CN108193218B - Application of the bismuth telluride nanometer sheet of Supported Co nickel molybdenum particle in hydrogen reduction field - Google Patents
Application of the bismuth telluride nanometer sheet of Supported Co nickel molybdenum particle in hydrogen reduction field Download PDFInfo
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- CN108193218B CN108193218B CN201810167601.XA CN201810167601A CN108193218B CN 108193218 B CN108193218 B CN 108193218B CN 201810167601 A CN201810167601 A CN 201810167601A CN 108193218 B CN108193218 B CN 108193218B
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Abstract
The present invention discloses application of the bismuth telluride nanometer sheet of Supported Co nickel molybdenum particle in hydrogen reduction field, utilize solvent-thermal method, hexagonal bismuth telluride nanometer sheet is prepared by controlling temperature, and the load of cobalt nickel molybdenum particle is carried out in bismuth telluride nanometer sheet using direct-reduction process, bismuth telluride nanometer sheet is in hexagon, on the evengranular surface for being distributed in bismuth telluride nanometer sheet of cobalt nickel molybdenum.Implementation cost of the present invention is low, easy to operate, and it is a kind of synthetic method of high-efficiency and economic, while material granule of the invention is more evenly distributed that pollution is low, and specific surface area is 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 technique
The catalysis material of known anode is mainly some noble metals, but due to expensive, is limited in all fields
Application.The invention proposes with Bi2Te3Semiconductor 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, there is good electric conductivity, the free electron of metalloid material, conducive to the transmitting (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 is in the transition series metal element left side has synergistic effect, cobalt and nickel in analysis oxygen with the nickel for being located at the right
Before can electrode surface formed one layer of very thin oxidation film, improve catalytic activity.
Summary of the invention
The object of the present invention is to provide the bismuth telluride nanometer sheets and its synthetic method of a kind of Supported Co nickel molybdenum particle, obtain one
More evenly, specific surface area is bigger for kind of distribution of particles, analyses the stronger nano material of oxygen performance, 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 as steps described below carry out:
Step 1, the preparation of bismuth telluride nanometer sheet: BiCl is taken3(production of this reagent Co., Ltd of Adama), Na2TeO3(north
The production of Jing Yinuokai company), PVP (Tianjin Heowns Biochemical Technology Co., Ltd. production, molecular weight w=40000), (day NaOH
The production of Jinshi City East China chemical reagent work) 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, drying to obtain tellurium after being distinguished eccentric cleaning 3 times with deionized water and dehydrated alcohol
Change bismuth nanometer sheet.
In ethylene glycol solution described in step 1, BiCl3Concentration is 0.0278M, Na2TeO3Concentration is that 0.0425M, PVP are dense
Degree is 0.00026M-0.000521M, NaOH concentration 0.415M-0.419M；
Step 2, bismuth telluride nanometer sheet alkali process obtained in step 1 is placed on the water in the source Co-Ni-Mo 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, and the concentration of nickel sulfate is 0.0285M-
0.0287M, the concentration of sodium molybdate are 0.00565M-0.00567M, and the concentration of cobalt nitrate is 0.000694M-0.0694M, lemon
The concentration of sour trisodium is 0.0249M-0.0251M, and the concentration of PVP is 0.0000625M, and the quality of reducing agent sodium borohydride is added
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 dehydrated alcohol from
The heart cleans 3 times to get the bismuth telluride nanometer sheet for arriving Supported Co nickel molybdenum particle.
Method cost of the invention is low, easy to operate, time-consuming shorter, compared with traditional preparation methods, mainly have with
Under several advantages: (1) solve the characteristics of particle agglomeration, cobalt nickel molybdenum particle 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).
Detailed description of the invention
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 particle, and curve (2) is load
Bismuth telluride nanometer sheet XRD spectrum after CoNiMo particle；
The bismuth telluride nanometer sheet for the load C oNiMo particle that Fig. 2 is the concentration of cobalt nitrate of the present invention when being 0.000694M
SEM pattern photo (FE-SEM, Hitachi S-4800)；
The bismuth telluride nanometer sheet for the load C oNiMo particle that Fig. 3 is the concentration of cobalt nitrate of the present invention when being 0.00694M
SEM pattern photo (FE-SEM, Hitachi S-4800)；
The SEM of the bismuth telluride nanometer sheet for the load C oNiMo particle that Fig. 4 is the concentration of cobalt nitrate of the present invention when being 0.0347M
Pattern photo (FE-SEM, Hitachi S-4800)；
The SEM of the bismuth telluride nanometer sheet for the load C oNiMo particle that Fig. 5 is the concentration of cobalt nitrate of the present invention when being 0.0694M
Pattern photo (FE-SEM, Hitachi S-4800)；
Fig. 6 is TEM pattern photo (TEM, the Philips of the bismuth telluride nanometer sheet of load C oNiMo particle of the present invention
Tecnai G2f20c)；
Fig. 7 is the hydrogen reduction of the bismuth telluride nanometer sheet of the load C oNiMo particle synthesized under the different nitric acid cobalt concentrations of the present invention
The hydrogen reduction of linear scan curve, the bismuth telluride nanometer sheet that wherein curve (1) is 0.0694M for the concentration in cobalt nitrate is linearly swept
Retouch curve, curve (2) be cobalt nitrate concentration be 0.000694M bismuth telluride nanometer sheet hydrogen reduction linear scan curve,
Curve (3) is the hydrogen reduction linear scan curve of Ni net.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, embodiment of the present invention is made below further
Ground detailed description.
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, dried for standby after being distinguished eccentric cleaning 3 times with deionized water and dehydrated alcohol.
After bismuth telluride nanometer sheet alkali process after taking 0.07g dry in the mixed solution of the source Co-Ni-Mo, in mixed solution
Ethylene glycol: the volume ratio of water is 1:1, solution total amount 20ml.The concentration of nickel sulfate is 0.0285M, the concentration of sodium molybdate in solution
For 0.00565M, the concentration of cobalt nitrate is 0.000694M, and the concentration of trisodium citrate is 0.0249M, and the concentration of PVP is
50min is stirred at room temperature in 0.0000625M, directly 0.08g sodium borohydride ultrasound 30min is added to restore mixed solution afterwards.
Solution taking-up is placed in water-bath 70min in 35 DEG C of water-baths, it is negative to get arriving with dehydrated alcohol eccentric cleaning 3 times afterwards
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, dried for standby after being distinguished eccentric cleaning 3 times with deionized water and dehydrated alcohol.
After bismuth telluride nanometer sheet alkali process after taking 0.07g dry in the mixed solution of the source Co-Ni-Mo, in mixed solution
Ethylene glycol: the volume ratio of water is 1:1, solution total amount 20ml.The concentration of nickel sulfate is 0.0287M, the concentration of sodium molybdate in solution
For 0.00567M, the concentration of cobalt nitrate is 0.00694M, and the concentration of trisodium citrate is 0.0251M, and the concentration of PVP is
70min is stirred at room temperature in 0.0000625M, directly 0.08g sodium borohydride ultrasound 30min is added to restore mixed solution afterwards.
Solution taking-up is placed in water-bath 50min in 45 DEG C of water-baths, it is negative to get arriving with dehydrated alcohol eccentric cleaning 3 times afterwards
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, dried for standby after being distinguished eccentric cleaning 3 times with deionized water and dehydrated alcohol.
After bismuth telluride nanometer sheet alkali process after taking 0.07g dry in the mixed solution of the source Co-Ni-Mo, in mixed solution
Ethylene glycol: the volume ratio of water is 1:1, solution total amount 20ml.The concentration of nickel sulfate is 0.0286M, the concentration of sodium molybdate in solution
For 0.00566M, the concentration of cobalt nitrate is 0.0347M, and the concentration of trisodium citrate is 0.0250M, and the concentration of PVP is
60min is stirred at room temperature in 0.0000625M, directly 0.08g sodium borohydride ultrasound 30min is added to restore mixed solution afterwards.
Solution taking-up is placed in water-bath 60min in 40 DEG C of water-baths, it is negative to get arriving with dehydrated alcohol eccentric cleaning 3 times afterwards
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, dried for standby after being distinguished eccentric cleaning 3 times with deionized water and dehydrated alcohol.
After bismuth telluride nanometer sheet alkali process after taking 0.07g dry in the mixed solution of the source Co-Ni-Mo, in mixed solution
Ethylene glycol: the volume ratio of water is 1:1, solution total amount 20ml.The concentration of nickel sulfate is 0.0286M, the concentration of sodium molybdate in solution
For 0.00566M, the concentration of cobalt nitrate is 0.0694M, and the concentration of trisodium citrate is 0.0249M, and the concentration of PVP is
60min is stirred at room temperature in 0.0000625M, directly 0.08g sodium borohydride ultrasound 30min is added to restore mixed solution afterwards.
Solution taking-up is placed in water-bath 60min in 40 DEG C of water-baths, it is negative to get arriving with dehydrated alcohol eccentric cleaning 3 times afterwards
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, dried for standby after being distinguished eccentric cleaning 3 times with deionized water and dehydrated alcohol.
After bismuth telluride nanometer sheet alkali process after taking 0.07g dry in the mixed solution of the source Co-Ni-Mo, in mixed solution
Ethylene glycol: the volume ratio of water is 1:1, solution total amount 20ml.The concentration of nickel sulfate is 0.0286M, the concentration of sodium molybdate in solution
For 0.00566M, the concentration of cobalt nitrate is 0.000694M, and the concentration of trisodium citrate is 0.0249M, and the concentration of PVP is
60min is stirred at room temperature in 0.0000625M, directly 0.05g sodium borohydride ultrasound 30min is added to restore mixed solution afterwards.
Solution taking-up is placed in water-bath 60min in 40 DEG C of water-baths, it is negative to get arriving with dehydrated alcohol eccentric cleaning 3 times afterwards
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, dried for standby after being distinguished eccentric cleaning 3 times with deionized water and dehydrated alcohol.
After bismuth telluride nanometer sheet alkali process after taking 0.07g dry in the mixed solution of the source Co-Ni-Mo, in mixed solution
Ethylene glycol: the volume ratio of water is 1:1, solution total amount 20ml.The concentration of nickel sulfate is 0.0286M, the concentration of sodium molybdate in solution
For 0.00566M, the concentration of cobalt nitrate is 0.000694M, and the concentration of trisodium citrate is 0.0249M, and the concentration of PVP is
60min is stirred at room temperature in 0.0000625M, directly 0.06g sodium borohydride ultrasound 30min is added to restore mixed solution afterwards.
Solution taking-up is placed in water-bath 60min in 40 DEG C of water-baths, it is negative to get arriving with dehydrated alcohol eccentric cleaning 3 times afterwards
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, dried for standby after being distinguished eccentric cleaning 3 times with deionized water and dehydrated alcohol.
After bismuth telluride nanometer sheet alkali process after taking 0.07g dry in the mixed solution of the source Co-Ni-Mo, in mixed solution
Ethylene glycol: the volume ratio of water is 1:1, solution total amount 20ml.The concentration of nickel sulfate is 0.0286M, the concentration of sodium molybdate in solution
For 0.00566M, the concentration of cobalt nitrate is 0.000694M, and the concentration of trisodium citrate is 0.0249M, and the concentration of PVP is
60min is stirred at room temperature in 0.0000625M, directly 0.07g sodium borohydride ultrasound 30min is added to restore mixed solution afterwards.
Solution taking-up is placed in water-bath 60min in 40 DEG C of water-baths, it is negative to get arriving with dehydrated alcohol eccentric cleaning 3 times afterwards
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. application of the bismuth telluride nanometer sheet of Supported Co nickel molybdenum particle in hydrogen reduction field, which is characterized in that in the load
In the bismuth telluride nanometer sheet of cobalt nickel molybdenum particle, bismuth telluride nanometer sheet is in hexagon, and cobalt nickel molybdenum is evengranular to be distributed in bismuth telluride
On the surface of nanometer sheet, and carry out as steps described below:
Step 1, the preparation of bismuth telluride nanometer sheet: BiCl is taken3、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, sample is taken out after reacting 36h, with deionized water and anhydrous
Drying to obtain bismuth telluride nanometer sheet after ethyl alcohol is distinguished eccentric cleaning 3 times；
In ethylene glycol solution described in step 1, BiCl3Concentration is 0.0278M, Na2TeO3Concentration is that 0.0425M, PVP concentration are
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 source 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, and the concentration of nickel sulfate is 0.0285M-
0.0287M, the concentration of sodium molybdate are 0.00565M-0.00567M, and the concentration of cobalt nitrate is 0.000694M-0.0694M, lemon
The concentration of sour trisodium is 0.0249M-0.0251M, and the concentration of PVP is 0.0000625M, and the quality of reducing agent sodium borohydride is added
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 be centrifuged with dehydrated alcohol it is clear
3 times are washed to get the bismuth telluride nanometer sheet for arriving Supported Co nickel molybdenum particle.
2. application of the bismuth telluride nanometer sheet of Supported Co nickel molybdenum particle according to claim 1 in hydrogen reduction field,
It is characterized in that, in the step 1, PVP concentration is 0.000347M, NaOH concentration 0.417M.
3. application of the bismuth telluride nanometer sheet of Supported Co nickel molybdenum particle according to claim 1 in hydrogen reduction field,
It is characterized in that, the concentration of cobalt nitrate is 0.00694M-0.0347M in the step 2, and the quality of reducing agent sodium borohydride is 6-7
A mass parts, each mass parts are 0.01g.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810167601.XA 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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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810167601.XA 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 |
| 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 |
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| CN201510163321.8A Division 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 |
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| CN201810167603.9A Expired - Fee Related CN108286058B (en) | 2015-04-08 | 2015-04-08 | The method for preparing the bismuth telluride nanometer sheet of Supported Co nickel molybdenum particle |
| 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 |
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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 |
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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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| CN101805910A (en) * | 2009-02-18 | 2010-08-18 | 黄富成 | Hydrogen-oxygen generating electrode plate and method for manufacturing the same |
| 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 |
| CN103974769A (en) * | 2011-09-01 | 2014-08-06 | 西蒙·特鲁德尔 | Electrocatalytic materials and methods for manufacturing same |
| CN104451797A (en) * | 2014-11-28 | 2015-03-25 | 鹏南电子科技（厦门）有限公司 | Tinning processing method for Bi2Te3 matrix and supplement |
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| US9718043B2 (en) * | 2009-02-24 | 2017-08-01 | Toyota Motor Engineering & Manufacturing North America, Inc. | Core-shell nanoparticles and process for producing the same |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101805910A (en) * | 2009-02-18 | 2010-08-18 | 黄富成 | Hydrogen-oxygen generating electrode plate and method for manufacturing the same |
| CN103974769A (en) * | 2011-09-01 | 2014-08-06 | 西蒙·特鲁德尔 | Electrocatalytic materials and methods for manufacturing same |
| 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 |
| CN104451797A (en) * | 2014-11-28 | 2015-03-25 | 鹏南电子科技（厦门）有限公司 | Tinning processing method for Bi2Te3 matrix and supplement |
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| CN108286058A (en) | 2018-07-17 |
| CN106140201A (en) | 2016-11-23 |
| CN106140201B (en) | 2018-08-31 |
| CN108193218A (en) | 2018-06-22 |
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