CN106076342A - NiFe alloy nano particle/graphite alkene composite and its preparation method and application - Google Patents
NiFe alloy nano particle/graphite alkene composite and its preparation method and application Download PDFInfo
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- CN106076342A CN106076342A CN201610518702.8A CN201610518702A CN106076342A CN 106076342 A CN106076342 A CN 106076342A CN 201610518702 A CN201610518702 A CN 201610518702A CN 106076342 A CN106076342 A CN 106076342A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
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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
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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
- H01M4/9041—Metals or alloys
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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
Abstract
The invention discloses a kind of NiFe alloy nano particle/graphite alkene composite and its preparation method and application, this preparation method includes: 1) be dispersed in water positive divalent nickel salt, ferrous salt and graphene oxide with prepared system one;2) hydrazine hydrate is mixed and in system one with prepared system two;3) system two is placed in airtight condition and carries out hydro-thermal reaction with prepared NiFe alloy nano particle/graphite alkene composite.The NiFe alloy nano particle/graphite alkene composite prepared by the method has a catalysis activity of excellence to OER, and this preparation method has simple to operate, mild condition and the high advantage of product purity.
Description
Technical field
The present invention relates to composite, in particular it relates to NiFe alloy nano particle/graphite alkene composite and preparation thereof
Methods and applications.
Background technology
Owing to Graphene has a superior electrical conductivity, and with the strong interaction of heterogeneous component, thus graphene-based compound
Material has excellent properties and important application prospect in fields such as energy conversion and storage, environmental improvement and catalysis sensings.Mesh
The research of front graphene-based composite is mainly transition metal oxide/graphene composite material and noble metal/Graphene
Composite.The material compound with Graphene for active transition metal and alloy nano particle thereof but rarely has report.Report
Employing synthetic method in a small amount of material is also that the hydrogen reducing by metal oxide/graphene composite material obtains, this
Method exists that step is tediously long and the defect such as safety is low.
Summary of the invention
It is an object of the invention to provide a kind of NiFe alloy nano particle/graphite alkene composite and preparation method thereof and answer
With, the NiFe alloy nano particle/graphite alkene composite prepared by the method has excellent catalysis activity to OER, and
And this preparation method has simple to operate, mild condition and the high advantage of product purity.
To achieve these goals, the invention provides the system of a kind of NiFe alloy nano particle/graphite alkene composite
Preparation Method, this preparation method includes:
1) positive divalent nickel salt, ferrous salt and graphene oxide are dispersed in water with prepared system one;
2) hydrazine hydrate is mixed and in system one with prepared system two;
3) system two is placed in airtight condition and carries out hydro-thermal reaction with prepared NiFe alloy nanoparticle/graphene oxide
Composite.
The invention provides and go back a kind of NiFe alloy nano particle/graphite alkene composite, this NiFe alloy nanoparticle/
Graphene composite material is prepared by above-mentioned method.
Invention further provides a kind of above-mentioned NiFe alloy nano particle/graphite alkene composite at catalysis OER
In application.
By technique scheme, the present invention is compound with system by NiFe alloy nanoparticle and graphene oxide being carried out
Obtaining NiFe alloy nano particle/graphite alkene composite, wherein, hydrazine hydrate, as reducing agent, will aoxidize stone in recombination process
Ink alkene is reduced into Graphene.This composite has the catalysis activity of excellence to OER (electro-catalysis oxygen evolution reaction), and this is prepared
Method has simple to operate, mild condition and the high advantage of product purity.
Other features and advantages of the present invention will be described in detail in detailed description of the invention part subsequently.
Accompanying drawing explanation
Accompanying drawing is used to provide a further understanding of the present invention, and constitutes the part of description, with following tool
Body embodiment is used for explaining the present invention together, but is not intended that limitation of the present invention.In the accompanying drawings:
Fig. 1 is the TEM detection figure of A1 in detection example 1;
Fig. 2 is the HRTEM detection figure of A1 in detection example 1;
Fig. 3 is the XRD detection figure of A1 and A2 in detection example 1;
Fig. 4 is the TEM detection figure of A2 in detection example 1;
Fig. 5 is the HRTEM detection figure of A2 in detection example 1;
Fig. 6 is the catalysis OER polarization curve of A1 in application examples 1;
Fig. 7 is the Detection of Stability result figure of the catalysis OER of A1 in application examples 1.
Detailed description of the invention
Hereinafter the detailed description of the invention of the present invention is described in detail.It should be appreciated that described herein specifically
Embodiment is merely to illustrate and explains the present invention, is not limited to the present invention.
The invention provides the preparation method of a kind of NiFe alloy nano particle/graphite alkene composite, this preparation method
Including:
1) positive divalent nickel salt, ferrous salt and graphene oxide are dispersed in water with prepared system one;
2) hydrazine hydrate is mixed and in system one with prepared system two;
3) system two is placed in airtight condition carry out hydro-thermal reaction and be combined with prepared NiFe alloy nano particle/graphite alkene
Material.
Step 1 in the preparation method that the present invention provides) in, the consumption of each material can select in wide scope, but
It is to improve the catalysis of prepared NiFe alloy nano particle/graphite alkene composite activity further, it is preferable that in step
1) in, relative to the positive divalent nickel salt of 1mmol, the consumption of ferrous salt is 0.01-2mmol, the consumption 0.01-of graphene oxide
20mg;It is highly preferred that the positive divalent nickel salt relative to 1mmol, the consumption of ferrous salt is 0.25-0.1mmol, graphene oxide
Consumption 5-7mg.
Step 1 in the preparation method that the present invention provides) in, the total concentration of iron ion and nickel ion can be in wide scope
Interior selection, but in order to improve the catalysis activity of prepared NiFe alloy nano particle/graphite alkene composite further, preferably
Ground, in system one, the total concentration of iron ion and nickel ion is 0.1-5mol/L;It is highly preferred that iron ion and nickel ion is total
Concentration is 0.7-0.8mol/L.
Meanwhile, the step 1 in the present invention) in, the consumption of water can select in wide scope, but in order to carry further
The catalysis activity of the high NiFe alloy nano particle/graphite alkene composite prepared, it is preferable that relative to the positive bivalence of 1mmol
Nickel salt, the consumption of water is 5-20mL.
In the present invention, positive divalent nickel salt, the concrete kind of ferrous salt can also select in wide scope, but in order to
Improve the catalysis activity of the NiFe alloy nano particle/graphite alkene composite prepared further, it is preferable that in step 1) in,
Positive divalent nickel salt, ferrous salt are each independently selected from nitrate and/or villaumite.
Step 2 in the present invention) in, the concentration of hydrazine hydrate can select in wide scope, but in order to carry further
The catalysis activity of the high NiFe alloy nano particle/graphite alkene composite prepared, it is preferable that in step 2) in, hydrazine hydrate
Concentration is 10-80 volume %;It is highly preferred that the concentration of hydrazine hydrate is 20-30 volume %.
Step 2 in the present invention) in, the consumption of hydrazine hydrate can select in wide scope, but in order to carry further
The catalysis activity of the high NiFe alloy nano particle/graphite alkene composite prepared, it is preferable that relative to the positive bivalence of 1mmol
Nickel salt, described hydrazine hydrate consumption be 1-10mL.
On the basis of the above, in step 3) in, the actual conditions of hydro-thermal reaction can select in wide scope,
But in order to improve reaction efficiency, it is preferable that hydro-thermal reaction at least meets following condition: reaction temperature is 100-220 DEG C, reaction
Time is 1-24h;It is highly preferred that hydro-thermal reaction at least meets following condition: reaction temperature is 120-180 DEG C, the response time is
6-12h。
The invention provides and go back a kind of NiFe alloy nano particle/graphite alkene composite, this NiFe alloy nanoparticle/
Graphene composite material is prepared by above-mentioned method.
Invention further provides a kind of above-mentioned NiFe alloy nano particle/graphite alkene composite at catalysis OER
In application.
Hereinafter will be described the present invention by embodiment.
Embodiment 1
First, by 6mg graphene oxide powder, the Ni (NO of 0.29g3)2·6H2The FeCl of O and 0.10g2·4H2O dissolves
In 15mL water;Then, add 5mL hydrazine hydrate (volumetric concentration is 25%) and be stirred vigorously;Then above-mentioned mixed system is shifted
Seal to 25mL autoclave, and at 180 DEG C, keep 12h;Finally, it is cooled to 25 DEG C, is centrifuged, washs and is dried, to obtain final product
To NiFe alloy nano particle/graphite alkene composite A 1.
Embodiment 2
Carry out preparing NiFe alloy nano particle/graphite alkene composite A 2 according to the method for embodiment 1, different
It is, by FeCl2·4H2The consumption of O changes 0.05g into.
Embodiment 3
Carry out preparing NiFe alloy nano particle/graphite alkene composite A 3 according to the method for embodiment 1, different
It is, by FeCl2·4H2The consumption of O changes 0.20g into.
Embodiment 4
Carry out preparing NiFe alloy nanoparticle graphene composite material A4 according to the method for embodiment 1, except that,
By FeCl2·4H2The consumption of O changes 0.20g into, by Ni (NO3)2·6H2The consumption of O changes 0.58g into, by graphene oxide powder
Consumption changes 12mg into.
Embodiment 5
Carry out preparing NiFe alloy nano particle/graphite alkene composite A 5 according to the method for embodiment 1, different
It is to be changed the temperature of hydro-thermal reaction into 120 DEG C by 180 DEG C.
Embodiment 6
Carry out preparing NiFe alloy nano particle/graphite alkene composite A 6 according to the method for embodiment 1, different
It is to be changed the time of hydro-thermal reaction into 6h by 12h, by FeCl2·4H2The consumption of O changes 0.20g into.
Comparative example 1
Carry out preparing NiFe alloy nanoparticle according to the method for embodiment 1, except that, do not use graphite oxide
Alkene.
Comparative example 2
Carry out preparing NiFe alloy nanoparticle/carbon black composite material according to the method for embodiment 1, except that, will
Graphene oxide changes white carbon black into.
Detection example 1
1) utilizing transmission electron microscope to characterize A1, result is shown in Fig. 1, utilizes high resolution transmission electron microscopy pair
A1 characterizes, and result is shown in Fig. 2, Fig. 1 and 2 understand NiFe nanoparticle and be dispersed on graphene nanometer sheet.
2) utilizing x-ray diffractometer to characterize A1 and A2, result is shown in Fig. 3, and in product, NiFe is conjunction as shown in Figure 3
Golden nanometer particle (contrasting with standard card, X-ray diffraction peak position is between Fe and Ni simple substance peak, belongs to alloy phase).
3) utilizing transmission electron microscope to characterize A2, result is shown in Fig. 4, utilizes high resolution transmission electron microscopy pair
A2 characterizes, and result is shown in Fig. 5, Figure 4 and 5 the size understanding the composite that different condition obtains can regulate and control.
It addition, TEM, HRTEM of A3-A6 keep consistent with the testing result of XRD with the testing result of A1-A2.
Application examples 1
1) preparation of working electrode
Nafion (5wt%) solution of NiFe alloy nano particle/graphite alkene composite A 1, the 10 μ L of 5mg is added
DMF/H to 1.0mL2In O mixed solvent, ultrasonic disperse uniformly prepares catalyst ink.Take 3.5 μ L catalyst inks and drop to glass
On carbon electrode (diameter 3mm), air dries prepared working electrode D1 naturally.
It is worth working electrode D2, except for the difference that by NiFe alloy nano particle/graphite alkene according to above-mentioned same method
Composite A 1 is changed to NiFe alloy nanoparticle.
It is worth working electrode D3, except for the difference that by NiFe alloy nano particle/graphite alkene according to above-mentioned same method
Composite A 1 is changed to NiFe alloy nanoparticle/carbon black composite material.
2) OER is catalyzed active testing
Employing three-electrode system is tested, and respectively using working electrode D1-D3 as working electrode, Pt plate electrode is to electrode,
Ag/AgCl electrode saturated for KCl is reference electrode, and electrochemical workstation is CHI660C (Shanghai occasion China).Electrolyte is O2Saturated
The KOH solution of 1.0M, use linear sweep voltammetry test O2Separating out signal, chronoptentiometry tests its catalytic stability,
Concrete outcome is shown in Fig. 6 and Fig. 7, and NiFe alloy nano particle/graphite alkene composite has the electro-catalysis work of excellence as seen from the figure
Property and stability.
It addition, the OER catalytic performance of A2-A6 generally maintains consistent with the OER catalytic of A1, NiFe alloy nanoparticle
Catalytic performance is significantly lower than the catalytic performance of NiFe alloy nano particle/graphite alkene composite.
The preferred embodiment of the present invention described in detail above, but, the present invention is not limited in above-mentioned embodiment
Detail, in the technology concept of the present invention, technical scheme can be carried out multiple simple variant, this
A little simple variant belong to protection scope of the present invention.
It is further to note that each the concrete technical characteristic described in above-mentioned detailed description of the invention, at not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to various can
The compound mode of energy illustrates the most separately.
Additionally, combination in any can also be carried out between the various different embodiment of the present invention, as long as it is without prejudice to this
The thought of invention, it should be considered as content disclosed in this invention equally.
Claims (10)
1. the preparation method of a NiFe alloy nano particle/graphite alkene composite, it is characterised in that described preparation method bag
Include:
1) positive divalent nickel salt, ferrous salt and graphene oxide are dispersed in water with prepared system one;
2) hydrazine hydrate is mixed and in described system one with prepared system two;
3) described system two is placed in airtight condition carry out hydro-thermal reaction and be combined with prepared NiFe alloy nano particle/graphite alkene
Material.
Preparation method the most according to claim 1, wherein, in step 1) in, relative to the positive divalent nickel salt of 1mmol, institute
The consumption stating ferrous salt is 0.01-2mmol, the consumption 0.01-20mg of described graphene oxide.
Preparation method the most according to claim 2, wherein, relative to the positive divalent nickel salt of 1mmol, the use of described ferrous salt
Amount is 0.25-0.1mmol, the consumption 5-7mg of described graphene oxide.
Preparation method the most according to claim 3, wherein, in described system one, iron ion and the total concentration of nickel ion
For 0.1-5mol/L.
Preparation method the most according to claim 4, wherein, in described system one, iron ion and the total concentration of nickel ion
For 0.7-0.8mol/L.
6. according to the preparation method described in any one in claim 1-5, wherein, relative to the positive divalent nickel salt of 1mmol, institute
The consumption stating water is 5-20mL;
Preferably, in step 1) in, described positive divalent nickel salt, ferrous salt are each independently selected from nitrate and/or villaumite.
Preparation method the most according to claim 6, wherein, in step 2) in, the concentration of described hydrazine hydrate is 10-80 body
Long-pending %;
Preferably, the concentration of described hydrazine hydrate is 20-30 volume %;
It is highly preferred that the positive divalent nickel salt relative to 1mmol, described hydrazine hydrate consumption be 1-10mL.
8., according to claim 1-5, preparation method described in 7, wherein, described hydro-thermal reaction at least meets following condition: reaction
Temperature is 100-220 DEG C, and the response time is 1-24h;
Preferably, described hydro-thermal reaction at least meets following condition: reaction temperature is 120-180 DEG C, and the response time is 6-12h.
9. a NiFe alloy nano particle/graphite alkene composite, it is characterised in that described NiFe alloy nanoparticle/stone
Ink alkene composite is prepared by the method described in any one in claim 1-8.
10. a NiFe alloy nano particle/graphite alkene composite as claimed in claim 9 application in catalysis OER.
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Cited By (2)
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CN108636425A (en) * | 2018-05-14 | 2018-10-12 | 潍坊学院 | Ferronickel sulfide-graphene composite material, preparation method and application |
WO2021114062A1 (en) * | 2019-12-10 | 2021-06-17 | 陈志勇 | Iron-nickel alloy hydrogenation catalyst and fabrication method therefor |
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