely dissolved;
adding 30g of boric acid, and heating to 40 ℃;
③ after the boric acid is completely dissolved, 1.6g of SrMoO4Dispersing the powder particles in the solution and uniformly stirring;
cutting the foam nickel with the thickness of 5mm to obtain the foam nickel with the surface size of 1cm multiplied by 2cm, removing oil from the cut foam nickel, washing with water, putting the foam nickel into the solution after activation to keep the cathode current density at 0.5A/dm2And taking out after 30s, and cleaning and drying to finish the preparation. The specific capacitance of the electrode after composite electroplating processing is 1106F g under the condition that the charging and discharging current density is 1A/g-1。
Example 4
Firstly, 260g of nickel sulfate is dissolved in distilled water, and 30g of nickel chloride is added and stirred for dissolution after the nickel sulfate is completely dissolved;
adding 30g of boric acid, and heating to 40 ℃;
③ after the boric acid is completely dissolved, 1.6g of SrMoO4Dispersing the powder particles in the solution and uniformly stirring;
cutting the foam nickel with the thickness of 5mm to obtain the foam nickel with the surface size of 1cm multiplied by 2cm, removing oil from the cut foam nickel, washing with water, activating, putting the foam nickel into the solution, and electrifying to 0.5A/dm2And taking out after 60s, and cleaning and drying to finish the preparation. The specific capacitance of the electrode after the composite electroplating processing is 680F g under the condition that the charge-discharge current density is 1A/g-1。
Example 5
Firstly, 260g of nickel sulfate is dissolved in distilled water, and 30g of nickel chloride is added and stirred for dissolution after the nickel sulfate is completely dissolved;
adding 30g of boric acid, and heating to 40 ℃;
③ after the boric acid is completely dissolved, 1.6g of SrMoO4Dispersing the powder particles in the solution and uniformly stirring;
cutting the foam nickel with the thickness of 5mm to obtain the foam nickel with the surface size of 1cm multiplied by 2cm, removing oil from the cut foam nickel, washing with water, putting the foam nickel into the solution after activation to keep the cathode current density at 0.5A/dm2And taking out after 60s, and cleaning and drying to finish the preparation. The specific capacitance of the electrode after the composite electroplating processing is 680F g under the condition that the charge-discharge current density is 1A/g-1。
Example 6
Firstly, 260g of nickel sulfate is dissolved in distilled water, and 30g of nickel chloride is added and stirred for dissolution after the nickel sulfate is completely dissolved;
adding 30g of boric acid, and heating to 40 ℃;
③ after the boric acid is completely dissolved, 1.6g of SrMoO4Dispersing the powder particles in the solution and uniformly stirring;
fourthly, the foam nickel is degreased, washed and activated, and then is put into the solution to keep the cathode current density at 0.6A/dm2And taking out after 60s, and cleaning and drying to finish the preparation. The specific capacitance of the electrode after composite electroplating processing is 620 F.g under the condition that the charge-discharge current density is 1A/g-1。
Example 7
Firstly, 260g of nickel sulfate is dissolved in distilled water, and 30g of nickel chloride is added and stirred for dissolution after the nickel sulfate is completely dissolved;
adding 30g of boric acid, and heating to 40 ℃;
③ after the boric acid is completely dissolved, 1.6g of SrMoO4Dispersing the powder particles in the solution and uniformly stirring;
fourthly, the foam nickel is degreased, washed and activated, and then is put into the solution to keep the cathode current density at 0.8A/dm2And taking out after 60s, and cleaning and drying to finish the preparation. After composite electroplating processingThe specific capacitance of the electrode (2) at a charge-discharge current density of 1A/g is 500 Fg-1。
Without being limited thereto, any changes or substitutions that are not thought of through the inventive work should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope defined by the claims.
Claims (5)
1. The preparation method of the electrochemical capacitor electrode is characterized by comprising
Firstly, preparing a powder material and preparing an electroplating solution;
and secondly, dispersing the powder in the electroplating solution, namely adding inorganic oxide powder into the electroplating solution and continuously stirring, wherein the inorganic oxide powder is SrMoO4Powder particles;
the third step is to put the electrode matrix into the electroplating solution and electroplate under certain conditions, which is to dip the electrode matrix into the nickel salt solution dispersed with inorganic oxide powder as the cathode, take the metal nickel plate as the anode, and the cathode current density is 0.3 or 0.5 or 0.6 or 0.8A/dm2And electrifying for 30s or 60s to form the electrode.
2. The method for producing an electrochemical capacitor electrode according to claim 1, wherein the number of plating times is one or more.
3. The method of claim 1, wherein the plating solution is a nickel salt and water, and the nickel salt is nickel sulfate, nickel chloride, nickel sulfamate, or a mixture thereof.
4. The method for preparing an electrochemical capacitor electrode according to claim 1, wherein the electrode substrate is a foamed nickel substrate, and the foamed nickel substrate is subjected to degreasing, washing and activating treatment before electroplating.
5. The method of claim 4, wherein the nickel foam substrate is cut to desired dimensions before or after processing.
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| US20060254922A1 (en) * | 2005-03-21 | 2006-11-16 | Science & Technology Corporation @ Unm | Method of depositing films on aluminum alloys and films made by the method |
| CN100486007C (en) * | 2005-12-21 | 2009-05-06 | 中国科学院大连化学物理研究所 | Process for preparing integrated renewable fuel double effect oxygen electrode diffusion layer |
| CN101503805B (en) * | 2009-01-24 | 2010-10-27 | 燕山大学 | Super capacitor and preparation of composite anode material of battery |
| CN102290244B (en) * | 2011-08-09 | 2012-07-18 | 淄博国利新电源科技有限公司 | Preparation method of asymmetrical high-power capacitor battery |
| CN107946089A (en) * | 2017-11-17 | 2018-04-20 | 常州大学 | A kind of MnFe2O4The preparation method of/rGO composite materials and its application as electrode material for super capacitor |
| CN108597893B (en) * | 2018-05-28 | 2020-08-28 | 江苏大学 | Preparation method of supercapacitor composite electrode material based on foamed nickel |
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