Metal sulfide film based on organic sulfur precursor and preparation method thereof

A metal sulfide and precursor technology, applied in metal material coating process, gaseous chemical plating, coating and other directions, can solve the problems that hinder the expansion and development of ALD new metal sulfide methods, safety hazards, etc., and achieve excellent electroplating. Catalytic performance, reducing safety hazards, and the effect of dense and uniform crystallinity

Active Publication Date: 2020-11-03
PEKING UNIV SHENZHEN GRADUATE SCHOOL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the sulfur source precursors used in the preparation of these metal sulfides by ALD are basically H 2 S gas, while H 2 As a highly toxic, flammable and corrosive gas, S gas has great safety hazards in the process of storage, transportation and use.
equipped with H 2 S cylinders need to be stored in a professional storage cabinet and equipped with a professional H 2 S gas sensor, use H 2 Strict and standardized operating procedures must be followed in the S process, and these problems have largely hindered the method expansion and development of ALD new metal sulfides

Method used

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  • Metal sulfide film based on organic sulfur precursor and preparation method thereof
  • Metal sulfide film based on organic sulfur precursor and preparation method thereof
  • Metal sulfide film based on organic sulfur precursor and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0070] 1. Nickel sulfide (NiS) based on organosulfur precursors x ) film preparation.

[0071]Place the pretreated substrate in the ALD reaction chamber, control the temperature in the reaction chamber to 200 ° C, and bis(nitrogen, nitrogen-di-tert-butylacetamidine) nickel (Ni(amd) 2 ) is heated to 70°C to form bis(nitrogen, nitrogen-di-tert-butylacetamido) nickel vapor, in high-purity N 2 With the assistance of carrier gas, 0.12 Torr s of bis(nitrogen, nitrogen-di-tert-butylacetamido) nickel vapor was introduced into the ALD reaction chamber, and then N was introduced into the ALD reaction chamber. 2 Purge for 30s for the first time to remove unreacted bis(nitrogen, nitrogen-di-tert-butylacetamido)nickel precursor and reaction by-products, then heat the tert-butyl disulfide (TBDS) precursor to 35°C, The formed TBDS vapor was filled into the gas collector, and the TBDS vapor in the 0.15 Torr·s gas collector was introduced into the ALD reaction chamber in a pulsed manner. Th...

Embodiment 2

[0087] 1. Nickel sulfide (NiS) based on organosulfur precursors x ) thin film carbon cloth-based catalytic electrode (NiS x / CNT / CC) preparation.

[0088] Carbon nanotube / carbon cloth (CNT / CC) substrates were fabricated by drop-coating carbon nanotube (CNT) suspensions onto carbon cloth (CC). Deposition of NiS on CNT / CC with TBDS as organosulfur precursor x Film, its deposition method and parameters are the same as in Example 1, the difference is that the number of ALD cycles is 500 times, and the oxygen evolution reaction electrode obtained is expressed as NiS x / CNT / CC. For comparison, the NiS x The film is deposited on a pretreated flat glassy carbon electrode, and the prepared oxygen evolution reaction electrode is denoted as NiS x / GC, and with RuO 2 The suspension was drop-coated onto the pretreated glassy carbon electrode to prepare a standard catalyst electrode expressed as RuO 2 / GC.

[0089] 2. NiS x / CNT / CC Catalytic Electrode Characterization.

[0090] (1...

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Abstract

The invention provides a metal sulfide film based on an organic sulfur precursor and a preparation method thereof. The preparation method comprises the steps that a metal precursor is introduced intoan atomic layer deposition reaction chamber in the presence of inert carrier gas by adopting an atomic layer deposition technology to deposit a metal monoatomic layer; and then the organic sulfur precursor is introduced into the atomic layer deposition reaction chamber in a pulse mode to obtain a metal sulfide molecular layer, the process of forming the molecular layer is taken as an ALD period, and the metal sulfide film based on the organic sulfur precursor is obtained by circulating the ALD period. According to the preparation method, the organosulfur compound is adopted to replace high-toxicity H2S gas to serve as the sulfur source precursor, potential safety hazards of the harmful gas to the film preparation process are reduced, the environmental friendliness is achieved, the metal sulfide film prepared through the method is compact, uniform, good in crystallinity and excellent in electro-catalytic performance, and the metal sulfide film can be applied to the field of electrocatalysis.

Description

technical field [0001] The invention relates to the technical field of metal sulfide film preparation, in particular to a metal sulfide film based on an organosulfur precursor and a preparation method thereof. Background technique [0002] Metal sulfide thin films have excellent electrical, optical, magnetic and electrochemical properties, so they have attracted extensive attention from researchers in various fields. They are currently used in integrated circuits, gas sensors, photodetectors, solar cells and electrochemical catalysis. Show great application potential. Traditional methods for synthesizing metal sulfide thin films mainly include electrodeposition, chemical water bath deposition, chemical vapor deposition, and physical vapor deposition. In recent years, atomic layer deposition (ALD) technology has gradually evolved into an important method for preparing high-quality metal sulfide thin films. ALD technology can grow uniform, continuous and precise thickness on ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C16/30C23C16/455
CPCC23C16/305C23C16/45527C23C16/45553C23C16/45555
Inventor 王新炜李豪
Owner PEKING UNIV SHENZHEN GRADUATE SCHOOL
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