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Method for preparing antimony sulfide film through low-temperature plasma vulcanization

A low-temperature plasma, antimony sulfide technology, applied in antimony sulfide, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of loose structure and composition deviation, increase of ambient temperature, increase of thermal motion of solid sulfur source, etc. Large size, flat structure, and the effect of low temperature growth

Pending Publication Date: 2020-06-30
KUNMING UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The present invention prepares Sb for existing thermal activation technology 2 S 3 Thin films are prone to problems such as loose structure and compositional deviation caused by volatilization of components. A method for preparing antimony sulfide thin films by low-temperature plasma vulcanization is provided, that is, in an inert gas environment such as argon, argon is plasmaized after being subjected to an electric field Highly active argon ions and electrons are obtained, and highly active argon ions and electrons collide with each other, and also collide with solid sulfur sources to generate plasma sulfur; the ambient temperature rise caused by the collisions between various particles increases the solid The thermal movement of the sulfur source further promotes the generation of plasma sulfur. Due to its high activity, plasma sulfur can quickly realize the sulfuration of metal antimony, antimony oxide or antimony hydroxide film to obtain antimony sulfide film.

Method used

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Embodiment 1

[0030] Embodiment 1: A kind of method for preparing antimony sulfide film by low-temperature plasma vulcanization, concrete steps are as follows:

[0031] (1) Metal antimony thin films were prepared by vapor deposition method (see figure 2 ):

[0032] with SbCl 3 (99.99% pure) with H 2 (99.99% purity) as raw material, deposit pure antimony film on soda-lime glass substrate: the deposition process is carried out in a quartz tube furnace, the deposition furnace is heated by resistance wire, and the power of the deposition system is controlled and adjusted by a thyristor voltage regulator , using Ni-Ni-Si thermocouple to measure the substrate temperature, using needle valve and flowmeter to control the SbCl 3 and H 2 The gas flow rate, the deposition temperature is about 400°C, and the mixed gas ratio is n(SbCl 3 ):n(H 2 )=1:2, the gas outlet of the deposition furnace is fed into saturated KOH solution and then ignited or emptied into the atmosphere; from the surface SEM i...

Embodiment 2

[0035] Embodiment 2: a kind of method for preparing antimony sulfide film by low-temperature plasma vulcanization, concrete steps are as follows:

[0036] (1) Prepare antimony oxide film by spray pyrolysis method: accurately weigh 10 g of analytically pure Sb(NO 3 ) 3 Dissolve in 250 ml dilute HNO with a mass fraction of 5% 3 In the solution, under the protective atmosphere of argon, the Sb(NO 3 ) 3 The solution is atomized into aerosol droplets, and a flat electric furnace with Mo conductive glass is placed in the system. The temperature of the flat electric furnace is 400 ° C. The antimony oxide film is deposited on Mo On the conductive glass, the tail gas is discharged after being neutralized by the alkali solution in the absorption bottle; the deposited antimony oxide film can be directly used as the precursor of the antimony sulfide film prepared by low-temperature plasma vulcanization; 2 Metal antimony film can be obtained by reduction under atmosphere for 30 minutes; ...

Embodiment 3

[0043] Embodiment 3: A kind of method for preparing antimony sulfide film by low-temperature plasma vulcanization, concrete steps are as follows:

[0044] (1) Preparation of antimony hydroxide thin film by chemical bath deposition method:

[0045] Antimony hydroxide film material is prepared by chemical bath deposition. Take 2.8501 grams of antimony trichloride solid raw material, 5 milliliters of ammonia water, and 25 milliliters of triethanolamine in a small beaker. After the dissolution and complexation are complete, pour it into a 250 milliliter volumetric flask Constant volume, the antimony concentration of the obtained solution is 0.05mol / L, adjust the pH value of the solution to 7.2 with hydrochloric acid or sodium hydroxide, put the solution in a 500 mL beaker, and put the washed and dried SnO plated in the beaker. 2 Glass (with a square resistance of 20Ω) was used as the experimental substrate material; the beaker was placed in a water bath at a temperature of 70°C, a...

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Abstract

The invention relates to a method for preparing an antimony sulfide film through low-temperature plasma vulcanization, and belongs to the technical field of photoelectric functional materials. The method comprises the steps: preparing a metal antimony, antimony oxide or antimony hydroxide film, carrying out low-temperature plasma treatment on a solid sulfur source by using a low-temperature plasmagenerator to form plasma-state sulfur, and carrying out low-temperature plasma vulcanization treatment on the film by using the plasma-state sulfur to obtain the antimony sulfide film. In an inert gas environment, inert gas is ionized under the action of an electric field to obtain high-activity inert gas ions and electrons, and the high-activity inert gas ions and electrons collide with a solidsulfur source to generate plasma-state sulfur; ambient temperature rise caused by mutual collision among various particles increases the thermal motion of the solid sulfur source, and further promotesthe generation of plasma-state sulfur. The plasma-state sulfur has high activity, so that vulcanization of the film can be quickly realized to obtain the antimony sulfide film. The antimony sulfide film is uniform in component, flat and compact in structure and large in grain size.

Description

technical field [0001] The invention relates to a method for preparing an antimony sulfide thin film by low-temperature plasma vulcanization, and belongs to the technical field of photoelectric functional materials. Background technique [0002] Antimony sulfide (Sb 2 S 3 ) crystal structure belongs to orthorhombic stibnite structure, antimony sulfide (Sb 2 S 3 ) is used in the field of solar cells, with a suitable band gap (1-1.72eV), large absorption coefficient (short-wavelength visible light absorption coefficient>10 5 cm -1 ), large relative permittivity (9.5, greater than 7.1 of CdTe), can be used as thin-film photovoltaic absorber material, photocatalytic material and electrocatalytic material. [0003] Sb 2 S 3 The composition and phase of the product are relatively simple, and there is only one phase composition at room temperature, which can effectively avoid the problem of impurity phase formation during the preparation process. Sb 2 S 3 The melting p...

Claims

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Application Information

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IPC IPC(8): C01G30/00H01L31/032
CPCC01G30/008H01L31/032C01P2004/03C01P2004/20C01P2002/82C01P2006/40
Inventor 杨佳欧于学刘国豪张君司圣和徐宝强李绍元万贺利杨斌马文会熊恒刘大春郁青春李一夫田阳蒋文龙戴永年宋宁
Owner KUNMING UNIV OF SCI & TECH
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