CN112342563A - Preparation method and application of nickel self-supporting electrode loaded with ferric hydroxide and manganese carbonate - Google Patents
Preparation method and application of nickel self-supporting electrode loaded with ferric hydroxide and manganese carbonate Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 37
- 235000006748 manganese carbonate Nutrition 0.000 title claims abstract description 19
- 239000011656 manganese carbonate Substances 0.000 title claims abstract description 19
- 229940093474 manganese carbonate Drugs 0.000 title claims abstract description 19
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 title claims abstract description 19
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 229960004887 ferric hydroxide Drugs 0.000 title claims description 11
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 title claims description 11
- 239000006260 foam Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000243 solution Substances 0.000 claims abstract description 14
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 12
- 239000011572 manganese Substances 0.000 claims abstract description 12
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 12
- 235000014413 iron hydroxide Nutrition 0.000 claims abstract description 11
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 claims abstract description 11
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims abstract description 9
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims abstract description 9
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000004202 carbamide Substances 0.000 claims abstract description 9
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 9
- 235000002867 manganese chloride Nutrition 0.000 claims abstract description 9
- 239000011565 manganese chloride Substances 0.000 claims abstract description 9
- 229940099607 manganese chloride Drugs 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 claims abstract description 5
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 14
- 230000008021 deposition Effects 0.000 claims description 8
- 239000000758 substrate Substances 0.000 claims description 8
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 7
- 239000012498 ultrapure water Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 150000002500 ions Chemical class 0.000 claims description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims 1
- 239000004810 polytetrafluoroethylene Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 7
- 238000004070 electrodeposition Methods 0.000 abstract description 5
- 230000003647 oxidation Effects 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 239000002135 nanosheet Substances 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 2
- 229910001220 stainless steel Inorganic materials 0.000 abstract description 2
- 239000010935 stainless steel Substances 0.000 abstract description 2
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 abstract 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 238000000151 deposition Methods 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 238000005520 cutting process Methods 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 229910000510 noble metal Inorganic materials 0.000 description 4
- 229910021607 Silver chloride Inorganic materials 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000004832 voltammetry Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
-
- 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
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electrodes For Compound Or Non-Metal Manufacture (AREA)
Abstract
一种负载氢氧化铁和碳酸锰的镍自支撑电极的制法及应用，其属于电催化纳米异质结材料。该方法为将泡沫镍超声洗涤后，加入到装有氯化锰和尿素混合溶液的不锈钢水热反应釜中，将泡沫镍浸没于溶液中进行水热反应；然后在硝酸铁的溶液中，采用三电极体系进行电沉积，最终得到氢氧化铁/碳酸锰‑泡沫镍的自支撑电极。该电极具有纳米片包覆的三维立方体结构，有利于增大材料的比表面积并且能够暴露更多的活性位点。同时电极中含有碳酸锰材料，锰元素具有丰富的价态结构，可以提高电荷的转移速率。该电极对于电催化水氧化具有高效的性能，具备很好的商业价值。
A preparation method and application of a nickel self-supporting electrode loaded with iron hydroxide and manganese carbonate belong to electrocatalytic nano-heterojunction materials. The method comprises ultrasonically washing the nickel foam, adding it to a stainless steel hydrothermal reactor equipped with a mixed solution of manganese chloride and urea, and immersing the nickel foam in the solution for hydrothermal reaction; then in the solution of iron nitrate, using Electrodeposition was carried out in a three-electrode system, and finally a self-supporting electrode of iron hydroxide/manganese carbonate-nickel foam was obtained. The electrode has a three-dimensional cubic structure covered by nanosheets, which is beneficial to increase the specific surface area of the material and expose more active sites. At the same time, the electrode contains manganese carbonate material, and the manganese element has a rich valence structure, which can improve the transfer rate of charges. The electrode has high performance for electrocatalytic water oxidation and has good commercial value.
Description
Technical Field
The invention belongs to an electro-catalytic nano heterojunction material, and particularly relates to a preparation method of a self-supporting foam nickel electrode loaded with ferric hydroxide and manganese carbonate for efficient electro-catalytic water oxidation.
Background
Due to the excessive use of traditional fossil energy (coal, oil and natural gas), serious problems of environmental pollution, greenhouse effect, energy crisis and the like are caused. This makes people to explore clean energy sources that can replace traditional fossil energy sources, and the clean energy sources that have been put into use at present are: solar energy, wind energy, geothermal energy, tidal energy, hydrogen energy, and the like. The hydrogen energy as a clean energy has the following advantages: (1) the source of hydrogen is wide; (2) hydrogen has a large energy density (120 mg/kJ); (3) the combustion product of the hydrogen is water, and has no pollution to the environment. Through years of research, people find that the electrocatalytic water decomposition hydrogen production is a high-efficiency and feasible technology. The water splitting reaction is divided into an anodic water oxidation reaction and a cathodic proton reduction reaction, wherein the water oxidation reaction requires high free energy through the transfer of multiple electrons and protons, and therefore the water oxidation reaction is a key reaction for restricting the water splitting. This requires a highly efficient water oxidation catalyst to catalyze the reaction. The catalysts which are put into practical use at present are often noble metal catalysts (ruthenium, iridium and platinum), but the noble metals are expensive and low in reserves, so that the noble metals cannot be put into large-scale application. Therefore, research into non-noble metal catalysts is currently being conducted. Secondly, the selection of the substrate is also important, the foamed nickel has a three-dimensional porous structure which is beneficial to the permeation of electrolyte and the exposure of active sites, and the iron hydroxide/manganese carbonate self-supporting electrode is prepared on the foamed nickel by a hydrothermal method and an electrodeposition method and has the shape of a three-dimensional cubic structure coated by nano-sheets, so that the specific surface area of the material is increased, and more active sites can be exposed. Meanwhile, the manganese element in the manganese carbonate has a rich valence structure, so that the transfer rate of charges can be improved.
Disclosure of Invention
The invention aims to provide a preparation method of a self-supporting foam nickel electrode loaded with ferric hydroxide and manganese carbonate for high-efficiency electrocatalytic water oxidation, which mainly solves the problems of low catalytic activity, high overpotential, poor stability and the like in the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a nickel self-supporting electrode loaded with ferric hydroxide and manganese carbonate comprises the following steps:
(S1) cutting the required substrate nickel foam into small pieces of 2 × 3cm, and ultrasonically washing the small pieces with dilute hydrochloric acid, absolute ethyl alcohol and ultrapure water for 20 minutes respectively;
(S2) adding a mixed solution of manganese chloride and urea into a 50ml of polytetrafluoroethylene-lined hydrothermal reaction kettle, immersing the foamed nickel subjected to ultrasonic washing in the mixed solution (S1), and carrying out hydrothermal reaction at 120 ℃ for 8-15h to obtain a manganese carbonate-loaded foamed nickel electrode; the concentration of the urea is 0.1-0.2 mol/L; the concentration of the manganese chloride solution is 0.01-0.05 mol/L;
(S3) cutting the manganese carbonate-loaded foamed nickel electrode obtained in the step (S2) into a size of 1 x 1cm, and then carrying out electrodeposition in a ferric nitrate solution by adopting a three-electrode system to obtain an iron hydroxide/manganese carbonate-foamed nickel self-supporting electrode, wherein the deposition potential is-0.8V-1.5V (vsAg/AgCl electrode), and the deposition time is 100-600S; the concentration of the ferric nitrate is 0.005-0.02 mol/L;
(S4) the obtained self-supporting electrode is washed with ultrapure water to remove surface residual ions, and then naturally dried.
The iron hydroxide/manganese carbonate-foamed nickel self-supporting electrode is applied to electrocatalysis water oxidation reaction.
Compared with the prior art, the invention has the following beneficial effects:
(1) the substrate foamed nickel adopted by the invention has a three-dimensional porous structure which is beneficial to the permeation of electrolyte and the exposure of active sites
(2) The iron hydroxide/manganese carbonate-foamed nickel self-supporting electrode prepared by the invention is a nanosheet-coated three-dimensional cubic structure, and the structure is favorable for increasing the specific surface area of the material and can expose more active sites.
(3) The manganese carbonate material in the electrode material prepared by the invention has a rich valence structure, and can improve the charge transfer rate.
Drawings
FIG. 1 is a schematic view of the flow structure of the present invention.
FIG. 2 is a scanning electron microscope photograph of the surface of the iron hydroxide/manganese carbonate-nickel foam self-supporting electrode at different hydrothermal temperatures.
FIG. 3 is a graph showing the catalytic performance and stability of the water oxidation reaction of the iron hydroxide/manganese carbonate-nickel foam self-supporting electrode of the present invention.
Detailed Description
The present invention is further illustrated by the following figures and examples, which include, but are not limited to, the following examples.
A preparation method of a self-supporting foam nickel electrode loaded with ferric hydroxide and manganese carbonate for high-efficiency electrocatalysis water oxidation comprises the following steps:
(S1) cutting the required substrate nickel foam into small pieces of 2 × 3cm, and ultrasonically washing the small pieces with dilute hydrochloric acid, absolute ethyl alcohol and ultrapure water for 20 minutes respectively;
(S2) adding a mixed solution of manganese chloride and urea into a 50ml of polytetrafluoroethylene-lined hydrothermal reaction kettle, immersing the foamed nickel subjected to ultrasonic washing in the mixed solution (S1), and carrying out hydrothermal reaction at 120 ℃ for 8-15h to obtain a manganese carbonate-loaded foamed nickel electrode; the concentration of the urea is 0.1-0.2 mol/L; the concentration of the manganese chloride solution is 0.01-0.05 mol/L;
(S3) cutting the manganese carbonate-loaded foamed nickel electrode obtained in the step (S2) into a size of 1 x 1cm, and then carrying out electrodeposition in a ferric nitrate solution by adopting a three-electrode system to obtain an iron hydroxide/manganese carbonate-foamed nickel self-supporting electrode, wherein the deposition potential is-0.8V-1.5V (vsAg/AgCl electrode), and the deposition time is 100-600S; the concentration of the ferric nitrate is 0.005-0.02 mol/L;
(S4) the obtained self-supporting electrode is washed with ultrapure water to remove surface residual ions, and then naturally dried.
The specific embodiments are as follows:
example 1
Fig. 1 is a flow chart of electrode preparation, which comprises the following specific steps: cutting the purchased foam nickel substrate into 3 x 2cm, and respectively carrying out ultrasonic washing for 20 minutes by using dilute hydrochloric acid, absolute ethyl alcohol and ultrapure water to remove oxides and organic impurities remained on the foam nickel. Then 40ml of mixed aqueous solution of manganese chloride and urea is added into a stainless steel hydrothermal reaction kettle, wherein the concentration of the manganese chloride solution is 0.025 mol/L, and the concentration of the urea solution is 0.125 mol/L. Immersing the foamed nickel in the solution to carry out hydrothermal reaction at 120 ℃ for 11 hours; then, electrodeposition was carried out in a 0.01 mol/L ferric nitrate solution using a three-electrode system at a deposition potential of-1V (vsAg/AgCl electrode) for a deposition time of 300 s. Finally obtaining the self-supporting electrode of ferric hydroxide/manganese carbonate-foamed nickel. A self-supporting electrode of iron hydroxide/manganese carbonate-nickel foam was applied to electrocatalytic water oxidation reactions.
As can be seen from fig. 2, at a hydrothermal temperature of 100 ℃, a cubic structure has not yet been formed; when the hydrothermal temperature is 120 ℃, the shape is a three-dimensional cubic structure coated by the nano-sheets; at a hydrothermal temperature of 150 ℃, the surfaces of the cubes become very smooth; at a hydrothermal temperature of 180 ℃, the cubic structure starts to crack.
As can be seen from FIG. 3, the electrodes were tested for their catalytic performance by linear voltammetry (LSV) at electrochemical workstation CHI660e, which showed the best electrocatalytic effect at a hydrothermal temperature of 120 ℃ and a current density of 10 mA/cm2When the voltage is high, the overpotential is only 213mV, and the Tafel slope is 31.8 mV/dec. Can be stabilized for more than 23h in the stability test of constant current long-time electrolysis, and the effect is basically kept unchanged.
The above embodiments are only preferred embodiments of the present invention, and are not intended to limit the scope of the present invention, but all changes that can be made by applying the principles of the present invention and performing non-inventive work on the basis of the principles shall fall within the scope of the present invention.
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|---|---|---|---|---|
| CN102655231A (en) * | 2012-05-08 | 2012-09-05 | 广州市香港科大霍英东研究院 | A new method for preparing LiMn2O4 cathode material for lithium-ion batteries with high power performance |
| CN105000598A (en) * | 2015-05-08 | 2015-10-28 | 青岛科技大学 | Method for preparing manganese carbonate hollow spheres |
| CN107195878A (en) * | 2017-05-08 | 2017-09-22 | 陕西科技大学 | A kind of preparation method of manganese monoxide/N doping redox graphene combination electrode material |
| CN107973333A (en) * | 2016-10-25 | 2018-05-01 | 中国科学院苏州纳米技术与纳米仿生研究所 | Metal composite oxide, its preparation method and application with hollow sea urchin shape structure |
| CN108557892A (en) * | 2018-06-07 | 2018-09-21 | 江苏大学 | A kind of oxide preparation method and application for the manganese that object is mutually controllable |
| CN110975907A (en) * | 2019-12-02 | 2020-04-10 | 大连理工大学 | Preparation method of foam nickel electrode loaded with iron and basic cobalt carbonate for catalyzing oxidation of water or organic matters |
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2020
- 2020-11-02 CN CN202011201891.9A patent/CN112342563A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102655231A (en) * | 2012-05-08 | 2012-09-05 | 广州市香港科大霍英东研究院 | A new method for preparing LiMn2O4 cathode material for lithium-ion batteries with high power performance |
| CN105000598A (en) * | 2015-05-08 | 2015-10-28 | 青岛科技大学 | Method for preparing manganese carbonate hollow spheres |
| CN107973333A (en) * | 2016-10-25 | 2018-05-01 | 中国科学院苏州纳米技术与纳米仿生研究所 | Metal composite oxide, its preparation method and application with hollow sea urchin shape structure |
| CN107195878A (en) * | 2017-05-08 | 2017-09-22 | 陕西科技大学 | A kind of preparation method of manganese monoxide/N doping redox graphene combination electrode material |
| CN108557892A (en) * | 2018-06-07 | 2018-09-21 | 江苏大学 | A kind of oxide preparation method and application for the manganese that object is mutually controllable |
| CN110975907A (en) * | 2019-12-02 | 2020-04-10 | 大连理工大学 | Preparation method of foam nickel electrode loaded with iron and basic cobalt carbonate for catalyzing oxidation of water or organic matters |
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Application publication date: 20210209 |