CN102424959A - Method for preparing cobalt sulfide thin film on indium tin oxide (ITO) substrate by microwave hydrothermal process - Google Patents

Method for preparing cobalt sulfide thin film on indium tin oxide (ITO) substrate by microwave hydrothermal process Download PDF

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CN102424959A
CN102424959A CN2011103758012A CN201110375801A CN102424959A CN 102424959 A CN102424959 A CN 102424959A CN 2011103758012 A CN2011103758012 A CN 2011103758012A CN 201110375801 A CN201110375801 A CN 201110375801A CN 102424959 A CN102424959 A CN 102424959A
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solution
reaction kettle
ito substrate
hydrothermal
hydrothermal reaction
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曹丽云
李碧
孙莹
黄剑锋
吴建鹏
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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Abstract

The invention discloses a method for preparing a cobalt sulfide thin film on an indium tin oxide (ITO) substrate by a microwave hydrothermal process, which comprises: adding cobaltous oxalate dehydrate into deionized water to obtain a solution A; adding thiourea into the solution A to obtain a solution B; adding H2O2 into the solution B to obtain a precursor film coating solution C; pouring the precursor film coating solution C into a hydrothermal reaction kettle; immersing the ITO substrate into the precursor film coating solution C in the reaction kettle; sealing the hydrothermal reaction kettle, and placing the hydrothermal reaction kettle into a microwave hydrothermal reaction device to perform a microwave hydrothermal reaction; and after the reaction is finished, naturally cooling to room temperature, taking the ITO substrate output, washing with distilled water and absolute ethanol, drying in a drying tank and obtaining the cobalt sulfide thin film on the surface of the indium tin oxide. The cobalt sulfide thin film prepared by the method has good crystallization property, and is uniform and insusceptible to breakage; and the preparation process is simple, the operation is convenient, the reaction period is short, the temperature is low, the energy consumption is small, and the preparation cost is low.

Description

A kind of microwave-hydrothermal method prepares the method for cobaltous sulfide film on ito substrate
Technical field
The invention belongs to the sulfide nano-material technical field, be specifically related to a kind of microwave-hydrothermal method prepares the cobaltous sulfide film on ito substrate method.
Background technology
Transient metal sulfide material as a kind of nontoxic, environmental protection; CoS has special 3d valence electron shell structure; Its energy gap is approximately 3.91eV [S.P.Tandon; J.P.Gupta.Measurement of Forbidden Energy Gap of Semiconductors by Diffuse Reflectance Technique.Physica Status Solidi (b); 1970,381 (1): 363-367], this makes it have good optical performance, electric property, magnetic performance, catalytic performance and lubricity etc. more.There is bibliographical information to obtain CoS film [the Zhenrui Yu that energy gap is about 1.1eV through control process parameters; Jinhui Du, Shuhua Guo, Jiayou Zhang; Yasuhiro Matsumoto.CoS thin films prepared with modified chemical bath deposition [J] .Thin Solid Films; 2002,415 (1-2): 173-176], and energy gap also can change along with the variation of processing parameter; Good sensitivity of light makes its application table aspect solar cell reveal very superior application prospect.As the electrode materials of electrical condenser, utilize the CoS plated film can replace best capacitance material ruthenium dioxide (RuO 2); And cobaltous sulfide is cheap, nontoxic, so good application prospects [Feng Tao, Yongqing Zhao are arranged aspect electrical condenser; Guoqing Zhang; Hulin Li.Electrochemical characterization on cobalt sulfide for supercapacitors [J] .Electrochemistry Communications, 2007,9 (6): 1282-1287].The preparation method of relevant cobaltous sulfide film mainly contains electroless plating, ion sputtering, vacuum plating, galvanic deposit and elevated temperature heat spraying etc. both at home and abroad at present.The comparative maturity of these method researchs, but to equipment requirements than higher, complex process, cost is than higher.
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.Certainly, microwave method also is a kind of effective ways that prepare film, and being combined into microwave-hydrothermal method with hydro-thermal has good effect for the preparation film.
Summary of the invention
The objective of the invention is to propose a kind of microwave-hydrothermal method prepares the cobaltous sulfide film on ito substrate method.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, and the cobaltous sulfide thin film crystallization of gained is intact, and the film quality homogeneous is repeatable high, and good using value is arranged.
For achieving the above object, the technical scheme that the present invention adopts is:
1) ito substrate that cleans up being put into mass concentration is that the toluene solution of 1% palmityl trimethyl ammonium chloride soaks;
2) get the analytical pure Diaquaoxalato cobalt (CoC of 0.73g-2.92g 2O 42H 2O) place small beaker, in small beaker, add deionized water, stir, be configured to the red clear solution A of 100mL;
3) get the thiocarbamide of 0.38g-1.52g, thiocarbamide added in the solution A, be stirred to dissolve solution B;
4) getting the 1mL-10mL mass concentration is 30% H 2O 2Add in the solution B, stir, be configured to forerunner's coating liquid C;
5) forerunner's coating liquid C is poured in the hydrothermal reaction kettle, the control compactedness is 50-80%; The ito substrate of then step 1) being handled is placed on reaction kettle and is dipped among forerunner's coating liquid C; The sealing hydrothermal reaction kettle puts it in the microwave hydrothermal reaction; Hydrothermal temperature is controlled at 160-220 ℃, reaction 10min-30min;
6) reaction naturally cools to room temperature after finishing, and takes out ito substrate, cleans with zero(ppm) water and absolute ethyl alcohol respectively, and the vacuum drying oven inner drying of putting into 40 ℃ again promptly obtains the cobaltous sulfide nano thin-film at substrate surface.
The cobaltous sulfide thin film crystallization of the present invention's preparation is good, and film is more even, and is not easy to crack; 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 the electron photomicrograph of the cobaltous sulfide film of the embodiment of the invention 1 preparation.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is done further explain.
1) ito substrate that cleans up being put into mass concentration is that the toluene solution of 1% palmityl trimethyl ammonium chloride soaks;
2) get the analytical pure Diaquaoxalato cobalt (CoC of 0.73g 2O 42H 2O) place small beaker, in small beaker, add deionized water, stir, be configured to the red clear solution A of 100mL;
3) get the thiocarbamide of 0.38g, thiocarbamide added in the solution A, be stirred to dissolve solution B;
4) getting the 2mL mass concentration is 30% H 2O 2Add in the solution B, stir, be configured to forerunner's coating liquid C;
5) forerunner's coating liquid C is poured in the hydrothermal reaction kettle, the control compactedness is 80%; The ito substrate of then step 1) being handled is placed on reaction kettle and is dipped among forerunner's coating liquid C; The sealing hydrothermal reaction kettle puts it in the microwave hydrothermal reaction; Hydrothermal temperature is controlled at 180 ℃, reaction 30min;
6) reaction naturally cools to room temperature after finishing, and takes out ito substrate, cleans with zero(ppm) water and absolute ethyl alcohol respectively, and the vacuum drying oven inner drying of putting into 40 ℃ again promptly obtains the cobaltous sulfide nano thin-film at substrate surface.
Prepared cobaltous sulfide nano thin-film is carried out observation analysis with sem, obtain the surface image (Fig. 1) of integral macroscopic.
Embodiment 2:
1) ito substrate that cleans up being put into mass concentration is that the toluene solution of 1% palmityl trimethyl ammonium chloride soaks;
2) get the analytical pure Diaquaoxalato cobalt (CoC of 1.56g 2O 42H 2O) place small beaker, in small beaker, add deionized water, stir, be configured to the red clear solution A of 100mL;
3) get the thiocarbamide of 0.76g, thiocarbamide added in the solution A, be stirred to dissolve solution B;
4) getting the 5mL mass concentration is 30% H 2O 2Add in the solution B, stir, be configured to forerunner's coating liquid C;
5) forerunner's coating liquid C is poured in the hydrothermal reaction kettle, the control compactedness is 60%; The ito substrate of then step 1) being handled is placed on reaction kettle and is dipped among forerunner's coating liquid C; The sealing hydrothermal reaction kettle puts it in the microwave hydrothermal reaction; Hydrothermal temperature is controlled at 160 ℃, reaction 30min;
6) reaction naturally cools to room temperature after finishing, and takes out ito substrate, cleans with zero(ppm) water and absolute ethyl alcohol respectively, and the vacuum drying oven inner drying of putting into 40 ℃ again promptly obtains the cobaltous sulfide nano thin-film at substrate surface.
Embodiment 3:
1) ito substrate that cleans up being put into mass concentration is that the toluene solution of 1% palmityl trimethyl ammonium chloride soaks;
2) get the analytical pure Diaquaoxalato cobalt (CoC of 1.25g 2O 42H 2O) place small beaker, in small beaker, add deionized water, stir, be configured to the red clear solution A of 100mL;
3) get the thiocarbamide of 1.00g, thiocarbamide added in the solution A, be stirred to dissolve solution B;
4) getting the 1mL mass concentration is 30% H 2O 2Add in the solution B, stir, be configured to forerunner's coating liquid C;
5) forerunner's coating liquid C is poured in the hydrothermal reaction kettle, the control compactedness is 50%; The ito substrate of then step 1) being handled is placed on reaction kettle and is dipped among forerunner's coating liquid C; The sealing hydrothermal reaction kettle puts it in the microwave hydrothermal reaction; Hydrothermal temperature is controlled at 220 ℃, reaction 10min;
6) reaction naturally cools to room temperature after finishing, and takes out ito substrate, cleans with zero(ppm) water and absolute ethyl alcohol respectively, and the vacuum drying oven inner drying of putting into 40 ℃ again promptly obtains the cobaltous sulfide nano thin-film at substrate surface.
Embodiment 4:
1) ito substrate that cleans up being put into mass concentration is that the toluene solution of 1% palmityl trimethyl ammonium chloride soaks;
2) get the analytical pure Diaquaoxalato cobalt (CoC of 2.00g 2O 42H 2O) place small beaker, in small beaker, add deionized water, stir, be configured to the red clear solution A of 100mL;
3) get the thiocarbamide of 1.52g, thiocarbamide added in the solution A, be stirred to dissolve solution B;
4) getting the 8mL mass concentration is 30% H 2O 2Add in the solution B, stir, be configured to forerunner's coating liquid C;
5) forerunner's coating liquid C is poured in the hydrothermal reaction kettle, the control compactedness is 70%; The ito substrate of then step 1) being handled is placed on reaction kettle and is dipped among forerunner's coating liquid C; The sealing hydrothermal reaction kettle puts it in the microwave hydrothermal reaction; Hydrothermal temperature is controlled at 200 ℃, reaction 20min;
6) reaction naturally cools to room temperature after finishing, and takes out ito substrate, cleans with zero(ppm) water and absolute ethyl alcohol respectively, and the vacuum drying oven inner drying of putting into 40 ℃ again promptly obtains the cobaltous sulfide nano thin-film at substrate surface.
Embodiment 5:
1) ito substrate that cleans up being put into mass concentration is that the toluene solution of 1% palmityl trimethyl ammonium chloride soaks;
2) get the analytical pure Diaquaoxalato cobalt (CoC of 2.46g 2O 42H 2O) place small beaker, in small beaker, add deionized water, stir, be configured to the red clear solution A of 100mL;
3) get the thiocarbamide of 1.20g, thiocarbamide added in the solution A, be stirred to dissolve solution B;
4) getting the 10mL mass concentration is 30% H 2O 2Add in the solution B, stir, be configured to forerunner's coating liquid C;
5) forerunner's coating liquid C is poured in the hydrothermal reaction kettle, the control compactedness is 55%; The ito substrate of then step 1) being handled is placed on reaction kettle and is dipped among forerunner's coating liquid C; The sealing hydrothermal reaction kettle puts it in the microwave hydrothermal reaction; Hydrothermal temperature is controlled at 190 ℃, reaction 25min;
6) reaction naturally cools to room temperature after finishing, and takes out ito substrate, cleans with zero(ppm) water and absolute ethyl alcohol respectively, and the vacuum drying oven inner drying of putting into 40 ℃ again promptly obtains the cobaltous sulfide nano thin-film at substrate surface.
Embodiment 6:
1) ito substrate that cleans up being put into mass concentration is that the toluene solution of 1% palmityl trimethyl ammonium chloride soaks;
2) get the analytical pure Diaquaoxalato cobalt (CoC of 2.92g 2O 42H 2O) place small beaker, in small beaker, add deionized water, stir, be configured to the red clear solution A of 100mL;
3) get the thiocarbamide of 1.35g, thiocarbamide added in the solution A, be stirred to dissolve solution B;
4) getting the 6mL mass concentration is 30% H 2O 2Add in the solution B, stir, be configured to forerunner's coating liquid C;
5) forerunner's coating liquid C is poured in the hydrothermal reaction kettle, the control compactedness is 75%; The ito substrate of then step 1) being handled is placed on reaction kettle and is dipped among forerunner's coating liquid C; The sealing hydrothermal reaction kettle puts it in the microwave hydrothermal reaction; Hydrothermal temperature is controlled at 210 ℃, reaction 15min;
6) reaction naturally cools to room temperature after finishing, and takes out ito substrate, cleans with zero(ppm) water and absolute ethyl alcohol respectively, and the vacuum drying oven inner drying of putting into 40 ℃ again promptly obtains the cobaltous sulfide nano thin-film at substrate surface.

Claims (1)

1. a microwave-hydrothermal method prepares the method for cobaltous sulfide film on ito substrate, it is characterized in that:
1) ito substrate that cleans up being put into mass concentration is that the toluene solution of 1% palmityl trimethyl ammonium chloride soaks;
2) get the analytical pure Diaquaoxalato cobalt (CoC of 0.73g-2.92g 2O 42H 2O) place small beaker, in small beaker, add deionized water, stir, be configured to the red clear solution A of 100mL;
3) get the thiocarbamide of 0.38g-1.52g, thiocarbamide added in the solution A, be stirred to dissolve solution B;
4) getting the 1mL-10mL mass concentration is 30% H 2O 2Add in the solution B, stir, be configured to forerunner's coating liquid C;
5) forerunner's coating liquid C is poured in the hydrothermal reaction kettle, the control compactedness is 50-80%; The ito substrate of then step 1) being handled is placed on reaction kettle and is dipped among forerunner's coating liquid C; The sealing hydrothermal reaction kettle puts it in the microwave hydrothermal reaction; Hydrothermal temperature is controlled at 160-220 ℃, reaction 10min-30min;
6) reaction naturally cools to room temperature after finishing, and takes out ito substrate, cleans with zero(ppm) water and absolute ethyl alcohol respectively, and the vacuum drying oven inner drying of putting into 40 ℃ again promptly obtains the cobaltous sulfide nano thin-film at substrate surface.
CN2011103758012A 2011-11-23 2011-11-23 Method for preparing cobalt sulfide thin film on indium tin oxide (ITO) substrate by microwave hydrothermal process Pending CN102424959A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104701018A (en) * 2015-01-29 2015-06-10 三峡大学 One-step solvothermal preparation method for dye-sensitized solar cell CoS counter electrode
CN105097295A (en) * 2015-07-23 2015-11-25 武汉理工大学 High-performance miniature supercapacitor and fabrication method thereof
CN112563487A (en) * 2020-11-18 2021-03-26 上海空间电源研究所 CoS for thermal battery2Method for producing a material

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5829881A (en) * 1981-08-13 1983-02-22 Matsushita Electric Ind Co Ltd Electric field luminescent element
CN101786671A (en) * 2009-10-30 2010-07-28 陕西科技大学 Method for preparing bar-shaped cobalt sulfide nanocrystalline
CN101838155A (en) * 2010-05-25 2010-09-22 陕西科技大学 Method for preparing hexagonal flaky cadmium sulphide membrane in microwave hydrothermal mode
CN101847583A (en) * 2010-05-25 2010-09-29 陕西科技大学 Method for preparing spherical cadmium sulfide (CdS) semiconductor film

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5829881A (en) * 1981-08-13 1983-02-22 Matsushita Electric Ind Co Ltd Electric field luminescent element
CN101786671A (en) * 2009-10-30 2010-07-28 陕西科技大学 Method for preparing bar-shaped cobalt sulfide nanocrystalline
CN101838155A (en) * 2010-05-25 2010-09-22 陕西科技大学 Method for preparing hexagonal flaky cadmium sulphide membrane in microwave hydrothermal mode
CN101847583A (en) * 2010-05-25 2010-09-29 陕西科技大学 Method for preparing spherical cadmium sulfide (CdS) semiconductor film

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104701018A (en) * 2015-01-29 2015-06-10 三峡大学 One-step solvothermal preparation method for dye-sensitized solar cell CoS counter electrode
CN105097295A (en) * 2015-07-23 2015-11-25 武汉理工大学 High-performance miniature supercapacitor and fabrication method thereof
CN105097295B (en) * 2015-07-23 2017-10-24 武汉理工大学 A kind of high-performance micro ultracapacitor and preparation method thereof
CN112563487A (en) * 2020-11-18 2021-03-26 上海空间电源研究所 CoS for thermal battery2Method for producing a material
CN112563487B (en) * 2020-11-18 2022-12-09 上海空间电源研究所 CoS for thermal battery 2 Method for producing a material

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Application publication date: 20120425