CN109267047B - Preparation method of flexible cloth electrode based on nickel-manganese hydroxide - Google Patents
Preparation method of flexible cloth electrode based on nickel-manganese hydroxide Download PDFInfo
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- CN109267047B CN109267047B CN201811278008.9A CN201811278008A CN109267047B CN 109267047 B CN109267047 B CN 109267047B CN 201811278008 A CN201811278008 A CN 201811278008A CN 109267047 B CN109267047 B CN 109267047B
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- 239000004744 fabric Substances 0.000 title claims abstract description 98
- FXOOEXPVBUPUIL-UHFFFAOYSA-J manganese(2+);nickel(2+);tetrahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[Mn+2].[Ni+2] FXOOEXPVBUPUIL-UHFFFAOYSA-J 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229920000742 Cotton Polymers 0.000 claims abstract description 59
- 239000007772 electrode material Substances 0.000 claims abstract description 40
- 238000004070 electrodeposition Methods 0.000 claims abstract description 23
- 238000007747 plating Methods 0.000 claims abstract description 23
- 239000008367 deionised water Substances 0.000 claims abstract description 22
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 22
- 239000011259 mixed solution Substances 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000005406 washing Methods 0.000 claims abstract description 17
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 239000000126 substance Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims abstract description 12
- 230000001235 sensitizing effect Effects 0.000 claims abstract description 12
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims abstract description 10
- 230000003213 activating effect Effects 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000011565 manganese chloride Substances 0.000 claims abstract description 10
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims abstract description 5
- 229910003286 Ni-Mn Inorganic materials 0.000 claims abstract description 5
- 235000002867 manganese chloride Nutrition 0.000 claims abstract description 5
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims abstract description 5
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 44
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 31
- 238000000151 deposition Methods 0.000 claims description 23
- 230000008021 deposition Effects 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 12
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims description 12
- 229910052697 platinum Inorganic materials 0.000 claims description 12
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 9
- 229910021205 NaH2PO2 Inorganic materials 0.000 claims description 7
- 229910002666 PdCl2 Inorganic materials 0.000 claims description 7
- 238000005520 cutting process Methods 0.000 claims description 7
- 239000008151 electrolyte solution Substances 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 238000002791 soaking Methods 0.000 claims description 7
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 7
- 239000001509 sodium citrate Substances 0.000 claims description 7
- 230000004913 activation Effects 0.000 claims description 4
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 4
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- 206010070834 Sensitisation Diseases 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000007772 electroless plating Methods 0.000 claims description 2
- 230000008313 sensitization Effects 0.000 claims description 2
- 239000003990 capacitor Substances 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 241000761557 Lamina Species 0.000 abstract 1
- 238000004769 chrono-potentiometry Methods 0.000 abstract 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 18
- ZAUUZASCMSWKGX-UHFFFAOYSA-N manganese nickel Chemical compound [Mn].[Ni] ZAUUZASCMSWKGX-UHFFFAOYSA-N 0.000 description 17
- 239000003792 electrolyte Substances 0.000 description 16
- 239000000463 material Substances 0.000 description 16
- 239000010410 layer Substances 0.000 description 12
- 238000002484 cyclic voltammetry Methods 0.000 description 11
- 229910000000 metal hydroxide Inorganic materials 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 6
- 150000004679 hydroxides Chemical class 0.000 description 6
- 238000001000 micrograph Methods 0.000 description 6
- 238000011056 performance test Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 125000004122 cyclic group Chemical group 0.000 description 5
- 239000011572 manganese Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 150000004692 metal hydroxides Chemical class 0.000 description 5
- 238000013112 stability test Methods 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 229910052759 nickel Inorganic materials 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 229910000428 cobalt oxide Inorganic materials 0.000 description 2
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- 229910001925 ruthenium oxide Inorganic materials 0.000 description 2
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 229910021503 Cobalt(II) hydroxide Inorganic materials 0.000 description 1
- 241000080590 Niso Species 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- ASKVAEGIVYSGNY-UHFFFAOYSA-L cobalt(ii) hydroxide Chemical compound [OH-].[OH-].[Co+2] ASKVAEGIVYSGNY-UHFFFAOYSA-L 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 150000003623 transition metal compounds Chemical class 0.000 description 1
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
- C23C18/28—Sensitising or activating
- C23C18/285—Sensitising or activating with tin based compound or composition
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
- C23C18/28—Sensitising or activating
- C23C18/30—Activating or accelerating or sensitising with palladium or other noble metal
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
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- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
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Abstract
A preparation method of a flexible cloth electrode based on nickel-manganese hydroxide comprises the following steps: (1) sensitizing cotton cloth; (2) activating cotton cloth; (3) performing chemical plating treatment on the activated cotton cloth; (4) performing constant-voltage electrodeposition on the nickel-plated conductive cotton cloth on an electrochemical workstation; (5) mixing and stirring nickel nitrate, manganous chloride, ammonium chloride and deionized water to obtain a mixed solution; (6) and carrying out electrochemical deposition on the current collector nickel-plated conductive cloth by using a chronopotentiometry, washing and drying to obtain a flower-shaped Ni-Mn bimetal hydroxide electrode material formed by combining a plurality of two-dimensional laminas. The preparation method has the advantages of simple synthesis path, easily obtained raw materials and low cost, and when the nickel-manganese hydroxide electrodeposited on the nickel-plated conductive cloth is used for the electrode material of the super capacitor, the specific capacitance is high and the rate capability is good.
Description
Technical Field
The invention relates to a preparation method of a flexible cloth electrode, in particular to a preparation method of a bimetal hydroxide flexible electrode, belonging to the field of electrode materials.
Background
With the rapid growth of the world population and the rapid development of socioeconomic performance, humans face the dual challenges of energy crisis and deterioration of the ecological environment. With the rapid development of science and technology, people require that the energy storage device has large capacitance, good cycle performance, low manufacturing cost and green and pollution-free manufacturing process. These are not met by ordinary batteries. Supercapacitors are emerging in the field of vision as emerging new energy storage devices.
The most important factor influencing the electrochemical performance of the supercapacitor is an electrode material, the performance of the electrode material directly determines the performance of the supercapacitor, and the electrode material can be divided into three types according to the physical and chemical properties of an active material on the electrode material: a carbon-based material, a transition metal compound, and a conductive polymer. Layered Double Hydroxides (LDHs), also known as hydrotalcite-like compounds or anionic clays, are Layered materials composed of Hydroxides of two or more metals. The layered structure and the controllable inter-layer ionic species and the adjustability of the number of the layers make the electrode material of the super capacitor occupy an important position. In scientific research, the combination of the optimal metal cations is researched, different anions are inserted between layers, the growth tendency and the morphology of the material are controlled, and the material composition with other advantages is developed, so that the electrochemical performance of the layered double hydroxide is optimized, and the layered double hydroxide is more suitable for the electrode material of the super capacitor.
Since the advent of the pseudocapacitor, metal oxides and hydroxides were the best choice for pseudocapacitor electrode materials, from the very beginning, expensive and toxic ruthenium oxide (RuO) was chosen2) The nickel oxide, the cobalt oxide and the cobalt oxide which are commonly used at present are published and developed,Manganese oxide, manganese dioxide, nickel hydroxide and cobalt hydroxide. In addition, in recent years, portable intelligent electronic devices are developed rapidly, and the development of the electronic devices does not leave corresponding high-efficiency flexible energy storage equipment, so that flexible capacitors made of carbon fibers, conductive gold metal fabrics and CNT (carbon nanotube) coated cotton fabrics/paper serving as substrates are produced. However, these substrates are expensive in manufacturing cost, have weak market economy competitiveness, and are difficult to be put into industrial production.
The preparation of the electrode material with high specific surface area is one of the ways to improve the electrochemical performance of the electrode material, and the lamellar electrode material has larger specific surface area, which means that the contact area of the electrode material and the electrolyte is increased, thereby shortening the electron transmission path, increasing the electron transfer efficiency and improving the electrochemical performance of the material. However, the manufacturing process of the conductive cloth material on the market is complicated and has high cost, and the deposition liquid which is physically quiet is not uniform, so that the final conductivity is not uniform.
Disclosure of Invention
In view of the problems in the prior art, the present invention aims to provide a method for preparing a flexible cloth electrode based on nickel-manganese hydroxide, so as to improve the preparation method of the electrode material of the flexible electrode, optimize the cost, optimize the morphology of the electrode material, improve the electrochemical performance and the electrochemical activity of the flexible cloth electrode material, simplify the manufacturing process, and improve the preparation efficiency.
In order to achieve the purpose, the invention adopts the technical scheme that: a preparation method of a flexible cloth electrode based on nickel-manganese hydroxide comprises the following steps:
(1) cutting pure cotton cloth into pieces of 1 × 2cm, and soaking the cotton cloth in sensitizing solution for sensitizing treatment;
(2) washing the sensitized cotton cloth with deionized water for at least three times, and then immersing the cotton cloth into an activating solution for activation treatment;
(3) washing the activated cotton cloth with deionized water, and then carrying out chemical plating treatment on the activated cotton cloth, wherein the pH value of the solution is adjusted to 9-10 by using ammonia water before plating treatment;
(4) taking the nickel-plated conductive cotton cloth obtained in the step (3) as a cathode, taking a 2 x 2cm Pt plate as an anode, and taking NiSO4、NH4Performing constant-voltage electrodeposition on the nickel-plated conductive cotton cloth on an electrochemical workstation by using Cl as an electrolyte solution, wherein the deposition voltage is 2V, and the deposition time is 8-10 min; cleaning and drying to obtain the nickel-plated conductive cloth;
(5) preparing a deposition solution required by electrodeposition, mixing and stirring nickel nitrate, manganous chloride, ammonium chloride and deionized water to obtain a mixed solution;
(6) and (3) starting an electrochemical workstation, placing the mixed solution obtained in the step (5) in a beaker, carrying out electrochemical deposition on the current collector nickel-plated conductive cloth by using a chronopotentiometric method under a three-electrode system with the current collector as a working electrode, the platinum electrode as a counter electrode and the saturated calomel electrode as a reference electrode, and washing and drying after the reaction is finished to obtain the Ni-Mn bimetal hydroxide electrode material.
Preferably, the sensitizing solution in step (1) comprises SnCl2And a few Sn particles, wherein SnCl2The mass ratio of HCl to HCl was 1:10 and the sensitization time was 10 min.
Preferably, the activating solution in step (2) comprises PdCl2And HCl, and activation time 10 min.
Preferably, the plating solution used for electroless plating in step (3) includes NiSO4、NH4Cl, sodium citrate and NaH2PO2And the chemical plating time is 2 hours.
Preferably, the mass ratio of the nickel nitrate to the manganous chloride in the mixed solution in the step (5) is 0.9: 1-1.5: 1.
Preferably, the conditions of the electrochemical deposition in step (6) are: current density 8mA cm-2Deposition time 900S.
Compared with the prior art, the preparation method of the flexible cloth electrode provided by the invention is characterized in that the insulated cotton cloth is processed into the nickel-coated cotton cloth through a series of chemical methods. The nickel-plated conductive cloth is a novel current collector synthesized in a chemical mode, has good conductivity of current collectors commonly used at present such as nickel nets, iron nets and the like, has a larger active substance bearing area, and is simple in synthesis path of nickel-coated cotton cloth, easy to obtain raw materials and low in cost. The sample prepared by the electrodeposition method has the advantages of short preparation time, high efficiency, experimental instruments, simple operation and the like, and the sedimentary deposit formed by electrodeposition is uniform and smooth, and more importantly, the thickness of the sedimentary deposit is controllable. When the nickel manganese hydroxide electrodeposited on the nickel plating conductive cloth is used for the electrode material of the super capacitor, the specific capacitance is high, and the rate capability is good.
Drawings
FIG. 1 is a scanning electron microscope image of a nickel-manganese double hydroxide, wherein (a), (b) and (c) are SEM images of nickel-manganese double hydroxides prepared under the conditions that the ratio of Ni to Mn is 1:1, 1:2 and 2:3 respectively;
fig. 2 is a graph showing electrochemical performance tests of the obtained nickel-manganese double hydroxide, wherein (a) is a graph showing CV curves of the nickel-manganese double hydroxide in different proportions, and (b) is a graph showing a GCD curve of the nickel-manganese double hydroxide in different proportions.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1:
a preparation method of a flexible cloth electrode based on nickel-manganese hydroxide comprises the following steps:
(1) cutting pure cotton cloth into pieces of 1 × 2cm, and soaking the cotton cloth in a solution containing 0.01Mol SnCl2Sensitizing in 0.1Mol HCl and a little Sn particles sensitizing solution for 10 min;
(2) the sensitized cotton cloth was washed with deionized water and then dipped in a solution containing 10. mu.g/mL of PdCl2Activating in 0.018Mol HCl activating solution for 10 min;
(3) washing activated cotton cloth with deionized water, and performing chemical plating treatment on the activated cotton cloth, wherein the plating solution comprises 0.0712Mol of NiSO4、0.561Mol NH4Cl, 0.034Mol sodium citrate and 0.0283Mol NaH2PO2The plating treatment time is 2 hours;
(4) in stepsThe nickel-plated conductive cotton cloth obtained in the step (3) is used as a cathode, a 2 x 2cm Pt plate is used as an anode, and 0.15Mol NiSO is used4、0.12Mol NH4Performing constant-voltage electrodeposition on the nickel-plated conductive cotton cloth on a CHI660E electrochemical workstation by using Cl as an electrolyte solution, wherein the deposition voltage is 2V, and the deposition time is 8-10 min;
(5) 0.58g of Ni (NO) was weighed3)2And 0.38g MnCl2Adding into 100mL deionized water, and magnetically stirring for 5min to obtain a mixed solution.
(6) Weighing 1.07gNH4And adding Cl into the mixed solution, and magnetically stirring for 5min to obtain the electrolyte.
(7) Taking the mixed solution obtained in the step (6) as an electrolyte, taking clean nickel-plated conductive cloth as a working electrode, taking a platinum electrode as a counter electrode and taking a saturated calomel electrode as a reference electrode, and carrying out constant-current electrodeposition reaction under an electrochemical workstation, wherein the area of the conductive cloth is 1 x 2cm2Current density of 8mA cm-2The electrodeposition time was 900S.
After the reaction is finished, the three-dimensional flower-shaped nickel-manganese double-metal hydroxide electrode material formed by combining a plurality of lamellar layers is obtained after ultrasonic washing and drying.
The nickel-manganese double metal hydroxide prepared by the embodiment shows a three-dimensional pattern-shaped space structure formed by combining two-dimensional lamellar layers, the specific surface area of the electrode material is large, and the pattern-shaped structure can be observed through a scanning electron microscope image.
The electrochemical performance test method comprises the following steps: the electrochemical performance of the working electrode is tested in a three-electrode system, the electrolyte is 1M KOH solution, a platinum sheet is used as a counter electrode, a Saturated Calomel Electrode (SCE) is used as a reference electrode, the three-electrode system is connected to an electrochemical workstation (CHI 660E), the electrochemical performance of the electrode is tested by utilizing Cyclic Voltammetry (CV), constant current charge and discharge (GCD) and Electrochemical Impedance (EIS) technologies, and the cyclic stability test is carried out on a blue-electricity battery test system.
The specific capacitance of the material prepared by the embodiment is 554F/g at 1A/g; the mass specific capacitance is 470F/g and the cycle efficiency is 80 percent after 2000 cycles of charge and discharge.
Example 2:
a preparation method of a flexible cloth electrode based on nickel-manganese hydroxide comprises the following steps:
(1) cutting pure cotton cloth into pieces of 1 × 2cm, and soaking the cotton cloth in a solution containing 0.01Mol SnCl2Sensitizing in 0.1Mol HCl and a little Sn particles sensitizing solution for 10 min;
(2) the sensitized cotton cloth was washed with deionized water and then dipped in a solution containing 10. mu.g/mL of PdCl2Activating in 0.018Mol HCl activating solution for 10 min;
(3) washing activated cotton cloth with deionized water, and performing chemical plating treatment on the activated cotton cloth, wherein the plating solution comprises 0.0712Mol of NiSO4、0.561Mol NH4Cl, 0.034Mol sodium citrate and 0.0283Mol NaH2PO2The plating treatment time is 2 hours;
(4) taking the nickel-plated conductive cotton cloth obtained in the step (3) as a cathode, a 2 x 2cm Pt plate as an anode and 0.15Mol NiSO4、0.12Mol NH4Performing constant-voltage electrodeposition on the nickel-plated conductive cotton cloth on a CHI660E electrochemical workstation by using Cl as an electrolyte solution, wherein the deposition voltage is 2V, and the deposition time is 8-10 min;
(5) 1.16g of Ni (NO) was weighed3)2And 1.14g MnCl2Adding into 100mL deionized water, and magnetically stirring for 5min to obtain a mixed solution.
(6) Weighing 1.07gNH4And adding Cl into the mixed solution, and magnetically stirring for 5min to obtain the electrolyte.
(7) Taking the mixed solution obtained in the step (6) as an electrolyte, taking clean conductive cloth as a working electrode, a platinum electrode as a counter electrode and a saturated calomel electrode as a reference electrode, and carrying out constant current point deposition reaction under an electrochemical workstation, wherein the area of the conductive cloth is 1 x 2cm2Current density of 8mA cm-2The electrodeposition time was 900S.
After the reaction is finished, the three-dimensional flower-shaped nickel-manganese double-metal hydroxide electrode material formed by combining a plurality of lamellar layers is obtained after ultrasonic washing and drying.
The nickel-manganese double metal hydroxide prepared by the embodiment shows a three-dimensional pattern-shaped space structure formed by combining two-dimensional lamellar layers, the specific surface area of the electrode material is large, and the pattern-shaped structure can be observed through a scanning electron microscope image.
The electrochemical performance test method comprises the following steps: the electrochemical performance of the working electrode is tested in a three-electrode system, the electrolyte is 1M KOH solution, a platinum sheet is used as a counter electrode, a Saturated Calomel Electrode (SCE) is used as a reference electrode, the three-electrode system is connected to an electrochemical workstation (CHI 660E), the electrochemical performance of the electrode is tested by utilizing Cyclic Voltammetry (CV), constant current charge and discharge (GCD) and Electrochemical Impedance (EIS) technologies, and the cyclic stability test is carried out on a blue-electricity battery test system.
The specific capacitance of the material prepared by the embodiment is 955F/g at 1A/g; the mass specific capacitance of the material is 764F/g after 2000 cycles of charge and discharge, and the cycle efficiency is 85%.
Example 3:
a preparation method of a flexible cloth electrode based on nickel-manganese hydroxide comprises the following steps:
(1) cutting pure cotton cloth into pieces of 1 × 2cm, and soaking the cotton cloth in a solution containing 0.01Mol SnCl2Sensitizing in 0.1Mol HCl and a little Sn particles sensitizing solution for 10 min;
(2) the sensitized cotton cloth was washed with deionized water and then dipped in a solution containing 10. mu.g/mL of PdCl2Activating in 0.018Mol HCl activating solution for 10 min;
(3) washing activated cotton cloth with deionized water, and performing chemical plating treatment on the activated cotton cloth, wherein the plating solution comprises 0.0712Mol of NiSO4、0.561Mol NH4Cl, 0.034Mol sodium citrate and 0.0283Mol NaH2PO2The plating treatment time is 2 hours;
(4) taking the nickel-plated conductive cotton cloth obtained in the step (3) as a cathode, a 2 x 2cm Pt plate as an anode and 0.15Mol NiSO4、0.12Mol NH4Performing constant-voltage electrodeposition on the nickel-plated conductive cotton cloth on a CHI660E electrochemical workstation by using Cl as an electrolyte solution, wherein the deposition voltage is 2V, and the deposition time is 8-10 min;
(5) 0.58g of Ni (NO) was weighed3)2And 0.76g MnCl2Adding into 100mL deionized water, and magnetically stirring for 5min to obtain a mixed solution.
(6) Weighing 1.07gNH4And adding Cl into the mixed solution, and magnetically stirring for 5min to obtain the electrolyte.
(7) Taking the mixed solution obtained in the step (6) as an electrolyte, taking clean conductive cloth as a working electrode, a platinum electrode as a counter electrode and a saturated calomel electrode as a reference electrode, and carrying out constant current point deposition reaction under an electrochemical workstation, wherein the area of the conductive cloth is 1 x 2cm2Current density of 8mA cm-2The electrodeposition time was 900S.
After the reaction is finished, the three-dimensional flower-shaped nickel-manganese double-metal hydroxide electrode material formed by combining a plurality of lamellar layers is obtained after ultrasonic washing and drying.
The nickel-manganese double metal hydroxide prepared by the embodiment shows a three-dimensional pattern-shaped space structure formed by combining two-dimensional lamellar layers, the specific surface area of the electrode material is large, and the pattern-shaped structure can be observed through a scanning electron microscope image.
The electrochemical performance test method comprises the following steps: the electrochemical performance of the working electrode is tested in a three-electrode system, the electrolyte is 1M KOH solution, a platinum sheet is used as a counter electrode, a Saturated Calomel Electrode (SCE) is used as a reference electrode, the three-electrode system is connected to an electrochemical workstation (CHI 660E), the electrochemical performance of the electrode is tested by utilizing Cyclic Voltammetry (CV), constant current charge and discharge (GCD) and Electrochemical Impedance (EIS) technologies, and the cyclic stability test is carried out on a blue-electricity battery test system.
The specific capacitance of the material prepared by the embodiment is 447F/g at 1A/g; the mass specific capacitance of the material is 366F/g after 2000 cycles of charge and discharge, and the cycle efficiency is 82%.
Example 4:
a preparation method of a flexible cloth electrode based on nickel-manganese hydroxide comprises the following steps:
(1) cutting pure cotton cloth into pieces of 1 × 2cm, and soaking the cotton cloth in a solution containing 0.01Mol SnCl2Sensitizing in 0.1Mol HCl and a little Sn particles sensitizing solution for 10 min;
(2) the sensitized cotton cloth was washed with deionized water and then dipped in a solution containing 10. mu.g/mL of PdCl2Activating in 0.018Mol HCl activating solution for 10 min;
(3) washing activated cotton cloth with deionized water, and performing chemical plating treatment on the activated cotton cloth, wherein the plating solution comprises 0.0712Mol of NiSO4、0.561Mol NH4Cl, 0.034Mol sodium citrate and 0.0283Mol NaH2PO2The plating treatment time is 2 hours;
(4) taking the nickel-plated conductive cotton cloth obtained in the step (3) as a cathode, a 2 x 2cm Pt plate as an anode and 0.15Mol NiSO4、0.12Mol NH4Performing constant-voltage electrodeposition on the nickel-plated conductive cotton cloth on a CHI660E electrochemical workstation by using Cl as an electrolyte solution, wherein the deposition voltage is 2V, and the deposition time is 8-10 min;
(5) 0.58g of Ni (NO) was weighed3)2And 0.38g MnCl2Adding into 100mL deionized water, and magnetically stirring for 5min to obtain a mixed solution.
(6) Weighing 1.07gNH4And adding Cl into the mixed solution, and magnetically stirring for 5min to obtain the electrolyte.
(7) Taking the mixed solution obtained in the step (6) as an electrolyte, taking clean conductive cloth as a working electrode, a platinum electrode as a counter electrode and a saturated calomel electrode as a reference electrode, and carrying out constant current point deposition reaction under an electrochemical workstation, wherein the area of the conductive cloth is 1 x 2cm2Current density of 4mA cm-2The electrodeposition time was 900S.
After the reaction is finished, the three-dimensional flower-shaped nickel-manganese double-metal hydroxide electrode material formed by combining a plurality of lamellar layers is obtained after ultrasonic washing and drying.
The nickel-manganese double metal hydroxide prepared by the embodiment shows a three-dimensional pattern-shaped space structure formed by combining two-dimensional lamellar layers, the specific surface area of the electrode material is large, and the pattern-shaped structure can be observed through a scanning electron microscope image.
The electrochemical performance test method comprises the following steps: the electrochemical performance of the working electrode is tested in a three-electrode system, the electrolyte is 1M KOH solution, a platinum sheet is used as a counter electrode, a Saturated Calomel Electrode (SCE) is used as a reference electrode, the three-electrode system is connected to an electrochemical workstation (CHI 660E), the electrochemical performance of the electrode is tested by utilizing Cyclic Voltammetry (CV), constant current charge and discharge (GCD) and Electrochemical Impedance (EIS) technologies, and the cyclic stability test is carried out on a blue-electricity battery test system.
The material prepared by the embodiment has a specific capacitance of 540F/g at 1A/g; the mass specific capacitance is 426F/g and the cycle efficiency is 79 percent after 2000 circles of charge and discharge are cycled.
Example 5:
a preparation method of a flexible cloth electrode based on nickel-manganese hydroxide comprises the following steps:
(1) cutting pure cotton cloth into pieces of 1 × 2cm, and soaking the cotton cloth in a solution containing 0.01Mol SnCl2Sensitizing in 0.1Mol HCl and a little Sn particles sensitizing solution for 10 min;
(2) the sensitized cotton cloth was washed with deionized water and then dipped in a solution containing 10. mu.g/mL of PdCl2Activating in 0.018Mol HCl activating solution for 10 min;
(3) washing activated cotton cloth with deionized water, and performing chemical plating treatment on the activated cotton cloth, wherein the plating solution comprises 0.0712Mol of NiSO4、0.561Mol NH4Cl, 0.034Mol sodium citrate and 0.0283Mol NaH2PO2At the position of the coatingThe processing time is 2 h;
(4) taking the nickel-plated conductive cotton cloth obtained in the step (3) as a cathode, a 2 x 2cm Pt plate as an anode and 0.15Mol NiSO4、0.12Mol NH4Performing constant-voltage electrodeposition on the nickel-plated conductive cotton cloth on a CHI660E electrochemical workstation by using Cl as an electrolyte solution, wherein the deposition voltage is 2V, and the deposition time is 8-10 min;
(5) 0.58g of Ni (NO) was weighed3)2And 0.38g MnCl2Adding into 100mL deionized water, and magnetically stirring for 5min to obtain a mixed solution.
(6) Weighing 1.07gNH4And adding Cl into the mixed solution, and magnetically stirring for 5min to obtain the electrolyte.
(7) Taking the mixed solution obtained in the step (6) as an electrolyte, taking clean conductive cloth as a working electrode, a platinum electrode as a counter electrode and a saturated calomel electrode as a reference electrode, and carrying out constant current point deposition reaction under an electrochemical workstation, wherein the area of the conductive cloth is 1 x 2cm2Current density of 8mA cm-2The electrodeposition time was 1800S.
After the reaction is finished, the three-dimensional flower-shaped nickel-manganese double-metal hydroxide electrode material formed by combining a plurality of lamellar layers is obtained after ultrasonic washing and drying.
The nickel-manganese double metal hydroxide prepared by the embodiment shows a three-dimensional pattern-shaped space structure formed by combining two-dimensional lamellar layers, the specific surface area of the electrode material is large, and the pattern-shaped structure can be observed through a scanning electron microscope image.
The electrochemical performance test method comprises the following steps: the electrochemical performance of the working electrode is tested in a three-electrode system, the electrolyte is 1M KOH solution, a platinum sheet is used as a counter electrode, a Saturated Calomel Electrode (SCE) is used as a reference electrode, the three-electrode system is connected to an electrochemical workstation (CHI 660e), the electrochemical performance of the electrode is tested by utilizing Cyclic Voltammetry (CV), constant current charge and discharge (GCD) and Electrochemical Impedance (EIS) technologies, and the cyclic stability test is carried out on a blue-electricity battery test system.
The specific capacitance of the material prepared by the embodiment is 500F/g at 1A/g; the mass specific capacitance of the material is 350F/g after 2000 cycles of charge and discharge, and the cycle efficiency is 70%.
In summary, the morphology of the prepared electrode material is shown in fig. 1, wherein (a) is an SEM image with a ratio of Ni to Mn of 1:1, and the structure shown in the figure is a truncated cone-shaped structure composed of two-dimensional nanosheet layered double hydroxides; (b) the figure is an SEM picture with a ratio of Ni to Mn being 1:2, and the structural sheet layered double hydroxide shown in the figure forms a truncated cone structure with larger gaps; (c) the figure is an SEM image with a ratio of Ni to Mn of 2:3, and the structure shown in the figure is a flower-like structure consisting of two-dimensional nanosheet layered double hydroxides. The following results are obtained through analysis and comparison: (c) the electrode material obtained in the figure has larger specific surface area, so the electrode material has more excellent electrochemical performance.
In FIG. 2, (a) is a graph illustrating cyclic voltammetry (cv) of electrode materials at different Ni/Mn ratios, the potential window of the electrode material is about 0-0.7V, and the wider potential window of the electrode material is shown. A pair of distinct redox peaks was observed for each CV curve, indicating that the capacitance of the electrode material is primarily derived from the pseudocapacitance generated during the redox process of nickel manganese double hydroxide. The oxidation peak and the reduction peak are both symmetrical about 0.4V, indicating that the electrode material has good reversibility. With the continuous increase of the scanning rate, the CV curve still has a more obvious oxidation reduction peak, which indicates that the material has better rate performance. The area of the CV curve represents the magnitude of the specific capacitance of this material, which is most pronounced in the three ratios, as is clear from the graph (a) when the Ni-Mn ratio is 2: 3; (b) the constant current charge-discharge test chart of the electrode material under different nickel-manganese ratios shows that the charge curve and the discharge curve have certain symmetry, which shows that the electrode material has good stability and high reversibility. Each charge-discharge curve has a pair of plateaus, which correspond to the positions of the redox peaks in the CV curve. The longer the discharge time of the GCD curve, the higher the specific capacitance of this material, given the same current density and potential window. It can also be seen from the graph (b) that when the Ni-Mn ratio is 2:3, the discharge time of the GCD curve is the longest and the specific capacitance is the largest among the three ratios.
Claims (6)
1. A preparation method of a flexible cloth electrode based on nickel-manganese hydroxide is characterized by comprising the following steps:
(1) cutting pure cotton cloth into pieces of 1 × 2cm, and soaking the cotton cloth in sensitizing solution for sensitizing treatment;
(2) washing the sensitized cotton cloth with deionized water for at least three times, and then immersing the cotton cloth into an activating solution for activation treatment;
(3) washing the activated cotton cloth with deionized water, and then carrying out chemical plating treatment on the activated cotton cloth, wherein the pH value of the solution is adjusted to 9-10 by using ammonia water before plating treatment;
(4) taking the nickel-plated conductive cotton cloth obtained in the step (3) as a cathode, taking a 2 x 2cm Pt plate as an anode, and taking NiSO4、NH4Performing constant-voltage electrodeposition on the nickel-plated conductive cotton cloth on an electrochemical workstation by using Cl as an electrolyte solution, wherein the deposition voltage is 2V, and the deposition time is 8-10 min; cleaning and drying to obtain the nickel-plated conductive cloth;
(5) preparing a deposition solution required by electrodeposition, mixing and stirring nickel nitrate, manganous chloride, ammonium chloride and deionized water to obtain a mixed solution;
(6) and (3) starting an electrochemical workstation, placing the mixed solution obtained in the step (5) in a beaker, carrying out electrochemical deposition on the current collector nickel-plated conductive cloth by using a chronopotentiometric method under a three-electrode system with the current collector as a working electrode, the platinum electrode as a counter electrode and the saturated calomel electrode as a reference electrode, and washing and drying after the reaction is finished to obtain the Ni-Mn bimetal hydroxide electrode material.
2. The method for preparing the flexible cloth electrode based on the nickel-manganese hydroxide according to claim 1, wherein the sensitizing solution in the step (1) comprises SnCl2And a few Sn particles, wherein SnCl2The mass ratio of HCl to HCl was 1:10 and the sensitization time was 10 min.
3. The method for preparing the nickel-manganese hydroxide-based flexible cloth electrode as claimed in claim 2, wherein the activating solution in the step (2) comprises PdCl2And HCl, and activation time 10 min.
4. The method for preparing a flexible cloth electrode based on nickel manganese hydroxide according to claim 1 or 2, wherein the electroless plating solution used in the step (3) comprises NiSO4、NH4Cl, sodium citrate and NaH2PO2And the chemical plating time is 2 hours.
5. The method for preparing the nickel-manganese hydroxide-based flexible cloth electrode according to claim 1 or 2, wherein the mass ratio of the nickel nitrate to the manganous chloride in the mixed solution in the step (5) is 0.9: 1-1.5: 1.
6. The method for preparing the nickel-manganese hydroxide-based flexible cloth electrode according to claim 1 or 2, wherein the conditions of the electrochemical deposition in the step (6) are as follows: current density 8mA cm-2Deposition time 900S.
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| CN110189924B (en) * | 2019-05-23 | 2022-01-07 | 潍坊学院 | Preparation method of linear Co-Mn bimetal hydroxide electrode material |
| CN110690057B (en) * | 2019-09-27 | 2021-02-02 | 同济大学 | Nickel intercalation manganese dioxide-based flexible symmetrical quasi-solid supercapacitor material and preparation method and application thereof |
| CN111825127B (en) * | 2020-07-07 | 2023-06-16 | 江苏大学 | Preparation method and application of metallic nickel-based nanomaterial |
| CN112768653A (en) * | 2021-01-08 | 2021-05-07 | 天津工业大学 | Preparation method and application of flexible nickel-cobalt double hydroxide/metal organic frame/fabric electrode |
| CN116199277B (en) * | 2023-04-28 | 2023-08-11 | 江苏正力新能电池技术有限公司 | Manganese-nickel bimetallic compound and preparation and application thereof |
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