CN102502888A - Microwave-hydrothermal preparation method for cobalt sulfide nanometer crystals - Google Patents

Microwave-hydrothermal preparation method for cobalt sulfide nanometer crystals Download PDF

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CN102502888A
CN102502888A CN2011103758027A CN201110375802A CN102502888A CN 102502888 A CN102502888 A CN 102502888A CN 2011103758027 A CN2011103758027 A CN 2011103758027A CN 201110375802 A CN201110375802 A CN 201110375802A CN 102502888 A CN102502888 A CN 102502888A
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microwave
reaction kettle
hydrothermal reaction
hydrothermal
cobalt sulfide
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CN102502888B (en
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曹丽云
李碧
孙莹
黄剑锋
吴建鹏
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Qidong Binhua water supply Co.,Ltd.
Shenzhen Pengbo Information Technology Co ltd
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Shaanxi University of Science and Technology
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Abstract

A microwave-hydrothermal preparation method for cobalt sulfide nanometer crystals includes steps of dissolving hexahydrated cobalt nitrate into deionized water to prepare liquor A; dissolving thioacetamide (TAA) into the liquor A to prepare liquor B; adding ammonia water into the liquor B to prepare aqueous liquor C with precipitate; uniformly adding the aqueous liquor C into a microwave-hydrothermal reaction kettle, sealing the hydrothermal reaction kettle, placing the sealed hydrothermal reaction kettle into a microwave-hydrothermal reaction instrument to realize reaction, and naturally cooling the hydrothermal reaction kettle to room temperature after reaction; and opening the microwave-hydrothermal reaction kettle, collecting samples by means of centrifugal separation, drying the samples in a vacuum drying tank, and obtaining black cobalt sulfide nanometer crystals. The cobalt sulfide nanometer crystals prepared by the aid of the microwave-hydrothermal preparation method are fine in crystallization, grains of the cobalt sulfide nanometer crystals are uniform, and the size of each crystal grain ranges from 10nm to 50nm. In addition, preparation process is simple, operation is convenient, reaction period is short, temperature is low, energy consumption is low, and preparation cost is also low.

Description

A kind of microwave hydrothermal prepares the method for cobalt sulfide nanocrystalline
Technical field
The invention belongs to the sulfide nano-material technical field, be specifically related to the method that a kind of microwave hydrothermal prepares the cobalt sulfide nanocrystalline material.
Technical background
The nano metal sulfide material has special non-linear nature, fluorescent characteristic, quantum size effect and other important physical chemical property, thereby is with a wide range of applications.Transient metal sulfide with 3d valence electron shell structure has performances such as good optical, electricity and magnetics especially, is widely used in high energy density cells, solar energy electric material, thereby receives extensive attention.And the energy level that nanometer sulfide brings owing to quantum size effect changes, energy gap broadens, and the emitted energy of particulate is increased, and optical absorption moves to the shortwave direction, has more excellent photoelectric catalytic activity.
Cobaltous sulfide is exactly a kind of material in the transient metal sulfide, as a kind of sulfide material of nontoxic, environmental protection, the increasing great attention that causes people of cobaltous sulfide.The nanometer cobaltous sulfide has the physics more superior than macrobead tradition cobaltous sulfide, chemistry, optics, pigment performance and purposes more widely.Such as nanometer cobaltous sulfide material good application prospects is just being arranged aspect the ultracapacitor, well-known, best capacitor material ruthenium dioxide (RuO 2) capacitance be 720-760Fg -1, and utilizing the material of nano Co S as electrical condenser, its capacitance can reach 508Fg -1[Shujuan Bao; Changming Li, Chunxian Guo, Yan Qiao.Biomolecule-assisted synthesis of cobalt sulfide nanowires for application in supercapacitors [J] .Journal of Power Sources; 2008; 180 (1): 676-681], and cobaltous sulfide is cheap, nontoxic, so aspect electrical condenser, good application prospects is arranged.Because the variety of its character; Later on will be at magneticsubstance, electronic material [Mingkui Wang; Alina M.Anghel; Benoit Marsan, Ngoc-Le Cevey Ha, Nuttapol Pootrakulchote; Shaik.M.Zakeeruddin; And Michael Gratzel.CoS Supersedes Pt as Efficient Electrocatalyst for Triiodide Reduction in Dye-Sensitized Solar Cells [J] .American Chemical Society.2009,44,131:15976-15977], aspect such as sintering of optical material and high-strength, high density material, catalysis, sensing gathers around and has broad application prospects.At present; Also few both at home and abroad about the report of the preparation of cobalt sulfide nanocrystalline; Mainly contain P.Justin; People [P.Justin, G.Ranga Rao.CoS spheres for high-rate electrochemical capacitive energy storage application [J] .International Journal of Hydrogen Energy.2010,35 (18): 9709-9715] such as G.Ranga Rao utilize Co (CH 3COOH) 2.2H 2O and L-halfcystine are that raw material has synthesized the cobaltous sulfide nano material, and people such as BaoShujuan are with CoCl 26H2O and L-halfcystine are raw material; Utilize biological auxiliary Hydrothermal Preparation to go out the cobaltous sulfide nano wire, people such as Q.R.Hu [Q.R.Hu, S.L.Wang; Y.Zhang; W.H.Tang.Synthesis of cobalt sulfide nanostructures by a facile solvothermal growth process [J] .Journal of Alloys and Compounds, 2010,491 (1-2): 707-711] with Co (NO 3) 26H 2O and thiocarbamide are raw material, utilize a kind of solvent thermal growth method of gentleness to prepare the cobaltous sulfide nanostructure.
Traditional hydrothermal synthesis method operational condition is complicated and comparatively harsh; Often need to add deleterious organism, perhaps in building-up process, need protection of inert gas as solvent, need be in HTHP or reaction for a long time at low temperatures; Reaction time is long, and cost is high.
Microwave is a kind of special type of heating, is the frequency hertzian wave in 300MHz～300GHz scope greatly, and it is between radiowave and ir radiation.Microwave with p.s. 300M～300G time periodically change, have penetrance and selectivity.This mode of motion can make the material any part moment that is in the microwave field receive microwave action; Thereby change the microscopic motion of polar particle; Be the dipole pilot polarization and the interfacial polarization of microwave-excitation polarity microcosmic particle, and force its mode of motion to move, make the ordering of rambling microcosmic particle trend according to microwave; This just causes the microscopic motion behavior of polar material to receive reinforcement and constraint that high frequency changes EM field, and the result causes energy waste.In the mechanism of microwave; The energy of loss is absorbed by polar material and transforms into other forms of energy such as heat energy; Interior motion and the collision between them, the friction of microcosmic particle are reinforced or weaken; Cause the microcosmic particle self-energy to change, thereby make it that some new physics, chemical transformation take place.Microwave method makes synthesizing nano-particle become efficiently as a kind of heating means evenly and rapidly, simple and repeatability height.
Summary of the invention
The objective of the invention is to propose the method that a kind of microwave hydrothermal prepares cobalt sulfide nanocrystalline.This method is simple to operate, need not protective atmosphere, and the reaction times is short, and temperature of reaction is low, and energy consumption is little, the cobalt sulfide nanocrystalline well-crystallized of gained, and particle size dispersion is better, complete shape and appearance, controllable diameter is repeatable high.
For achieving the above object, the technical scheme that the present invention adopts is:
1) gets the analytical pure Cobaltous nitrate hexahydrate (Co (NO of 0.58g-4.64g 3) 26H 2O) be dissolved in the deionized water, be configured to the red clear solution A of 40mL-80mL;
2) get the analytical pure thioacetamide (TAA) of 0.15g-1.20g, be dissolved in the solution A, stir solution B;
3) in solution B, adding the 0.2-4.0mL mass concentration is 5% ammoniacal liquor, obtains containing sedimentary aqueous solution C;
4) aqueous solution C is joined in the microwave hydrothermal reaction kettle uniformly, controlling its packing ratio is 40%-80%; Put into microwave hydrothermal reaction behind the sealing hydrothermal reaction kettle; Hydrothermal temperature is controlled at 150-220 ℃, reaction 20-120min, and reaction naturally cools to room temperature after finishing;
5) after reaction finishes, open microwave hydrothermal reaction kettle, collect sample, the sample of collecting is carried out drying with the vacuum drying oven of putting into 60 ℃ after deionized water, the washing with alcohol respectively, obtain the cobalt sulfide nanocrystalline of black through spinning.
The cobalt sulfide nanocrystalline well-crystallized of the present invention's preparation, uniform particles, grain-size is about 10-50nm; And preparation technology is simple, and is easy to operate, and reaction time is short, and temperature is low, and energy consumption is little, and preparation cost is lower.
Description of drawings
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of the cobalt sulfide nanocrystalline of the embodiment of the invention 1 preparation;
Fig. 2 is the transmission electron micrograph of the cobalt sulfide nanocrystalline of the embodiment of the invention 1 preparation.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is done further explain.
Embodiment 1:
1) gets the analytical pure Cobaltous nitrate hexahydrate (Co (NO of 1.16g 3) 26H 2O) be dissolved in the deionized water, be configured to the red clear solution A of 40mL;
2) get the analytical pure thioacetamide (TAA) of 0.30g, be dissolved in the solution A, stir solution B;
3) in solution B, adding the 1.0mL mass concentration is 5% ammoniacal liquor, obtains containing sedimentary aqueous solution C;
4) aqueous solution C is joined in the microwave hydrothermal reaction kettle uniformly, controlling its packing ratio is 60%; Put into microwave hydrothermal reaction behind the sealing hydrothermal reaction kettle; Hydrothermal temperature is controlled at 180 ℃, reaction 60min, and reaction naturally cools to room temperature after finishing;
5) after reaction finishes, open microwave hydrothermal reaction kettle, collect sample, the sample of collecting is carried out drying with the vacuum drying oven of putting into 60 ℃ after deionized water, the washing with alcohol respectively, obtain the cobalt sulfide nanocrystalline of black through spinning.
The cobalt sulfide nanocrystalline product of gained is analyzed with x-ray diffractometer, found that product is that JCPDS is numbered 65-3418 (Fig. 1).This sample is observed with sem, can be found out that prepared sample size is about 20nm (Fig. 2).
Embodiment 2:
1) gets the analytical pure Cobaltous nitrate hexahydrate (Co (NO of 0.58g 3) 26H 2O) be dissolved in the deionized water, be configured to the red clear solution A of 50mL;
2) get the analytical pure thioacetamide (TAA) of 0.15g, be dissolved in the solution A, stir solution B;
3) in solution B, adding the 2.3mL mass concentration is 5% ammoniacal liquor, obtains containing sedimentary aqueous solution C;
4) aqueous solution C is joined in the microwave hydrothermal reaction kettle uniformly, controlling its packing ratio is 80%; Put into microwave hydrothermal reaction behind the sealing hydrothermal reaction kettle; Hydrothermal temperature is controlled at 170 ℃, reaction 60min, and reaction naturally cools to room temperature after finishing;
5) after reaction finishes, open microwave hydrothermal reaction kettle, collect sample, the sample of collecting is carried out drying with the vacuum drying oven of putting into 60 ℃ after deionized water, the washing with alcohol respectively, obtain the cobalt sulfide nanocrystalline of black through spinning.
Embodiment 3:
1) gets the analytical pure Cobaltous nitrate hexahydrate (Co (NO of 0.87g 3) 26H 2O) be dissolved in the deionized water, be configured to the red clear solution A of 60mL;
2) get the analytical pure thioacetamide (TAA) of 0.45g, be dissolved in the solution A, stir solution B;
3) in solution B, adding the 1.6mL mass concentration is 5% ammoniacal liquor, obtains containing sedimentary aqueous solution C;
4) aqueous solution C is joined in the microwave hydrothermal reaction kettle uniformly, controlling its packing ratio is 40%; Put into microwave hydrothermal reaction behind the sealing hydrothermal reaction kettle; Hydrothermal temperature is controlled at 150 ℃, reaction 120min, and reaction naturally cools to room temperature after finishing;
5) after reaction finishes, open microwave hydrothermal reaction kettle, collect sample, the sample of collecting is carried out drying with the vacuum drying oven of putting into 60 ℃ after deionized water, the washing with alcohol respectively, obtain the cobalt sulfide nanocrystalline of black through spinning.
Embodiment 4:
1) gets the analytical pure Cobaltous nitrate hexahydrate (Co (NO of 2.32g 3) 26H 2O) be dissolved in the deionized water, be configured to the red clear solution A of 70mL;
2) get the analytical pure thioacetamide (TAA) of 0.60g, be dissolved in the solution A, stir solution B;
3) in solution B, adding the 3.5mL mass concentration is 5% ammoniacal liquor, obtains containing sedimentary aqueous solution C;
4) aqueous solution C is joined in the microwave hydrothermal reaction kettle uniformly, controlling its packing ratio is 70%; Put into microwave hydrothermal reaction behind the sealing hydrothermal reaction kettle; Hydrothermal temperature is controlled at 200 ℃, reaction 50min, and reaction naturally cools to room temperature after finishing;
5) after reaction finishes, open microwave hydrothermal reaction kettle, collect sample, the sample of collecting is carried out drying with the vacuum drying oven of putting into 60 ℃ after deionized water, the washing with alcohol respectively, obtain the cobalt sulfide nanocrystalline of black through spinning.
Embodiment 5:
1) gets the analytical pure Cobaltous nitrate hexahydrate (Co (NO of 3.40g 3) 26H 2O) be dissolved in the deionized water, be configured to the red clear solution A of 80mL;
2) get the analytical pure thioacetamide (TAA) of 0.85g, be dissolved in the solution A, stir solution B;
3) in solution B, adding the 0.2mL mass concentration is 5% ammoniacal liquor, obtains containing sedimentary aqueous solution C;
4) aqueous solution C is joined in the microwave hydrothermal reaction kettle uniformly, controlling its packing ratio is 50%; Put into microwave hydrothermal reaction behind the sealing hydrothermal reaction kettle; Hydrothermal temperature is controlled at 220 ℃, reaction 20min, and reaction naturally cools to room temperature after finishing;
5) after reaction finishes, open microwave hydrothermal reaction kettle, collect sample, the sample of collecting is carried out drying with the vacuum drying oven of putting into 60 ℃ after deionized water, the washing with alcohol respectively, obtain the cobalt sulfide nanocrystalline of black through spinning.
Embodiment 6:
1) gets the analytical pure Cobaltous nitrate hexahydrate (Co (NO of 4.64g 3) 26H 2O) be dissolved in the deionized water, be configured to the red clear solution A of 50mL;
2) get the analytical pure thioacetamide (TAA) of 1.20g, be dissolved in the solution A, stir solution B;
3) in solution B, adding the 4.0mL mass concentration is 5% ammoniacal liquor, obtains containing sedimentary aqueous solution C;
4) aqueous solution C is joined in the microwave hydrothermal reaction kettle uniformly, controlling its packing ratio is 80%; Put into microwave hydrothermal reaction behind the sealing hydrothermal reaction kettle; Hydrothermal temperature is controlled at 160 ℃, reaction 100min, and reaction naturally cools to room temperature after finishing;
5) after reaction finishes, open microwave hydrothermal reaction kettle, collect sample, the sample of collecting is carried out drying with the vacuum drying oven of putting into 60 ℃ after deionized water, the washing with alcohol respectively, obtain the cobalt sulfide nanocrystalline of black through spinning.

Claims (1)

1. a microwave hydrothermal prepares the method for cobalt sulfide nanocrystalline, it is characterized in that:
1) gets the analytical pure Cobaltous nitrate hexahydrate (Co (NO of 0.58g-4.64g 3) 26H 2O) be dissolved in the deionized water, be configured to the red clear solution A of 40mL-80mL;
2) get the analytical pure thioacetamide (TAA) of 0.15g-1.20g, be dissolved in the solution A, stir solution B;
3) in solution B, adding the 0.2-4.0mL mass concentration is 5% ammoniacal liquor, obtains containing sedimentary aqueous solution C;
4) aqueous solution C is joined in the microwave hydrothermal reaction kettle uniformly, controlling its packing ratio is 40%-80%; Put into microwave hydrothermal reaction behind the sealing hydrothermal reaction kettle; Hydrothermal temperature is controlled at 150-220 ℃, reaction 20-120min, and reaction naturally cools to room temperature after finishing;
5) after reaction finishes, open microwave hydrothermal reaction kettle, collect sample, the sample of collecting is carried out drying with the vacuum drying oven of putting into 60 ℃ after deionized water, the washing with alcohol respectively, obtain the cobalt sulfide nanocrystalline of black through spinning.
CN201110375802.7A 2011-11-23 2011-11-23 Microwave-hydrothermal preparation method for cobalt sulfide nanometer crystals Active CN102502888B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106799242A (en) * 2015-11-26 2017-06-06 中国科学院大连化学物理研究所 A kind of surface amphiphilic nano vulcanization Co catalysts and preparation method and application
CN106799260A (en) * 2015-11-26 2017-06-06 中国科学院大连化学物理研究所 Surface amphiphilic nano composite sulfuration nickel cobalt iron catalyst and preparation method and application
CN108821348A (en) * 2018-09-17 2018-11-16 陕西科技大学 A kind of cobalt sulfide nanometer sheet material and preparation method thereof
CN111943277A (en) * 2020-08-19 2020-11-17 北京理工大学 Preparation method of core-shell structure amorphous cobalt sulfide particles

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Publication number Priority date Publication date Assignee Title
CN101746837A (en) * 2009-12-24 2010-06-23 东北师范大学 Preparation method of cobalt sulfide micro tube with hiberarchy structure
CN101786671A (en) * 2009-10-30 2010-07-28 陕西科技大学 Method for preparing bar-shaped cobalt sulfide nanocrystalline

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101786671A (en) * 2009-10-30 2010-07-28 陕西科技大学 Method for preparing bar-shaped cobalt sulfide nanocrystalline
CN101746837A (en) * 2009-12-24 2010-06-23 东北师范大学 Preparation method of cobalt sulfide micro tube with hiberarchy structure

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Title
WENJUN DONG ET AL.: "Hydrothermal synthesis and structure evolution of hierarchical cobalt sulfide nanostructures", 《DALTON TRANS.》 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106799242A (en) * 2015-11-26 2017-06-06 中国科学院大连化学物理研究所 A kind of surface amphiphilic nano vulcanization Co catalysts and preparation method and application
CN106799260A (en) * 2015-11-26 2017-06-06 中国科学院大连化学物理研究所 Surface amphiphilic nano composite sulfuration nickel cobalt iron catalyst and preparation method and application
CN106799260B (en) * 2015-11-26 2019-08-02 中国科学院大连化学物理研究所 Surface amphiphilic nano composite sulfuration nickel cobalt iron catalyst and the preparation method and application thereof
CN106799242B (en) * 2015-11-26 2019-08-09 中国科学院大连化学物理研究所 A kind of surface amphiphilic nano vulcanization Co catalysts and the preparation method and application thereof
CN108821348A (en) * 2018-09-17 2018-11-16 陕西科技大学 A kind of cobalt sulfide nanometer sheet material and preparation method thereof
CN108821348B (en) * 2018-09-17 2021-02-19 陕西科技大学 Cobalt sulfide nanosheet material and preparation method thereof
CN111943277A (en) * 2020-08-19 2020-11-17 北京理工大学 Preparation method of core-shell structure amorphous cobalt sulfide particles

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