CN108048869B - A kind of Ni-based active electrode material and preparation method thereof being embedded in ruthenium hafnium composite oxides - Google Patents
A kind of Ni-based active electrode material and preparation method thereof being embedded in ruthenium hafnium composite oxides Download PDFInfo
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Abstract
The present invention provides a kind of Ni-based active electrode material and preparation method thereof for being embedded in ruthenium hafnium composite oxides, the average grain diameter of the ruthenium hafnium composite oxides is 12 nm, and wherein the molar ratio of Hf and (Hf+Ru) are (0.35~0.45): 1.The present invention uses composite electric plating method, and nickel and ruthenium hafnium composite oxides are deposited simultaneously, obtains the Ni-based active electrode material of insertion ruthenium hafnium composite oxides.Resulting materials have superior hydrogen evolution activity, and preparation method is simple, and strong operability, raw material is easy to get, at low cost.
Description
Technical field
The invention belongs to the electrode material fields of Applied Electrochemistry and energy industry, and in particular to one kind has high catalytic property
The electrode material and preparation method thereof of energy.
Background technique
After the advent of electrodes containing metal oxide containing precious metals in 1967, it has been found that there is this type oxide very high electricity to urge
Change activity, therefore referred to as activating oxide material, or referred to as active material.Active material the most superior is aoxidized containing ruthenium
The comprehensive performance of the anode material containing ruthenium, Er Qieke not only can be improved by adulterating non-noble metal j element in object, numerous studies discovery
To be substantially reduced the cost of manufacture of the anode containing ruthenium, so that composite oxides containing ruthenium be made largely to be answered in many electrochemical industries
With.The application of active anode is greatly improved the analysis chlorine and oxygen evolution activity of electrode material, reduces power consumption.Relative to anode
Material, it is more weak to the research of cathode material, electro catalytic activity and the lower nickel gold of stability are still used in many occasions
Belong to or titanium be as cathode material, seriously constrain related electrochemical industry field (including chlorine industry, chloric acid salt industrial,
Pharmaceuticals industry and new energy industry etc.) development.
Before 20 years, external expert's discovery adds the higher constituent element of activity in nickel metal and forms mixture, can make cathode
The activity of material significantly improves (referring to " Ni+RuO2 co-deposited electrodes for hydrogen
Evolution ", " Electrochemical Acta ", 2000, page 45,4195-4202).Later, in electrochemical industry
Ni-based ruthenic oxide (Ni+RuO is succeeded in developing2) active cathode material, i.e., unit oxide is embedded in nickel metal
RuO2.However up to the present, how people are designing the cathode material with embedded structure, and how to introduce doping member
Element, the catalytic activity and corrosion resistance of Lai Tigao insert, does not occur new breakthrough, this to be formed with being constantly progressive for anode material
Contrast.
For this purpose, project of national nature science fund project is presided over by this Research Team, containing for insert can be made by being on the one hand directed to
RuO2The cathode behavior of composite oxides has carried out series of studies (referring to " preparation of Ru-Mn oxide coating Ti cathode and liberation of hydrogen
Performance ", " metal heat treatmet ", 2009,34(11), 36-39 pages), on the other hand for the anode material with embedded structure
Related Mechanism have made intensive studies (referring to " Adding a Spinodal Decomposition Retarder:An
Approach to Improving Electrochemical Properties of Ruthenium–Tin Complex
Oxides ", " Journal of Electrochemical Society ", 2014,161(10), E119-E127 pages).Pass through
The analysis and research of system find that only a few adulterates RuO2It is suitable as the active insert of cathode material.Wherein, it adds
The mixed oxide of the hafnium element of certain content can prepare cathode activity insert, be adaptable to acid medium to develop
New Nickel base composite oxidate active cathode material.
Summary of the invention
The purpose of the present invention is to provide a kind of Ni-based active electrode material for being embedded in ruthenium hafnium composite oxides and its preparations
Method, resulting materials have superior hydrogen evolution activity, and preparation method is simple, and strong operability, raw material is easy to get, cost
It is low.
To achieve the above object, the present invention adopts the following technical scheme:
Routine can be used in a kind of Ni-based active electrode material being embedded in ruthenium hafnium composite oxides, the ruthenium hafnium composite oxides
Thermal decomposition or co-deposition method preparation, wherein the molar ratio of Hf and (Hf+Ru) are (0.35~0.45): 1, ruthenium hafnium combined oxidation
The average grain diameter of object is 12 nm.
The preparation method of the Ni-based active electrode material of the insertion ruthenium hafnium composite oxides, is by Ni-based material degreasing, 6
After being etched 1 hour in the aqueous sulfuric acid of mol/L, rinsed with deionized water, it is dry, it is then immersed in plating solution, is stirring
Under the conditions of be electroplated, pH value that plating solution is controlled during this is 4.4~4.6, and coating bath temperature is 48 DEG C, current density 40
mA·cm-2, electricity is 110 Ccm-2, that is, the Ni-based active electrode material of insertion ruthenium hafnium composite oxides is made；
The Ni-based material is industrial pure ni, nickel screen or nickel plate material；Contain 1.2 mol/L of nickel sulfate hexahydrate, six in the plating solution
0.18 mol/L of hydrated nickel chloride, 0.42 mol/L of boric acid, ruthenium hafnium composite oxides 30g/L.
Remarkable advantage of the invention:
A) present invention is embedded in the ruthenium hafnium composite oxides (Ru that average dimension is 12 nm in nickel-base material1-xHfxO2), make
With the more appropriate nanometer embedded structure of electro-catalysis, the final institutional framework for obtaining high degree of dispersion and high uniformity distribution
Activated centre, so that its more traditional Ni-base cathode material of activity be made to be greatly improved, it may have than Ni-based ruthenic oxide material
More superior comprehensive performance.
B) present invention introduces a high proportion of hafnium oxide in ruthenium hafnium composite oxides insert, can efficiently use dioxy
The high corrosion-resistant for changing hafnium makes the electrode material obtained have good stability in the evolving hydrogen reaction of acid medium, and due to adopting
Precious metal element ruthenium is partially replaced with hafnium, so that cost of manufacture significantly reduces.
C) preparation method of the Ni-based active electrode material of present invention insertion ruthenium hafnium composite oxides, is electroplated using watt type
Method deposits nickel and ruthenium hafnium composite oxides simultaneously that is, on the pure nickel substrate of etched processing, compound to obtain insertion ruthenium hafnium
The Ni-based active electrode material of oxide.
D) the Ni-based active electrode material of present invention gained insertion ruthenium hafnium composite oxides can make cathode assembly, apply
In the electrochemical industries such as chlor-alkali, chlorate, water electrolysis, organic solution electrolysis, electrochemical capacitance, hydrogen storage battery, fuel cell, especially
Evolving hydrogen reaction suitable for acid medium.
E) present invention prepares that raw material is simple, is easy to get, and process stabilizing can reach practical and industrial applications conditions.
Specific embodiment
The present invention uses composite plating method, obtains the Ni-based ruthenium hafnium composite oxides active electrode material with embedded structure
Material, the preparation step of the active electrode material are as follows:
1) processing of Ni-based material: industrial pure ni, nickel screen or nickel plate material degreasing are carved in the aqueous sulfuric acid of 6 mol/L
After erosion 1 hour, rinsed with deionized water, it is dry；
2) 1.2 mol/L of nickel sulfate hexahydrate, 0.18 mol/L of Nickel dichloride hexahydrate, boric acid 0.42 preparation of plating solution: are pressed
The concentration preparation plating solution of mol/L, ruthenium hafnium composite oxides 30g/L；Hf:(Hf+Ru in the ruthenium hafnium composite oxides) mole
Than for 0.35~0.45:1；
3) it is electroplated: Ni-based material after processing being immersed in plating solution, is electroplated under mechanical agitation；Electroplating process
Middle control bath pH value is 4.4~4.6, and coating bath temperature is 48 DEG C, 40 mAcm of current density-2, 110 Ccm of electricity-2,
The Ni-based active electrode material of insertion ruthenium hafnium composite oxides is made.
Three examples of implementation of the invention are described in detailed below, but the present invention is not limited to this.
Embodiment 1
1) use industrial pure ni N6 web material for Ni-based material, using 10% detergent degreasing, then in 50 DEG C, 6 mol/L
It is etched 1 hour in aqueous sulfuric acid, deionized water is rinsed, dry；
2) containing 1.2 mol/L nickel sulfate hexahydrates, 0.18 mol/L Nickel dichloride hexahydrate and 0.42 mol/L boric acid
In solution, (Hf:Hf+Ru moles of composite oxides of ruthenium hafnium that the average dimension through thermolysis process preparation is 12 nm or so is added
Than plating solution is made for 30 g/L of 0.35:1)；
3) plating solution is heated to 48 DEG C, is 4.5 with the pH value that 5 mol/L HCl adjust plating solution, carries out under mechanical stirring
Current density is 40 mAcm-2Constant current electro-deposition, electricity be 110 Ccm-2, that is, insertion ruthenium hafnium composite oxides are made
Ni-based active electrode material.
Using electrochemical workstation, using three-electrode system, with saturated calomel electrode (SCE) for reference electrode, electrolyte
For 0.5 M H2SO4Solution, 25 DEG C of tests.The Tafel slope for measuring the electrode material liberation of hydrogen is 55 mVdecade-1, say
It is bright its with significant electro catalytic activity.
Embodiment 2
1) use industrial pure ni N6 web material for Ni-based material, using 10% detergent degreasing, then in 50 DEG C, 6 mol/L
It is etched 1 hour in aqueous sulfuric acid, deionized water is rinsed, dry；
2) containing 1.2 mol/L nickel sulfate hexahydrates, 0.18 mol/L Nickel dichloride hexahydrate and 0.42 mol/L boric acid
In solution, (Hf:Hf+Ru moles of composite oxides of ruthenium hafnium that the average dimension through thermolysis process preparation is 12 nm or so is added
Than plating solution is made for 30 g/L of 0.45:1)；
3) plating solution is heated to 48 DEG C, is 4.6 with the pH value that 5 mol/L HCl adjust plating solution, carries out under mechanical stirring
Current density is 40 mAcm-2Constant current electro-deposition, electricity be 110 Ccm-2, that is, insertion ruthenium hafnium composite oxides are made
Ni-based active electrode material.
Using electrochemical workstation, using three-electrode system, with saturated calomel electrode (SCE) for reference electrode, electrolyte
For 0.5 M H2SO4Solution, 25 DEG C of tests.The Tafel slope for measuring the electrode material liberation of hydrogen is 56 mVdecade-1, say
It is bright its with significant electro catalytic activity.
Embodiment 3
1) use industrial pure ni N6 web material for Ni-based material, using 10% detergent degreasing, then in 50 DEG C, 6 mol/L
It is etched 1 hour in aqueous sulfuric acid, deionized water is rinsed, dry；
2) containing 1.2 mol/L nickel sulfate hexahydrates, 0.18 mol/L Nickel dichloride hexahydrate and 0.42 mol/L boric acid
Solution in, adding the ruthenium hafnium composite oxides that the average dimension through thermolysis process preparation is 12 nm or so, (Hf:Hf+Ru rubs
You are than being 0.42:1) 30 g/L, plating solution is made；
3) plating solution is heated to 48 DEG C, is 4.6 with the pH value that 5 mol/L HCl adjust plating solution, carries out under mechanical stirring
Current density is 40 mAcm-2Constant current electro-deposition, electricity be 110 Ccm-2, that is, insertion ruthenium hafnium composite oxides are made
Ni-based active electrode material.
Using electrochemical workstation, using three-electrode system, with saturated calomel electrode (SCE) for reference electrode, electrolyte
For 0.5 M H2SO4Solution, 25 DEG C of tests.The Tafel slope for measuring the electrode material liberation of hydrogen is 53 mVdecade-1, say
It is bright its with significant electro catalytic activity.
Comparative example
1) use industrial pure ni N6 web material for Ni-based material, using 10% detergent degreasing, then in 50 DEG C, 6 mol/L
It is etched 1 hour in aqueous sulfuric acid, deionized water is rinsed, dry；
2) containing 1.2 mol/L nickel sulfate hexahydrates, 0.18 mol/L Nickel dichloride hexahydrate and 0.42 mol/L boric acid
In solution, 30 g/L of ruthenic oxide that the average dimension through thermolysis process preparation is 12 nm or so is added, plating solution is made；
3) plating solution is heated to 48 DEG C, is 4.6 with the pH value that 5 mol/L HCl adjust plating solution, carries out under mechanical stirring
Current density is 40 mAcm-2Constant current electro-deposition, electricity be 110 Ccm-2, that is, the titanium dioxide that insertion is free of hafnium is made
The Ni-based active electrode material of ruthenium.
Using electrochemical workstation, using three-electrode system, with saturated calomel electrode (SCE) for reference electrode, electrolyte
For 0.5 M H2SO4Solution, 25 DEG C of tests.The Tafel slope for measuring the electrode material liberation of hydrogen is 93 mVdecade-1。
Comparative illustration, new electrode materials proposed by the present invention have significant electro catalytic activity.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (3)
1. a kind of Ni-based active electrode material for being embedded in ruthenium hafnium composite oxides, it is characterised in that: the ruthenium hafnium composite oxides
The molar ratio of middle Hf and (Hf+Ru) are (0.35~0.45): 1；
The average grain diameter of the ruthenium hafnium composite oxides is 12 nm.
2. Ni-based active electrode material according to claim 1, it is characterised in that: by Ni-based material degreasing, in 6 mol/L
Aqueous sulfuric acid in etch 1 hour after, rinsed with deionized water, it is dry, be then immersed in plating solution, under agitation
It is electroplated, the pH value that plating solution is controlled during this is 4.4~4.6, and coating bath temperature is 48 DEG C, and current density is 40 mA
cm-2, electricity is 110 Ccm-2, that is, the Ni-based active electrode material of insertion ruthenium hafnium composite oxides is made；
Contain 1.2 mol/L of nickel sulfate hexahydrate, 0.18 mol/L of Nickel dichloride hexahydrate, 0.42 mol/L of boric acid, ruthenium in the plating solution
Hafnium composite oxides 30g/L.
3. Ni-based active electrode material according to claim 2, it is characterised in that: the Ni-based material is industrial pure ni, nickel
Net or nickel plate material.
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