CN106486680A - A kind of preparation method of phosphatization stainless steel electrolytic water catalysis material - Google Patents
A kind of preparation method of phosphatization stainless steel electrolytic water catalysis material Download PDFInfo
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- CN106486680A CN106486680A CN201610973167.5A CN201610973167A CN106486680A CN 106486680 A CN106486680 A CN 106486680A CN 201610973167 A CN201610973167 A CN 201610973167A CN 106486680 A CN106486680 A CN 106486680A
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- stainless steel
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/9016—Oxides, hydroxides or oxygenated metallic salts
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M8/00—Fuel cells; Manufacture thereof
- H01M8/10—Fuel cells with solid electrolytes
- H01M8/1016—Fuel cells with solid electrolytes characterised by the electrolyte material
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- 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
- Y02E60/50—Fuel cells
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- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Abstract
The invention belongs to electrocatalysis material preparing technical field and in particular to a kind of preparation method of electrolysis water catalysis material and its full hydrogen production by water decomposition produce oxygen in terms of application.The present invention, with rustless steel as substrate, calcines the phosphatization rustless steel of preparation as electrolysis water catalyst using hypophosphites for phosphorus source in an inert atmosphere together.This phosphatization rustless steel elctro-catalyst not only greatly reduces the overpotential needed for electrolysis water, significantly improves the catalytic performance of electrolysis water, and raw material is cheap and easy to get, simple to operate, is conducive to large-scale industrial production.
Description
Technical field
The invention belongs to electrocatalysis material preparing technical field is and in particular to a kind of phosphatization stainless steel electrolytic water catalysis material
Preparation method.
Background technology
With the continuous development of modern society, the pollution that Fossil fuel produces is also increasingly serious, and this problem causes
The concern of more and more many people, the vital problem that people take up in research and solve this impact human survival, base
In this trend, find that new environmentally friendly and the reproducible energy itself becomes the task of top priority with fuel material.Hydrogen is exactly
A kind of preferable novel energy, and be expected to become topmost energy substance in future.Hydrogen is most plentiful element in the universe,
On earth, ocean occupies 72% surface area, and therefore tellurian protium is almost unlimited.If Hydrogen Energy is made
To utilize for the energy, water circulation as main support system, Hydrogen Energy using can avoid leading to using Fossil fuel in a large number
Atmospheric carbon dioxide concentration increase.The main method of hydrogen manufacturing at present:Fossil fuel hydrogen manufacturing, Methanol Decomposition hydrogen manufacturing, ammonolysis craft system
Hydrogen, the steam reforming reaction hydrogen manufacturing of methane, biological hydrogen production, electrolysis water hydrogen making etc..But as a kind of secondary energy sources, hydrogen
Certain processing can be needed just to obtain, therefore, it is desirable to thoroughly depart from Fossil fuel, the hydrogen energy source realizing cleaning is thus protecting field
Ball border is it should using substantial amounts of natural energy resources with regenerative resource come hydrogen making, meanwhile can not produce new pollution
Thing.In view of the situation, the hydrogen manufacturing of electrocatalytic decomposition water is the technology having application prospect most.The research of nearly more than ten years shows, in water
Remain several big problems in this approach of decomposing hydrogen-production, how to improve efficiency, stability, reduce overpotential, reduce into
This etc., is to be expected to solve one of most effective approach of these problems using catalyst.However, so far, maximally effective product hydrogen
Or produce VPO catalysts be still made up of noble metal, such as Pt (CN201510412672.8, ZL201310020844.8,
US20150072852, JP2004008963) and Ru(DE102011083528、WO2013045318)It is used for producing Deng noble metal
Hydrogen.But the cost of noble metal great number seriously hinders the large-scale production of solar energy fuel.Therefore, for reduces cost, exploitation
Become urgent all the more by the elementary composition available moisture solution catalyst of rich content.The oxide of base metal iron-cobalt-nickel and hydrogen
Oxide etc. is also all demonstrated by excellent electrolysis aqueouss energy, and such as nickel foam (ACS Catal. 2016,6,714 721) is base
The electrolysis water catalyst at bottom, but the mechanical strength of nickel foam is little, complicated process of preparation, condition harshness etc..Rustless steel is extensive
For electrochemistry in industry, its good conductivity, mechanical strength is good.For this reason, we adopt one-step calcination method by rustless steel phosphatization, then
It is directly used in electrocatalytic decomposition water, raw material is cheap and easy to get, technique and its simple, it is easy to accomplish large-scale production.
Content of the invention
It is an object of the invention to provide a kind of cheap preparation method being easily electrolysed water catalyst.With cheap and easy to get
Rustless steel is substrate, by preparing with hypophosphites one-step calcination.Prepared material has good electrocatalytic decomposition Aquatic product
The full decomposability of hydrogen, product oxygen and water.
The present invention provides a kind of preparation method of the electrocatalyst materials of electrocatalytic decomposition water, comprises the following steps:With not
Rust steel is substrate, is obtained through one-step calcination with hypophosphites.The preparation method of the present invention is simple, equipment requirements are low, cheap,
Stable performance, possess the advantage being prepared on a large scale, and the catalytic performance of resulting materials be notable, be expected to produce well society and
Economic benefit;
The calcining heat of methods described is 300-600 DEG C, is incubated 1-5 hour;
The features such as material prepared by the present invention has that cheap, catalytic performance is good, is easy to industrialization.
Brief description
Fig. 1 is the XRD figure of phosphatization stainless steel foam elctro-catalyst prepared by embodiment 1;
Fig. 2 is the SEM figure of phosphatization stainless steel foam elctro-catalyst prepared by embodiment 1;
Fig. 3 and Fig. 4 is respectively HER the and OER figure that phosphatization stainless steel foam elctro-catalyst prepared by embodiment 1 is electrolysed water.
Specific embodiment
Below in conjunction with the accompanying drawings and be embodied as example and further illustrate the present invention it should be appreciated that following embodiment is only used for
The present invention is described, and the unrestricted present invention;
As a kind of preferred version, with stainless steel foam as source metal;
As a kind of preferred version, Sodium Hypophosphite is phosphorus source;
As a kind of preferred version, the calcining heat of step 1 methods described is 500 DEG C;
The performance of above-mentioned electrocatalyst materials is estimated by electrocatalytic decomposition Aquatic product hydrogen and product oxygen, and experimentation is as follows:
With above-mentioned phosphatization stainless steel foam as working electrode, platinum electrode is to electrode, and silver/silver chloride electrode is reference electrode, adopts three
Electrode system carries out electro chemical analysis test in 1M KOH solution;
The structure characterization methods of above-mentioned electrocatalyst materials are:X-ray powder diffraction(XRD)Analysis crystallization situation, scanning electron microscope
(SEM)Observe material morphology,(XPS)The surface chemistry composition of analysis of material.
The invention has benefit that:The present invention provides a kind of electro-catalysis to prepare water decomposition for method of simple and fast
Agent.It is initiation material using rustless steel cheap and easy to get.The present invention obtain decomposition water electrocatalyst materials have inexpensive, efficient,
The advantages of stablize, be easy to large-scale production, substantially reduces electrolysis Aquatic product hydrogen, the overpotential of product oxygen.In addition, the preparation side of the present invention
Method very simple, equipment requirements are low, possess the advantage being prepared on a large scale, and the catalytic performance of resulting materials is notable, be expected to produce
Raw good Social and economic benef@;
Enumerate embodiment further below to describe the present invention in detail.It will similarly be understood that following examples are served only for the present invention
It is further described it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art is according to the present invention's
Some nonessential improvement that the above is made and adjustment belong to protection scope of the present invention.The specific technique of following example
Parameter etc. is also only one of OK range example, and that is, those skilled in the art can pass through the explanation of this paper in suitable model
Enclose interior selection, rather than the concrete numerical value being only defined in hereafter example.
Embodiment 1
A kind of preparation method of water decomposition elctro-catalyst is as follows:By 1cm2Stainless steel foam piece put respectively with 2 grams of sodium hypophosphites
In tube furnace, lower 500 DEG C of argon protection is calcined 2 hours, obtains phosphatization stainless steel foam electrolysis water catalyst;
With the phosphatization stainless steel foam that obtains as working electrode, platinum electrode is to electrode, and silver/silver chloride electrode is reference electrode,
Electro chemical analysis test is carried out in 1M KOH solution using three-electrode system.Result shows that this electrocatalysis material has well
Produce hydrogen and produce oxygen performance, produce hydrogen with producing oxygen and reach 10mA/cm2Overpotential needed for electric current density is respectively 206mv and 298mv;
Embodiment 2
Method is with embodiment 1:By 1cm2Stainless steel foam piece and 2 grams of sodium hypophosphites be individually placed in tube furnace, argon protect
Calcine 2 hours for lower 600 DEG C, obtain phosphatization stainless steel foam electrolysis water catalyst;
Result shows to produce hydrogen and produce oxygen to reach 10mA/cm2Overpotential needed for electric current density is respectively 236mv and 313mv;
Embodiment 3
Method is with embodiment 1:By 1cm2Stainless steel foam piece and 2 grams of sodium hypophosphites be individually placed in tube furnace, argon protect
Calcine 2 hours for lower 400 DEG C, obtain phosphatization stainless steel foam electrolysis water catalyst;
Result shows to produce hydrogen and produce oxygen to reach 10mA/cm2Overpotential needed for electric current density is respectively 242mv and 323mv;
Embodiment 4
In order to investigate the impact to catalyst performance for the calcining heat, apart from the temperature, other reaction conditions such as proportioning raw materials etc. all with
Embodiment 1 is identical.Result shows, improves temperature and has an impact to improving electrolysis water H2-producing capacity, but temperature has an optimum;
Fig. 1 is the XRD figure of prepared electrolysis water catalysis material, as can be seen from the figure still keeps stainless skeleton knot after phosphatization
Structure;
Fig. 2 is the SEM figure of prepared electrolysis water catalysis material, and as can be seen from the figure catalysis material is in sclay texture;
Fig. 3 and Fig. 4 is respectively HER the and OER figure of phosphatization stainless steel electrolytic water, as seen from the figure electrolysis Aquatic product hydrogen and product oxygen after phosphatization
Performance is all remarkably reinforced, and produces hydrogen and overpotential respectively 206mv and 298mv producing oxygen.
Claims (5)
1. a kind of preparation method of phosphatization stainless steel electrolytic water catalysis material it is characterised in that:By stainless steel base and hypophosphorous acid
Salt calcining obtains.
2. method according to claim 1, it is characterised in that calcining heat is 300-600 DEG C, is incubated 1-5 hour.
3. according to claim 1 and 2 methods describeds it is characterised in that stainless steel base includes stainless steel foam, stainless steel fibre
Band, stainless steel cloth etc. have the rustless steel of open structure.
4. according to claim 1 and 2 methods describeds it is characterised in that hypophosphites include sodium hypophosphite, potassium hypophosphite, hypophosphorous acid
The hypophosphites such as calcium.
5. the electrocatalyst materials according to the preparation of Claims 1-4 methods described are it is characterised in that this catalysis material can be used for electricity
The full decomposition of catalytic decomposition Aquatic product hydrogen, product oxygen and water.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109364953A (en) * | 2018-10-30 | 2019-02-22 | 长安大学 | A kind of ferronickel doping sheet MoS2Electro-catalysis hydrogen manufacturing material and preparation method thereof |
CN110093623A (en) * | 2019-04-30 | 2019-08-06 | 苏州科技大学 | Phosphatization stainless steel material and its preparation method and application |
WO2020107952A1 (en) * | 2018-11-30 | 2020-06-04 | 清华大学 | Efficient and stable stainless steel-based electrolytic water catalytic electrode and preparation method therefor and application thereof |
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CN105826573A (en) * | 2016-05-12 | 2016-08-03 | 湖北大学 | Surface treatment method for improving electro-catalysis hydrogen production performance |
CN105839131A (en) * | 2016-06-13 | 2016-08-10 | 成都玖奇新材料科技有限公司 | Water electrolytic hydrogen production catalytic electrode of self-supporting metal-doped cobalt phosphide nano structure |
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CN105951123A (en) * | 2016-05-06 | 2016-09-21 | 湖北大学 | Preparation method for NiCoP nanowire electro-catalytic electrode |
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CN103466574A (en) * | 2013-09-17 | 2013-12-25 | 天津工业大学 | Method for preparing three-dimensional macroporous metal phosphide |
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Cited By (5)
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CN109364953A (en) * | 2018-10-30 | 2019-02-22 | 长安大学 | A kind of ferronickel doping sheet MoS2Electro-catalysis hydrogen manufacturing material and preparation method thereof |
CN109364953B (en) * | 2018-10-30 | 2021-07-27 | 长安大学 | Nickel-iron-doped flaky MoS2Electrocatalytic hydrogen production material and preparation method thereof |
WO2020107952A1 (en) * | 2018-11-30 | 2020-06-04 | 清华大学 | Efficient and stable stainless steel-based electrolytic water catalytic electrode and preparation method therefor and application thereof |
CN110093623A (en) * | 2019-04-30 | 2019-08-06 | 苏州科技大学 | Phosphatization stainless steel material and its preparation method and application |
CN110093623B (en) * | 2019-04-30 | 2020-10-27 | 苏州科技大学 | Phosphated stainless steel material, and preparation method and application thereof |
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Application publication date: 20170308 |