CN110055477A - A kind of nanoporous ni-based amorphous alloy material and its application in water electrolysis hydrogen production - Google Patents
A kind of nanoporous ni-based amorphous alloy material and its application in water electrolysis hydrogen production Download PDFInfo
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- CN110055477A CN110055477A CN201910159551.5A CN201910159551A CN110055477A CN 110055477 A CN110055477 A CN 110055477A CN 201910159551 A CN201910159551 A CN 201910159551A CN 110055477 A CN110055477 A CN 110055477A
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Abstract
The present invention relates to a kind of nanoporous ni-based amorphous alloy material and its applications in water electrolysis hydrogen production；Selection and alloy preparation, preparation Ni-Ti-Zr amorphous alloy ribbon and then removal alloying by alloying component prepare nanoporous ni-based amorphous alloy epidermis；Amorphous metal thin strip is cut into section, 30~50min of immersion treatment in 0.1M hydrofluoric acid corrosive liquid is placed it at room temperature, dissolve part Ti, Zr element on surface, form nanoporous ni-based amorphous alloy epidermis, then it impregnates again in deionized water, residual contaminants are dissolved, nanoporous ni-based amorphous alloy material is obtained.The material can effectively reduce the overpotential of hydrogen evolution in alkaline environment to 40mV or less, and integral electrode can be directly prepared by engineering science appropriate design, reduce the complexity of technology for preparing electrode, it is suitble to produce in enormous quantities, provides new thinking and strategy for guide design and the performance optimization of alkaline environment liberation of hydrogen catalyst.
Description
Technical field
The present invention relates to a kind of nanoporous ni-based amorphous alloy materials, can be used for water electrolysis hydrogen production, belong to new material skill
Art and field of new energy technologies.Especially propose a kind of nanoporous ni-based amorphous alloy material and its in water electrolysis hydrogen production
Application.
Background technique
With the worsening of energy problem and environmental problem, hydrogen energy source enters big as a kind of reproducible clean energy resource
Many sights, secondary energy sources of the hydrogen energy source as high effect cleaning are considered as one of following most potential new energy.Hydrogen energy source
Appearance can solve the two large problems that human survival faces, and reach green, sustainable development mode.However substitution fossil energy
Need a large amount of hydrogen.Hydrogen preparation method common at present has water electrolysis hydrogen production, biological hydrogen production, photocatalysis hydrogen production and fossil combustion
Expect the methods of hydrogen manufacturing.In numerous hydrogen production process, the advantage of water electrolysis hydrogen production technology hydrogen feedstock the most significant is at low cost, provides
Source is wide, equipment cost is low, hydrogen purity is high and carbon emission problem is not present.But current water electrolysis hydrogen production technology, because of analysis
Hydrogen electrode overpotential is high, causes production energy consumption larger, to limit the development of hydrogen energy source.Therefore, the liberation of hydrogen for improving electrode is urged
Change activity to have a very big significance.
Precious metals pt, Pd etc. have good electro catalytic activity and lower overpotential of hydrogen evolution as electrode material, still
Since these noble metals are expensive, it is difficult to widely apply in the industrial production, to hinder the universal of hydrogen energy source.And transition
Metallic nickel has resource reserve more abundant, and has certain cathode catalysis liberation of hydrogen ability, is acknowledged as noble metal ideal
Alternate material.The catalytic hydrogen evolution ability of pure metallic nickel still has larger gap with noble metal, suitably takes the mode of alloying can
To promote the catalytic activity of metallic nickel.
The efficient catalytic hydrogen evolution cathode material of hydrogen manufacturing demand is industrialized, i.e., is had under electrode unit geometrical surface standard
There is lower overpotential.This demand makes cathode material that should be provided simultaneously with two elements: the preferably intrinsic catalysis of 1. catalyst
Activity；2. entire cathode has biggish electrochemical surface, to increase effective catalytic site quantity.Traditional galvanoplastic, ball
Although the alloying of metallic nickel may be implemented in the methods of mill method, to improve intrinsic catalytic capability, big electrochemistry table is being constructed
The aspect of area is limited to micro-meter scale rank to the adjusting of catalyst particle size substantially, it is difficult to obtain more preferably effect.
In particular, theoretically there is biggish specific surface area, but after it is prepared into hydrogen-precipitating electrode for powder-type catalyst, due to
There are problems that inevitable particle agglomeration, so that effective catalytic surface product is generally much less than the real table area of catalyst,
The catalytic hydrogen evolution overpotential of electrode is difficult to further decrease.Therefore, find have both good catalytic activity for hydrogen evolution and it is biggish effectively
The Ni-based cathode hydrogen evolution material of catalytic surface is one and significantly works.
Summary of the invention
The purpose of the present invention is there are problems for above-mentioned, a kind of nanoporous ni-based amorphous alloy material is provided, is used in combination
Make cathode hydrogen evolution catalyst, overpotential of hydrogen evolution is effectively reduced, it can steady operation in strong basicity environment.
Technical solution of the present invention:
A kind of nanoporous ni-based amorphous alloy material, geometry are divided into metal inside and porous nickel alloy epidermis two
Point, inner core is ni-based amorphous alloy, outside package one layer of nanoporous ni-based amorphous alloy epidermis, the amorphous alloy inner core at
It is divided into Ni45+b(Ti20Zr35)55-b(b=0~5) at.%, the original of metallic element in the nanoporous ni-based amorphous alloy epidermis
Sub- percentage is Ni:(Ti+Zr)=80+a:20-a (a=0~16), wherein two kinds of elements of Ti, Zr are with oxidation state shape
Formula exists.
The pore size distribution range of the nanoporous ni-based amorphous alloy material nano porous structure is 1~100nm.
The preparation method of nanoporous ni-based amorphous alloy material of the invention, it is characterized in that being prepared by the following steps institute
:
1) selection of alloying component and alloy preparation
It is Ni according to alloying component point45+b(Ti36Zr64)55-b(b=0~5) at.% selects metal material, and raw material is respectively
Mass percent purity be 99.9% pure nickel, 99.9% pure titanium, 99.9% pure zirconium, by the conjunction of arc melting hereafter
Raw material of the gold as preparation precursor strip, after melting, Ni-Ti-Zr alloy cast ingot is made in furnace cooling；
2) Ni-Ti-Zr amorphous alloy ribbon is prepared
Above-mentioned Ni-Ti-Zr alloy pig is removed into superficial oxidation skin, heats alloy pig to molten condition, then by melting
Ni-Ti-Zr alloy gets rid of carrying device preparation Ni-Ti-Zr amorphous alloy ribbon with vacuum；
3) removal alloying prepares nanoporous ni-based amorphous alloy epidermis
The amorphous metal thin strip that step 2) is obtained is cut into section, places it in 0.1M hydrofluoric acid corrosive liquid and soaks at room temperature
Bubble 30~50min of processing, dissolves part Ti, Zr element on surface, forms nanoporous ni-based amorphous alloy epidermis, then soak again
Bubble in deionized water, dissolves residual contaminants, obtains nanoporous ni-based amorphous alloy material.
Nanoporous ni-based amorphous alloy material of the invention is used as the evolving hydrogen reaction catalyst during electrolysis water.
The nanoporous nickel-base alloy that the present invention obtains mainly exists as an amorphous form, reduces alloying element and occurs partially
The tendency of analysis constitutes Ni/ so that Ti, Zr element of alloy surface are uniformly distributed in metallic nickel and exist with oxidation states
TixZryOzType metal/oxide composite catalyzing site.On the one hand, the disperse shape distribution of Ti, Zr element can promote unit electrochemistry
Ni/Ti on surfacexZryOzThe quantity of type catalytic site.Wherein, Ti, Zr of oxidation state can optimize the electronic structure of W metal,
Ni-H bond strength is reduced, the desorption of absorption hydrogen is promoted to be precipitated；Meanwhile Ti, Zr of oxidation state are conducive to the HO- in activated water molecule
H key promotes the Dissociative process of hydrone in alkaline environment.On the other hand, nano-porous structure can effectively increase material
Electrochemical surface area.Above-mentioned two aspects factor synergistic effect can significant increase material catalytic hydrogen evolution activity.
The present invention also remains the amorphous state object of alloy skeleton while the nano-porous structure for constructing high surface area
Phase, the remaining metal element Ti of material surface, Zr exist in the form of oxidation state.The material can effectively reduce electrolysis water liberation of hydrogen
Overpotential, and can be with stably catalyzed liberation of hydrogen 60 hours or more to 40mV hereinafter, reduce the power consumption of water electrolysis hydrogen production process.It is logical
Electrode structural designs appropriate are crossed, can be prepared into " collector-catalyst " integrated type composite material, liberation of hydrogen electricity can be directly used as
Pole.Material catalytic hydrogen evolution of the present invention is functional, and core preparation process has certain universality, convenient for design and exploitation
At various geometries and the integral type hydrogen-precipitating electrode of dimensional parameters, to meet the use demand of different type electrolysis unit.It is suitable
It closes and produces in enormous quantities, provide new thinking and strategy for guide design and the performance optimization of alkaline environment liberation of hydrogen catalyst.
Detailed description of the invention
Fig. 1 shines for the surface microhardness scanning electron microscope of nanoporous ni-based amorphous alloy material obtained in the present invention
Piece.
Fig. 2 is the transmission electron microscope photo of nanoporous ni-based amorphous alloy material obtained in the present invention.
Fig. 3 is the high-resolution-ration transmission electric-lens photo of nanoporous ni-based amorphous alloy material obtained and corresponding in the present invention
Fourier transformation figure.
Fig. 4 is the X ray diffracting spectrum of nanoporous ni-based amorphous alloy material obtained in the present invention.
Fig. 5 is the X-ray photoelectricity of Ti, Zr element of nanoporous ni-based amorphous alloy material surface obtained in the present invention
Sub- power spectrum (XPS) figure.
Polarization curve of the Fig. 6 for nanoporous ni-based amorphous alloy material obtained in the present invention in 1M KOH electrolyte
(LSV) figure.
Long period analysis of the Fig. 7 for nanoporous ni-based amorphous alloy material obtained in the present invention in 1M KOH electrolyte
Stabilized hydrogen test result figure.
Polarization curve of the Fig. 8 for nanoporous ni-based amorphous alloy material obtained in the present invention in 1M KOH electrolyte
(LSV) figure.
Specific embodiment
It is described further technical solution of the invention below in conjunction with specific embodiment, these embodiments cannot manage
It solves to be the limitation to technical solution.
Embodiment 1:
1) selection of alloying component and alloy preparation
It is Ni according to alloying component point45Ti20Zr35(b=0) at.% selects metal material, and raw material is respectively quality percentage
Than purity be 99.9% pure nickel, 99.9% pure titanium, 99.9% pure zirconium, and by this alloy of well known arc melting work
For the raw material for preparing precursor strip, after melting, Ni-Ti-Zr alloy cast ingot is made in furnace cooling；
2) Ni-Ti-Zr precursor amorphous alloy ribbon is prepared
Above-mentioned Ni-Ti-Zr alloy pig is removed into superficial oxidation skin, heats alloy pig to molten condition, then by melting
Ni-Ti-Zr alloy gets rid of carrying device preparation Ni-Ti-Zr amorphous alloy ribbon with vacuum；
3) removal alloying prepares nanoporous ni-based amorphous alloy epidermis
4cm length will be intercepted on Ni-Ti-Zr amorphous alloy thin band made from step 2), place it in 0.1M at room temperature
It carries out freely taking off alloy treatment 30min in hydrofluoric acid corrosive liquid, then the product of acquisition is impregnated in deionized water, is dissolved residual
Pollutant is stayed, the nanoporous ni-based amorphous alloy material with interlayer structure, ingredient Ni are obtained80(Ti+Zr)20。
Fig. 1 shines for the surface microhardness scanning electron microscope of nanoporous ni-based amorphous alloy material obtained in the present invention
Piece.
Fig. 2 is the transmission electron microscope photo of nanoporous ni-based amorphous alloy material obtained in the present invention, which has
Hole abundant can effectively increase electrochemical surface area.
Fig. 3 be nanoporous ni-based amorphous alloy material obtained in the present invention high-resolution-ration transmission electric-lens photo (A1,
B1) and corresponding Fourier transformation figure (A2, B2), by high-resolution-ration transmission electric-lens photo it can be seen that the not formed long-range of the material has
The atomic arrangement structure of sequence does not occur diffraction ring it can be seen from its Fourier transformation figure, therefore can determine and be with amorphous phase
Main object phase.
Fig. 4 is the X ray diffracting spectrum of nanoporous ni-based amorphous alloy material obtained in the present invention.XRD diffraction pattern
Do not occur the diffraction maximum of obvious crystalline phase in spectrum, shows that main object is mutually amorphous phase.
Fig. 5 is the X-ray photoelectricity of Ti, Zr element of nanoporous ni-based amorphous alloy material surface obtained in the present invention
Sub- power spectrum (XPS) figure.Ti element 2p3/2 and 2p1/2 characteristic peak respectively appears near 458.8eV and 464.4eV, corresponding oxidation
The Ti of valence state；Zr element 3d5/2 and 2p3/2 characteristic peak mainly appears near 182.5eV and 184.9eV, corresponding oxidation state
Zr, separately there is lesser 3d5/2 characteristic peak to appear near 178.8eV, the Zr of corresponding metal state.XPS is the result shows that nanometer
Porous Ni-base amorphous alloy material Ti, Zr element remained on surface exists in the form of the oxide substantially.In alkaline environment, table
Face oxide can activated water molecule, be conducive to electrochemistry liberation of hydrogen process.
Polarization curve of the Fig. 6 for nanoporous ni-based amorphous alloy material obtained in the present invention in 1M KOH electrolyte
(LSV) figure.Compared to metal nickel electrode (overpotential of hydrogen evolution about 270mV), nanoporous ni-based amorphous alloy material can reduce analysis
Hydrogen overpotential is to 40mV hereinafter, effectively reducing additional energy consumption.
Long period analysis of the Fig. 7 for nanoporous ni-based amorphous alloy material obtained in the present invention in 1M KOH electrolyte
Stabilized hydrogen test result figure, which can continue catalytic hydrogen evolution in alkaline environment can still keep lower after 60 hours
Overpotential shows with good stability.
Embodiment 2:
1) selection of alloying component and alloy preparation
It is Ni according to alloying component point50Ti18Zr32At.% selects metal material, and raw material is respectively mass percent purity
For 99.9% pure nickel, 99.9% pure titanium, 99.9% pure zirconium, and pass through this alloy of well known arc melting as preparation
The raw material of precursor strip, after melting, Ni-Ti-Zr alloy cast ingot is made in furnace cooling；
2) Ni-Ti-Zr precursor amorphous alloy ribbon is prepared
Above-mentioned Ni-Ti-Zr alloy pig is removed into superficial oxidation skin, heats alloy pig to molten condition, then by melting
Ni-Ti-Zr alloy gets rid of carrying device preparation Ni-Ti-Zr amorphous alloy ribbon with vacuum；
3) removal alloying prepares nanoporous ni-based amorphous alloy epidermis
4cm length will be intercepted on Ni-Ti-Zr amorphous alloy thin band made from step 2), place it in 0.1M at room temperature
It carries out freely taking off alloy treatment 40min in hydrofluoric acid corrosive liquid, then impregnates the product of acquisition 5 minutes in deionized water,
Residual contaminants are dissolved, the nanoporous ni-based amorphous alloy material with interlayer structure, ingredient Ni are obtained96(Ti+Zr)4。
Fig. 8 is bent for polarization of the nanoporous ni-based amorphous alloy material obtained in the present embodiment in 1M KOH electrolyte
Line (LSV) figure.In 10mA/cm2Cathode-current density standard under, overpotential of hydrogen evolution 32mV.
Embodiment 3:
1) selection of alloying component and alloy preparation
It is Ni according to alloying component point47.5Ti18.9Zr33.6At.% selects metal material, and raw material is respectively mass percent
Purity be 99.9% pure nickel, 99.9% pure titanium, 99.9% pure zirconium, and pass through this alloy conduct of well known arc melting
The raw material for preparing precursor strip, after melting, Ni-Ti-Zr alloy cast ingot is made in furnace cooling；
2) Ni-Ti-Zr precursor amorphous alloy ribbon is prepared
Above-mentioned Ni-Ti-Zr alloy pig is removed into superficial oxidation skin, heats alloy pig to molten condition, then by melting
Ni-Ti-Zr alloy gets rid of carrying device preparation Ni-Ti-Zr amorphous alloy ribbon with vacuum；
3) removal alloying prepares nanoporous ni-based amorphous alloy epidermis
4cm length will be intercepted on Ni-Ti-Zr amorphous alloy thin band made from step 2), place it in 0.1M at room temperature
It carries out freely taking off alloy treatment 40min in hydrofluoric acid corrosive liquid, then the product of acquisition is impregnated in deionized water, is dissolved residual
Pollutant is stayed, the nanoporous ni-based amorphous alloy material with interlayer structure, ingredient Ni are obtained85(Ti+Zr)15。
Nanoporous ni-based amorphous alloy material obtained is in 1M KOH electrolyte in the present embodiment, 10mA/cm2Yin
Under electrode current density criterion, overpotential of hydrogen evolution 30mV illustrates that precursor alloying component changes not in a small range in conjunction with example 2
The catalytic hydrogen evolution performance of final resulting materials can be significantly affected.In actual industrial preparation process, the consistency of final products
It is often difficult to strictly accurately control, and the permission of this precursor ingredient small range fluctuation, be conducive to avoid the consistent of material
The harsh limitation of property.
All methods and technology of preparing that the present invention is disclosed and proposed, those skilled in the art can be by using for reference in this paper
Hold, the links such as appropriate feed change and process route are realized, are preferably implemented although method and technology of preparing of the invention has passed through
Example is described, related technical personnel obviously can not depart from the content of present invention, in spirit and scope to as described herein
Methods and techniques route is modified or reconfigures, to realize final technology of preparing.In particular, it should be pointed out that Suo Youxiang
Similar replacement and change is apparent to those skilled in the art, they are considered as being included in essence of the invention
In mind, range and content.
Claims (4)
1. a kind of nanoporous ni-based amorphous alloy material, it is characterised in that the crystallographic structure of the material is amorphous state, is had both
Nano-porous structure, and the atomic percentage ratio of the metallic element of material surface is Ni:(Ti+Zr)=80+a:20-a (a=0
~16)；Wherein, two kinds of elements of Ti, Zr exist in the form of oxidation state.
2. nanoporous ni-based amorphous alloy material as described in claim 1, it is characterized in that the aperture of nano-porous structure point
Cloth range is 1~100nm.
3. the preparation method of nanoporous ni-based amorphous alloy material as described in claim 1, it is characterized in that by following steps
Preparation gained:
1) selection of alloying component and alloy preparation
It is Ni according to alloying component point45+b(Ti36Zr64)55-b(b=0~5) at.% selects metal material, and raw material is respectively quality
Percent purity be 99.9% pure nickel, 99.9% pure titanium, 99.9% pure zirconium, make by arc melting alloy hereafter
For the raw material for preparing precursor strip, after melting, Ni-Ti-Zr alloy cast ingot is made in furnace cooling；
2) Ni-Ti-Zr amorphous alloy ribbon is prepared
Above-mentioned Ni-Ti-Zr alloy pig is removed into superficial oxidation skin, heats alloy pig to molten condition, then by the Ni- of melting
Ti-Zr alloy gets rid of carrying device preparation Ni-Ti-Zr amorphous alloy ribbon with vacuum；
3) removal alloying prepares nanoporous ni-based amorphous alloy epidermis
The amorphous metal thin strip that step 2) is obtained is cut into section, is placed it in 0.1M hydrofluoric acid corrosive liquid at room temperature at immersion
30~50min is managed, part Ti, Zr element on surface is dissolved, nanoporous ni-based amorphous alloy epidermis is formed, is then immersed in again
In deionized water, residual contaminants are dissolved, obtain nanoporous ni-based amorphous alloy material.
4. nanoporous ni-based amorphous alloy material as described in claim 1 is used as the evolving hydrogen reaction catalysis during electrolysis water
Agent.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110408950A (en) * | 2019-08-30 | 2019-11-05 | 南通大学 | A kind of electrolysis water cathode and preparation method thereof based on microcosmic blasting technology |
| CN110648852A (en) * | 2019-10-09 | 2020-01-03 | 温州大学 | Counter electrode and quantum dot sensitized solar cell |
| CN110923752A (en) * | 2019-10-29 | 2020-03-27 | 东北大学 | Transition metal powder with high specific surface area and preparation method thereof |
| CN113668005A (en) * | 2021-09-08 | 2021-11-19 | 四川华能氢能科技有限公司 | Porous nickel electrode and preparation method thereof |
| CN114855104A (en) * | 2022-04-27 | 2022-08-05 | 南京理工大学 | Method for regulating amorphous energy state to enhance catalytic performance |
| CN115558951A (en) * | 2022-10-18 | 2023-01-03 | 海南大学 | Amorphous nano porous nickel alloy integrated electrode, preparation method and application thereof |
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| JP2001316724A (en) * | 2000-05-10 | 2001-11-16 | Alps Electric Co Ltd | Method for manufacturing high frequency core |
| CN108707922A (en) * | 2018-05-03 | 2018-10-26 | 北京科技大学 | A kind of flexible nano is porous/amorphous composite material and preparation method thereof |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110408950A (en) * | 2019-08-30 | 2019-11-05 | 南通大学 | A kind of electrolysis water cathode and preparation method thereof based on microcosmic blasting technology |
| CN110408950B (en) * | 2019-08-30 | 2021-04-27 | 南通大学 | Electrolytic water cathode based on microscopic blasting process and preparation method thereof |
| CN110648852A (en) * | 2019-10-09 | 2020-01-03 | 温州大学 | Counter electrode and quantum dot sensitized solar cell |
| CN110923752A (en) * | 2019-10-29 | 2020-03-27 | 东北大学 | Transition metal powder with high specific surface area and preparation method thereof |
| CN113668005A (en) * | 2021-09-08 | 2021-11-19 | 四川华能氢能科技有限公司 | Porous nickel electrode and preparation method thereof |
| CN114855104A (en) * | 2022-04-27 | 2022-08-05 | 南京理工大学 | Method for regulating amorphous energy state to enhance catalytic performance |
| CN114855104B (en) * | 2022-04-27 | 2024-01-30 | 南京理工大学 | Method for regulating amorphous energy state to enhance catalytic performance |
| CN115558951A (en) * | 2022-10-18 | 2023-01-03 | 海南大学 | Amorphous nano porous nickel alloy integrated electrode, preparation method and application thereof |
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Application publication date: 20190726 |