Preparation method of CZTSSe thin film and application of CZTSSe thin film in lithium ion battery

A thin film and plasma technology, applied in the field of lithium-ion battery preparation, can solve the problems affecting the performance of materials, uneven crystallinity of prepared materials, etc.

Active Publication Date: 2019-07-19
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Ge eYeongKim (SolarEnergy Materials and Solar Cells, 2014, 127: 129-135) and others used Cu, ZnS and SnS to sputter the prefabricated layer of CZTS, and then used Se to directly realize selenization under an inert atmosphere. Although this method can CZTSSe thin film is prepar

Method used

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  • Preparation method of CZTSSe thin film and application of CZTSSe thin film in lithium ion battery
  • Preparation method of CZTSSe thin film and application of CZTSSe thin film in lithium ion battery

Examples

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Embodiment 1

[0044] Soak the copper foil in 10wt% hydrochloric acid for 12 hours, dry it with alcohol after cleaning and cut it into small pieces of 2cm×2cm. Coat its A side with chloroform in which 5g of Se powder is dissolved, and dry it. Then fix the copper foil on the target stage, and control the sputtering of the material to the B surface. The target material is Cu, Zn, Sn target, three targets co-sputtering, and the atmosphere is adjusted to H 2 S, the total addition amount of controlled atmosphere is 220ml. At the same time, the heating program of the substrate was started, and the temperature was raised to 300°C. After pre-sputtering for 10mins, remove the baffle, adjust the power to 60W, and sputter for 60mins. Finally, the CZTSSe film obtained by sputtering was placed in a tube furnace, and the temperature was raised to 800° C. at a rate of 5° C. / min for high-temperature calcination for 100 mins to obtain the CZTSSe film. The thickness of the film is 0.74 μm, and the atomic r...

Embodiment 2

[0049] Soak the copper foil in 12wt% hydrochloric acid for 12 hours, dry it with alcohol after cleaning and cut it into small pieces of 2cm×2cm. Coat its A side with chloroform in which 5g of Se powder is dissolved, and dry it. Then fix the copper foil on the target stage, and control the sputtering of the material to the B surface. The target material is Cu, Zn, and Sn targets for three-target co-sputtering, and the atmosphere is adjusted to Ar / H 2 S(1:1), the total amount of control gas added is 400ml. At the same time, the heating program of the substrate was started, and the temperature was raised to 500°C. After pre-sputtering for 10mins, remove the baffle, adjust the power to 40W, and sputter for 60mins. Finally, the CZTSSe film obtained by sputtering was placed in a tube furnace, and the temperature was raised to 900° C. at a rate of 5° C. / min for high-temperature calcination for 30 minutes to obtain the CZTSSe film. The thickness of the film is 0.68 μm, and the atom...

Embodiment 3

[0052] Soak the copper foil in 15wt% sulfuric acid for 12h, dry it with alcohol after cleaning and cut it into small pieces of 2cm×2cm. Coat its A side with chloroform in which 5g of Se powder is dissolved, and dry it. Then fix the copper foil on the target stage, and control the sputtering of the material to the B surface. The target material is Cu, Zn, and Sn targets for three-target co-sputtering, and the atmosphere is adjusted to Ar / H 2 S (1:10), the total amount of control gas added is 200ml. At the same time, the heating program of the substrate was started, and the temperature was raised to 250°C. After pre-sputtering for 10mins, remove the baffle, adjust the power to 80W, and sputter for 10mins. Finally, the CZTSSe film obtained by sputtering was placed in a tube furnace, and the temperature was raised to 650° C. at a rate of 10° C. / min for high-temperature calcination for 180 minutes to obtain the CZTSSe film. The thickness of the film is 0.80 μm, and the atomic ra...

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Abstract

The invention discloses a preparation method of a copper-zinc-tin sulfide-selenide (CZTSSe) thin film and application of the thin film in a lithium ion battery. By means of a magnetron sputtering method, by means of copper foil treated with Se, the atmosphere with Se and S plasma is created in a sputtering cavity, and a Cu-Zn-Sn-S-Se precursor is synthesized through reactive sputtering. The thin film is arranged in the protective atmosphere, and after high-temperature annealing, the CZTSSe thin film is obtained. The preparation method is simple and effective, the uniformity and the stability of the preparation material are guaranteed, meanwhile, the material integrates the advantages of metal sulfide-selenide and has high energy density and circulating stability, and the discharge performance of the battery is effectively improved.

Description

technical field [0001] The invention relates to a preparation method of a CZTSSe thin film and its application in lithium ion batteries, belonging to the field of lithium ion battery preparation. Background technique [0002] Energy is the main material basis for developing the national economy and improving people's living standards, and it is also an important factor that directly affects economic development. Since the beginning of the 21st century, problems such as resource shortage, environmental pollution, and greenhouse effect caused by traditional energy utilization methods have become increasingly prominent. Improving the energy structure and developing efficient and clean new energy sources has become a global consensus. Lithium-ion batteries are favored by people because of their superior properties such as safety, environmental protection, high specific energy and good electrochemical performance. In order to meet the requirements of the energy miniaturization o...

Claims

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Application Information

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IPC IPC(8): C23C14/35C23C14/06C23C14/58H01M4/58H01M10/0525
CPCC23C14/0057C23C14/0623C23C14/352C23C14/5806H01M4/581H01M4/5815H01M10/0525Y02E60/10
Inventor 赖延清张治安王麒羽汪齐刘芳洋洪波张凯李劼
Owner CENT SOUTH UNIV
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