CN107217219A - It is a kind of for Fe Co P C systems amorphous elctro-catalyst of efficient evolving hydrogen reaction and preparation method thereof - Google Patents
It is a kind of for Fe Co P C systems amorphous elctro-catalyst of efficient evolving hydrogen reaction and preparation method thereof Download PDFInfo
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- CN107217219A CN107217219A CN201710429114.1A CN201710429114A CN107217219A CN 107217219 A CN107217219 A CN 107217219A CN 201710429114 A CN201710429114 A CN 201710429114A CN 107217219 A CN107217219 A CN 107217219A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/02—Amorphous alloys with iron as the major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/11—Making amorphous alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/003—Making ferrous alloys making amorphous alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/04—Amorphous alloys with nickel or cobalt as the major constituent
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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
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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
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
- C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
- C25B11/061—Metal or alloy
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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
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention discloses a kind of for Fe Co P C systems amorphous elctro-catalyst of efficient evolving hydrogen reaction and preparation method thereof, it is characterised in that:Elctro-catalyst is Fe Co P C systems amorphous alloy strips, and its composition is Fe80‑xCoxP20‑yCy, 0≤x≤50,0≤y≤15, wherein x and y are respectively the atomic percentage of Co elements and C element in Fe Co P C systems amorphous alloy strips.The elctro-catalyst of the present invention is prepared using melt spinning method method, and preparation method is simple, easy to operate, cost is low, environment-friendly, and whole preparation process does not need special installation, can carry out large-scale industrial production, and obtained alloy strip steel rolled stock quality is higher;Fe Co P C frenulums materials prepared by the inventive method can realize the advantages of good conductivity, avtive spot are more, electro catalytic activity is high simultaneously, be a kind of Electrocatalytic Activity for Hydrogen Evolution Reaction material with extensive industrial applications prospect.
Description
Technical field
The present invention relates to the preparation of amorphous alloy strip steel rolled stock and electrocatalysis material application field, and in particular to one kind is used for
The Fe-Co-P-C systems amorphous elctro-catalyst of efficient evolving hydrogen reaction.
Background technology
Hydrogen is expected to substitute fossil fuels as a kind of preferable energy carrier as one kind cleaning, regenerative resource.Water
It is a kind of effective ways for obtaining hydrogen energy source that electrolysis, which produces hydrogen,.Evolving hydrogen reaction is used as one of electro-catalysis hydrolysis important half
Reaction, is the focus of current people's research.
Early stage evolving hydrogen reaction elctro-catalyst is studied, people's perpetual object is mainly the precious metal materials such as Pt, Pd.Your gold
Category material limits the broad commercial applications of itself due to high cost and scarcity.With research and development in recent years,
In order to avoid high use cost, transition metal alloy and its nitride, boride, carbide, sulfide and phosphide
Research in terms of evolving hydrogen reaction electro-catalysis receives extensive attention.A series of transistion metal compounds are prepared out and opened up
Reveal excellent electrocatalysis characteristic.Hereafter related material turns into the study hotspot of electrocatalysis material always.
Non-crystalline material, such as glassy metal (also referred to as glass metal or alloy), it is fine due to having in corrosive medium
Stability and high catalytic activity, thus a kind of potential elctro-catalyst is considered by everybody.Recently, noble metal base
Pd40Ni10Cu30P20With iron-based Fe40Ni40P20The electricity that glassy metal is found to have brilliance urges performance.And Fe bases nanometer material
Material has also met low cost benefit by many experiments confirmation, and with good corrosion resistance characteristic and electro catalytic activity.With
The material of general wet chemical method synthesis is different, and glassy metal is generally mass produced by melt spinning method method, can realized
Widespread commercial application.In view of the premium properties of glassy metal, including excellent mechanical performance, low production cost and good
Good corrosion resistance, designs a kind of non-crystaline amorphous metal based on transition-metal Fe, Co bases and realizes urging for high electrocatalytic properties of hydrogen evolution
Agent be instantly in the urgent need to.Test result indicates that, Fe-Co-P-C amorphous alloy materials are a kind of good elctro-catalysts,
There are high electrocatalytic active and long-time stability in an acidic solution.Based on its superior mechanical performance and low production cost,
Current Fe-Co-P-C is likely to represent a kind of new electrocatalyst materials, with great commercial application prospect.
The content of the invention
The purpose of the present invention is to prepare a series of Fe-Co-P-C systems with superior electric catalytic activity and high stability
Amorphous alloy strips are used for efficient evolving hydrogen reaction, so as to solve that existing elctro-catalyst current density is low, overpotential is high, stability is poor
The problem of.
The present invention adopts the following technical scheme that to realize goal of the invention:
The present invention is used for the Fe-Co-P-C systems amorphous elctro-catalyst of efficient evolving hydrogen reaction, and its feature is:The electro-catalysis
Agent is Fe-Co-P-C systems amorphous alloy strips, and its composition is Fe80-xCoxP20-yCy, 0≤x≤50,0≤y≤15, wherein x and y
The atomic percentage of Co elements and C element respectively in Fe-Co-P-C systems amorphous alloy strips.
The present invention is used for the Fe-Co-P-C systems amorphous elctro-catalyst of efficient evolving hydrogen reaction, and its feature is lain also in:
Alloy raw material Fe, Co purity used in Fe-Co-P-C systems amorphous alloy strips are 99.9wt.%, remaining
Material purity is not less than 99.00wt.%.
The thickness range of described Fe-Co-P-C systems amorphous alloy strips is 10-60 μm.
The preparation method of above-mentioned Fe-Co-P-C systems amorphous elctro-catalyst, comprises the following steps:
(1) preparation of master alloy ingot
According to nominal composition Fe80-xCoxP20-yCy, Fe powder, Co powder, P powder and C powder are subjected to dispensing, then in high-purity Ar gas
Under atmosphere protection, with vacuum arc furnace melting, in order to ensure that the composition of alloying component is uniform, foundry alloy overturns melting repeatedly in stove
More than 4 times, obtain mother alloy ingot;
(2) high vacuum gets rid of band
Mother alloy ingot made from step (1) is melted using the mode of sensing heating, then using melt spinning method method,
Molten state alloy is ejected on the copper roller of rotation at a high speed under high vacuum condition, it is by the heat conduction of copper roller that molten state alloy is quick
Cooling (because this cooling velocity is very fast, can reach the 104K/s-106K/s orders of magnitude, so as to when room temperature solidifies
Continue to keep the disordered structure of its liquid to suppress crystallization, obtain amorphous alloy strip steel rolled stock), obtain for as elctro-catalyst
Fe-Co-P-C systems amorphous alloy strips.
The present invention has the beneficial effect that:
1st, Fe-Co-P-C systems amorphous alloy strips of the invention show excellent glass in wider composition range
Change Forming ability and good electro catalytic activity, be good evolving hydrogen reaction elctro-catalyst, before widespread commercialization application
Scape.
2nd, elctro-catalyst of the invention is prepared using melt spinning method method, and preparation method is simple, easy to operate, cost is low, environment
Close friend, whole preparation process does not need special installation, can carry out large-scale industrial production, obtained alloy strip steel rolled stock quality compared with
It is high;Fe-Co-P-C frenulums material prepared by the inventive method can realize that good conductivity, avtive spot be more, electro catalytic activity is high simultaneously
The advantages of.
Brief description of the drawings
Fig. 1 is the Fe prepared by embodiment 140Co40P13C7The X ray diffracting spectrum and progress 20h of amorphous alloy strips
Electrocatalytic reaction after sample X ray diffracting spectrum;
Fig. 2 is the Fe prepared by embodiment 140Co40P13C7The transmission electron microscope figure of amorphous alloy strips;
Fig. 3 is the Fe prepared by embodiment 140Co40P13C7Amorphous alloy strips are in 0.5M H2SO4It is linear in electrolyte
Scan voltammetry performance curve.
Embodiment
The Fe-Co-P-C systems amorphous alloy strips of following embodiments are prepared using melt spinning method method, device therefor model:
WK, Beijing thing section, China.
The amorphous characteristic of Fe-Co-P-C systems amorphous alloy strips is examined using X-ray diffraction method (XRD) obtained by following embodiments
Survey, device therefor model:X ' Pert Pro MPD X-ray diffractometers, PANalytical (Panalytical), Holland.
The electro catalytic activity of Fe-Co-P-C systems amorphous alloy strips is obtained using electrochemical workstation obtained by following embodiments
, device therefor model:CHI 760E, Shanghai morning is magnificent, China.
Embodiment 1
The present embodiment prepares Fe as follows40Co40P13C7Amorphous alloy strips:
(1) preparation of master alloy ingot
According to nominal composition Fe40Co40P13C7, purity is not less than for 99.9wt.% Fe powder, Co powder and purity
99.00wt.%P powder and C powder carry out dispensing, then under high-purity Ar gas shielded, with vacuum arc furnace melting, in order to ensure alloy
The composition of composition is uniform, and foundry alloy overturns melting more than 4 times repeatedly in stove, slowly melting phosphorus of being tried one's best in each fusion process
Iron and carbon dust, prevent temperature is too high from causing raw material to volatilize, and mother alloy ingot is obtained after finally cooling down.
(2) high vacuum gets rid of band
Using the mode of sensing heating by mother alloy ingot refuse made from step (1), melt spinning method is then utilized
Molten state alloy, is ejected on the copper roller of rotation at a high speed, is closed molten state by the heat conduction of copper roller by method in high vacuum conditions
Golden quick cooling, with obtain wide~2mm, thickness~35 μm Fe40Co40P13C7Amorphous alloy strips.
Fe obtained by the present embodiment is characterized with X-ray diffraction method40Co40P13C7Amorphous alloy strips (the As- in corresponding diagram
Prepared structure), as a result as shown in figure 1, only existing unique width on the XRD spectral lines of non-crystaline amorphous metal and the broad peak of disperse,
Do not see that substantially diffraction maximum corresponding with crystal phase is present, this is the characteristic feature of non-crystaline amorphous metal, can be concluded that these alloys
Band is complete amorphous microstructure.The Fe of the present embodiment40Co40P13C7After electrocatalytic reaction of the amorphous alloy strips through 20h
(the 20h tested in corresponding diagram), its XRD result, which is shown, still has obvious amorphous peak, illustrates that this kind of FeCo bases amorphous is closed
Gold ribbon material has good corrosion resistance.
Reduction processing is carried out to non-crystaline amorphous metal obtained by the present embodiment using Ion Beam Thinner, then passes through transmission electron microscope table again
Surface topography is levied, as shown in Fig. 2 there is not obvious lattice fringe, diffraction spot and crystal diffraction ring, is proved again
Gained alloy is amorphous structure.
Under the conditions of microwave power 100W, by the Fe obtained by the present embodiment40Co40P13C7Amorphous alloy strips are in acetone
Ultrasound 30 minutes, is then washed, vacuum drying chamber is dried, and obtains the test of surface cleaning with deionized water and absolute ethyl alcohol successively
Sample;Gained test specimens are used for electrolysis water (evolving hydrogen reaction) electrocatalytic reaction, electro-chemical activity test is carried out:Test specimens are clipped in
On corresponding electrode holder, tested using three-electrode system with linear sweep voltammetry, electrolyte is 0.5M H2SO4Solution,
Measurement under speed is swept for 100mV/s in sweep speed, as a result shows that sample current density can reach in overpotential 124mV
10mAcm-2。
Embodiment 2
The present embodiment prepares Fe-Co-P-C systems amorphous elctro-catalyst by the identical method of embodiment 1, differs only in change
Nominal composition during each feed proportioning, to obtain the band of heterogeneity.The dimensional parameters of gained sample are as shown in table 1, through table
Levy, each sample is all amorphous structure, and with good electro catalytic activity.
The composition and dimensional parameters of the Fe-Co-P-C systems amorphous alloy strips sample segment of table 1
Sample composition | Width (mm) | Thickness (um) |
Fe72Co8P13C7 | 2.99 | 39 |
Fe64Co16P13C7 | 1.80 | 51 |
Fe56Co24P13C7 | 1.86 | 31 |
Fe48Co32P13C7 | 2.30 | 47 |
Fe40Co40P13C7 | 2.04 | 35 |
Fe26Co44P15C15 | 2.24 | 29 |
Fe45Co35P20 | 1.99 | 28 |
These are only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all the present invention spirit and
Any modifications, equivalent substitutions and improvements made within principle etc., should be included in the scope of the protection.
Claims (4)
1. a kind of Fe-Co-P-C systems amorphous elctro-catalyst for efficient evolving hydrogen reaction, it is characterised in that:The elctro-catalyst is
Fe-Co-P-C systems amorphous alloy strips, its composition is Fe80-xCoxP20-yCy, 0≤x≤50,0≤y≤15, wherein x and y difference
For the atomic percentage of Co elements and C element in Fe-Co-P-C systems amorphous alloy strips.
2. Fe-Co-P-C systems amorphous elctro-catalyst according to claim 1, it is characterised in that:The Fe-Co-P-C systems are non-
Alloy raw material Fe, Co purity used in peritectic alloy band is 99.9wt.%, and remaining material purity is not less than
99.00wt.%.
3. Fe-Co-P-C systems amorphous elctro-catalyst according to claim 1 or 2, it is characterised in that:Described Fe-Co-P-
The thickness range of C systems amorphous alloy strips is 10-60 μm.
4. the preparation method of Fe-Co-P-C systems amorphous elctro-catalyst described in any one, its feature in a kind of claims 1 to 3
It is, comprises the following steps:
(1) preparation of master alloy ingot
According to nominal composition Fe80-xCoxP20-yCy, Fe powder, Co powder, P powder and C powder are subjected to dispensing, then in high-purity Ar gas shielded
Under, with vacuum arc furnace melting, in order to ensure that the composition of alloying component is uniform, foundry alloy overturn melting repeatedly in stove 4 times with
On, obtain mother alloy ingot;
(2) high vacuum gets rid of band
Mother alloy ingot made from step (1) is melted using the mode of sensing heating, then using melt spinning method method, in Gao Zhen
Molten state alloy is ejected on the copper roller of rotation at a high speed under empty condition, by the heat conduction of copper roller by the fast quickly cooling of molten state alloy
But, obtain for the Fe-Co-P-C systems amorphous alloy strips as elctro-catalyst.
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CN108325544A (en) * | 2018-01-31 | 2018-07-27 | 中国科学院合肥物质科学研究院 | A kind of ternary Cu-Co-P nanometer rods and the preparation method and application thereof |
CN108660474A (en) * | 2018-06-01 | 2018-10-16 | 北京航空航天大学 | (FeaCobNic)xMyRzSystem's analysis oxygen catalysis material and the application on Oxygen anodic evolution electrode |
CN108914156A (en) * | 2018-08-30 | 2018-11-30 | 合肥工业大学 | A kind of Fe-Co-Mo-P-C system amorphous alloy elctro-catalyst and its preparation method and application |
CN109023161A (en) * | 2018-08-30 | 2018-12-18 | 合肥工业大学 | A kind of Fe-Ni-P-C system amorphous alloy elctro-catalyst and its preparation method and application |
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CN110339850A (en) * | 2019-08-21 | 2019-10-18 | 合肥工业大学 | A kind of Fe-Co-Ni-P-C system high-entropy alloy elctro-catalyst and preparation method thereof for evolving hydrogen reaction |
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CN115044841A (en) * | 2022-05-13 | 2022-09-13 | 大连理工大学 | Co-based bulk amorphous alloy with high saturation magnetic induction and large supercooling liquid phase region and preparation method thereof |
CN116334663A (en) * | 2023-05-29 | 2023-06-27 | 中石油深圳新能源研究院有限公司 | Method and device for preparing amorphous transition metal nitride electrocatalyst |
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