化学气相沉积法制备智能窗用热致变色VO2薄膜的研究进展

doi:10.15541/jim20230386

无机材料学报 ›› 2024, Vol. 39 ›› Issue (3): 233-258.DOI: 10.15541/jim20230386 CSTR: 32189.14.10.15541/jim20230386

• 综述 • 下一篇

化学气相沉积法制备智能窗用热致变色VO₂薄膜的研究进展

鲍可¹^,²(), 李西军¹^,²^,³()

1.西湖大学先进微纳加工与测试平台, 杭州 310024
2.浙江省3D微纳加工和表征研究重点实验室, 杭州 310024
3.西湖大学芯片数字化生产技术研究中心, 杭州 310024

收稿日期:2023-08-28 修回日期:2023-09-29 出版日期:2024-03-20 网络出版日期:2023-11-28
通讯作者: 李西军, 研究员. E-mail: lixijun@westlake.edu.cn
作者简介:鲍可(1984-), 女, 博士. E-mail: baoke@westlake.edu.cn
基金资助:
西湖大学微纳平台建设专项经费(201046011801)

Chemical Vapor Deposition of Vanadium Dioxide for Thermochromic Smart Window Applications

BAO Ke¹^,²(), LI Xijun¹^,²^,³()

1. Westlake Center for Micro/Nano Fabrication, Westlake University, Hangzhou 310024, China
2. Key Laboratory of 3D Micro/Nano Fabrication and Characterization of Zhejiang Province, Hangzhou 310024, China
3. Research Center for Digitalized Manufacturing Technology of Integrated Circuits, Westlake University, Hangzhou 310024, China

Received:2023-08-28 Revised:2023-09-29 Published:2024-03-20 Online:2023-11-28
Contact: LI Xijun, professor. E-mail: lixijun@westlake.edu.cn
About author:BAO Ke (1984-), female, PhD. E-mail: baoke@westlake.edu.cn
Supported by:
Operation Fund of Westlake Center for Micro/Nano Fabrication(201046011801)

摘要/Abstract

摘要：

热致变色智能窗是通过在玻璃上沉积温度刺激响应型材料, 实现根据环境温度调控窗户玻璃的太阳光透过率, 减少建筑物能耗的节能窗户。二氧化钒(VO₂)是一种典型的热致相变材料, 在~68 ℃发生金属-绝缘体相变, 相变前后伴随光学性能的显著变化, 在智能窗等多个领域有潜在的技术应用。然而, 当前VO₂基热致变色智能窗的应用仍存在着相变温度(τ_c)偏高、可见光透过率(T_lum)低和太阳能调节效率(ΔT_sol)不足等问题, 无法满足实际建筑节能的需求。为了解决这些问题, 研究人员开展了广泛而深入的工作。化学气相沉积法(Chemical vapor deposition, CVD)能够以合理的成本生产高质量、大面积的VO₂薄膜, 受到研究者青睐。本文总结了近年来利用CVD技术制备VO₂薄膜的研究进展, 系统介绍常压化学气相沉积、气溶胶辅助化学气相沉积、低压化学气相沉积、金属有机物化学气相沉积、原子层沉积和等离子体增强化学气相沉积等CVD工艺, 分析了反应物种类及比例、反应温度、压力、载体流量等因素对VO₂薄膜质量的影响, 并结合元素掺杂、纳米复合薄膜、多层膜结构等对VO₂薄膜的性能调控与优化进行总结, 最后对未来等离子体增强化学气相沉积制备VO₂薄膜的研究前景做出展望。

关键词: 二氧化钒, 热致变色, 智能窗, 化学气相沉积, 薄膜, 综述

Abstract:

Smart windows have gained tremendous attention because of their ability to dynamically modulate the solar radiation to minimize energy consumption and improve indoor living comfort. Vanadium dioxide (VO₂) is one of the most attractive thermochromic materials for energy-saving smart windows due to its reversible metal-to-insulator transition at a critical temperature of ~68 ℃ and accompanying great change of its optical transmittance. However, VO₂ itself has a couple of significant limitations as a smart window material: high phase transition temperature (τ_c), low luminous transmittance (T_lum) and insufficient solar energy modulation ability (ΔT_sol). Several methods have been used to grow VO₂ thin films with improved properties to meet the specific requirements for smart windows applications. The phase transition temperature (τ_c) should be reduced to near room temperature, in the meantime luminous transmittance (T_lum) and solar energy modulation ability (ΔT_sol) should be high enough for the modulation of indoor temperature self-adapted to seasons and climate. The most common way to reduce τ_c is by doping. To enhance T_lum and ΔT_sol, multilayer structures and/or nanocomposite film have been widely adopted. Chemical vapor deposition (CVD) is a promising technique to produce high quality and highly uniform VO₂ thin film with different morphologies in large scale and at low costs. In this paper, various CVD techniques, such as atmospheric pressure chemical vapor deposition (APCVD), aerosol-assisted chemical vapor deposition (AACVD), low-pressure chemical vapor deposition (LPCVD), metal-organic chemical vapor deposition (MOCVD), atomic layer deposition (ALD) and plasma-enhanced chemical vapor deposition (PECVD), are examined with respect to their advantages for VO₂ deposition, film quality and the strategies for film quality improvement. Finally, challenges and opportunities for further research and development of VO₂ thermochromic films using PECVD technique are emphasized.

Key words: vanadium dioxide, thermochromism, smart window, chemical vapor deposition, thin film, review

中图分类号:

TQ174

鲍可, 李西军. 化学气相沉积法制备智能窗用热致变色VO₂薄膜的研究进展[J]. 无机材料学报, 2024, 39(3): 233-258.

BAO Ke, LI Xijun. Chemical Vapor Deposition of Vanadium Dioxide for Thermochromic Smart Window Applications[J]. Journal of Inorganic Materials, 2024, 39(3): 233-258.

图/表 42

图1 热致变色智能窗[7]

Fig. 1 Schematic of thermochromic smart window[7]

图2 VO2的晶体结构和能带结构

Fig. 2 Schematics of the crystal structures and band structures of VO2 (a, b) Schematic depictions of the crystal structures of the high- temperature tetragonal rutile R phase (a) and low-temperature monoclinic M phase (b)[13]; (c, d) Schematic of the VO2 band structure in the metallic (c) and insulating (d) states[14]

图3 辐射冷却调节智能窗的结构与工作原理[27]

Fig. 3 Structure and concept of an RCRT window[27] (a) Schematic structure of the RCRT window; (b, c) Working principle of RCRT window in summer (b) and winter (c)

图4 1 atm下V-O系统相图[38]

Fig. 4 Phase diagram of the V-O system at 1 atm[38]

图5 CVD反应过程示意图[72]

Fig. 5 Schematic of general elementary steps of a typical CVD process[72]

表1 CVD制备VO2薄膜采用的钒前驱体的蒸气压

Table 1 Vapor pressure of the vanadium precursorscompounds used for the CVD of VO2 thin films

V valence	Compound/Molecular formula	Vapor pressure	Ref.
+3	V(acac)₃/V(C₅H₇O₂)₃	Not volatile, sublimes@220 ℃	[75]
+3	V(amd)₃/C₂₄H₅₁N₆V	6.6 Pa@70 ℃, 2.6 Pa@120 ℃	[76-78]
+4	TDMAV/C₈H₂₄N₄V	133 Pa@64 ℃	[79]
+4	TEMAV/C₁₂H₃₂N₄V	13 Pa@25 ℃, 57 Pa@82 ℃, 133 Pa@107 ℃	[79-81]
+4	VCl₄	780 Pa@20 ℃, 13.3 kPa@100 ℃	[82]
+4	VO(acac)₂/VO(C₅H₇O₂)₂	0.21 Pa@96 ℃	[77, 83]
+4	VO(thd)₂/VO(C₁₁H₁₉O₂)₂	0.27 Pa@96 ℃	[77, 83]
+4	VO(hfa)₂/VO(C₅H₂F₆O₂)₂	0.18 Pa@57 ℃	[83]
+5	VO(OC₃H₇)₃	6 Pa@20 ℃, 38.6 Pa@45 ℃, 268 Pa@82 ℃	[[79, [84-85]
+5	VOCl₃	1.84 kPa@20 ℃, 9.3 kPa@55 ℃	[82]

图6 APCVD装置示意图[36]

Fig. 6 Schematic diagram for APCVD system[36]

图7 APCVD以不同VCl4和H2O比例在450 ℃制备的氧化钒薄膜[90]

Fig. 7 Vanadium oxide thin films grown by APCVD at 450 ℃ using different gas precursor ratios[90] (a) XRD patterns for the samples grown using VCl4: H2O ratios of 1 : 1, 1 : 2 and 1 : 3; (b-d) SEM images of as-deposited (b) V2O3, (c) VO2 and (d) V2O5 thin films

图8 VO(acac)2和不同氧化剂通过APCVD反应生成的VO2薄膜的SEM照片(沉积温度500 ℃)[96]

Fig. 8 FE-SEM images of VO2 films obtained via APCVD with VO(acac)2 and different oxygen sources at 500 ℃[96] VO2 obtained using (a) ethanol; (b) propanol; (c) O2 gas

图9 外电场辅助APCVD装置示意图[97]

Fig. 9 Schematic of electric field EAAPCVD rig[97]

表2 APCVD制备VO2薄膜的工艺条件

Table 2 Range of conditions for the vanadium oxide thin films prepared by APCVD

Vanadium precursor	Bubbler temperature/℃	Oxygen source	Precursor ratio	Substrate temperature/℃	Carrier gas flow (N₂)/ (L·min^-1)	*τ_c of VO₂/℃	Ref.
VCl₄	100	H₂O	1 : 10	350-550	0.2	68	[86]
VCl₄	80	H₂O	(0.43-1.08) : 1	350-450	12	-	[92]
VCl₄	80	C₄H₈O₂	2 : 1	550	23.2	68	[91]
VOCl₃	90	H₂O	1.0 : 3.4	350-650	1.0	67	[89]
VO(acac)₂	200	O₂	-	500-575	0.4	51.5	[93]
VO(OC₃H₇)₃	50	-	-	450	3-4	65.5	[94]

图10 AACVD的工作原理和系统构成[36,100]

Fig. 10 Mechanism and system configuration for AACVD[36,100]

图11 通过AACVD在400~750 ℃下以不同VO(acac)2溶液制备的VO2薄膜以及基底[9]

Fig. 11 Substrates and VO2 films deposition via AACVD at 400-750 ℃ using different solutions of VO(acac)2[9] (a, c) Photographs (a) and XRD patterns (c) of VO2 films from methanol solution of VO(acac)2; (b, d) Photographs (b) and XRD patterns (d) of VO2 films from water solution of VO(acac)2

图12 通过AACVD以VO(acac)2水溶液为前驱体在650 ℃制得的VO2薄膜的SEM照片[9]

Fig. 12 SEM images of the VO2 films deposited via AACVD at 650 ℃ using a water solution of VO(acac)2[9] (a) Surface SEM image of the VO2 films at low magnification; (b) Surface SEM image of the VO2 films at high magnification; (c) Cross-sectional SEM image of the VO2 films

图13 LPCVD装置及沉积过程示意图[103]

Fig. 13 Schematic representation of LPCVD and the CVD reaction process[103]

图14 LPCVD以V(acac)3为前驱体在不同时间下制得的VO2薄膜(350 ℃下沉积30~120 min, 并在350 ℃下退火2 h)[103]

Fig. 14 VO2 films deposited via LPCVD from V(acac)3 at 350 ℃ for 30-120 min and then annealed at 350 ℃ for 2 h[103] (a) Raman spectra of VO2 films; (d) XRD patterns of VO2 films; (b, c, e, f) SEM photographs of VO2 films deposited for (b) 30, (c) 60, (e) 90, and (f) 120 min, respectively

表3 MOCVD制备VO2薄膜的工艺条件

Table 3 Conditions for VO2 thin films deposited by MOCVD

Vanadium precursor	Evaporator temperature/℃	Reactor pressure/Pa	Substrate temperature/℃	O₂ flow	Carrier gas flow (Ar)	τ_c of VO₂/℃	Ref.
VO(acac)₂	150-175	2000	475-520	20-60 sccm	50-100 sccm	66-72	[107]
VO(acac)₂/methanol	150	101325	375-450	0.02-0.08 L/min	0.98 L/min	60	[108]
VO(acac)₂	120-150	266.6	390-490	Flow rate of O₂ to Ar 0.2	-	62±1	[105]
VO(acac)₂	170	399.9	200-750	150 sccm	150 sccm	-	[106]
VO(acac)₂	185	2559.36	520-550	50 sccm	100 sccm	61.0-68.5	[109]
VO(hfa)₂/H₂O	100-120	350	390-600	-	3.6-5.0 L/h	60	[110-111]

图15 二区卧式MOCVD反应器示意图[105]

Fig. 15 Scheme of a two-zone horizonal MOCVD reactor for VO2 film growth[105]

图16 MOCVD以VO(acac)2为前驱体在200~350 ℃制备的VO2薄膜的SEM照片[106]

Fig. 16 SEM morphologies of VO2 films prepared with MOCVD using VO(acac)2 in the range of 200-350 ℃[106] (a) 200 ℃; (b) 300 ℃; (c) 350 ℃

图17 MOCVD以VO(hfa)2/H2O为反应物制备VO2薄膜[110-111]

Fig. 17 Experimental details of VO2 film deposition based on MOCVD using reaction between VO(hfa)2 and H2O vapors[110-111] (a) Scheme of the MOCVD apparatus; (b) Scheme of pyrohydrolysis of VO(hfa)2 molecules resulting in the VO2 film growth

图18 MOCVD以VO(hfa)2/H2O为反应物制备的VO2薄膜及退火后的SEM照片[111]

Fig. 18 SEM images of VO2 films deposited by MOCVD using VO(hfa)2/H2O[111] (a) As-deposited VO2 film at 390 ℃; (b, c) VO2 films after annealed at (b) 575 and (c) 600 ℃ for 60 min

图19 ALD反应流程图[113]

Fig. 19 Schematic of ALD cycle[113] (a) Precursor A reacts with the substrate; (b) Excess precursor A and reaction byproducts are purged from the chamber; (c) Precursor B is pulsed into the chamber and reacts with the surface; (d) Excess precursor B and reaction products are purged from the chamber

表4 ALD制备VO2薄膜的工艺条件

Table 4 Summary of the ALD parameters used for the growth of VOx thin films

Vanadium precursor	Evaporator temperature/℃	Oxidant	Substrate temperature/℃	Annealing conditions	τ_c of VO₂/℃	Ref.
VO(acac)₂	150	O₂	400-475	-	66-70	[120]
VO(acac)₂	-	O₂	400-450	550-850 ℃ for 3 min	-	[121]
VO(OC₃H₇)₃	RT	H₂O	60-90	Ar plasma-annealing at 550 ℃ in vacuum	68	[79]
TEMAV	105	O₃	150	450 ℃ in He/O₂	68	[122]
TEMAV	105	O₃	150	2 h at 585 ℃ in 1.333×10^-3 Pa O₂	68	[123]
TEMAV	105	H₂O	150	450 ℃ in O₂/Ar (13.33 Pa)	70.1	[80]
TDMAV	RT	H₂O/O₃	50-200	550-800 ℃ in N₂ for 2 h	-	[119]
TDMAV	60	H₂O	150-200	475 ℃ in Ar for 100 min	72	[124]
VCl₄	-	H₂O	350	≥500 ℃ in 90% N₂/10% H₂ for 60 min	68	[125]

图20 ALD制备的氧化钒薄膜经过不同温度退火后的SEM照片[121]

Fig. 20 SEM images of ALD VO2 films annealed at different temperatures[121] (a) 550 ℃; (b) 700 ℃; (c) 850 ℃

图21 ALD以TEMAV/O3为反应物制得的氧化钒薄膜(衬底为c-Al2O3)的XPS图谱[123]

Fig. 21 XPS spectra of ALD VO2 films using TEMAV/O3 as reactants on c-Al2O3[123] (a) XPS spectra of as-deposited (black) and annealed (red) VO2 films; (b) Raman spectra of as-deposited (black) and annealed (red) VO2 films

图22 ALD以TEMAV/H2O为反应物制得的VO2薄膜经退火后的SEM和AFM照片[133]

Fig. 22 SEM and AFM images of annealed H2O-based ALD VO2 films [133] (a) 28 nm; (b) 8 nm; (c) 4 nm

图23 单脉冲和多脉冲两种模式的ALD方法制备VO2薄膜[80]

Fig. 23 Schematic of SP and MP modes employed in the ALD process[80] (a) Typical sequence of the SP and MP modes of the ALD process; (b) Resistivity as a function of temperature and its derivative for the annealed VO2 thickness indicating the transition temperatures during heating and cooling cycle for depositions in SP and MP modes

图24 ALD以TDMAV/H2O为反应物在50 ℃下制备的VOx薄膜[119]

Fig. 24 ALD VOx films deposited with TDMAV/H2O at 50 ℃[119] (a) XRD patterns of VOx film before and after 2 h annealing at 800 ℃ under N2; (b) SEM images of as-deposited and annealed VOx films

图25 ALD以TDMAV/H2O为反应物在150~200 ℃制备的VOx薄膜(在475 ℃氩气中退火100 min)[124]

Fig. 25 ALD VO2 films deposited from TDMAV/H2O at 150-200 ℃ and annealed at 475 ℃ for 100 min in Ar[124] (a-c) AFM images of VO2 films deposited at (a) 150, (b) 175 and (c) 200 ℃; (d) V2p XPS spectrum for the annealed VO2 film deposited at 200 ℃

图26 ALD以VCl4/H2O为反应物制得的VO2薄膜(在500和550 ℃退火)[125]

Fig. 26 ALD VO2 films deposited from VCl4/H2O and subsequently annealed at 500 and 550 ℃[125] (a) Raman spectra of as-deposited sample (black) and annealed samples at 500 (blue) and 550 ℃ (red); (b) XRD patterns of as-deposited and annealed VO2 films

图27 PECVD成膜的反应过程示意图[145]

Fig. 27 Schematic representation of the PECVD reaction process[145]

图28 RF-PECVD反应装置示意图[151]

Fig. 28 Schematic diagram of RF-PECVD system[151]

图29 WxV1-xO2d 晶体结构示意图[158]

Fig. 29 Crystalline structures of the WxV1-xO2[158] (a) Crystal structure relationship diagram of R and M1 phases; (b) Schematic diagram of local rutile structure around W dopant

表5 CVD方法制备W掺杂VO2薄膜的工艺条件

Table 5 Summary of the CVD conditions for the synthesis of W-doped VO2 thin films

Vanadium precursor	Oxygen source	Dopant precursor	CVD process	Substrate/ temperature/℃	Doping level/% (in atomic)	τ_c of VO₂/℃	Ref.
VOCl₃	H₂O	WCl₆	APCVD	Glass/500-650 ℃	1.9	29	[159]
VCl₄	H₂O	W(OC₂H₅)₆	APCVD	Glass/500-600 ℃	0.3	50	[161]
VCl₄	H₂O	WCl₆	APCVD	Glass/550 ℃	0.12-1.75	55.0-5.5	[162]
VO(acac)₂	2O₂/98N₂	WCl₆	APCVD	Glass/525 ℃	0.5	55	[163]
VO(acac)₂	O₂	W(OC₂H₅)₅	MOCVD	Glass/450 ℃	2	35	[164]
VO(acac)₂	-	W(OC₂H₅)₅	AACVD	Glass/550 ℃	0.175-1.98	47-28	[165]
TEMAV	O₂	W(CO)₆	ALD	Si/200 ℃	1.63	32	[29]

表6 部分掺杂元素对氧化钒薄膜热致变色性能的影响

Table 6 Effect of dopants on the thermochromic performance of VO2 thin films

Dopant (s), (in atom)	τ_c	ΔT_sol	T_lum/%	Ref.
W⁶⁺/0.6%	~21.6 ℃/%	11.4%	50.8	[170]
Mo⁶⁺	~5 ℃/%	-	-	[171]
Nb⁵⁺/10%	52.2 ℃	-	-	[172]
Ta⁵⁺/4%	24.8 ℃	6.8%	47.1	[173]
Zr⁴⁺/9.8%	64.3 ℃	14.1%	60.4	[174]
Mg²⁺/7%	~3 ℃/%	4.8%	51	[167]
Co²⁺/10%	44 ℃	3%	79	[175]
Tb³⁺/2%	65 ℃	8.3%	54	[176]
La³⁺/4%	~1.1 ℃/%	10.3	50.1	[177]
Eu³⁺/4%	~6.5 ℃/%	6.7%	54	[178]
Si⁴⁺/3%	63.1 ℃	13.9%	54.7	[179]
Fe³⁺/Mg²⁺	38.2 ℃	12.8%	42.1	[180]
Mg²⁺/W⁶⁺	35 ℃	4.3%	81.3	[168]
Tb³⁺/W⁶⁺	40.8 ℃	6.3%	40	[181]
Zr³⁺/W⁶⁺	28.6 ℃	4.9%	48.6	[174]

图30 APCVD以VOCl3/TTIP/H2O为反应物在650 ℃下得到VO2/TiO2复合薄膜表征[183]

Fig. 30 Characterization of VO2/TiO2 film formed by the APCVD reaction of VOCl3/TTIP/H2O at 650 ℃[183] (a) XRD pattern; (b) Raman spectrum; (c) SEM image; (d) Variable temperature transmission plot at 2.5 μm

图31 组合APCVD制备VO2/TiO2复合薄膜[184]

Fig. 31 Combinatorial APCVD for the synthesis of VO2/TiO2 composite film[184] (a) Schematic of the APCVD apparatus; (b) Picture of the entire graded VO2/TiO2 composite film formed

图32 在VO2薄膜上应用折射率可调减反层的效果图[191]

Fig. 32 Schematic illustrating the concept of the RI-tunable ARC applied on the VO2 substrate[191]

图33 APCVD制备的单层和双层薄膜的SEM照片[193]

Fig. 33 SEM images of the monolayer and multilayer samples prepared by APCVD[193] (a) VO2 film; (b) TiO2 film; (c) Multilayer of TiO2 over VO2; (d) Multilayer of VO2 over TiO2

表7 APCVD制备VO2/SiO2/TiO2三层薄膜的工艺参数[195]

Table 7 APCVD conditions of the VO2/SiO2/TiO2 films[195]

Layer	Precursor	Bubbler temperature /℃	N₂ flow rate /(L·min^-1)	Thickness /nm
VO₂	VCl₄/C₄H₈O₄	80/40	0.7/0.2	~300
SiO₂	SiC₈H₂₀O₄/C₄H₈O₄	130/40	0.7/0.2	~1300
TiO₂	TiCl₄/C₄H₈O₄	75/40	0.6/0.6	~100

图34 APCVD制备的VO2/SiO2/TiO2三层薄膜的SEM照片[195]

Fig. 34 SEM images of multi-layered VO2/SiO2/TiO2 films using APCVD[195] (a) Typical VO2 coating on glass; (b) Porous structure of the SiO2 interlayer, as deposited on VO2 coating; (c) Typical surface morphology of the TiO2 layer in the VO2/SiO2/TiO2 system; (d) Side-on SEM image of VO2/SiO2/TiO2 film

图35 VO2薄膜和SiO2/VO2双层薄膜的SEM和AFM照片[196]

Fig. 35 SEM and AFM images of VO2 and SiO2/VO2 thin films[196] (a, b) SEM and (c) AFM images of the pristine VO2 thin film; (d, e) SEM and (f) AFM images of SiO2/VO2 thin film

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化学气相沉积法制备智能窗用热致变色VO₂薄膜的研究进展

Chemical Vapor Deposition of Vanadium Dioxide for Thermochromic Smart Window Applications

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