CN108286058A - The method for preparing the bismuth telluride nanometer sheet of Supported Co nickel molybdenum particle - Google Patents
The method for preparing the bismuth telluride nanometer sheet of Supported Co nickel molybdenum particle Download PDFInfo
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Abstract
Using solvent-thermal method hexagonal bismuth telluride nanometer sheet is prepared by controlling temperature, and carry out the load of cobalt nickel molybdenum particle in bismuth telluride nanometer sheet using direct-reduction process in the method that the present invention discloses the bismuth telluride nanometer sheet for preparing Supported Co nickel molybdenum particle.Implementation cost of the present invention is low, easy to operate, and pollution is low, is a kind of synthetic method of high-efficiency and economic, while the material granule of the present invention is more evenly distributed, specific surface area bigger, and analysis oxygen performance is stronger.
Description
The present patent application is parent application " a kind of the bismuth telluride nanometer sheet and its synthetic method of Supported Co nickel molybdenum particle "
The applying date of divisional application, parent application is on April 8th, 2015, and application No. is 2015101633218.
Technical field
The present invention relates to a kind of novel nano-material and its synthetic method more particularly to a kind of telluriums of Supported Co nickel molybdenum particle
Change bismuth nanometer sheet and its synthetic method.
Background technology
The catalysis material of known anode is mainly some noble metals, but due to expensive, is limited in all fields
Application.The present invention, which proposes, uses Bi2Te3Semi-conducting material is as anode, and there is no similar researchs before this.It is proposed this idea
It is main to consider the following：(1)Bi2Te3Crystal structure is closely similar with the crystal structure of graphite, is easy dissociation slabbing, dissociation
Face is smooth, and has metallic luster, has good electric conductivity, the free electron of metalloid material to be conducive to the transmission (2) of electronics
Bi2Te3It is that thermal conductivity is low, conductivity is high, and conductivity varies with temperature obviously.Temperature necessarily rises after electrified regulation, can inspire
Its topological insulator characteristic of more electronics (3) is a kind of novel substance state with unusual Quantum Properties.
Cobalt, nickel, molybdenum particle have good application in terms of Electrochemical oxygen evolution, and the alkali resistance of nickel is strong, oxygen evolution potential also compared with
Low and be widely used, molybdenum, which is in the transition series metal element left side and the nickel positioned at the right, has synergistic effect, cobalt and nickel in analysis oxygen
Before can electrode surface formed one layer of very thin oxidation film, improve catalytic activity.
Invention content
The object of the present invention is to provide a kind of the bismuth telluride nanometer sheets and its synthetic method of Supported Co nickel molybdenum particle, obtain one
Evenly, specific surface area bigger analyses the stronger nano material of oxygen performance for kind of distribution of particles, the method have it is at low cost, prepared
The simple feature of journey.
The purpose of the present invention is achieved by following technical proposals：
A kind of bismuth telluride nanometer sheet of Supported Co nickel molybdenum particle, bismuth telluride nanometer sheet are in hexagon, and cobalt nickel molybdenum particle is uniform
Be distributed on the surface of bismuth telluride nanometer sheet, and carry out as steps described below：
Step 1, the preparation of bismuth telluride nanometer sheet：Take BiCl3(production of this reagent Co., Ltd of Adama), Na2TeO3(north
Jing Yinuokai companies produce), PVP (Tianjin Heowns Biochemical Technology Co., Ltd. produce, molecular weight w=40000), (days NaOH
Jinshi City East China chemical reagent work produces) in ethylene glycol, 2h is stirred at room temperature, is then transferred in polytetrafluoroethylene (PTFE) pyroreaction kettle, it is permanent
220 DEG C of temperature takes out sample after reacting 36h, with drying to obtain tellurium after deionized water and absolute ethyl alcohol difference eccentric cleaning 3 times
Change bismuth nanometer sheet.
In ethylene glycol solution described in step 1, BiCl3A concentration of 0.0278M, Na2TeO3A concentration of 0.0425M, PVP are dense
Degree is 0.00026M-0.000521M, NaOH concentration 0.415M-0.419M；
Step 2, by bismuth telluride nanometer sheet alkali process obtained is placed on the water in the sources Co-Ni-Mo in step 1 and ethylene glycol mixes
It closes in solution, 50-70min is stirred at room temperature, then directly sodium borohydride ultrasound 30min is added to restore mixed solution；
Ethylene glycol in mixed solution described in step 2：The volume ratio of water is 1:1, a concentration of 0.0285M- of nickel sulfate
0.0287M, a concentration of 0.00565M-0.00567M of sodium molybdate, a concentration of 0.000694M-0.0694M of cobalt nitrate, lemon
The quality of reducing agent sodium borohydride is added in a concentration of 0.0000625M of a concentration of 0.0249M-0.0251M of sour trisodium, PVP
For 5-8 mass parts, each mass parts are 0.01g；
Step 3, by step 2 solution taking-up be placed in water-bath 50-70min in 35-45 DEG C of water-bath, afterwards with absolute ethyl alcohol from
The heart cleans 3 times to get to the bismuth telluride nanometer sheet of Supported Co nickel molybdenum particle.
The present invention method cost it is low, it is easy to operate, take it is shorter, compared with traditional preparation methods, mainly have with
Under several advantages：(1) it solves the characteristics of particle agglomeration, cobalt nickel molybdenum particle is made to be evenly distributed on bismuth telluride nanometer sheet (such as attached drawing 6
It is shown)；(2) reaction time greatly shortens, and easy to operate；(3) it is tested using electrochemical workstation GAMRY 04084,
The bismuth telluride nanometer sheet hydrogen reduction linear scan highest current density of Supported Co nickel molybdenum particle, shows that this material has in the present invention
Higher production oxygen performance, can be used for hydrogen reduction field ((as shown in Fig. 7).
Description of the drawings
Fig. 1 is XRD spectrum (XRD, the Rigaku of the bismuth telluride nanometer sheet nano material of Supported Co nickel molybdenum particle of the present invention
D/max-Ra), wherein curve (1) is the bismuth telluride nanometer sheet XRD spectrum of unsupported CoNiMo particles, and curve (2) is load
Bismuth telluride nanometer sheet XRD spectrum after CoNiMo particles；
The bismuth telluride nanometer sheet of load C oNiMo particles when Fig. 2 is a concentration of 0.000694M of cobalt nitrate of the present invention
SEM patterns photo (FE-SEM, Hitachi S-4800)；
The bismuth telluride nanometer sheet of load C oNiMo particles when Fig. 3 is a concentration of 0.00694M of cobalt nitrate of the present invention
SEM patterns photo (FE-SEM, Hitachi S-4800)；
The SEM of the bismuth telluride nanometer sheet of load C oNiMo particles when Fig. 4 is a concentration of 0.0347M of cobalt nitrate of the present invention
Pattern photo (FE-SEM, Hitachi S-4800)；
The SEM of the bismuth telluride nanometer sheet of load C oNiMo particles when Fig. 5 is a concentration of 0.0694M of cobalt nitrate of the present invention
Pattern photo (FE-SEM, Hitachi S-4800)；
Fig. 6 is TEM pattern photos (TEM, the Philips of the bismuth telluride nanometer sheet of load C oNiMo particles of the present invention
Tecnai G2f20c)；
Fig. 7 is the hydrogen reduction of the bismuth telluride nanometer sheet of the load C oNiMo particles synthesized under the different nitric acid cobalt concentrations of the present invention
Linear scan curve, wherein curve (1) are linearly to be swept in the hydrogen reduction of bismuth telluride nanometer sheet of a concentration of 0.0694M of cobalt nitrate
Curve is retouched, curve (2) is the hydrogen reduction linear scan curve in the bismuth telluride nanometer sheet of a concentration of 0.000694M of cobalt nitrate,
Curve (3) is the hydrogen reduction linear scan curve of Ni nets.
Specific implementation mode
To make the object, technical solutions and advantages of the present invention clearer, embodiment of the present invention is made below further
It is described in detail on ground.
Embodiment 1
Take 0.315gBiCl3、0.34gNa2TeO3, 0.48gPVP (w=40000), 0.58gNaOH in 36ml ethylene glycol,
2h is stirred at room temperature.
It is transferred to above-mentioned in polytetrafluoroethylene (PTFE) pyroreaction kettle, 220 DEG C of constant temperature, 36h.
Sample is taken out, with dried for standby after deionized water and absolute ethyl alcohol difference eccentric cleaning 3 times.
After bismuth telluride nanometer sheet alkali process after taking 0.07g to dry in the mixed solution of the sources Co-Ni-Mo, in mixed solution
Ethylene glycol：The volume ratio of water is 1:1, solution total amount 20ml.A concentration of 0.0285M of nickel sulfate, the concentration of sodium molybdate in solution
For 0.00565M, a concentration of 0.000694M of cobalt nitrate, a concentration of 0.0249M of trisodium citrate, PVP's is a concentration of
50min is stirred at room temperature in 0.0000625M, directly 0.08g sodium borohydride ultrasounds 30min is added to restore mixed solution afterwards.
Solution taking-up is placed in water-bath 70min in 35 DEG C of water-baths, afterwards with absolute ethyl alcohol eccentric cleaning 3 times to get to negative
Carry the bismuth telluride nanometer sheet of cobalt nickel molybdenum particle.
Embodiment 2
Take 0.315gBiCl3、0.34gNa2TeO3, 0.52gPVP (w=40000), 0.62gNaOH in 36ml ethylene glycol,
2h is stirred at room temperature.
It is transferred to above-mentioned in polytetrafluoroethylene (PTFE) pyroreaction kettle, 220 DEG C of constant temperature, 36h.
Sample is taken out, with dried for standby after deionized water and absolute ethyl alcohol difference eccentric cleaning 3 times.
After bismuth telluride nanometer sheet alkali process after taking 0.07g to dry in the mixed solution of the sources Co-Ni-Mo, in mixed solution
Ethylene glycol：The volume ratio of water is 1:1, solution total amount 20ml.A concentration of 0.0287M of nickel sulfate, the concentration of sodium molybdate in solution
For 0.00567M, a concentration of 0.00694M of cobalt nitrate, a concentration of 0.0251M of trisodium citrate, PVP's is a concentration of
70min is stirred at room temperature in 0.0000625M, directly 0.08g sodium borohydride ultrasounds 30min is added to restore mixed solution afterwards.
Solution taking-up is placed in water-bath 50min in 45 DEG C of water-baths, afterwards with absolute ethyl alcohol eccentric cleaning 3 times to get to negative
Carry the bismuth telluride nanometer sheet of cobalt nickel molybdenum particle.
Embodiment 3
Take 0.315gBiCl3、0.34gNa2TeO3, 0.50gPVP (w=40000), 0.60gNaOH in 36ml ethylene glycol,
2h is stirred at room temperature.
It is transferred to above-mentioned in polytetrafluoroethylene (PTFE) pyroreaction kettle, 220 DEG C of constant temperature, 36h.
Sample is taken out, with dried for standby after deionized water and absolute ethyl alcohol difference eccentric cleaning 3 times.
After bismuth telluride nanometer sheet alkali process after taking 0.07g to dry in the mixed solution of the sources Co-Ni-Mo, in mixed solution
Ethylene glycol：The volume ratio of water is 1:1, solution total amount 20ml.A concentration of 0.0286M of nickel sulfate, the concentration of sodium molybdate in solution
For 0.00566M, a concentration of 0.0347M of cobalt nitrate, a concentration of 0.0250M of trisodium citrate, PVP's is a concentration of
60min is stirred at room temperature in 0.0000625M, directly 0.08g sodium borohydride ultrasounds 30min is added to restore mixed solution afterwards.
Solution taking-up is placed in water-bath 60min in 40 DEG C of water-baths, afterwards with absolute ethyl alcohol eccentric cleaning 3 times to get to negative
Carry the bismuth telluride nanometer sheet of cobalt nickel molybdenum particle.
Embodiment 4
Take 0.315gBiCl3、0.34gNa2TeO3, 0.50gPVP (w=40000), 0.60gNaOH in 36ml ethylene glycol,
No less than 2h is stirred at room temperature.
It is transferred to above-mentioned in polytetrafluoroethylene (PTFE) pyroreaction kettle, 220 DEG C of constant temperature, 36h.
Sample is taken out, with dried for standby after deionized water and absolute ethyl alcohol difference eccentric cleaning 3 times.
After bismuth telluride nanometer sheet alkali process after taking 0.07g to dry in the mixed solution of the sources Co-Ni-Mo, in mixed solution
Ethylene glycol：The volume ratio of water is 1:1, solution total amount 20ml.A concentration of 0.0286M of nickel sulfate, the concentration of sodium molybdate in solution
For 0.00566M, a concentration of 0.0694M of cobalt nitrate, a concentration of 0.0249M of trisodium citrate, PVP's is a concentration of
60min is stirred at room temperature in 0.0000625M, directly 0.08g sodium borohydride ultrasounds 30min is added to restore mixed solution afterwards.
Solution taking-up is placed in water-bath 60min in 40 DEG C of water-baths, afterwards with absolute ethyl alcohol eccentric cleaning 3 times to get to negative
Carry the bismuth telluride nanometer sheet of cobalt nickel molybdenum particle.
Embodiment 5
Take 0.315gBiCl3、0.34gNa2TeO3, 0.50gPVP (w=40000), 0.60gNaOH in 36ml ethylene glycol,
No less than 2h is stirred at room temperature.
It is transferred to above-mentioned in polytetrafluoroethylene (PTFE) pyroreaction kettle, 220 DEG C of constant temperature, 36h.
Sample is taken out, with dried for standby after deionized water and absolute ethyl alcohol difference eccentric cleaning 3 times.
After bismuth telluride nanometer sheet alkali process after taking 0.07g to dry in the mixed solution of the sources Co-Ni-Mo, in mixed solution
Ethylene glycol：The volume ratio of water is 1:1, solution total amount 20ml.A concentration of 0.0286M of nickel sulfate, the concentration of sodium molybdate in solution
For 0.00566M, a concentration of 0.000694M of cobalt nitrate, a concentration of 0.0249M of trisodium citrate, PVP's is a concentration of
60min is stirred at room temperature in 0.0000625M, directly 0.05g sodium borohydride ultrasounds 30min is added to restore mixed solution afterwards.
Solution taking-up is placed in water-bath 60min in 40 DEG C of water-baths, afterwards with absolute ethyl alcohol eccentric cleaning 3 times to get to negative
Carry the bismuth telluride nanometer sheet of cobalt nickel molybdenum particle.
Embodiment 6
Take 0.315gBiCl3、0.34gNa2TeO3, 0.50gPVP (w=40000), 0.60gNaOH in 36ml ethylene glycol,
No less than 2h is stirred at room temperature.
It is transferred to above-mentioned in polytetrafluoroethylene (PTFE) pyroreaction kettle, 220 DEG C of constant temperature, 36h.
Sample is taken out, with dried for standby after deionized water and absolute ethyl alcohol difference eccentric cleaning 3 times.
After bismuth telluride nanometer sheet alkali process after taking 0.07g to dry in the mixed solution of the sources Co-Ni-Mo, in mixed solution
Ethylene glycol：The volume ratio of water is 1:1, solution total amount 20ml.A concentration of 0.0286M of nickel sulfate, the concentration of sodium molybdate in solution
For 0.00566M, a concentration of 0.000694M of cobalt nitrate, a concentration of 0.0249M of trisodium citrate, PVP's is a concentration of
60min is stirred at room temperature in 0.0000625M, directly 0.06g sodium borohydride ultrasounds 30min is added to restore mixed solution afterwards.
Solution taking-up is placed in water-bath 60min in 40 DEG C of water-baths, afterwards with absolute ethyl alcohol eccentric cleaning 3 times to get to negative
Carry the bismuth telluride nanometer sheet of cobalt nickel molybdenum particle.
Embodiment 7
Take 0.315gBiCl3、0.34gNa2TeO3, 0.50gPVP (w=40000), 0.60gNaOH in 36ml ethylene glycol,
No less than 2h is stirred at room temperature.
It is transferred to above-mentioned in polytetrafluoroethylene (PTFE) pyroreaction kettle, 220 DEG C of constant temperature, 36h.
Sample is taken out, with dried for standby after deionized water and absolute ethyl alcohol difference eccentric cleaning 3 times.
After bismuth telluride nanometer sheet alkali process after taking 0.07g to dry in the mixed solution of the sources Co-Ni-Mo, in mixed solution
Ethylene glycol：The volume ratio of water is 1:1, solution total amount 20ml.A concentration of 0.0286M of nickel sulfate, the concentration of sodium molybdate in solution
For 0.00566M, a concentration of 0.000694M of cobalt nitrate, a concentration of 0.0249M of trisodium citrate, PVP's is a concentration of
60min is stirred at room temperature in 0.0000625M, directly 0.07g sodium borohydride ultrasounds 30min is added to restore mixed solution afterwards.
Solution taking-up is placed in water-bath 60min in 40 DEG C of water-baths, afterwards with absolute ethyl alcohol eccentric cleaning 3 times to get to negative
Carry the bismuth telluride nanometer sheet of cobalt nickel molybdenum particle.
Illustrative description has been done to the present invention above, it should explanation, the case where not departing from core of the invention
Under, any simple deformation, modification or other skilled in the art can not spend the equivalent replacement of creative work equal
Fall into protection scope of the present invention.
Claims (3)
1. the method for preparing the bismuth telluride nanometer sheet of Supported Co nickel molybdenum particle, which is characterized in that bismuth telluride nanometer sheet is in hexagon,
Cobalt nickel molybdenum is evengranular to be distributed on the surface of bismuth telluride nanometer sheet, and is carried out as steps described below：
Step 1, the preparation of bismuth telluride nanometer sheet：Take BiCl3、Na2TeO3, PVP, NaOH in ethylene glycol, 2h is stirred at room temperature, so
After be transferred in polytetrafluoroethylene (PTFE) pyroreaction kettle, 220 DEG C of constant temperature takes out sample after reacting 36h, with deionized water and anhydrous
Ethyl alcohol distinguishes drying to obtain bismuth telluride nanometer sheet after eccentric cleaning 3 times.
In ethylene glycol solution described in step 1, BiCl3A concentration of 0.0278M, Na2TeO3A concentration of 0.0425M, PVP are a concentration of
0.00026M-0.000521M, NaOH concentration 0.415M-0.419M；
Step 2, by bismuth telluride nanometer sheet alkali process obtained in step 1 be placed on the sources Co-Ni-Mo water and ethylene glycol mix it is molten
In liquid, 50-70min is stirred at room temperature, then directly sodium borohydride ultrasound 30min is added to restore mixed solution.
Ethylene glycol in mixed solution described in step 2：The volume ratio of water is 1:1, a concentration of 0.0285M- of nickel sulfate
0.0287M, a concentration of 0.00565M-0.00567M of sodium molybdate, a concentration of 0.000694M-0.0694M of cobalt nitrate, lemon
The quality of reducing agent sodium borohydride is added in a concentration of 0.0000625M of a concentration of 0.0249M-0.0251M of sour trisodium, PVP
For 5-8 mass parts, each mass parts are 0.01g；
Step 3, solution taking-up in step 2 is placed in water-bath 50-70min in 35-45 DEG C of water-bath, after centrifuged with absolute ethyl alcohol it is clear
3 times are washed to get to the bismuth telluride nanometer sheet of Supported Co nickel molybdenum particle.
2. the method for the bismuth telluride nanometer sheet according to claim 1 for preparing Supported Co nickel molybdenum particle, which is characterized in that institute
It states in step (1), a concentration of 0.000347M of PVP, NaOH concentration 0.417M.
3. the method for the bismuth telluride nanometer sheet according to claim 1 for preparing Supported Co nickel molybdenum particle, which is characterized in that institute
A concentration of 0.00694M-0.0347M of cobalt nitrate in step (2) is stated, the quality of reducing agent sodium borohydride is 6-7 mass parts,
Each mass parts are 0.01g.
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| CN201510163321.8A CN106140201B (en) | 2015-04-08 | 2015-04-08 | A kind of the bismuth telluride nanometer sheet and its synthetic method of Supported Co nickel molybdenum particle |
| CN201810167603.9A CN108286058B (en) | 2015-04-08 | 2015-04-08 | The method for preparing the bismuth telluride nanometer sheet of Supported Co nickel molybdenum particle |
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| CN201510163321.8A Expired - Fee Related CN106140201B (en) | 2015-04-08 | 2015-04-08 | A kind of the bismuth telluride nanometer sheet and its synthetic method of Supported Co nickel molybdenum particle |
| CN201810167601.XA Expired - Fee Related CN108193218B (en) | 2015-04-08 | 2015-04-08 | Application of the bismuth telluride nanometer sheet of Supported Co nickel molybdenum particle in hydrogen reduction field |
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| CN201810167601.XA Expired - Fee Related CN108193218B (en) | 2015-04-08 | 2015-04-08 | Application of the bismuth telluride nanometer sheet of Supported Co nickel molybdenum particle in hydrogen reduction field |
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| CN112436159B (en) * | 2020-11-06 | 2022-09-02 | 扬州大学 | Alcohol fuel cell anode catalyst, preparation method and application thereof |
| CN113937311B (en) * | 2021-10-11 | 2023-01-31 | 福州大学 | Preparation method of two-dimensional porous silica non-carbon carrier supported platinum-copper-nickel catalyst |
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| CN101549405A (en) * | 2009-05-19 | 2009-10-07 | 燕山大学 | High-pressure sintering preparation method of high-densification high-performance nano crystal block thermoelectric material |
| JP2013522860A (en) * | 2009-02-24 | 2013-06-13 | トヨタ モーター エンジニアリング アンド マニュファクチャリング ノース アメリカ，インコーポレイティド | Core-shell nanoparticles and manufacturing method |
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| CN103606660A (en) * | 2013-11-06 | 2014-02-26 | 中国科学院化学研究所 | Alumina-coated granules, as well as preparation method and application thereof |
| CN104451797B (en) * | 2014-11-28 | 2016-10-26 | 鹏南电子科技（厦门）有限公司 | The tin plating processing method of a kind of Tellurobismuthite. matrix and a kind of supplement |
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| CN101549405A (en) * | 2009-05-19 | 2009-10-07 | 燕山大学 | High-pressure sintering preparation method of high-densification high-performance nano crystal block thermoelectric material |
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