CN107398564B - A kind of preparation method of ultra-thin CoNi alloy nano piece - Google Patents
A kind of preparation method of ultra-thin CoNi alloy nano piece Download PDFInfo
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- CN107398564B CN107398564B CN201710614134.6A CN201710614134A CN107398564B CN 107398564 B CN107398564 B CN 107398564B CN 201710614134 A CN201710614134 A CN 201710614134A CN 107398564 B CN107398564 B CN 107398564B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0551—Flake form nanoparticles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses a kind of preparation methods of ultra-thin CoNi alloy nano piece, this method first prepares cobalt nickel cyanogen glue using cobalt chloride and four Potassium Tetracyanonickelates as precursor, then using sodium borohydride as reducing agent, cobalt nickel cyanogen glue can be reduced into the ultra-thin CoNi alloy nano piece of regular shape, size uniformity using the method heated in aqueous solution.Preparation method of the present invention is simple, economical, it is suitble to industrialization large-scale production, and the ultra-thin CoNi alloy nano piece of gained is with good stability and water-soluble, has good OER catalytic activity and stability in alkaline potassium hydroxide solution, has a good application prospect in terms of electrochemistry.
Description
Technical field
The invention belongs to catalyst preparation technical fields, and in particular to a kind of preparation side of ultra-thin CoNi alloy nano piece
Method, the CoNi alloy nano piece show higher catalytic activity and stabilization to oxygen evolution reaction under alkaline condition as catalyst
Property.
Background technique
In recent years, due to Precious Metals Resources rareness, expensive, more and more people begin one's study base metal substance,
Especially non-noble metal alloy.And magnetic metal (such as cobalt, nickel) and its alloy material have high intensity, anticorrosion, high firmly because of it
Degree, ferromagnetism, high catalytic performance etc. and be concerned.The study found that the catalytic performance of special appearance structure is far superior to common
Spheroidal particle.Cobalt-nickel alloy is a kind of typical magnetic alloy, and cobalt-nickel alloy material has good corrosion resistance and thermostabilization
Property, compared to simple substance cobalt, nickel, cobalt-nickel alloy shows more excellent performance in many cases, in magnetic material, fuel electricity
The fields such as pond, electronics and opto-electronic device, biological engineering material are with a wide range of applications, but currently, cobalt-nickel alloy is main
Different-shape is prepared by the way that surfactant or microwave method is added, preparation method is complex.
Summary of the invention
Technical problem to be solved by the present invention lies in provide it is a kind of simply prepare size uniformity, morphology controllable it is ultra-thin
The method of CoNi alloy nano piece.
Solving technical solution used by above-mentioned technical problem is: cobalt chloride solution and four Potassium Tetracyanonickelate aqueous solutions are mixed
It closes uniformly, cobalt nickel cyanogen glue is obtained after standing, sodium borohydride aqueous solution is then added, in room temperature to reduction reaction 1~24 at 80 DEG C
Hour, centrifuge separation, washing, vacuum drying obtain ultra-thin CoNi alloy nano piece.
The concentration of cobalt chloride is 1.5~2.0mol/L, four cyanogen in four Potassium Tetracyanonickelate aqueous solutions in above-mentioned cobalt chloride solution
The concentration of nickel acid potassium is 0.9~1.0mol/L, and the molar ratio of four Potassium Tetracyanonickelates and cobalt chloride is 1:1.5~2.
In above-mentioned preparation method, preferably cobalt chloride solution is uniformly mixed with four Potassium Tetracyanonickelate aqueous solutions, room temperature extremely
4~12 hours are stood at 50 DEG C, obtains cobalt nickel cyanogen glue.
In above-mentioned preparation method, preferably the molar ratio of four Potassium Tetracyanonickelates and sodium borohydride is 1:250~300.
In above-mentioned preparation method, reduction reaction 4~8 hours further preferably at 60~70 DEG C.
Beneficial effects of the present invention are as follows:
1, the present invention first prepares cobalt nickel cyanogen glue using cobalt chloride and four Potassium Tetracyanonickelates as precursor, is then also with sodium borohydride
Former agent restores cobalt nickel cyanogen glue using the method heated in aqueous solution, ultra-thin CoNi alloy nano piece can be obtained, wherein boron hydrogen
The reduction rate of divalent cobalt and nickelous can be accelerated by changing sodium, ensure that the reduction rate gap of product is smaller, keep cobalt nickel synchronous also
Original, to obtain the ultra-thin CoNi alloy nano piece of regular shape, size uniformity.
2, operation of the present invention is simple, and product yield is high, purity is high, and homogeneity is good, is suitble to large-scale production.
3, ultra-thin CoNi alloy nano piece prepared by the present invention is compared with traditional iridium C catalyst, to voltage compared with Gao Shiyou
Preferably analysis oxygen electro catalytic activity uses potentiality with huge in electro-catalysis application aspect.
Detailed description of the invention
Fig. 1 is the TEM figure of ultra-thin CoNi alloy nano piece prepared by embodiment 1.
Fig. 2 is the partial enlarged view of Fig. 1.
Fig. 3 is the Co of ultra-thin CoNi alloy nano piece prepared by embodiment 12pXPS high-resolution be fitted spectrogram.
Fig. 4 is the Ni of ultra-thin CoNi alloy nano piece prepared by embodiment 12pXPS high-resolution be fitted spectrogram.
Fig. 5 is the SEM figure of ultra-thin CoNi alloy nano piece prepared by embodiment 2.
Fig. 6 is the TEM figure of ultra-thin CoNi alloy nano piece prepared by embodiment 3.
Fig. 7 is the test of ultra-thin CoNi nanometer sheet prepared by embodiment 1 and commercialization iridium C catalyst oxygen evolution reaction performance
Figure.
Specific embodiment
The present invention is described in more detail with reference to the accompanying drawings and examples, but protection scope of the present invention and not only limits
In these embodiments.
Embodiment 1
The four Potassium Tetracyanonickelate aqueous solutions of the cobalt chloride solution of 0.5mL 2.0mol/L, 0.5mL 1.0mol/L are added
In 5mL beaker, it is uniformly mixed, stands 8 hours at 40 DEG C, obtain cobalt nickel cyanogen glue, 50mL is then added under agitation
The sodium borohydride aqueous solution of 3.0mol/L, wherein the molar ratio of four Potassium Tetracyanonickelates and cobalt chloride, sodium borohydride is 1:2:300,
Reduction reaction 6 hours, are cooled to room temperature at 70 DEG C, are centrifugated, are washed with deionized, 60 DEG C of dryings in vacuum drying oven,
Up to ultra-thin CoNi alloy nano piece (see Fig. 1~4).
Embodiment 2
5mL is added in the cobalt chloride solution of 0.5mL 1.5mol/L, tetra- Potassium Tetracyanonickelate aqueous solution of 0.5mL 1.0mol/L
In beaker, it is uniformly mixed, stands 8 hours at 40 DEG C, obtain cobalt nickel cyanogen glue, 36mL is then added under agitation
The sodium borohydride aqueous solution of 3.5mol/L, wherein the molar ratio of four Potassium Tetracyanonickelates and cobalt chloride, sodium borohydride is 1:1.5:250,
Reduction reaction 6 hours, are cooled to room temperature at 70 DEG C, are centrifugated, are washed with deionized, and do for 60 DEG C in vacuum drying oven
It is dry to get ultra-thin CoNi alloy nano piece (see Fig. 5).
Embodiment 3
5mL is added in the four Potassium Tetracyanonickelate aqueous solutions of the cobalt chloride solution of 1mL 2.0mol/L, 1mL 1.0mol/L to burn
It in cup, is uniformly mixed, stands 12 hours at room temperature, obtain cobalt nickel cyanogen glue, 100mL is then added under agitation
The sodium borohydride aqueous solution of 3.0mol/L, wherein the molar ratio of four Potassium Tetracyanonickelates and cobalt chloride, sodium borohydride is 1:2:300,
Reduction reaction 24 hours at room temperature are centrifugated, are washed with deionized, and 60 DEG C of dryings are in vacuum drying oven to get ultra-thin
CoNi alloy nano piece (see Fig. 6).
The ultra-thin CoNi alloy nano piece electro-catalysis analysis oxygen that inventor is obtained using embodiment 1, method particularly includes: by 2mg
Ultra-thin CoNi alloy nano piece is added in 1mL aqueous solution, is uniformly mixed, and gained 4 μ L of mixed liquor is taken to be added dropwise on platinum carbon electrode, to
Electro-chemical test is used for after drying, test result to be shown in Fig. 7.As seen from Figure 7, compared with business iridium carbon (IrC) catalyst, the present invention
The ultra-thin CoNi alloy nano piece of preparation has good electro catalytic activity when voltage is higher to electro-catalysis analysis oxygen.
Claims (5)
1. a kind of preparation method of ultra-thin CoNi alloy nano piece, it is characterised in that: by cobalt chloride solution and four Potassium Tetracyanonickelates
Aqueous solution is uniformly mixed, and cobalt nickel cyanogen glue is obtained after standing, sodium borohydride aqueous solution is then added, anti-to reduction at 80 DEG C in room temperature
It answers 1~24 hour, centrifuge separation, washing, vacuum drying obtain ultra-thin CoNi alloy nano piece.
2. the preparation method of ultra-thin CoNi alloy nano piece according to claim 1, it is characterised in that: the cobalt chloride water
The concentration of Chlorine in Solution cobalt is 1.5~2.0mol/L, in four Potassium Tetracyanonickelate aqueous solutions the concentration of four Potassium Tetracyanonickelates be 0.9~
The molar ratio of 1.0mol/L, four Potassium Tetracyanonickelates and cobalt chloride is 1:1.5~2.
3. the preparation method of ultra-thin CoNi alloy nano piece according to claim 1 or 2, it is characterised in that: by cobalt chloride
Aqueous solution is uniformly mixed with four Potassium Tetracyanonickelate aqueous solutions, in room temperature to standing 4~12 hours at 50 DEG C, obtains cobalt nickel cyanogen glue.
4. the preparation method of ultra-thin CoNi alloy nano piece according to claim 1, it is characterised in that: the four cyanogen nickel acid
The molar ratio of potassium and sodium borohydride is 1:250~300.
5. the preparation method of ultra-thin CoNi alloy nano piece according to claim 1, it is characterised in that: at 60~70 DEG C
Reduction reaction 4~8 hours.
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| CN109254048B (en) * | 2018-11-05 | 2021-03-16 | 济南大学 | Preparation method and application of nitrofuran antibiotic sensor based on cobalt-nickel oxide |
| CN109637826B (en) * | 2018-12-14 | 2020-09-08 | 江苏科技大学 | Preparation method and application of cobaltosic oxide-nickel oxide/graphene foam composite electrode material |
| CN113155910B (en) * | 2020-12-18 | 2022-07-19 | 中国石油大学(华东) | Preparation method and application of carbon quantum dot-cobalt tetracyanide nickelate composite material ammonia gas sensor |
| CN112838224B (en) * | 2021-01-25 | 2022-06-10 | 中国科学院大连化学物理研究所 | Proton exchange membrane fuel cell membrane electrode anti-reversal additive and preparation method thereof |
| CN113529107B (en) * | 2021-08-19 | 2022-11-04 | 西安热工研究院有限公司 | Silver nanowire and cobalt-nickel alloy composite oxygen evolution catalytic material and preparation method thereof |
| CN114204043A (en) * | 2021-12-10 | 2022-03-18 | 先进能源产业研究院(广州)有限公司 | Alkaline system hydrazine hydrate fuel cell cathode material and preparation method thereof |
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| CN102796999B (en) * | 2012-08-02 | 2014-04-16 | 黑龙江大学 | Method for preparing two-dimensional self-supporting ultrathin transition metal sheets |
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