CN107398564A - A kind of preparation method of ultra-thin CoNi alloy nanos piece - Google Patents
A kind of preparation method of ultra-thin CoNi alloy nanos piece Download PDFInfo
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- CN107398564A CN107398564A CN201710614134.6A CN201710614134A CN107398564A CN 107398564 A CN107398564 A CN 107398564A CN 201710614134 A CN201710614134 A CN 201710614134A CN 107398564 A CN107398564 A CN 107398564A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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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- 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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- 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
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The invention discloses a kind of preparation method of ultra-thin CoNi alloy nanos 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, using the method heated in aqueous cobalt nickel cyanogen glue can be reduced into regular shape, size uniformity ultra-thin CoNi alloy nanos piece.Preparation method of the present invention is simple, economical, it is adapted to industrialization large-scale production, and the ultra-thin CoNi alloy nanos piece of gained has good stability and water solubility, there is good OER catalytic activity and stability in alkaline potassium hydroxide solution, there is good application prospect in terms of electrochemistry.
Description
Technical field
The invention belongs to catalyst preparation technical field, and in particular to a kind of preparation side of ultra-thin CoNi alloy nanos piece
Method, the CoNi alloy nanos piece show higher catalytic activity and stably as catalyst to oxygen evolution reaction in the basic conditions
Property.
Background technology
In recent years, expensive because Precious Metals Resources are rare, increasing people begins one's study base metal material,
Especially non-noble metal alloy.And magnetic metal (such as cobalt, nickel) and its alloy material have high intensity, anticorrosion, high hard because of it
Degree, ferromagnetism, high catalytic performance etc. and receive much concern.Research finds 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 under many circumstances, in magnetic material, fuel electricity
The field such as pond, electronics and opto-electronic device, biological engineering material is with a wide range of applications, but at present, cobalt-nickel alloy is main
Different-shape is prepared by adding surfactant or microwave method, and preparation method is complex.
The content of the invention
The technical problems to be solved by the invention be to provide it is a kind of it is simple prepare size uniformity, morphology controllable it is ultra-thin
The method of CoNi alloy nano pieces.
Technical scheme is used by solving above-mentioned technical problem：Cobalt chloride solution and the four Potassium Tetracyanonickelate aqueous solution are mixed
Close uniformly, cobalt nickel cyanogen glue is obtained after standing, then adds sodium borohydride aqueous solution, in room temperature to reduction reaction 1~24 at 80 DEG C
Hour, centrifuge, wash, vacuum drying, obtaining ultra-thin CoNi alloy nanos piece.
The concentration of cobalt chloride is 1.5~2.0mol/L in above-mentioned cobalt chloride solution, four cyanogen in the four Potassium Tetracyanonickelate aqueous solution
The concentration of nickel acid potassium is 0.9~1.0mol/L, and the mol ratio of four Potassium Tetracyanonickelates and cobalt chloride is 1:1.5~2.
In above-mentioned preparation method, preferably cobalt chloride solution is well mixed with the four Potassium Tetracyanonickelate aqueous solution, in room temperature extremely
4~12 hours are stood at 50 DEG C, obtains cobalt nickel cyanogen glue.
In above-mentioned preparation method, preferably the mol 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：
1st, the present invention first prepares cobalt nickel cyanogen glue using cobalt chloride and four Potassium Tetracyanonickelates as precursor, then using sodium borohydride as also
Former agent, cobalt nickel cyanogen glue is reduced using the method heated in aqueous, you can obtain ultra-thin CoNi alloy nanos piece, wherein boron hydrogen
The reduction rate of divalence cobalt and nickelous can be accelerated by changing sodium, ensure that the reduction rate gap of product is smaller, cobalt nickel is synchronously gone back
Original, so as to obtain regular shape, size uniformity ultra-thin CoNi alloy nanos piece.
2nd, the present invention is simple to operate, and product yield is high, and purity is high, and homogeneity is good, is adapted to large-scale production.
3rd, ultra-thin CoNi alloy nanos 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, has huge use potentiality in electro-catalysis application aspect.
Brief description of the drawings
Fig. 1 is the TEM figures of ultra-thin CoNi alloy nanos piece prepared by embodiment 1.
Fig. 2 is Fig. 1 partial enlarged drawing.
Fig. 3 is the Co of ultra-thin CoNi alloy nanos piece prepared by embodiment 12pXPS high-resolution fitting spectrogram.
Fig. 4 is the Ni of ultra-thin CoNi alloy nanos piece prepared by embodiment 12pXPS high-resolution fitting spectrogram.
Fig. 5 is the SEM figures of ultra-thin CoNi alloy nanos piece prepared by embodiment 2.
Fig. 6 is the TEM figures of ultra-thin CoNi alloy nanos piece prepared by embodiment 3.
Fig. 7 is the test of ultra-thin CoNi nanometer sheets and commercialization iridium C catalyst oxygen evolution reaction performance prepared by embodiment 1
Figure.
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
0.5mL 2.0mol/L cobalt chloride solution, 0.5mL the 1.0mol/L four Potassium Tetracyanonickelate aqueous solution are added
In 5mL beakers, it is well mixed, stands 8 hours at 40 DEG C, obtain cobalt nickel cyanogen glue, then add 50mL under agitation
3.0mol/L sodium borohydride aqueous solution, wherein the mol ratio of four Potassium Tetracyanonickelates and cobalt chloride, sodium borohydride is 1:2:300,
Reduction reaction 6 hours, are cooled to normal temperature at 70 DEG C, centrifuge, are washed with deionized, 60 DEG C of dryings in vacuum drying oven,
Produce ultra-thin CoNi alloy nanos piece (see Fig. 1~4).
Embodiment 2
0.5mL 1.5mol/L cobalt chloride solution, the Potassium Tetracyanonickelate aqueous solution of 0.5mL 1.0mol/L tetra- are added into 5mL
In beaker, it is well mixed, stands 8 hours at 40 DEG C, obtain cobalt nickel cyanogen glue, then add 36mL under agitation
3.5mol/L sodium borohydride aqueous solution, wherein the mol ratio of four Potassium Tetracyanonickelates and cobalt chloride, sodium borohydride is 1:1.5:250,
Reduction reaction 6 hours, are cooled to normal temperature at 70 DEG C, centrifuge, are washed with deionized, and are done for 60 DEG C in vacuum drying oven
It is dry, produce ultra-thin CoNi alloy nanos piece (see Fig. 5).
Embodiment 3
1mL 2.0mol/L cobalt chloride solution, 1mL the 1.0mol/L four Potassium Tetracyanonickelate aqueous solution are added into 5mL to burn
In cup, it is well mixed, stands 12 hours at room temperature, obtain cobalt nickel cyanogen glue, then add 100mL under agitation
3.0mol/L sodium borohydride aqueous solution, wherein the mol ratio of four Potassium Tetracyanonickelates and cobalt chloride, sodium borohydride is 1:2:300,
Reduction reaction 24 hours at room temperature, centrifuge, be washed with deionized, 60 DEG C of dryings in vacuum drying oven, produce ultra-thin
CoNi alloy nanos piece (see Fig. 6).
The ultra-thin CoNi alloy nanos piece electro-catalysis analysis oxygen that inventor is obtained using embodiment 1, specific method are：By 2mg
Ultra-thin CoNi alloy nanos piece is added in the 1mL aqueous solution, is well mixed, and is taken the gained μ L of mixed liquor 4 to be added dropwise on platinum carbon electrode, is treated
It is used for electro-chemical test after drying, test result is shown in Fig. 7.As seen from Figure 7, compared with business iridium carbon (IrC) catalyst, the present invention
The ultra-thin CoNi alloy nanos piece prepared has good electro catalytic activity when voltage is higher to electro-catalysis analysis oxygen.
Claims (5)
- A kind of 1. preparation method of ultra-thin CoNi alloy nanos piece, it is characterised in that：By cobalt chloride solution and four Potassium Tetracyanonickelates The aqueous solution is well mixed, and cobalt nickel cyanogen glue is obtained after standing, then adds sodium borohydride aqueous solution, anti-to reduction at 80 DEG C in room temperature Answer 1~24 hour, centrifuge, wash, vacuum drying, obtaining ultra-thin CoNi alloy nanos piece.
- 2. the preparation method of ultra-thin CoNi alloy nanos 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 the four Potassium Tetracyanonickelate aqueous solution concentration of four Potassium Tetracyanonickelates for 0.9~ The mol 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 nanos piece according to claim 1 or 2, it is characterised in that：By cobalt chloride The aqueous solution is well mixed with the four Potassium Tetracyanonickelate aqueous solution, 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 nanos piece according to claim 1, it is characterised in that：The four cyanogen nickel acid The mol ratio of potassium and sodium borohydride is 1:250~300.
- 5. the preparation method of ultra-thin CoNi alloy nanos piece according to claim 1, it is characterised in that：At 60~70 DEG C Reduction reaction 4~8 hours.
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Cited By (6)
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| CN109254048A (en) * | 2018-11-05 | 2019-01-22 | 济南大学 | A kind of preparation method and application of the Nitrofuran antibiotics sensor based on cobalt-nickel oxide |
| CN109637826A (en) * | 2018-12-14 | 2019-04-16 | 江苏科技大学 | A kind of preparation method and applications of cobaltosic oxide-nickel oxide/grapheme foam combination electrode material |
| CN112838224A (en) * | 2021-01-25 | 2021-05-25 | 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 |
| CN113155910A (en) * | 2020-12-18 | 2021-07-23 | 中国石油大学(华东) | Preparation method and application of carbon quantum dot-cobalt tetracyanide nickelate composite material ammonia gas sensor |
| CN113529107A (en) * | 2021-08-19 | 2021-10-22 | 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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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109254048A (en) * | 2018-11-05 | 2019-01-22 | 济南大学 | A kind of preparation method and application of the Nitrofuran antibiotics sensor based on cobalt-nickel oxide |
| CN109637826A (en) * | 2018-12-14 | 2019-04-16 | 江苏科技大学 | A kind of preparation method and applications of cobaltosic oxide-nickel oxide/grapheme foam combination electrode material |
| 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 |
| CN113155910A (en) * | 2020-12-18 | 2021-07-23 | 中国石油大学(华东) | Preparation method and application of carbon quantum dot-cobalt tetracyanide nickelate composite material ammonia gas sensor |
| CN112838224A (en) * | 2021-01-25 | 2021-05-25 | 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 |
| CN113529107A (en) * | 2021-08-19 | 2021-10-22 | 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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