CN106140201A - The Tellurobismuthite. nanometer sheet of a kind of Supported Co nickel molybdenum granule and synthetic method thereof - Google Patents

The Tellurobismuthite. nanometer sheet of a kind of Supported Co nickel molybdenum granule and synthetic method thereof Download PDF

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CN106140201A
CN106140201A CN201510163321.8A CN201510163321A CN106140201A CN 106140201 A CN106140201 A CN 106140201A CN 201510163321 A CN201510163321 A CN 201510163321A CN 106140201 A CN106140201 A CN 106140201A
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tellurobismuthite
nanometer sheet
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CN106140201B (en
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尹凯
梁砚琴
崔振铎
杨贤金
朱胜利
李朝阳
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Tianjin University
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Abstract

The present invention discloses Tellurobismuthite. nanometer sheet and the synthetic method thereof of a kind of Supported Co nickel molybdenum granule, Tellurobismuthite. nanometer sheet is hexagon, on the evengranular surface being distributed in Tellurobismuthite. nanometer sheet of cobalt nickel molybdenum, utilize solvent-thermal method, prepare hexagonal Tellurobismuthite. nanometer sheet by controlling temperature, and utilize direct-reduction process to carry out the load of cobalt nickel molybdenum granule in Tellurobismuthite. nanometer sheet.Implementation cost of the present invention is low, easy and simple to handle, pollutes low, is the synthetic method of a kind of high-efficiency and economic, and the material granule of the present invention is more evenly distributed simultaneously, and specific surface area is bigger, and analysis oxygen performance is higher.

Description

The Tellurobismuthite. nanometer sheet of a kind of Supported Co nickel molybdenum granule and synthetic method thereof
Technical field
The present invention relates to a kind of novel nano-material and synthetic method thereof, particularly relate to the telluride of a kind of Supported Co nickel molybdenum granule Bismuth nanometer sheet and synthetic method thereof.
Background technology
The catalysis material of known anode is mainly some noble metals, but due to expensive, limits in all fields Application.The present invention proposes and uses Bi2Te3Semi-conducting material, as anode, is not similar to research before this.Propose this to think Method mainly consider following some: (1) Bi2Te3Crystal structure is closely similar with the crystal structure of graphite, easily dissociates in flakes Shape, face of dissociating is smooth, and has metallic luster, has good electric conductivity, the free electron of metalloid material, is beneficial to electricity Transmission (2) Bi of son2Te3Being that thermal conductivity is low, electrical conductivity is high, and electrical conductivity varies with temperature substantially.Temperature after electrified regulation Necessarily rising, can inspire its topological insulator characteristic of more electronics (3) is a kind of new thing with unusual Quantum Properties Matter state.
Cobalt, nickel, molybdenum granule have good application in terms of Electrochemical oxygen evolution, and the alkali resistance of nickel is strong, and oxygen evolution potential is the most relatively Low and be widely used, molybdenum is in the transition series metal element left side and is positioned at the nickel on the right has synergism, cobalt and nickel in analysis One layer of oxidation film the thinnest can be formed at electrode surface before oxygen, carry high catalytic activity.
Summary of the invention
It is an object of the invention to provide Tellurobismuthite. nanometer sheet and the synthetic method thereof of a kind of Supported Co nickel molybdenum granule, it is thus achieved that a kind of Evenly, specific surface area is bigger for distribution of particles, and the nano material that analysis oxygen performance is higher, the method has low cost, preparation The simple feature of process.
The purpose of the present invention is achieved by following technical proposals:
The Tellurobismuthite. nanometer sheet of a kind of Supported Co nickel molybdenum granule, Tellurobismuthite. nanometer sheet is hexagon, and cobalt nickel molybdenum is evengranular It is distributed on the surface of Tellurobismuthite. nanometer sheet, and carries out as steps described below:
Step 1, the preparation of Tellurobismuthite. nanometer sheet: take BiCl3(production of this reagent company limited of Adama), Na2TeO3 (production of Beijing Yi Nuokai company), PVP (Tianjin Heowns Biochemical Technology Co., Ltd. produces, molecular weight w=40000), NaOH (production of East China, Tianjin chemical reagent work), in ethylene glycol, is stirred at room temperature 2h, is then transferred to politef high In temperature reactor, constant temperature 220 DEG C, takes out sample after reaction 36h, by deionized water and dehydrated alcohol eccentric cleaning respectively Drying to obtain Tellurobismuthite. nanometer sheet after 3 times.
Described in step 1 in ethylene glycol solution, BiCl3Concentration is 0.0278M, Na2TeO3Concentration is 0.0425M, PVP Concentration is 0.00026M-0.000521M, NaOH concentration is 0.415M-0.419M；
Step 2, water and ethylene glycol that the Tellurobismuthite. nanometer sheet alkali prepared in step 1 process is placed on Co-Ni-Mo source mix Close in solution, 50-70min is stirred at room temperature, the most directly add sodium borohydride ultrasonic 30min reduction mixed solution；
Ethylene glycol in mixed solution described in step 2: the volume ratio of water is 1:1, the concentration of nickel sulfate is 0.0285M-0.0287M, the concentration of sodium molybdate is 0.00565M-0.00567M, and the concentration of cobalt nitrate is 0.000694M-0.0694M, the concentration of trisodium citrate is that the concentration of 0.0249M-0.0251M, PVP is 0.0000625M, the quality adding borane reducing agent sodium hydride is 5-8 mass parts, and each mass parts is 0.01g；
Step 3, by step 2 solution take out be placed in water-bath 50-70min in 35-45 DEG C of water-bath, after use dehydrated alcohol Eccentric cleaning 3 times, i.e. obtains the Tellurobismuthite. nanometer sheet of Supported Co nickel molybdenum granule.
The method cost of the present invention is low, easy and simple to handle, the shortest, compared with traditional preparation methods, mainly There is following advantage: (1) solves the feature of particle agglomeration, make cobalt nickel molybdenum granule be evenly distributed on Tellurobismuthite. nanometer Sheet (as shown in Figure 6)；(2) response time is greatly shortened, and simple to operate；(3) electrochemical operation is used The GAMRY 04084 that stands tests, the Tellurobismuthite. nanometer sheet hydrogen reduction linear scanning of Supported Co nickel molybdenum granule in the present invention Highest current density, shows that this material has higher product oxygen performance, can be used for hydrogen reduction field ((as shown in Figure 7).
Accompanying drawing explanation
Fig. 1 is XRD figure spectrum (XRD, the Rigaku of the Tellurobismuthite. nanometer sheet nano material of Supported Co nickel molybdenum granule of the present invention D/max-Ra), wherein curve (1) is the Tellurobismuthite. nanometer sheet XRD figure spectrum of unsupported CoNiMo granule, curve (2) Compose for the Tellurobismuthite. nanometer sheet XRD figure after load C oNiMo granule；
Fig. 2 be the concentration of cobalt nitrate of the present invention be the Tellurobismuthite. nanometer sheet of load C oNiMo granule during 0.000694M SEM pattern photo (FE-SEM, Hitachi S-4800)；
Fig. 3 be the concentration of cobalt nitrate of the present invention be the Tellurobismuthite. nanometer sheet of load C oNiMo granule during 0.00694M SEM pattern photo (FE-SEM, Hitachi S-4800)；
Fig. 4 be the concentration of cobalt nitrate of the present invention be the Tellurobismuthite. nanometer sheet of load C oNiMo granule during 0.0347M SEM pattern photo (FE-SEM, Hitachi S-4800)；
Fig. 5 be the concentration of cobalt nitrate of the present invention be the Tellurobismuthite. nanometer sheet of load C oNiMo granule during 0.0694M SEM pattern photo (FE-SEM, Hitachi S-4800)；
Fig. 6 is TEM pattern photo (TEM, the Philips of the Tellurobismuthite. nanometer sheet of load C oNiMo granule of the present invention Tecnai G2f20c)；
Fig. 7 is the hydrogen reduction of the Tellurobismuthite. nanometer sheet of the load C oNiMo granule of synthesis under difference cobalt nitrate concentration of the present invention Linear scanning curve, wherein curve (1) is the hydrogen reduction line of the Tellurobismuthite. nanometer sheet that concentration is 0.0694M at cobalt nitrate Property scanning curve, curve (2) is linearly to sweep in the hydrogen reduction of the Tellurobismuthite. nanometer sheet that concentration is 0.000694M of cobalt nitrate Retouching curve, curve (3) is the hydrogen reduction linear scanning curve of Ni net.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearer, below embodiment of the present invention is made further Describe in detail.
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 politef pyroreaction still, constant temperature 220 DEG C, 36h.
Sample is taken out, by dried for standby after deionized water and dehydrated alcohol respectively eccentric cleaning 3 times.
Take after 0.07g dried Tellurobismuthite. nanometer sheet alkali processes in the mixed solution of Co-Ni-Mo source, in mixed solution Ethylene glycol: the volume ratio of water is 1:1, solution total amount 20ml.In solution, the concentration of nickel sulfate is 0.0285M, sodium molybdate Concentration is 0.00565M, and the concentration of cobalt nitrate is 0.000694M, and the concentration of trisodium citrate is 0.0249M, PVP's Concentration is 0.0000625M, and 50min is stirred at room temperature, and the most directly adds 0.08g sodium borohydride ultrasonic 30min reduction mixing molten Liquid.
Solution is taken out and is placed in water-bath 70min in 35 DEG C of water-baths, use dehydrated alcohol eccentric cleaning 3 times afterwards, i.e. born Carry the Tellurobismuthite. nanometer sheet of cobalt nickel molybdenum granule.
Embodiment 2
Take 0.315gBiCl3、0.34gNa2TeO3, 0.52gPVP (w=40000), 0.62gNaOH be in 36ml ethylene glycol In, 2h is stirred at room temperature.
It is transferred to above-mentioned in politef pyroreaction still, constant temperature 220 DEG C, 36h.
Sample is taken out, by dried for standby after deionized water and dehydrated alcohol respectively eccentric cleaning 3 times.
Take after 0.07g dried Tellurobismuthite. nanometer sheet alkali processes in the mixed solution of Co-Ni-Mo source, second in mixed solution Glycol: the volume ratio of water is 1:1, solution total amount 20ml.In solution, the concentration of nickel sulfate is 0.0287M, sodium molybdate Concentration is 0.00567M, and the concentration of cobalt nitrate is 0.00694M, and the concentration of trisodium citrate is the dense of 0.0251M, PVP Degree is 0.0000625M, and 70min is stirred at room temperature, and the most directly adds 0.08g sodium borohydride ultrasonic 30min reduction mixed solution.
Solution is taken out and is placed in water-bath 50min in 45 DEG C of water-baths, use dehydrated alcohol eccentric cleaning 3 times afterwards, i.e. born Carry the Tellurobismuthite. nanometer sheet of cobalt nickel molybdenum granule.
Embodiment 3
Take 0.315gBiCl3、0.34gNa2TeO3, 0.50gPVP (w=40000), 0.60gNaOH be in 36ml ethylene glycol In, 2h is stirred at room temperature.
It is transferred to above-mentioned in politef pyroreaction still, constant temperature 220 DEG C, 36h.
Sample is taken out, by dried for standby after deionized water and dehydrated alcohol respectively eccentric cleaning 3 times.
Take after 0.07g dried Tellurobismuthite. nanometer sheet alkali processes in the mixed solution of Co-Ni-Mo source, second in mixed solution Glycol: the volume ratio of water is 1:1, solution total amount 20ml.In solution, the concentration of nickel sulfate is 0.0286M, sodium molybdate Concentration is 0.00566M, and the concentration of cobalt nitrate is 0.0347M, and the concentration of trisodium citrate is the dense of 0.0250M, PVP Degree is 0.0000625M, and 60min is stirred at room temperature, and the most directly adds 0.08g sodium borohydride ultrasonic 30min reduction mixed solution.
Solution is taken out and is placed in water-bath 60min in 40 DEG C of water-baths, use dehydrated alcohol eccentric cleaning 3 times afterwards, i.e. born Carry the Tellurobismuthite. nanometer sheet of cobalt nickel molybdenum granule.
Embodiment 4
Take 0.315gBiCl3、0.34gNa2TeO3, 0.50gPVP (w=40000), 0.60gNaOH be in 36ml ethylene glycol In, it is stirred at room temperature no less than 2h.
It is transferred to above-mentioned in politef pyroreaction still, constant temperature 220 DEG C, 36h.
Sample is taken out, by dried for standby after deionized water and dehydrated alcohol respectively eccentric cleaning 3 times.
Take after 0.07g dried Tellurobismuthite. nanometer sheet alkali processes in the mixed solution of Co-Ni-Mo source, second in mixed solution Glycol: the volume ratio of water is 1:1, solution total amount 20ml.In solution, the concentration of nickel sulfate is 0.0286M, sodium molybdate Concentration is 0.00566M, and the concentration of cobalt nitrate is 0.0694M, and the concentration of trisodium citrate is the dense of 0.0249M, PVP Degree is 0.0000625M, and 60min is stirred at room temperature, and the most directly adds 0.08g sodium borohydride ultrasonic 30min reduction mixed solution.
Solution is taken out and is placed in water-bath 60min in 40 DEG C of water-baths, use dehydrated alcohol eccentric cleaning 3 times afterwards, i.e. born Carry the Tellurobismuthite. nanometer sheet of cobalt nickel molybdenum granule.
Embodiment 5
Take 0.315gBiCl3、0.34gNa2TeO3, 0.50gPVP (w=40000), 0.60gNaOH be in 36ml ethylene glycol In, it is stirred at room temperature no less than 2h.
It is transferred to above-mentioned in politef pyroreaction still, constant temperature 220 DEG C, 36h.
Sample is taken out, by dried for standby after deionized water and dehydrated alcohol respectively eccentric cleaning 3 times.
Take after 0.07g dried Tellurobismuthite. nanometer sheet alkali processes in the mixed solution of Co-Ni-Mo source, second in mixed solution Glycol: the volume ratio of water is 1:1, solution total amount 20ml.In solution, the concentration of nickel sulfate is 0.0286M, sodium molybdate Concentration is 0.00566M, and the concentration of cobalt nitrate is 0.000694M, and the concentration of trisodium citrate is 0.0249M, PVP's Concentration is 0.0000625M, and 60min is stirred at room temperature, and the most directly adds 0.05g sodium borohydride ultrasonic 30min reduction mixing molten Liquid.
Solution is taken out and is placed in water-bath 60min in 40 DEG C of water-baths, use dehydrated alcohol eccentric cleaning 3 times afterwards, i.e. born Carry the Tellurobismuthite. nanometer sheet of cobalt nickel molybdenum granule.
Embodiment 6
Take 0.315gBiCl3、0.34gNa2TeO3, 0.50gPVP (w=40000), 0.60gNaOH be in 36ml ethylene glycol In, it is stirred at room temperature no less than 2h.
It is transferred to above-mentioned in politef pyroreaction still, constant temperature 220 DEG C, 36h.
Sample is taken out, by dried for standby after deionized water and dehydrated alcohol respectively eccentric cleaning 3 times.
Take after 0.07g dried Tellurobismuthite. nanometer sheet alkali processes in the mixed solution of Co-Ni-Mo source, second in mixed solution Glycol: the volume ratio of water is 1:1, solution total amount 20ml.In solution, the concentration of nickel sulfate is 0.0286M, sodium molybdate Concentration is 0.00566M, and the concentration of cobalt nitrate is 0.000694M, and the concentration of trisodium citrate is 0.0249M, PVP's Concentration is 0.0000625M, and 60min is stirred at room temperature, and the most directly adds 0.06g sodium borohydride ultrasonic 30min reduction mixing molten Liquid.
Solution is taken out and is placed in water-bath 60min in 40 DEG C of water-baths, use dehydrated alcohol eccentric cleaning 3 times afterwards, i.e. born Carry the Tellurobismuthite. nanometer sheet of cobalt nickel molybdenum granule.
Embodiment 7
Take 0.315gBiCl3、0.34gNa2TeO3, 0.50gPVP (w=40000), 0.60gNaOH be in 36ml ethylene glycol In, it is stirred at room temperature no less than 2h.
It is transferred to above-mentioned in politef pyroreaction still, constant temperature 220 DEG C, 36h.
Sample is taken out, by dried for standby after deionized water and dehydrated alcohol respectively eccentric cleaning 3 times.
Take after 0.07g dried Tellurobismuthite. nanometer sheet alkali processes in the mixed solution of Co-Ni-Mo source, second in mixed solution Glycol: the volume ratio of water is 1:1, solution total amount 20ml.In solution, the concentration of nickel sulfate is 0.0286M, sodium molybdate Concentration is 0.00566M, and the concentration of cobalt nitrate is 0.000694M, and the concentration of trisodium citrate is 0.0249M, PVP's Concentration is 0.0000625M, and 60min is stirred at room temperature, and the most directly adds 0.07g sodium borohydride ultrasonic 30min reduction mixing molten Liquid.
Solution is taken out and is placed in water-bath 60min in 40 DEG C of water-baths, use dehydrated alcohol eccentric cleaning 3 times afterwards, i.e. born Carry the Tellurobismuthite. nanometer sheet of cobalt nickel molybdenum granule.
Above the present invention is done exemplary description, it should explanation, in the situation of the core without departing from the present invention Under, any simple deformation, amendment or other those skilled in the art can not spend the equivalent of creative work to replace Change and each fall within protection scope of the present invention.

Claims (6)

1. the Tellurobismuthite. nanometer sheet of a Supported Co nickel molybdenum granule, it is characterised in that Tellurobismuthite. nanometer sheet is hexagon, cobalt nickel On the evengranular surface being distributed in Tellurobismuthite. nanometer sheet of molybdenum, and carry out as steps described below:
Step 1, the preparation of Tellurobismuthite. nanometer sheet: take BiCl3、Na2TeO3, PVP (w=40000), NaOH be in second two In alcohol, 2h is stirred at room temperature, is then transferred in politef pyroreaction still, constant temperature 220 DEG C, will after reaction 36h Sample takes out, by drying to obtain Tellurobismuthite. nanometer sheet after deionized water and dehydrated alcohol respectively eccentric cleaning 3 times.
Described in step 1 in ethylene glycol solution, BiCl3Concentration is 0.0278M, Na2TeO3Concentration is 0.0425M, PVP Concentration is 0.00026M-0.000521M, NaOH concentration is 0.415M-0.419M；
Step 2, water and ethylene glycol that the Tellurobismuthite. nanometer sheet alkali prepared in step 1 process is placed on Co-Ni-Mo source mix Close in solution, 50-70min is stirred at room temperature, the most directly add sodium borohydride ultrasonic 30min reduction mixed solution；
Ethylene glycol in mixed solution described in step 2: the volume ratio of water is 1:1, the concentration of nickel sulfate is 0.0285M-0.0287M, the concentration of sodium molybdate is 0.00565M-0.00567M, and the concentration of cobalt nitrate is 0.000694M-0.0694M, the concentration of trisodium citrate is that the concentration of 0.0249M-0.0251M, PVP is 0.0000625M, the quality adding borane reducing agent sodium hydride is 5-8 mass parts, and each mass parts is 0.01g；
Step 3, by step 2 solution take out be placed in water-bath 50-70min in 35-45 DEG C of water-bath, after use dehydrated alcohol Eccentric cleaning 3 times, i.e. obtains the Tellurobismuthite. nanometer sheet of Supported Co nickel molybdenum granule.
The Tellurobismuthite. nanometer sheet of Supported Co nickel molybdenum granule the most according to claim 1, it is characterised in that described step (1) In, PVP concentration is 0.000347M, NaOH concentration is 0.417M.
The Tellurobismuthite. nanometer sheet of Supported Co nickel molybdenum granule the most according to claim 1, it is characterised in that described step (2) The concentration of middle cobalt nitrate is 0.00694M-0.0347M, and the quality of borane reducing agent sodium hydride is 6-7 mass parts, Mei Gezhi Amount part is 0.01g.
4. the synthetic method of the Tellurobismuthite. nanometer sheet of a Supported Co nickel molybdenum granule, it is characterised in that Tellurobismuthite. nanometer sheet is hexagonal Shape, on the evengranular surface being distributed in Tellurobismuthite. nanometer sheet of cobalt nickel molybdenum, and is carried out as steps described below:
Step 1, the preparation of Tellurobismuthite. nanometer sheet: take BiCl3、Na2TeO3, PVP (w=40000), NaOH be in second two In alcohol, 2h is stirred at room temperature, is then transferred in politef pyroreaction still, constant temperature 220 DEG C, will after reaction 36h Sample takes out, by drying to obtain Tellurobismuthite. nanometer sheet after deionized water and dehydrated alcohol respectively eccentric cleaning 3 times.
Described in step 1 in ethylene glycol solution, BiCl3Concentration is 0.0278M, Na2TeO3Concentration is 0.0425M, PVP Concentration is 0.00026M-0.000521M, NaOH concentration is 0.415M-0.419M；
Step 2, water and ethylene glycol that the Tellurobismuthite. nanometer sheet alkali prepared in step 1 process is placed on Co-Ni-Mo source mix Close in solution, 50-70min is stirred at room temperature, the most directly add sodium borohydride ultrasonic 30min reduction mixed solution；
Ethylene glycol in mixed solution described in step 2: the volume ratio of water is 1:1, the concentration of nickel sulfate is 0.0285M-0.0287M, the concentration of sodium molybdate is 0.00565M-0.00567M, and the concentration of cobalt nitrate is 0.000694M-0.0694M, the concentration of trisodium citrate is that the concentration of 0.0249M-0.0251M, PVP is 0.0000625M, the quality adding borane reducing agent sodium hydride is 5-8 mass parts, and each mass parts is 0.01g；
Step 3, by step 2 solution take out be placed in water-bath 50-70min in 35-45 DEG C of water-bath, after use dehydrated alcohol Eccentric cleaning 3 times, i.e. obtains the Tellurobismuthite. nanometer sheet of Supported Co nickel molybdenum granule.
The synthetic method of the Tellurobismuthite. nanometer sheet of Supported Co nickel molybdenum granule the most according to claim 4, it is characterised in that institute Stating in step (1), PVP concentration is 0.000347M, NaOH concentration is 0.417M.
The synthetic method of the Tellurobismuthite. nanometer sheet of Supported Co nickel molybdenum granule the most according to claim 4, it is characterised in that institute Stating the concentration of cobalt nitrate in step (2) is 0.00694M-0.0347M, and the quality of borane reducing agent sodium hydride is 6-7 quality Part, each mass parts is 0.01g.
CN201510163321.8A 2015-04-08 2015-04-08 A kind of the bismuth telluride nanometer sheet and its synthetic method of Supported Co nickel molybdenum particle Expired - Fee Related CN106140201B (en)

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