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Growth of nbs by an atomic layer deposition technique x thin film method

A technique of atomic layer deposition and technology, applied in the direction of nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problems of difficult storage and transportation, strong toxicity, difficult operation, etc., and achieve the effect of good effect, reduced toxicity and easy operation

Active Publication Date: 2020-11-03
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, the sulfur source used in the preparation of other related sulfides by the ALD method is hydrogen sulfide gas, which is not easy to store and transport, and has strong toxicity and is not easy to handle.

Method used

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  • Growth of nbs by an atomic layer deposition technique <sub>x</sub> thin film method
  • Growth of nbs by an atomic layer deposition technique <sub>x</sub> thin film method
  • Growth of nbs by an atomic layer deposition technique <sub>x</sub> thin film method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] A Nb(OCH 2 CH 3 ) 5 As Nb source, NbS with tert-butyl mercaptan (t-Bu-SH) as sulfur source x Thin film atomic layer deposition method, including the following processes:

[0056] (1) with TiO 2 is the substrate, the deposition temperature is 240°C, the Nb source Nb(OCH 2 CH 3 ) 5 The heating temperature is 75°C to make it vaporized, and high-purity nitrogen is used as the carrier gas, and the gas phase Nb(OCH 2 CH 3 ) 5 , the carrier gas flow rate is 20sccm; the pulse time is 12s, and the waiting time is 10s;

[0057] (2) Use high-purity nitrogen to clean after completing a pulse, and the cleaning time is 25s;

[0058] (3) The heating temperature of the sulfur source t-Bu-SH is 60°C to make it vaporize, using high-purity nitrogen as the carrier gas, the flow rate of the carrier gas is 60 sccm, and the t-Bu-SH is passed into t-Bu-SH in the form of pulses, and the pulse time is 5s , the waiting time is 20s;

[0059] After completing a pulse, use high-purity ni...

Embodiment 2

[0065] Example 2: Preparation of NbS from different sulfur sources x film

[0066] The sulfur source in embodiment 1 is replaced by n-butyl mercaptan (n-Bu-SH), isopropyl mercaptan (i-Pr-SH), n-propyl mercaptan (n-Pr-SH) respectively, other The operating steps and parameters remain the same.

[0067] The results show that after repeating the cycle 100 times, the obtained NbS x The film thicknesses are 4nm, 5nm and 4.6nm, respectively.

Embodiment 3

[0069] A Nb(OCH 2 CH 3 ) 5 As Nb source, NbS with n-butyl mercaptan (n-Bu-SH) as sulfur source x Thin film atomic layer deposition method, comprising the following processes:

[0070] (1) With porous alumina as the substrate, the deposition temperature is 265°C, and the Nb source Nb(OCH 2 CH 3 ) 5 The heating temperature is 120°C to vaporize it, and high-purity argon is used as the carrier gas, and the gaseous Nb(OCH 2 CH 3 ) 5 , the carrier gas flow rate is 80sccm; the pulse time is 6s, and the waiting time is 20s;

[0071] (2) Use high-purity argon to clean after completing a pulse, and the cleaning time is 45s;

[0072] (3) The heating temperature of the sulfur source n-Bu-SH is 40°C, high-purity argon is used as the carrier gas, the flow rate of the carrier gas is 20 sccm, and the n-Bu-SH is fed into the n-Bu-SH in the form of pulses, the pulse time is 15s, and the waiting time is 15s;

[0073] (4) Use high-purity argon to clean after completing a pulse, and the...

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Abstract

The invention discloses an atomic layer deposition technology to grow NbS x The thin film method belongs to the technical field of nanomaterial preparation. The method of the present invention includes the following steps: (1) Place the substrate in a reaction chamber, and under vacuum conditions, introduce a gas phase Nb source into the reaction chamber in the form of pulses for deposition to obtain a substrate with Nb source deposited on it. The Nb source is Nb(OCH 2 CH3) 5 ; (2) Fill the system with inert gas for purging; (3) Pulse mercaptan as a sulfur source into the reaction chamber and react with the Nb source deposited on the substrate to obtain nano-NbS x Thin film; (4) Fill the system with inert gas and complete an ALD cycle. Repeat the above cycle process multiple times to obtain NbS with a certain thickness. x film. The present invention can be deposited on a substrate to form NbS-containing materials with better shape retention properties. x sedimentary layer.

Description

technical field [0001] The invention relates to an atomic layer deposition technique for growing NbS x The thin film method belongs to the technical field of nanometer material preparation. Background technique [0002] Nanostructured transition metal sulfides have excellent magnetic, electronic, and optical properties. Among them, transition metal sulfides have attracted extensive attention in the field of photo(electro)catalytic hydrogen production because of their better catalytic activity and lower cost. Nb-based nanomaterials are considered to have good hydrogen evolution catalytic performance. In addition, atomic layer deposition (ALD) has gradually become a cutting-edge technology for preparing nanostructured materials. The self-limiting surface chemical reaction of ALD allows nanomaterials to be deposited on various complex surfaces or three-dimensional structures with remarkable reproducibility and precise control over film thickness, material composition, and di...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C23C16/30C23C16/455B82Y30/00B82Y40/00B01J27/04
CPCC23C16/305C23C16/45527B82Y30/00B82Y40/00B01J27/04B01J35/39
Inventor 丁玉强杜立永王科炎
Owner JIANGNAN UNIV