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Preparation method of step confinement two-dimensional tungsten nitride on surface of tungsten single crystal

A tungsten nitride and single crystal technology, applied in the field of nanomaterials, can solve problems such as the inability to observe the growth process, the uncontrollability of the preparation process, and the lack of guiding significance for the growth behavior of thin films.

Active Publication Date: 2021-09-10
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are very few methods for preparing two-dimensional tungsten nitride thin films, and the currently obtained two-dimensional tungsten nitride is a nanosheet powder material obtained by liquid-phase reaction followed by high-temperature calcination, and its growth process cannot be observed. , the preparation process is uncontrollable and lacks guiding significance for film growth behavior

Method used

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  • Preparation method of step confinement two-dimensional tungsten nitride on surface of tungsten single crystal
  • Preparation method of step confinement two-dimensional tungsten nitride on surface of tungsten single crystal
  • Preparation method of step confinement two-dimensional tungsten nitride on surface of tungsten single crystal

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Embodiment 1

[0040] Preparation of two-dimensional tungsten nitride with surface step confinement at medium temperature

[0041] 1) Processing single crystal W (110)

[0042] In the ultra-high vacuum chamber, the temperature is 1000°C, O 2 The pressure is 1.0×10 -7Under the condition of Torr, the single crystal W is subjected to oxygen burning for 10 minutes, and then the single crystal W is heated and kept at a high temperature of 1500-1600°C for 2 minutes for annealing, that is, kept at 1500-1600°C for 2 minutes, and then cooled until the low-energy electrons Microscope and low-energy electron diffraction did not observe any impurities, and a clean single crystal W(110) substrate was obtained.

[0043] 2) Growth of step-confined two-dimensional tungsten nitride on the surface of single crystal W(110)

[0044] The cleaned W(110) substrate was heated and maintained at 620°C, and 2.0×10 -7 Torr's ammonia gas, ammonia dissociates on the substrate and further combines with tungsten atoms ...

Embodiment 2

[0049] Preparation of two-dimensional tungsten nitride with surface step confinement at high temperature

[0050] 1) Processing single crystal W (110)

[0051] In an ultra-high vacuum chamber at 1000°C, 1.0×10 -7 TorrO 2 The single crystal W was oxidized for 10 minutes under certain conditions, and then the single crystal W was heated and kept at 1500-1600 ° C for 2 minutes for high temperature annealing, until no impurities were observed under the low-energy electron microscope and low-energy electron diffraction spots.

[0052] 2) Growth of step-confined two-dimensional tungsten nitride on the surface of W(110)

[0053] Heat and maintain the cleaned W(110) substrate at 670°C, and pass through 1.0×10 -6 Torr's ammonia gas, ammonia gas dissociates on the substrate and further combines with substrate tungsten atoms to form tungsten nitride, Figure 5 Low-energy electron microscope images obtained by real-time imaging and in-situ observation during the growth process of tung...

Embodiment 3

[0057] Preparation of Surface Tungsten Nitride at Low Temperature

[0058] 1) Processing single crystal W (110)

[0059] In an ultra-high vacuum chamber at 1000°C, 1.0×10 -7 TorrO 2 The single crystal W was oxidized under certain conditions for 10 minutes, and then the single crystal W was heated and kept at 1500-1600 ° C for 2 minutes for high temperature annealing until no impurities were observed by low-energy electron microscopy and low-energy electron diffraction.

[0060] 2) Growth of tungsten nitride on the surface of W(110)

[0061] Heat and maintain the cleaned W(110) substrate at 600°C, and pass through 1.0×10 -7 Torr's ammonia, ammonia dissociates on the substrate and further combines with tungsten atoms on the surface of the substrate to form tungsten nitride. Due to the lower growth temperature, the nucleation density is larger ( Figure 6 a), and the growth rate is slow, the growth of tungsten nitride only shows the splicing between different small islands ( ...

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Abstract

The invention relates to a preparation method of step confinement two-dimensional tungsten nitride on the surface of tungsten single crystal. The preparation method mainly comprises the following steps that surface pretreatment is carried out on a single crystal W; and the pretreated W substrate is heated to 600-670 DEG C, ammonia gas is introduced, the pressure of the ammonia gas is 1 * 10 <-7 > - 1 * 10 <-6 > Torr, real-time imaging is carried out through a surface imaging instrument, growth of tungsten nitride on the surface of the single crystal W is observed in situ, after tungsten nitride reaches the needed coverage degree, cooling is carried out under the ammonia gas, and the two-dimensional tungsten nitride is obtained. The preparation method for directly nitriding the substrate by modulating the temperature and the atmosphere pressure is simple and easy to implement, and the surface imaging instrument is used for real-time imaging in the preparation process, so that the structure of the preparation method is easy to control, the preparation method can be expanded to controllable preparation of other transition metal nitrides, and a good foundation is laid for controllable preparation and application research of subsequent nitride film materials.

Description

technical field [0001] The invention belongs to the technical field of nanometer materials, and in particular relates to a preparation method of step-confined two-dimensional tungsten nitride on the surface of a tungsten single crystal. Background technique [0002] Tungsten nitride thin film has a wide range of applications because of its special physical and chemical properties. In microelectronics, due to its high thermal conductivity and electrical conductivity, it is used as a barrier layer to inhibit copper diffusion and electrodes in semiconductor devices; in engineering, it is used on the surface of wear-resistant and anti-oxidation materials due to its high hardness coefficient In heterogeneous catalysis, because the electrochemical properties and catalytic properties exhibited are very similar to those of Pt-based noble metals, they are used in catalytic ammonia synthesis, hydrocarbon reforming, CO oxidation, hydrodesulfurization, and hydrodenitrogenation reactions...

Claims

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Application Information

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IPC IPC(8): C23C26/00C01B21/06B82Y30/00B82Y40/00B01J27/24
CPCC23C26/00C01B21/062B82Y30/00B82Y40/00B01J27/24C01P2004/20C01P2002/70C01P2004/01B01J35/33
Inventor 傅强孟彩霞包信和
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI