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Effect of Oxygen Deposition Pressure on the Structure and the Metal Insulator Transition in Pulsed Laser Deposited VO2 Films on Soda Lime Glass

NM Ndiaye, M Thiam, BD Ngom , O Sakho, M Chaker, N Manyala, AC Beye
American Journal of Nanomaterials. 2017, 5(2), 59-67. DOI: 10.12691/ajn-5-2-3
Published online: October 14, 2017

Abstract

Vanadium dioxide thin films nanostructures were synthesized by pulsed laser deposition on soda lime glass at a substrate temperature of 600°C and the effects of the oxygen deposition pressure on the crystalline structure and the phase transition characteristics of VO2 nanostructured films were investigated. The structure and microstructure of the films have been examined by X-ray diffraction (XRD) and scanning electron microscopy (SEM). Results indicate that the crystal structure of the films is strongly sensitive to the oxygen deposition pressure; exhibiting sharp a-axis diffraction peaks, showing a texturation along (1 0 0) plane. A detailed description of the growth mechanisms and the substrate–film interaction is given, and the characteristics of the electronic transition and hysteresis of the phase transition are described in terms of the morphology, grain boundary structure and crystal orientation. The sharpness of the transition and the hysteresis upon heating and cooling are found to be strong functions of the crystal structure and microstructure (grain size).

1. Introduction

Large number of transition metal oxides and sulphides are semi-conducting and metallic at low temperatures and high temperatures, respectively 1. In vanadium oxide compounds categorized as Mott insulators, this semi-conducting / metal phase transition is a first-order type as observed in V2O3, V3O5, V4O7, VO2 2. The fascinating properties and wide range applications of vanadium oxides family, especially in thin film form, have attracted considerable interest 3. Vanadium dioxide (VO2), which is part of the several vanadium oxide phases such as the Magneli (VnO2n1) and Wadsley phases (V2nO5n2), is studied widely due to its abrupt change of reflectance in the infrared range near room temperature 4, 5.

Vanadium dioxide (VO2) manifests a femtosecond 1st order semiconductor/metal transition (SMT) at a temperature TSMT ~ 68°C. At temperatures higher than the critical temperature which is TSMT ~ 68°C, it transforms to a narrow gap (0.7 eV) 6, 7. Below TSMT, the semiconductor VO2 exhibits a monoclinic structure, with lattice constants a ~0.575 nm, b~0.4526 nm and c~0.5383 nm. Above TSMT, the metallic behavior is characterized by a tetragonal rutile-type structure, with lattice constants a~0.455nm and c~0.285 nm. This tetragonal rutile (P42 /mnm) structure has chains of edge-shared VO6 octahedral along the c-axis and the V–V distance along the chains is 0.2851 nm. In the semiconducting monoclinic (P21/c) crystal structure, the dimerized vanadium atoms have alternate V–V distances of ~0.2619 and ~0.312 nm 4.

As a consequence of such a femtosecond electronic/ crystallographic and reversible SMT phase transition, the optical dielectric constant and thus the refractive index of VO2 exhibits a temperature modulation, which translates in a large reversible optical properties. This singular and unique property of VO2 makes it a multifunctional optical candidate of choice for smart windows applications, optical switching devices, field effect transistors, ultrafast tunable nano-plasmonics and optical limiting devices as well as ultrafast opto-electronic gates among others. Through this reversible SMT near room temperature, VO2 is considered also as a material having high potential for various applications other than thermochromic smart coatings, which include electronic switches and thermal sensors 8, 9, 10.

The nature of the electronic and structural phase transition has been a matter of research and debate for over three decades with many recent experiments shedding additional light on the issue 11. But during this period the hysteretic nature of VO2 has received much less attention. The hysteresis nature and mechanism in VO2 are still open questions, which are interesting from a basic research point of view and might provide both information regarding the SMT mechanism and hysteresis in general in VO2. It is also of vast importance from a technological aspect. For example, for optical memory-type applications, a large hysteresis is needed, while a small hysteresis is preferable in VO2-based room-temperature bolometers for UV detectors. So, understanding the origin of the hysteresis can lead to a better control of its properties as reported by J.-G. Ramírez et al. 11. The VO2 thermal hysteresis characteristics are found to vary between samples grown under different conditions and resulting samples conditions, growth temperature, choice of substrate, as well as growth atmospheric pressure 11. And film thickness and grain size respectively 11.

There are many reports on controlling the transition temperature of VO2 thin film, either by doping 12, 13 or applying stress 14, 15. Due to the small compositional differences between the numerous phases of vanadium oxide, VO2 preparation requires a stringently controlled process that provides the desired oxygen stoichiometry and correct crystalline structure. Consequently, oxygen pressure is a critical parameter in growing the films 16. In search of such a process, VO2 films have been produced by a number of methods, including DC and RF reactive magnetron sputtering 8, 17, 18, reactive ion-beam sputtering 19, 20, reactive evaporation 21, 22, chemical vapor deposition 23, 24, pulsed laser deposition (PLD) 2, 3, 25, electrochemical (anodic) oxidation 26, 27 and sol–gel processes 28, 29. Given the requirement for accurate optimization to obtain the correct VO2 polycrystalline structure, and due to the numerous electronic valences of vanadium and its high affinity for oxygen, it is challenging to synthesize large thermochromic VO2-based coatings using such techniques. PLD has been found to be efficient and cost effective technique to produce, large amounts of thermochromic coatings. This technique is known for its rational fabrication of smart and functional high-quality metal oxide particulate thin films and coatings. Some of the synthesis methods have produced amorphous or quasi-amorphous films; others have produced polycrystalline films, and still others have produced oriented epitaxial films. The resultant films structures vary, depending on the crystallographic relationship between the growing VO2 and the substrate, as well as on other factors, such as the growth temperature 30 and oxygen pressure.

In this paper we report on PLD-grown thin films, with a-axis orientation, influenced by the oxygen deposition pressure. It was determined that the manner of growth of a-axis oriented VO2 thin films on a glass substrate has a direct bearing on the characteristics of these films. As the hysteresis nature and mechanism in VO2 are still an open question, which is interesting from a basic research viewpoint. This contribution will shed light on the effect of oxygen deposition pressure on the structural and micro-structural properties of the VO2 thin films and consequently on its hysteresis characteristics and transition temperature.

2. Experimental Details

The VO2 thin films were deposited using pulsed laser ablation deposition on a soda lime glass substrate maintained at a temperature of 600°C. The oxygen deposition pressure was varied from 3 to 15 mTorr to prepare various samples. The deposition time was set and maintained at 45 minutes corresponding to a deposition rate of 1,78 nm/min. This gives a thickness of 80 nm for each sample. We used a KrF excimer laser of wavelength of 248 nm, which has been focused onto the rotating target metal vanadium. The laser fluence was maintained at 1.7J/cm2 and the repetition rate at 10 hertz, and 30 ns of pulse duration. The target-substrate distance was maintained at 6 cm. After deposition all samples were cooled in a vacuum with a cooling rate of 50°C/min. The crystallographic structure of thin films of VO2 was characterized and confirmed by the technique of X-ray diffraction using a Bruker D8 diffractometer model powder Bragg-Brentano geometry. The intensity of the direct beam is obtained using a variable tube current of 40 kV and 40 mA with Cu radiation of wavelengths Kα1 length. The goniometer comprises a set up with N -1 Vantec detector and filter 4 degrees of Soller slit and providing narrow symmetrical profiles instrumental (PI) to the desired angular range. The spectra of X-ray diffraction of the samples were recorded in the range (2θ = 12°-80°) using in each case a step size of 0.02° and a count time of 20 s per step without moving the sample. The instrumental profile was obtained experimentally by collecting diffraction data of a standard Al2O3 powder by fitting with pseudo-Voigt functions and setting changes on the value of the width at half height. A Scanning electronic microscope (SEM) SEM 230 Nano secondary electron mode was used for analysis of the surface morphology of the films after deposition and the UV-Vis-NIR spectroscopy data of the VO2 samples were collected in the wavelength range of 350 – 1100 nm using a CECIL 2000 Spectrophotometer incorporated with Peltier thermoelectric heating and cooling stage.

3. Results and Discussions

Figure 1a shows the XRD patterns characteristics of VO2 thin films deposited on soda-lime glass substrate at different oxygen deposition pressures ranging from 3 mTorr to 15 mTorr, and cooled down to room temperature at a rate of 50°C/min in vacuum after deposition. The patterns show peaks due to the VO2 thin layer at angles of 18.48°, 27.97°, 37.18°, 39.98° and 55.72° and a broad peak due to the glass substrate at an angle around 20°. Following the calculated pattern description of the monoclinic structure of VO2 (JCPDS No: 43-1051), these peaks can be indexed as the reflections on the (1 0 0), (0 1 1), (2 0 0), (0 2 0) and (0 2 2) planes respectively. After a qualitative phase analysis (search match) carried out using the PANAlytical X'pert Highscore plus software employing the ICDD PDF database, no additional peaks due to others impurities were observed. It should be noted that although the multiple valence states of vanadium ions lead to several vanadium oxide phases such as Magneli phases (VnO2n−1) and Wadsley phases (V2nO5n−2), no other peak corresponding to any other vanadium oxide phases mentioned is present in the XRD spectra, indicating the exclusive formation of single-phase VO2 films on the glass substrate.

However it can be seen that the sample prepared with an oxygen pressure of 3 mTorr is completely amorphous with the broard peak around 20° coming from the substrate, while the other samples prepared in the range of 5 to 12 mTor of oxygen pressure, present the same XRD patterns with a preferential orientation along the <1 0 0> direction. The sample prepared with an oxygen pressure of 15 mTorr presents the very same characteristic of monoclinic VO2 that is usually reported into the literature with a preferentiel growth along the <0 1 1> direction.

In an attempt to study and try to understand the mechanism that govern the preferential structural growth of our reported VO2 (1 0 0), we have look at the evolution of the intensity of the (0 1 1) plane with respect to the (1 0 0) plane, as a function of oxygen deposition pressure and it is shown in Figure 1b. When the oxygen pressure increases, it is observed that the intensity of the reflection coming from the (1 0 0) diffraction plane increases, while the intensity of the (0 1 1) diffraction plane decreases. These observations indicate an enhancement of the texture of the VO2 thin films along the <1 0 0> direction within the increasing of oxygen pressure. It should be noted that mostly reported work on the structural properties of VO2 on glass show only a preferential growth along the <0 1 1> direction. But recently a report by Ngom et al, 29, whom worked out the crystal structure and morphology of vanadium dioxide (VO2) nanostructures, showed a preferential orientation of VO2 along the <1 0 0> direction. They have synthesized their VO2 thin film by pulsed laser deposition on soda-lime glass substrate in pure oxygen at a pressure of 15 mTorr by controlling the cooling rate of the substrate from 5°C/min to 25°C/min after deposition in vacuum.

On the work done by Ngom et al., the presented results, as supported by both their SEM and XRD findings, and specially by the evolution of the crystalline growth along the (1 0 0) plane, showed that the growth mechanism that can be considered is the competitive texturation to explain the origin of the structural preferential growth along the VO2 (1 0 0) plane.

As shown in Figure 1b, it should be noticed that a “growth competition” is not the a better explanation of the origin of the preferential orientation since as the oxygen pressure increases, it is observed that the intensity of the reflection coming from the (1 0 0) diffraction plane increases, while the one of the (0 1 1) diffraction plane decreases. At maximum oxygen deposition pressure of 15 mTorr there is a restructuring and a change in the preferential orientation. Therefore there should be another mechanism that govern the preferential orientation along (1 0 0), which is not really very understand because of luck of enough information.

Figure 1c show the evolution of the d-spacings as a function of the deposition pressure along the (1 0 0) and (0 1 1) planes respectively. The reported values for the d-spacings agree with those of the monoclinic structure of VO2 (JCPDS No. 43-1051). Figure 1c shows a continuous, almost linear decrease of the d-spacing along the (0 1 1) plane, which may suggest that the films are under strain during growth along the (0 1 1) direction. This is illustrated by the evolution of the crystallite size obtained using the well-known Debye Scherrer formula, as presented in Figure 1d. While the crystalline grains size follow a linear trend along the (0 1 1) plane it is not the case along the (1 0 0).

The observed variation of the surface morphology as reported in Figure 2, of the VO2 nanostructures with oxygen pressure, may be due to the nucleation of the glass substrate, which occurs at around 575°C and is followed by the process of crystallization of the VO2. 30. Increasing the pressure up to 12 mTorr leads to preferential crystal growth along the (1 0 0) plane, while longitudinal grain growth leading to very well-dispersed nanorods-like edge shapes are taking off parallel to the surface of the substrate are observed. At a pressure of 15 mTorr grains dominate the surface morphology and there is a complete change on surface morphology, which can be correlated to the XRD results. In Figure 2, the SEM images of the films prepared at 3mTorr and 5mTorr there is some cracks, the origin of this, can be discussed in terms of films stress.

To investigate the effect of deposition pressure on the thermo-optical properties and the SMT phase transition characteristics in the V02 films deposited on soda lime, the transmittance measurements were carried while heating and cooling the sample at different temperatures from room temperature to 100°C. Figure 3a shows the thermal hysteresis loops of the optical transmittance (Tr) at a fixed wavelength of 1100 nm for VO2 thin films deposited at different oxygen pressure. We see qualitatively different hysteresis shapes for the films for different oxygen pressure as shown in Figure 3a.

To evaluate the transition temperature and the hysteresis width as functions of the deposition pressure, derivatives of the transmittance (Tr) and its temperature dependence (dTr/dT) were extracted for the VO2 thin films at different temperatures. A plot of (dTr/dT) was obtained from the transmittance (Tr)–temperature (T) data for each sample. The maximum temperatures corresponding to (dTr/dT) were defined as the phase temperatures in the heating and cooling cycles, THeating and TCooling, respectively.

The SMT temperature (TSMT) was defined as

The hysteresis width can be defined by

We can observe that the transition temperature follows the same trend as the crystalline size along the (1 0 0) plane of the VO2, within the increase of the deposition pressure. The Highest transition temperature was obtained at the higher crystalline sizes. This is to demonstrate how the crystalline grains sizes affect the transition temperature, but seems to be contradicting with what have been reported in the literature so far. Suh et al. 31 undertook a careful study of the SMT transition of VO2 films on (1 0 0) silicon substrates as a function of annealing time and found that the microstructure of the films changed from nanocrystalline nearly amorphous to crystals with a diameter of 200 nm. In the early stages, the film showed that as the grain size increased, the SMT decreased, but hysteresis continued to increase. The changes of the thermo-optical properties of VO2 thin films are usually explained as results of the competing effects between grains size, nucleation defects, grain boundaries and crystal imperfections 32, 33. Therefore the differences in the morphologies and crystal orientations of the films lead to the distinctive SMT characteristics seen in the curves of Figs 3b but not only because of the variation in crystal grain sizes.

J. B. Kana Kana et al 16 have reported high substrate temperature induced anomalous phase transition temperature shift in sputtered VO2 thin films on corning glass. They have observed that at higher substrate temperature from 550 to 600°C led to a transition temperature of 75°C and 80°C, respectively and these values are closer to our reported values but a little bit higher and this may be due to the difference in glass substrate type used. As reported by J.B. Kana Kana et al 15, the major two effects that could led to this higher VO2 transition temperature are a slight stoichiometry deviation and/or a possible diffusion of some element from the glass substrate to the films such as Al, Na or Ca. This would explain why we have observed higher transition temperature at higher crystal grain sizes, which may be related to some effect induced by the substrate glass transition temperature reported to be around 575°C during the 600°C thin films growth since thickness of the samples are the same.

As reported in fig. 3b it is interesting to notice that the hysteresis width increase linearly with the increase in deposition pressure with a smallest width of 7°C obtained at a deposition pressure of 5 mTorr and a maximum of 14°C obtained at a deposition pressure of 12 mTorr. While the sample prepared at a deposition pressure of 15 mTorr, which presents the preferential orientation along (0 1 1) plane of VO2 gave a hysteresis of 13°C. These values agree with the usual reported values into the literature for such (0 1 1) oriented VO2 34, 35. The smaller hysteresis of the films is obtained at lower oxygen pressure and this could be explained by the texture obtained at this oxygen pressure as reported in Figure 1a.

4. Conclusion

In this paper we have reported on the deposition and characterization of VO2 thin film samples, to study how the deposition oxygen pressures affects the crystal structure, grain size and shape of VO2 grown via the pulsed laser deposition technique on soda-lime glass substrate. Results on the surface morphology, the texturation is also presented. This study has shown that a-axis textured VO2 can be grown on glass owing at a substrate temperature of 600°C at an oxygen deposition pressure lower than 15 mTorr. And that the thermo-optical properties of the films are very sensitive to the crystal preferential orientation.

Acknowledgments

We are grateful for financial support from the, World Federation of Scientists, and also Thanks to the EMT-INRS, Canada, for the use of their facilities.

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Published with license by Science and Education Publishing, Copyright © 2017 NM Ndiaye, M Thiam, BD Ngom, O Sakho, M Chaker, N Manyala and AC Beye

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Normal Style
NM Ndiaye, M Thiam, BD Ngom, O Sakho, M Chaker, N Manyala, AC Beye. Effect of Oxygen Deposition Pressure on the Structure and the Metal Insulator Transition in Pulsed Laser Deposited VO2 Films on Soda Lime Glass. American Journal of Nanomaterials. Vol. 5, No. 2, 2017, pp 59-67. http://pubs.sciepub.com/ajn/5/2/3
MLA Style
Ndiaye, NM, et al. "Effect of Oxygen Deposition Pressure on the Structure and the Metal Insulator Transition in Pulsed Laser Deposited VO2 Films on Soda Lime Glass." American Journal of Nanomaterials 5.2 (2017): 59-67.
APA Style
Ndiaye, N. , Thiam, M. , Ngom, B. , Sakho, O. , Chaker, M. , Manyala, N. , & Beye, A. (2017). Effect of Oxygen Deposition Pressure on the Structure and the Metal Insulator Transition in Pulsed Laser Deposited VO2 Films on Soda Lime Glass. American Journal of Nanomaterials, 5(2), 59-67.
Chicago Style
Ndiaye, NM, M Thiam, BD Ngom, O Sakho, M Chaker, N Manyala, and AC Beye. "Effect of Oxygen Deposition Pressure on the Structure and the Metal Insulator Transition in Pulsed Laser Deposited VO2 Films on Soda Lime Glass." American Journal of Nanomaterials 5, no. 2 (2017): 59-67.
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  • Figure 1a. XRD patterns characteristic of VO2 thin films deposited at different oxygen pressures on soda-lime glass substrate and cooled down to room temperature at a rate of 50°C/min in vacuum
  • Figure 1d. Evolution of the crystallite size along the (100) and the crystallite size along the (0 1 1) planes respectively as a function of the deposition oxygen pressure
  • Figure 3a. Optical transmittance (%) hysteresis loop vs. temperature of VO2 thin films deposited on a soda-lime glass substrate at different deposition oxygen
  • Figure 3b. Evolution of the hysteresis and transition temperature characteristics of VO2 thin films deposited on a soda-lime at different deposition oxygen pressure
[1]  D. Adler, Mechanisms for Metal-Nonmental Transitions in Transition-Metal Oxides and Sulfides, Rev. Mod. Phys. 40 (4) (1968) 714.
In article      View Article
 
[2]  M. Maaza , K. Bouziane, J. Maritz, D. S. McLachlan, R. Swanepool, J. M. Frigerio, M. Every, Direct production of thermochromic VO2 thin film coatings by pulsed laser ablation, Optical Materials. Vol .15, Iss. 1 (2000) 41-45.
In article      View Article
 
[3]  A. Kaushal, N. Choudhary, N. Kaur, D. Kaur, VO2–WO3 nanocomposite thin films synthesized by pulsed laser deposition technique, Applied Surface Science. Vol.257, Iss. 21, (2011) 8937-8944.
In article      View Article
 
[4]  F. J. Morin, Physical Review Letters. Oxides Which Show a Metal-to-Insulator Transition at the Neel Temperature, 3 (1959) 34.
In article      View Article
 
[5]  J. B. Goodenough, The two components of the crystallographic transition in VO2, Journal of Solid State Chemistry. Vol.3, Iss.4 (1971) 490-500.
In article      View Article
 
[6]  T. W. Chiu, R. T. Hong, K. Tonooka, N. Kikuchi, Microstructure of orientation controlled VO2 thin films via ZnO buffer, Thin Solid Films. 529 (2013) 119-122.
In article      View Article
 
[7]  L. Zhao, L. Miao, S. Tanemura, J. Zhou, L. Chen, X. Xiao, G. Xu, A low cost preparation of VO2 thin films with improved thermochromic properties from a solution-based process, Thin Solid Films. 543 (2013) 157-161.
In article      View Article
 
[8]  C. H. Griffiths and H. K. Eastwood, Influence of stoichiometry on the metal‐semiconductor transition in vanadium dioxide, Journal of Applied Physics. Vol.45, Iss.5 (1974) 2201.
In article      View Article
 
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