Chemical Vapor Deposition of Vanadium Dioxide for Thermochromic Smart Window Applications

doi:10.15541/jim20230386

Abstract

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

CLC Number:

TQ174

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.

Figures/Tables 42

Fig. 1 Schematic of thermochromic smart window[7]

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]

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)

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

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

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]

Fig. 6 Schematic diagram for APCVD system[36]

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

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

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

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]

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

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

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

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

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]

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

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 ℃

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

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

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

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]

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

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

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

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

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

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 ℃

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

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

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

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

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]

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]

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

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

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

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

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

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

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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