应用等离子体辉光监控反馈控制反应气体流量制备VO2 薄膜的研究

doi:10.15541/jim20150302

摘要/Abstract

摘要：

采用等离子体辉光监控系统(PEM)反馈控制反应溅射过程, 在石英基底上制备出单斜相VO₂薄膜, 并研究了反馈控制下反应溅射的等离子体相对辉光强度与氧气流量的关系。实验结果表明: 在不同的反应压强(0.8 Pa、0.5 Pa、0.2 Pa)下, 通过调整相对辉光强度值(REI)均可稳定获得单斜相VO₂薄膜, 对应的REI值分别为0.6~0.65、0.65、0.6。XRD测试结果表明VO₂薄膜具有明显的(011)晶面取向, XPS测试结果表明薄膜的化学计量比为VO_2.02。VO₂薄膜在2.5 μm处的变温透过率测试结果显示薄膜在相变前后的透过率变化达到65%, 相变温度确定为66℃。

关键词: 二氧化钒, 等离子辉光监控, 反馈控制, 反应溅射, 薄膜

Abstract:

Monoclinic VO₂ film was deposited on quartz substrate by reactive sputtering using the plasma emission monitor (PEM) system as reactive gas flow rate feedback control. Relationship between oxygen flow rate and plasma emission intensity was studied. It was found that single-phase VO₂(M) could be obtained steadily at specific relative emission intensity (REI), which were determined as 0.6-0.65, 0.65 and 0.6 for total deposition pressure of 0.8 Pa, 0.5 Pa and 0.2 Pa, respectively. XRD measurement indicated that the deposited VO₂ films were strongly oriented of (011) and the XPS measurements verified stoichiometry of the films as VO_2.02. Optical transmission measurement of VO₂ film exhibited an abrupt change of transmittance from 81% to 16% as VO₂ film switched from semiconductor state to metallic state, at transition temperature of 66℃.

Key words: vanadium dioxide, plasma emission monitor, feedback control, reactive sputtering, thin films

中图分类号:

TQ174

王孝, 闫璐, 李莹, 曹韫真. 应用等离子体辉光监控反馈控制反应气体流量制备VO₂ 薄膜的研究[J]. 无机材料学报, 2015, 30(11): 1228-1232.

WANG Xiao, YAN Lu, LI Ying, CAO Yun-Zhen. Sputtering Deposition of VO₂ Film Using Plasma Emission Monitor as Reactive Gas Flow Rate Feedback Control[J]. Journal of Inorganic Materials, 2015, 30(11): 1228-1232.

图/表 5

Fig. 1 Schematic diagram of the experiment setup and control loop of PEM system

Fig. 2 The relative emission intensity (Vreactive/Vmetallic) vs oxygen flow curves (a) Oxygen flow rate was controlled by MFC and relative emission intensity was merely recorded; (b) Oxygen flow was feedback controlled by PEM system and the flow rate was recorded. The three curves were obtained under the total pressure of 0.8 Pa, 0.5 Pa and 0.2 Pa, respectively

Table 1 Deposition parameters and corresponding crystalline structures of the films

Samples	Total pressure/Pa	Relative emission intensity(V_reactive/V_metallic)	Oxygen flow/sccm	Crystalline structures
1#	0.8	0.7	2.4-2.3	V₅O₉
2#	0.8	0.65	2.7-2.5	VO₂(M)
3#	0.8	0.6	2.9-2.8	VO₂(M)
4#	0.8	0.5	2.9-2.8	VO₂(B),V₂O₅,V₆O₁₃
5#	0.8	0.4	2.9-2.8	VO₂(B)
6#	0.5	0.7	2.4-2.2	V₅O₉
7#	0.5	0.65	2.8-2.6	VO₂(M)
8#	0.5	0.6	3.0-2.8	V₃O₇, VO₂(B)
9#	0.2	0.65	2.9-2.7	V₅O₉
10#	0.2	0.6	3.2-3.0	VO₂(M)
11#	0.2	0.55	3.3-3.1	VO₂(B), V₃O₇, V₂O₅

Fig. 3 XRD pattern of VO2 (M) film (a) and XPS spectrum of VO2 (M) film (b)

Fig. 4 Temperature dependence of transmittance of VO2 film at wavelength of 2.5 μm (a) and derivative dTrans/dTemp curve for the heating cycle with dot line indicating its Gaussian fitting (b)

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应用等离子体辉光监控反馈控制反应气体流量制备VO₂ 薄膜的研究

Sputtering Deposition of VO₂ Film Using Plasma Emission Monitor as Reactive Gas Flow Rate Feedback Control

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