CN105148920A - Self-supporting transition metal-metal alloy catalyst as well as preparation method and application of self-supporting transition metal-metal alloy catalyst - Google Patents
Self-supporting transition metal-metal alloy catalyst as well as preparation method and application of self-supporting transition metal-metal alloy catalyst Download PDFInfo
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Abstract
The invention provides a self-supporting transition metal-metal alloy catalyst as well as a preparation method and an application of the self-supporting transition metal-metal alloy catalyst and belongs to fields of alkaline oxygen evolution and water decomposition of a whole electrolytic tank. The catalyst is prepared according to steps as follows: two or more kinds of metal salt of transition metal elements are mixed, and electrolyte is obtained; electrolytic deposition is performed in the electrolyte with a transition metal conductive substrate as a working electrode, and the self-supporting transition metal-metal alloy catalyst is obtained. The invention provides the self-supporting transition metal-metal alloy catalyst obtained with the preparation method. The prepared self-supporting transition metal-metal alloy catalyst is applied in the electrolytic tank and has excellent electro-catalytic hydrogen evolution and oxygen evolution performance.
Description
Technical field
The present invention relates to the full electrolytic cell water decomposition field of alkalescence, be specifically related to a kind of self-supporting transition metal-metal alloy catalyst and its preparation method and application.
Background technology
Enter 21 century, the increase of energy resource consumption and the quick use of fossil fuel make facing mankind the Tough questions of the exploitation High-efficiency Sustainable energy.Therefore, in order to realize the sustainable development of human society, the regenerative resource that exploitation is cleaned is extremely urgent.Hydrogen is a kind of new forms of energy with the replaceable conventional fossil of petering out of gravimetric energy density.But the production of current Hydrogen Energy also mainly relies on the reformation of coal, natural gas to obtain, and this will inevitably aggravate the consumption of non-regeneration energy and bring problem of environmental pollution.It is store intermittent solar energy and wind energy to provide a possible approach that brine electrolysis prepares hydrogen and oxygen.Utilizing solar energy to carry out photocatalytic water or light helps brine electrolysis, will be the ideal scheme of a kind of " sunlight economy ".Realize electric energy electrolysis or light helps brine electrolysis, the high performance catalyst that preparation possesses liberation of hydrogen ability seems most important.But due to the existence of overpotential of hydrogen evolution (the major cell voltage of commercialization electrolyzer is 1.8-2.0 volt, higher than theoretical minimum value 1.23 volts), make electrolytic process middle slot press large, energy consumption is high.Cathode hydrogen evolution and Oxygen anodic evolution reaction all need efficient electric catalyst to overcome high hydrolysis voltage and then make electrolytic process more efficient.At present, the compound based on iridium and ruthenium illustrates the highest oxygen evolution activity, and platinum group metal is then the most effective liberation of hydrogen catalyst, but rarity and high cost limits its extensive use.The transition-metal catalyst abundant based on the earth's crust that can replace noble metal catalyst in research and development makes great progress.Typical oxygen-separating catalyst comprises based on cobalt (Angew.Chem.Int.Ed., 2009,48,1841; Science, 2008,321,1072), nickel (J.Am.Chem.Soc., 2012,134,6801; Energ.Environ.Sci., 2013,6,2921) and iron (J.Am.Chem.Soc., 2010,132,10990; Nat.Chem., 2011,3,807).And typical liberation of hydrogen catalyst has molybdenum (Nat.Mater., 2012,11,963; Adv.Mater., 2014,26,5702), nickel (Nat.Commun., 2014,5,4695; J.Am.Chem.Soc., 2013,135,9267) and cobalt (J.Am.Chem.Soc., 2014,136,7587; Angew.Chem.Int.Ed., 2014,126,5531) etc.
Development and Design has both the non-precious metal catalyst electrode that high liberation of hydrogen analyses oxygen double function characteristic and receives much concern in same electrolyte.
on commercialization nickel screen, prepare ferronickel layered double-hydroxide etc. being recently reported, and it can be used as liberation of hydrogen to analyse oxygen bifunctional catalyst for alkaline water electrolytic, its current density can reach 10 milliamperes/centimetre under 1.7 volts of voltage
2, corresponding nickel hydroxide catalyst then needs 1.82 volts just can reach same current density (Science2014,345,1593).But its catalytic performance still needs to be further improved, exploitation high-performance liberation of hydrogen oxygen-separating catalyst has huge challenge.
Summary of the invention
The present invention solves the technical problem that existing catalyst activity is low or preparation flow is complicated, and provides a kind of self-supporting transition metal-metal alloy catalyst and its preparation method and application.
The invention provides the preparation method of a kind of self-supporting transition metal-metal alloy catalyst, the method comprises:
Step one: the slaine of two or more transition metal is mixed, obtains electrolyte;
Step 2: with transition metal conductive substrates for working electrode, carries out electro-deposition in the electrolyte that step one obtains, and obtains self-supporting transition metal-metal alloy catalyst.
Preferably, the slaine of described transition metal is one or more in the nitrate of iron, cobalt, nickel, copper, molybdenum or tungsten, chloride, acetate, sulfuric acid, oxalic acid, citric acid, tartaric acid, carbonate.
Preferably, the slaine of described transition metal is cobalt chloride, cobaltous sulfate, ferrous sulfate or nickelous sulfate.
Preferably, described transition metal conductive substrates is nickel screen, titanium net, nickel foil, copper mesh, Copper Foil, stainless (steel) wire, stainless steel foil, ferronickel net, cobalt paper tinsel, titanium net, titanium sheet, molybdenum foil or tungsten paper tinsel.
Preferably, the electrodeposition temperature of described step 2 is 25 DEG C.
Preferably, the described deposition number of turns is 10 ~ 120 circles.
Self-supporting transition metal-metal alloy catalyst that the present invention also provides above-mentioned preparation method to obtain.
The present invention also provides the application of above-mentioned self-supporting transition metal-metal alloy catalyst in electrolytic cell.
Beneficial effect of the present invention
The invention provides a kind of self-supporting transition metal-metal alloy catalyst and preparation method thereof, this catalyst is mixed by the slaine of two or more transition metal, obtains electrolyte; Then with transition metal conductive substrates for working electrode, in the electrolyte obtained, carry out electro-deposition, obtain self-supporting transition metal-metal alloy catalyst.Above-mentioned preparation method is simple, low production cost, and preparation-obtained alloy catalyst is applied in electrolytic cell, has excellent electrocatalytic hydrogen evolution oxygen evolve.
Accompanying drawing explanation
Fig. 1 is the surface sweeping electromicroscopic photograph figure of the nickel-ferro alloy nano-chip arrays that embodiment 1 prepares;
Fig. 2 is the nickel-ferro alloy nano-chip arrays polarization curve in the basic conditions that embodiment 1 prepares;
Fig. 3 is the stereoscan photograph figure of iron-cobalt alloy nano-chip arrays that embodiment 2 prepares;
Fig. 4 is iron-cobalt alloy nano-chip arrays polarization curve in the basic conditions that embodiment 2 prepares.
Detailed description of the invention
The invention provides the preparation method of a kind of self-supporting transition metal-metal alloy catalyst, the method comprises:
Step one: the slaine of two or more transition metal is mixed, obtains electrolyte;
Step 2: with transition metal conductive substrates for working electrode, carries out electro-deposition in the electrolyte that step one obtains, and obtains self-supporting transition metal-metal alloy catalyst.
According to the present invention, the metal salt face of two or more transition metal is mixed, preferably under the condition of magnetic agitation, the slaine of two or more transition metal is dissolved in deionized water respectively, and then mix, obtain electrolyte; The slaine of described transition metal is preferably mole mixing such as grade of two or three, the slaine of described transition metal be preferably in the nitrate of iron, cobalt, nickel, copper, molybdenum or tungsten, chloride, acetate, sulfuric acid, oxalic acid, citric acid, tartaric acid, carbonate one or more, be more preferably cobalt chloride, cobaltous sulfate, ferrous sulfate or nickelous sulfate.
According to the present invention, using transition metal conductive substrates as working electrode, graphite flake is for utilizing electrochemical workstation (CHI660D) electrodepositing transition metal-metal alloy to pole, silver/silver chlorate for reference electrode, depositing temperature is preferably 25 DEG C, the deposition number of turns is preferably 10 ~ 120 circles, be more preferably 30 ~ 60 circles, post-depositional sample can be obtained the transition metal-metal alloy catalyst of self-supporting preferably by with after deionized water and ethanol washing.Described transition metal conductive substrates is preferably nickel screen, titanium net, nickel foil, copper mesh, Copper Foil, stainless (steel) wire, stainless steel foil, ferronickel net, cobalt paper tinsel, titanium sheet, molybdenum foil or tungsten paper tinsel.
Self-supporting transition metal-metal alloy catalyst that the present invention also provides said method to prepare.
The present invention also provides the application of above-mentioned self-supporting transition metal-metal alloy catalyst in electrolytic cell, above-mentioned self-supporting transition metal-metal alloy catalyst is helped battery as the assembling of negative electrode, anode or negative and positive level, utilizes CHI660D type electrochemical workstation to test the electrocatalytic hydrogen evolution oxygen evolve of this electrode in alkaline electrolyte.
Below in conjunction with embodiment, the present invention will be further described in detail.
Embodiment 1
The nickelous sulfate and 0.2 that rubs the 0.2 respectively ferrous sulfate that rubs is dissolved in deionized water, and then mixes, and obtains electrolyte; By nickel screen watery hydrochloric acid, ethanol, deionization cleaning, then add in above-mentioned solution, using nickel screen as working electrode, graphite flake for pole, silver/silver chlorate for reference electrode utilize electrochemical workstation (CHI660D) under 25 DEG C of conditions between-0.2 ~-1.4 volt with cyclic voltammetry deposition 60 circle, nickel screen obtains nickel-ferro alloy nano-chip arrays.
Fig. 1 is the surface sweeping electromicroscopic photograph figure of the nickel-ferro alloy nano-chip arrays that embodiment 1 prepares, wherein figure a is the stereoscan photograph under 20 microns of scales, figure b is the stereoscan photograph under 500 m-n, the figure illustrates nickel screen to be covered completely by nickel-ferro alloy nano-chip arrays, its length is about 0.5 ~ 1 micron, and thickness is 5 ~ 20 nanometers.Fig. 2 is nickel-ferro alloy nano-chip arrays (1 molar potassium hydroxide in the basic conditions that embodiment 1 prepares, pH=14) polarization curve, this figure illustrates that the nickel-ferro alloy nano-chip arrays that the present embodiment 1 obtains carries out performance performance test, works as j=10mAcm
-2time nickel-ferro alloy nano-chip arrays electrode be 1.64 volts relative to current potential during standard hydrogen electrode.
Embodiment 2
The ferrous sulfate and 0.1 that rubs the 0.1 respectively cobalt chloride that rubs is dissolved in deionized water, and then mixes, and obtains electrolyte; By titanium net watery hydrochloric acid, ethanol, deionization cleaning, then add in above-mentioned mixed solution, using titanium net as working electrode, graphite flake for pole, silver/silver chlorate for reference electrode utilize electrochemical workstation (CHI660D) under 25 DEG C of conditions between-0.2 ~-1.4 volt with cyclic voltammetry deposition 30 circle, obtain iron-cobalt alloy nano-chip arrays on the net at titanium.
Fig. 3 is the surface sweeping electromicroscopic photograph figure of iron-cobalt alloy nano-chip arrays that embodiment 2 prepares, wherein figure a is the stereoscan photograph under 50 microns of scales, figure b is the stereoscan photograph under 500 m-n, the figure illustrates titanium net and is covered completely by iron-cobalt alloy nano-chip arrays.Iron embodiment 2 obtained-cobalt alloy nano-chip arrays carries out performance test, works as j=10mAcm
-2shi Tie-cobalt alloy nano-chip arrays catalyst electrode is 1.74 volts (Fig. 4) relative to current potential during standard hydrogen electrode.
Embodiment 3
The cobaltous sulfate and 0.1 that rubs the 0.1 respectively nickelous sulfate that rubs is dissolved in deionized water, and then mixes, and obtains electrolyte; By nickel screen watery hydrochloric acid, ethanol, deionization cleaning, then add in above-mentioned mixed solution, using nickel screen as working electrode, graphite flake for pole, silver/silver chlorate for reference electrode utilize electrochemical workstation (CHI660D) under 25 DEG C of conditions between-0.25 ~-1.35 volt with cyclic voltammetry deposition 30 circle, nickel screen obtains cobalt-nickel alloy nano-chip arrays catalyst.
Cobalt-nickel alloy nano-chip arrays embodiment 3 obtained carries out performance test, works as j=10mAcm
-2time cobalt-nickel alloy nano-chip arrays electrode be 1.76 volts relative to current potential during standard hydrogen electrode.
Embodiment 4
The cobaltous sulfate, 0.1 that rubs 0.1 respectively nickelous sulfate and 0.1 ferrous sulfate that rubs that rubs is dissolved in deionized water, and then mixes, and obtains electrolyte; By nickel screen watery hydrochloric acid, ethanol, deionization cleaning, then add in above-mentioned mixed solution, using nickel screen as working electrode, graphite flake for pole, silver/silver chlorate for reference electrode utilize electrochemical workstation (CHI660D) under 25 DEG C of conditions between-0.2 ~-1.4 volt with cyclic voltammetry deposition 30 circle, nickel screen obtains Co-Ni-Fe alloy nano chip arrays catalyst.
Co-Ni-Fe alloy nano chip arrays embodiment 3 obtained carries out performance test, works as j=10mAcm
-2time Co-Ni-Fe alloy nano chip arrays electrode be 1.72 volts relative to current potential during standard hydrogen electrode.
Claims (8)
1. a preparation method for self-supporting transition metal-metal alloy catalyst, it is characterized in that, the method comprises:
Step one: the slaine of two or more transition metal is mixed, obtains electrolyte;
Step 2: with transition metal conductive substrates for working electrode, carries out electro-deposition in the electrolyte that step one obtains, and obtains self-supporting transition metal-metal alloy catalyst.
2. the preparation method of a kind of self-supporting transition metal-metal alloy catalyst according to claim 1, it is characterized in that, the slaine of described transition metal is one or more in the nitrate of iron, cobalt, nickel, copper, molybdenum or tungsten, chloride, acetate, sulfuric acid, oxalic acid, citric acid, tartaric acid, carbonate.
3. the preparation method of a kind of self-supporting transition metal-metal alloy catalyst according to claim 3, is characterized in that, the slaine of described transition metal is cobalt chloride, cobaltous sulfate, ferrous sulfate or nickelous sulfate.
4. the preparation method of a kind of self-supporting transition-metal alloy catalyst according to claim 1, it is characterized in that, described transition metal conductive substrates is nickel screen, titanium net, nickel foil, copper mesh, Copper Foil, stainless (steel) wire, stainless steel foil, ferronickel net, cobalt paper tinsel, titanium sheet, molybdenum foil or tungsten paper tinsel.
5. the preparation method of a kind of self-supporting transition metal-metal alloy catalyst according to claim 1, is characterized in that, the depositing temperature of described step 2 is 25 DEG C.
6. the preparation method of a kind of self-supporting transition metal-metal alloy catalyst according to claim 1, is characterized in that, the described deposition number of turns is 10 ~ 120 circles.
7. self-supporting transition metal-metal alloy catalyst of obtaining of the preparation method of claim 1-6 described in any one.
8. the application of self-supporting transition metal-metal alloy catalyst according to claim 7 in electrolytic cell.
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Cited By (8)
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| CN106917105A (en) * | 2017-01-13 | 2017-07-04 | 太原理工大学 | A kind of water decomposition preparation method of self-supporting transient metal sulfide foam electrode |
| CN107805826A (en) * | 2016-09-08 | 2018-03-16 | 中国海洋大学 | Possess ferro-phosphorus modified electrode and preparation method that electrocatalytic oxidation separates out performance |
| CN109423660A (en) * | 2017-09-01 | 2019-03-05 | 中国科学院大连化学物理研究所 | A kind of water oxygen elctro-catalyst and preparation method thereof for electrocatalytic decomposition water |
| CN110592614A (en) * | 2019-09-27 | 2019-12-20 | 西南石油大学 | Three-dimensional self-supporting electrocatalyst for preparing hydrogen by water decomposition and preparation method thereof |
| CN112156788A (en) * | 2020-07-28 | 2021-01-01 | 中南大学 | Quaternary Ni-Fe-W-Mo alloy high-efficiency oxygen evolution electrocatalyst and preparation method and application thereof |
| CN113430553A (en) * | 2021-07-23 | 2021-09-24 | 华北电力大学 | Bifunctional catalytic electrode based on transition metal heterogeneous layered structure and preparation method thereof |
| CN113846349A (en) * | 2021-09-28 | 2021-12-28 | 安徽师范大学 | Co-doped molybdenum selenide nanosheet/Mo foil composite material, preparation method and application thereof |
| CN114150343A (en) * | 2022-01-19 | 2022-03-08 | 西南石油大学 | Nano-antler-shaped NiMoCu catalyst and preparation method thereof |
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| CN107805826A (en) * | 2016-09-08 | 2018-03-16 | 中国海洋大学 | Possess ferro-phosphorus modified electrode and preparation method that electrocatalytic oxidation separates out performance |
| CN107805826B (en) * | 2016-09-08 | 2019-07-02 | 中国海洋大学 | Have performance is precipitated in electrocatalytic oxidation ferro-phosphorus modified electrode and preparation method |
| CN106917105B (en) * | 2017-01-13 | 2019-05-31 | 太原理工大学 | A kind of preparation method of water decomposition self-supporting transient metal sulfide foam electrode |
| CN106917105A (en) * | 2017-01-13 | 2017-07-04 | 太原理工大学 | A kind of water decomposition preparation method of self-supporting transient metal sulfide foam electrode |
| CN109423660B (en) * | 2017-09-01 | 2021-02-09 | 中国科学院大连化学物理研究所 | Water oxidation electrocatalyst for electrocatalytic water decomposition and preparation method thereof |
| CN109423660A (en) * | 2017-09-01 | 2019-03-05 | 中国科学院大连化学物理研究所 | A kind of water oxygen elctro-catalyst and preparation method thereof for electrocatalytic decomposition water |
| CN110592614A (en) * | 2019-09-27 | 2019-12-20 | 西南石油大学 | Three-dimensional self-supporting electrocatalyst for preparing hydrogen by water decomposition and preparation method thereof |
| CN112156788A (en) * | 2020-07-28 | 2021-01-01 | 中南大学 | Quaternary Ni-Fe-W-Mo alloy high-efficiency oxygen evolution electrocatalyst and preparation method and application thereof |
| CN113430553A (en) * | 2021-07-23 | 2021-09-24 | 华北电力大学 | Bifunctional catalytic electrode based on transition metal heterogeneous layered structure and preparation method thereof |
| CN113430553B (en) * | 2021-07-23 | 2024-03-08 | 华北电力大学 | Double-function catalytic electrode based on transition metal heterogeneous layered structure and preparation method thereof |
| CN113846349A (en) * | 2021-09-28 | 2021-12-28 | 安徽师范大学 | Co-doped molybdenum selenide nanosheet/Mo foil composite material, preparation method and application thereof |
| CN113846349B (en) * | 2021-09-28 | 2023-02-21 | 安徽师范大学 | Co-doped molybdenum selenide nanosheet/Mo foil composite material, preparation method and application thereof |
| CN114150343A (en) * | 2022-01-19 | 2022-03-08 | 西南石油大学 | Nano-antler-shaped NiMoCu catalyst and preparation method thereof |
| CN114150343B (en) * | 2022-01-19 | 2024-02-06 | 西南石油大学 | Nanometer antler-shaped NiMoCu catalyst and preparation method thereof |
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