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Method for preparing Mo-doped VO2 thermochromic film through atomic layer deposition method

An atomic layer deposition method, VO2 technology, applied in the direction of coating, metal material coating process, gaseous chemical plating, etc., can solve the problems of limited practical application, high human hazard, high phase transition temperature, etc., and achieve excellent thermal induction Phase change characteristics, large-scale mass production, and simple operation

Inactive Publication Date: 2018-05-22
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, ALD was used to prepare doped VO 2 The study of thin films to change their phase transition temperature has never been reported
While the pure phase VO 2 Higher phase transition temperature limits ALD VO 2 practical application of
[0004] Mo-doped VO 2 The preparation of materials is mainly through chemical synthesis methods such as sol-gel method and hydrothermal method. The precursors are highly dangerous and harmful to humans, and it is difficult to achieve large-scale mass production.

Method used

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  • Method for preparing Mo-doped VO2 thermochromic film through atomic layer deposition method
  • Method for preparing Mo-doped VO2 thermochromic film through atomic layer deposition method
  • Method for preparing Mo-doped VO2 thermochromic film through atomic layer deposition method

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Experimental program
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Effect test

Embodiment 1

[0054] The precursor V(NMe 2 ) 4 and Mo(CO) 6 Heat to 50°C, and pulse alternately into the ALD reaction chamber, the chamber temperature is controlled at 160°C. The gas flow is set to 300sccm, and the reaction pressure is 0.5mbar, O 2 The plasma power was set to 80W. an ALD VO 2 The pulse purge program is V(NMe 2 ) 4 (3s)—Ar(8s)—H 2 O(0.6s)—Ar(3s), an ALD MoO 3 The pulse purge program for Mo(CO) 6 (1s)—Ar(4s)—O 2 (1s)—Ar(3s). Pass 2 ALD MoOs 3 Subloop and 98 ALD VO 2 The sub-loop is repeated 5 times alternately to obtain MoO 3 Cycle ratio of 2% VO 2 / MoO 3 Nano lamination. The nano-stack was incubated at 500°C in a vacuum (about 1 Pa) for 120 min to obtain crystallized V 1-x Mo x o 2 film.

[0055] to get V 1-x Mo x o 2 The film was tested, and the phase composition of the film was checked by X-ray diffractometer ( figure 1 ); using a field emission scanning electron microscope to observe the morphology of the film ( figure 2 ); The variable temperatu...

Embodiment 2

[0057] The precursor V(NMe 2 ) 4 and Mo(CO) 6 Heat to 50°C, and pulse alternately into the ALD reaction chamber, the chamber temperature is controlled at 180°C. The gas flow is set to 300sccm, and the reaction pressure is 0.5mbar, O 2 The plasma power was set to 60W. an ALD VO 2 The pulse purge program for H 2 O(0.6s)—Ar(3s)—V(NMe 2 ) 4 (3s)—Ar(8s), an ALD MoO 3 The pulse purge program is O 2 (1s)—Ar(3s)—Mo(CO) 6 (1s)—Ar(4s). By combining 5 ALD MoO 3 Subcycle and 95 ALD VO 2 The sub-loop is repeated 5 times alternately to obtain MoO 3 Cycle ratio of 5% VO 2 / MoO 3 Nano lamination. The nanostack was incubated in vacuum at 500 °C for 60 min to obtain crystallized V 1-x Mo x o 2 film.

[0058] to get V 1-x Mo x o 2 The film was tested, and the phase composition of the film was checked by X-ray diffractometer ( figure 1 ); using a field emission scanning electron microscope to observe the morphology of the film ( figure 2 ); The variable temperature resis...

Embodiment 3

[0060] The precursor V(NMe 2 ) 4 and Mo(CO) 6 Heat to 50°C, and pulse alternately into the ALD reaction chamber, and the chamber temperature is controlled at 150°C. The gas flow is set to 300sccm, and the reaction pressure is 0.5mbar, O 2 The plasma power was set at 100W. an ALD VO 2 The pulse purge program is V(NEtMe) 4 (3s)—Ar(8s)—O 3 (0.6s)—Ar(3s), an ALD MoO 3 The pulse purge program for Mo(CO) 6 (1s)—Ar(4s)—O 2 (1s)—Ar(3s). Pass 7 ALD MoOs 3 Subcycle and 93 ALD VO 2 The sub-loop is repeated 5 times alternately to obtain MoO 3 Cycle ratio of 7% VO 2 / MoO 3 The nano-stack was incubated in a vacuum at 500°C for 60 minutes to obtain crystallized V 1-x Mo x o 2 film.

[0061] to get V 1-x Mo x o 2 The film was tested, and the phase composition of the film was checked by X-ray diffractometer ( figure 1 ); using a field emission scanning electron microscope to observe the morphology of the film ( figure 2 ); the transmittance ( Figure 5 ) and the calcul...

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Abstract

The invention relates to a method for preparing a Mo-doped VO2 thermochromic film through an atomic layer deposition method. The chemical constitution of the Mo-doped VO2 film is V1-xMoxO2, wherein xis greater than or equal to 0.02 but less than or equal to 0.1. The Mo-doped VO2 film is obtained according to the steps that a VO2 / MoO3 nanometer laminated layer is obtained by alternately and circularly depositing VO2 and MoO3 on a substrate through the atomic layer deposition method and then conducting annealing. The V1-xMoxO2 film has good visible light transmittance and thermochromic characteristics, and is expected to be applied to intelligent windows and other fields.

Description

technical field [0001] The invention belongs to the field of thin film materials prepared by atomic layer deposition, and particularly relates to the preparation of Mo-doped VO by atomic layer deposition. 2 A method for thermochromic thin films. Background technique [0002] Vanadium dioxide (VO 2 ) is a thermochromic material with metal-semiconductor phase transition properties. Pure phase VO 2 The phase transition temperature is 68°C. When the temperature is higher than 68°C, it is a metal phase (R) with a rutile structure; when the temperature is lower than 68°C, it is a semiconductor phase with a monoclinic structure (M1). Before and after phase transition, VO 2 The resistivity changes by 4 orders of magnitude, and the infrared region changes from high transmittance (M1 phase) to high reflectivity (R phase). VO 2 The phase transition temperature can be significantly reduced to around room temperature by doping Mo. In addition, Mo doping can cause a blue shift in th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C16/40C23C16/455C23C16/56
CPCC23C16/405C23C16/45525C23C16/56
Inventor 曹韫真吕欣瑞李莹闫璐宋力昕
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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