VO2FTO复合薄膜的制备及其光电特性研究

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3.0 侯斌 2024-11-19 4 4 2.37MB 39 页 15积分

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摘要

根据外界环境温度变化而改变自身红外透过率的窗户就是智能窗，智能窗能

够有效的降低能耗起到节能环保的作用。因为 VO2薄膜材料独特的光电特性即：

在相变温度前后，其红外透过率、反射率和电阻率都会发生突变，这种突变具有

可逆性，相变速度快达皮秒量级，因此备受人们的关注。这使得 VO2薄膜在智能

窗应用领域中有着非常广阔的前景。

本文介绍了制备复合薄膜的几种方法，选取掺氟的 SnO2(FTO)导电玻璃作为衬

底，采用磁控溅射法制备了 V/FTO 复合薄膜样品，将制备的多个 V/FTO 复合薄膜

样品在不同比例的氮气（N2）和氧气（O2）混合气氛中退火，从而制备了多个

VO2/FTO 复合薄膜样品。经过多次试验发现，VO2/FTO 复合薄膜的厚度与其透过

率成反比关系，即厚度越厚透过率越低，热滞回线变宽，相变温度降低，究其原

因主要是受复合薄膜的结晶性影响。

从降低 VO2薄膜相变温度，缩窄热滞回线温宽和减小其相变前后红外透过率

差值等角度出发，开展了 VO2/FTO 复合薄膜制备工艺的探索。将制备的 V/FTO 复

合薄膜样品在不同混合比例的 N2和O2，以及相同比例的 N2和O2气氛不同退火时

间条件下形成的 VO2/FTO 复合薄膜的光电特性进行分析，摸索出 400℃条件下最

佳的退火氛围和时间。同时还研究并分析了一些工艺参数对复合薄膜特性的影响，

完善了制备 VO2/FTO 复合薄膜的工艺流程，从而获得了最佳工艺参数。

利用原子力显微镜(AFM)、X射线衍射仪（XRD）、分光光度计（250～2500nm）、

四探针测试仪和 4200-SCS 型半导体特性分析系统配合 M150 探针台分别对

VO2/FTO 复合薄膜样品的物理结构、光学特性和电学特性进行测试与分析。结果

表明，最佳工艺参数下制备的薄膜结晶程度较高，表面平滑致密，具有很好的一

致性，衬底上的 FTO 并没有改变 VO2择优取向生长，却使得 VO2的表面形貌特征

有很大改变。与 VO2薄膜的典型相变温度 68℃比较而言，VO2/FTO 复合薄膜的相

变温度降低了20℃，热滞回线收窄到 5℃，相变前后的红外透过率分别为 45%和

22%，相变前电阻率是相变后电阻率的 1.43×103倍，VO2/FTO 复合薄膜优良的光

电特性对新型光电薄膜器件的设计开发和应用具有重要意义。

关键词：VO2 FTO 氮氧混合热致变色智能窗

ABSTRACT

The smart windows can change its infrared transmittance according to the outside

temperature, so it can effectively reduce energy consumption which plays an important

role in energy conservation and environmental protection. VO2 attract a lot of people

because of its unique properties that infrared transmittance, reflectance and resistivity

will mutation before and after the phase transition, and the phase transition is reversible

as also as the time of phase transition only needs few picoseconds. This means the VO2

films has a very broad application prospects in the field of smart windows.

This paper introduce some methods to prepare composite film, we choose fluorine

doped SnO2 (FTO) conducting glass as substrate, VO/FTO composite films were

prepared by magnetron sputtering. And then we put the prepared VO/FTO composite

films in different mixing ratios of N2 and O2 annealing conditions to get the VO2/FTO

composite films. We can get the conclusions that, transmission of VO2/FTO composite

films is inversely proportional to its thickness, which means that the thicker of

VO2/FTO composite films the lower transmittance permeability, wider of thermal

hysteresis loop, lower phase transition temperature. The main reason is due to the

crystalline of the composite films.

In order to lower the phase transition temperature, narrow the wide temperature of

the thermal hysteresis loop and reduce infrared transmittance difference before and after

the phase transition of VO2/FTO composite films, we do this study for VO2/FTO

composite film preparation process. The prepared V/FTO composite film samples were

put in different mixing ratios of N2 and O2, or the same ratios of N2 and O2 atmosphere

with different annealing time and then we tested the photoelectric properties of

VO2/FTO composite films. We find out the best annealing mixing ratios of N2 and O2

and annealing time (in 400℃ annealing temperature) to form high quality VO2/FTO

composite films. We also studied and analyzed some process parameters which have

impact on the VO2/FTO composite films preparation process. In the same time we

improved the preparation process for preparing VO2/FTO composite films.

Tested the physical structure, the optical properties and electrical properties of

VO2/FTO composite films by atomic force microscopy (AFM), X-ray diffraction (XRD),

spectrophotometer (250~2500nm), four-probe tester and Model 4200-SCS

Semiconductor Characterization System with M150 probe station. The pure vanadium

metal thin films were fabricated on the SnO2 doped F conductive glass(FTO) substrates

by DC magnetron sputtering at room temperature, then the VO2 /FTO composite films

were prepared by annealing process in a mixture of N2 and O2. The structure and

optical-electrical properties of the composite films were analyzed by instruments. AFM

results show that the crystallinity of the thin film is improved significantly with smooth

and uniform surface morphology. Results show that VO2 /FTO composite films do not

change the preferred orientation growth of VO2 thin films, but significantly change its

surface morphology characteristics. Compared with the VO2 thin films that the phase

transition temperature of the VO2 /FTO composite films is decreased about 20℃, the

width of thermal hysteresis is narrowed by about 5℃, and the infrared transmittances

before and after phase transition are 45% and 22% respectively. The resistivity variation

is up to three orders of magnitude before and after transition. This brings about many

new opportunities for optoelectronic devices and industrial production.

Key words: VO2, FTO, N2-O2 mixture, Thermochromic, Smart

Windows

中文摘要

ABSTRACT

第一章绪论 .....................................................................................................................1

1.1 引言 ........................................................................................................................1

1.2 国内外研究现状 ....................................................................................................3

1.3 VO2薄膜的应用......................................................................................................4

1.4 课题研究的目的和意义 ........................................................................................5

1.5 课题研究的创新点 ................................................................................................6

1.6 本章小结 ................................................................................................................6

第二章 VO2/FTO 复合薄膜的设计与制备.....................................................................7

2.1 薄膜的制备方法概述 .............................................................................................7

2.1.1 真空溅射法 .....................................................................................................7

2.1.2 真空蒸发镀膜 .................................................................................................9

2.1.3 真空离子镀膜 ...............................................................................................10

2.1.4 化学气相沉积 ...............................................................................................10

2.1.5 液相沉积 .......................................................................................................11

2.2 直流磁控溅射法制备复合薄膜 ..........................................................................12

2.3 本章小结 ..............................................................................................................15

第三章制备工艺对 VO2/FTO 复合薄膜特性的影响..................................................16

3.1 影响 V/FTO 复合薄膜的工艺要素 .....................................................................16

3.1.1 真空度对 V/FTO 复合薄膜的影响 ..............................................................16

3.1.2 工作压力对 V/FTO 复合薄膜的影响 ..........................................................17

3.1.3 溅射功率对 V/FTO 复合薄膜的影响 ..........................................................18

3.1.4 溅射时间对 V/FTO 复合薄膜的影响 ..........................................................19

3.2 退火时不同氧气氮气比例和退火时间对 VO2/FTO 复合薄膜的影响.............20

3.3 本章小结 ..............................................................................................................21

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摘要：

摘要根据外界环境温度变化而改变自身红外透过率的窗户就是智能窗，智能窗能够有效的降低能耗起到节能环保的作用。因为VO2薄膜材料独特的光电特性即：在相变温度前后，其红外透过率、反射率和电阻率都会发生突变，这种突变具有可逆性，相变速度快达皮秒量级，因此备受人们的关注。这使得VO2薄膜在智能窗应用领域中有着非常广阔的前景。本文介绍了制备复合薄膜的几种方法，选取掺氟的SnO2(FTO)导电玻璃作为衬底，采用磁控溅射法制备了V/FTO复合薄膜样品，将制备的多个V/FTO复合薄膜样品在不同比例的氮气（N2）和氧气（O2）混合气氛中退火，从而制备了多个VO2/FTO复合薄膜样品。经过多次试验发现，VO2/FT...

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