The Fluorite Phase Transition in SnO2 under Uniaxial Compression

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The Fluorite Phase Transition in SnO2 under Uniaxial Compression and 500 K Tingting Ji, Yang Gao, Donghui Yue, Wenshu Shen, Yalan Yan, and Yonghao Han J. Phys. Chem. C, Just Accepted Manuscript • DOI: 10.1021/acs.jpcc.8b11846 • Publication Date (Web): 15 Jan 2019 Downloaded from http://pubs.acs.org on January 25, 2019

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The Journal of Physical Chemistry

The Fluorite Phase Transition in SnO2 under Uniaxial Compression and 500 K Tingting Ji,† Yang Gao,*‡ Donghui Yue,† Wenshu Shen,† Yalan Yan,† and Yonghao Han*†

†

State Key Laboratory of Superhard Materials, Physics Department, Jilin University,

Changchun 130012, China

‡

Department of Mechanical Engineering, Texas Tech University, Lubbock, Texas

79409, USA

AUTHOR INFORMATION Corresponding Author *To whom correspondence should be addressed. Yang Gao, E-mail: [email protected] Yonghao Han, E-mail: [email protected]

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ABSTRACT: The fluorite phase of SnO2 is discovered to demonstrate superior electrical conductivity compared to its rutile phase. Achieving SnO2’s fluorite phase at reduced pressure and intercepting it to ambient condition is of major significance. In this paper, we performed systematic investigations on SnO2’s phase transformations and physical properties under heating and non-hydrostatic compression using in-situ XRD and electrical measurements. Compared to previous XRD experiments (21 GPa, room temperature), it is discovered that cubic fluorite SnO2 can be achieved and retained to ambient condition at reduced pressure, 12.0 GPa, after heating to 500 K. The electrical measurements show that the fluorite phase of SnO2 has about 10 times higher conductivity than its rutile phase and can be quenched to ambient after the sample was heated to 500 K at 12.0 GPa.


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INTRODUCTION Abnormal and new physical properties as well as phases of materials have been observed under compression in the fields of earth, planetary and material sciences with the development of high-pressure science and technology.1-4 Unfortunately, plenty of these properties either arise at pressures too high for application or vanish as pressure is released.5-7 As a result, reducing the pressure requirements for materials’ highpressure phases, retaining them at ambient conditions and maintaining their remarkable properties at practicable conditions have become the top priorities for new materials’ preparation. Tin oxide (SnO2) is a typical semiconductor with wide band gap. It demonstrates both high conductivity and high transparency and thus has been widely exploited for application in solar cells, thermoelectric, photovoltaic and gas sensitive materials.8-12 To promote its application, efforts have been devoted in optimizing SnO2’s properties using both physical and chemical methods, such as grain size alteration and structural transformation induction as well as chemical doping.13-15 Pressure has been proved effective enhancing SnO2’s electrical properties by altering its interatomic spacing and electron configuration through lattice structure optimization.16 Extensive high-pressure investigations have been performed on SnO2. Haines et al. performed in situ XRD measurements on bulk SnO2 to 49 GPa (silicon oil as pressure transmitting medium) and discovered that bulk SnO2 (rutile-type) undergoes three structural phase transitions to CaCl2-type structure (orthorhombic) at 4.7 GPa, α-PbO23 ACS Paragon Plus Environment


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type structure (orthorhombic) at 12.6 GPa, and finally the fluorite-type structure (cubic) at 21 GPa.17 As pressure was released, a mixture of rutile-type and α-PbO2-type SnO2 was discovered in lack of fluorite-type SnO2.17 He et al. carried out in-situ XRD measurements on both bulk and nanocrystalline SnO2 to 40 GPa (methanol, ethanol and H2O mixture as pressure transmitting medium) and discovered that SnO2 transformed to fluorite-type structure at 23 and 29 GPa with bulk and nanocrystalline sample, respectively.18 Shieh et al. investigated the phase transition of bulk SnO2 by in situ XRD experiments using liquid Ar as the pressure medium. They found that the CaCl2type phase at 13.6 GPa and the cubic fluorite phase appeared at 28.8 GPa.19 Zhao et al. compressed 1-μm-diameter SnO2 nanowires to 34 GPa (with silicon oil as pressure transmitting medium) and discovered the formation of cubic fluorite SnO2 at 25GPa.20 As pressure was released, a mixture of rutile-type, α-PbO2-type and fluorite-type SnO2 was discovered in the sample at close-to-ambient condition.20 Furthermore, One et al. compressed SnO2 using multi-anvil press and discovered the formation of cubic fluorite SnO2 at 1100 K and significantly reduced pressure, 16.4 GPa.21 As the sample cooled to room temperature, the fluorite-type SnO2 was preserved to ambient condition. As demonstrated above, high temperature is essential reducing fluorite-type SnO2’s formation pressure and guaranteeing its preservation after quenching besides the grain size and non-hydrostatic status. In this paper, in-situ high-pressure XRD measurements on bulk SnO2 under nonhydrostatic condition were performed to 26.7 GPa. Pressure induced phase transitions 4 ACS Paragon Plus Environment

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were observed and the high-pressure phases were identified according to the reference. The samples were then heated to 500 K at different pressures and then quenched to ambient condition. Fluorite-type SnO2 was discovered in the sample heated to 500 K at 12.0 GPa, when pressure induced electrical conductivity was observed in simultaneously. It is discovered that the such enhanced conductivity was preserved under atmospheric pressure. EXPERIMENTAL METHODS

Figure 1. (a) Section view of the high-pressure high-temperature diamond anvil cell, (b) Schematic diagram of the parallel plate electrode.

The bulk SnO2 powder (99.996% purity) was purchased from Alfa Aesar Company. In the experiment, a special diamond anvil cell (DAC) set-up was introduced to satisfy pressure generation, sample heating and electrical resistance measurements at the same time, and to provide better thermal circumstance under compression. The detailed DAC set-up and sample loading schemes are shown in Figure 1. The DAC with a pair of 400 μm anvils was employed to generate high pressure. T301 steel wafer pressed to 63 μm in thickness was used as the gasket. A 300 μm hole was drilled in the center of the indentation. Al2O3 powder was put into the hole compressed solidly. A new hole with 5 ACS Paragon Plus Environment


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a diameter of 200 μm was then drilled at the center of the compressed Al2O3 as the sample chamber. Powdered sample and a small ruby ball were placed into the sample chamber and the pressure was gauged by the R1 ruby fluorescence method. Two K-type thermocouples were employed to calibrate the two anvils’ temperature.

Two mica

plates with 0.8-mm thickness were inserted in between the anvil seats and the DAC body to reduce heat flux from the furnaces to the DAC’s body during heating. The temperature of the sample was recorded when two thermocouples demonstrated the same reading. The electrical transport properties of the sample were measured using parallel plate electrodes. The metal molybdenum electrodes were fabricated on diamond anvils by magnetron sputtering and photolithography methods. The two resistance furnaces were respectively allocated on the two seats respectively. The details of electrode preparation have been illustrated in Ref 22. No pressure transmitting medium was introduced. The experiment was divided into four steps. In stage 1, in-situ angle dispersive XRD measurements of SnO2 were performed to 26.7 GPa at room temperature to map SnO2’s pressure-phase diagram under uniaxial compression. In stage 2, new samples were compressed to specific pressures, 6.3, 9.1, 12.0 and 15.6 GPa, respectively, and then heated to 500 K before quenching (cooling and depressurization). The quenched samples were subjected to XRD measurements for comparison with those acquired in stage 1. In stage 3, the electrical resistance measurements were performed on new sample up to 27.3 GPa (non-heated) to confirm the transport mechanism of SnO2 under 6 ACS Paragon Plus Environment

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high pressure. In stage 4, in-situ electrical resistivity under specific pressure (3.1, 6.3, 9.0, 12.0 GPa) after each operation (pressurization, heating and cooling, depressurization) were measured. All diffraction experiments were performed at BL15U1 beamline of Shanghai Synchrotron Radiation Facility and BL4W2 beamline of Beijing Synchrotron Radiation Facility, using angle-dispersive XRD mode (λ=0.6199 Å). CeO2 was used as standard material to do the calibration of instrument parameters. RESULTS AND DISCUSSION The initial diffraction pattern of SnO2 at room temperature corresponds to the rutiletype (P42/mnm) SnO2 (Figure 2). Width broadening and position shift of diffraction peaks were observed with elevated pressure. At 18.2 GPa, one new peak emerged between the (110) and (101) peaks of the rutile phase and indicated the initiation of a 1st order phase transformation. The intensity of the rutile-phase peaks decreased while that of the new phase increased with further pressurization to 26.7 GPa. As pressure was released, the high-pressure phase was preserved till ambient condition. The highpressure phase was assigned to SnO2’s cubic fluorite (𝑃𝑎3̅) phase according to the reference.18 The reduced onset pressure was ascribed to the non-hydrostatic effects induced by uniaxial compression. The preservation of the high-pressure phase indicates that the fluorite phase of SnO2 acquired under uniaxial compression remains stable at ambient condition. Yet the previously reported splitting of SnO2’s (211) peak at around 12.0 GPa16 had not been observed in this experiment, indicating that the CaCl2 phase 7 ACS Paragon Plus Environment


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of SnO2 did not arise under uniaxial compression. Furthermore, fluorite SnO2 was discovered at reduced pressures, 12.0 and 15.6 GPa, in heated samples (Figure 2) and preserved to ambient conditions. These results and some earlier reports21, 23 show that the non-hydrostatic effect and heating play a decisive role in initiating and accelerating this rutile to fluorite phase transformation of SnO2 at reduced pressures and preserving the fluorite phase to ambient condition. He et al. found the onset pressure of rutile to cubic fluorite structure phase transition increased with the decrease of nanoscale.18 In our study, due to the sample is bulk and in a non-hydrostatic compression, the cubic fluorite phase appears at 18.2 GPa, which is earlier than that of nano SnO2. The onset phase transition pressure of SnO2 here is different from the both in Ref. 17 and 18, which is due to the inhomogeneity of nonhydrostatic effects.

Figure 2. Selected XRD patterns of SnO2. The numbers represent the corresponding pressures in GPa at which the pattern is acquired. 8 ACS Paragon Plus Environment

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In-situ alternate current impedance spectroscopy measurements were performed to investigate the behavior of internal carriers in SnO2 under uniaxial compression (Figure 3) at room temperature. The impedance spectra of SnO2 consisted of only one single semi-circular response that corresponded to the grain’s contribution. No obvious contribution from the grain boundary was observed at ambient condition. With pressure elevation, the semi-circle became smaller with no evident change in shape. This indicates that the electrical transport mechanism of SnO2 remained unchanged under uniaxial compression. Furthermore, a two-stage resistance-pressure variation curve was observed. A positive linear correlation between the pressure and the sample’s resistance was observed below 19.5 GPa. Such correlation was ascribed to the reduced barriers and improved connectivity between sample’s grains under uniaxial compression.15 At pressures above 19.5 GPa, an evident slope change was observed indicating a 1st order phase transformation as the carriers’ behavior was extremely sensitive to lattice structure variation.24,25 In this case, SnO2’s rutile-fluorite phase transformation was believed to be responsible.

Figure 3. (a) SnO2’s Real Z′ verses imaginary Z″ components of impedance under various pressures at room temperature, (b) SnO2’s resistance dependency on pressure. 9 ACS Paragon Plus Environment


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The resistivity of SnO2 was then systematically measured at different pressures, ambient to 12.0 GPa, and different temperatures, 300 to 500 K (Figure 4a). Under ambient pressure, the resistivity of SnO2 demonstrated a negative correlation with temperature and remained close to its original value after a heating-cooling cycle. Similar negative correlations with temperature and pressure was observed (Figure 4b, 4c), yet on the contrary the ending value of SnO2’s resistivity was decreased by one order of magnitude after cooling under compression. Samples still maintain the semiconductor properties. These results revealed that pressure is more essential in regulating SnO2’s resistivity within the measurement condition range. The temperature dependence of SnO2’s resistivity under variated pressures was demonstrated in Figure 4d in form of Arrhenius plots. As an n-type semiconductor, the activation energy (Et) of SnO2 corresponded to the donor energy level activation energy, whose relationship with the resistivity was expressed by Arrhenius formula: ρ=ρ0 exp(Et /2kBT), (Ref 26) where T is the temperature, kB is the Boltzmann constant and ρ0 is the pre-exponential factor. (please refer to the supporting information for the specific fitting data). The correlation was discovered between Et and pressure is negative. The resistivity decreased with increasing temperature indicates the energy barrier is reduced under compression and the conductivity during heating is enhanced. The donor level in the band gap of SnO2 was also revealed according to Et at variable temperatures, for which the ionized defects such as oxygen vacancies were believed to be responsible.27 10 ACS Paragon Plus Environment

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Figure 4. (a) Resistivity of SnO2 in a heating-cooling cycle at ambient pressure. (b) The pressure dependence of SnO2’s resistivity during heating. (c) The pressure dependence of SnO2’s resistivity during cooling. (d) Arrhenius plot of the temperature dependence of SnO2’s resistivity under different pressures.

In-situ resistivity measurements were performed after each heating cycle to monitor SnO2’s resistivity variation during depressurization (Figure 5). In the cases with lower pressurization results (3.1, 6.3 and 9.0 GPa), the resistivity didn’t return to its exact initial values after processing but remained close to those before pressurization and heating, indicating that the resistivity variation of SnO2 was partially reversible with pressure and temperature. However, in the case of 12.0 GPa, the resistivity was significantly reduced and remained almost constant as pressure was released, indicating an irreversible transformation had occurred. Compared with the impedance spectra in Figure 3, such irreversible change in resistivity was ascribed to SnO2’s rutile to fluorite phase transformation.



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Figure 5. The resistivity’s dependency on pressure during depressurization from variated pressures.

Due to the relatively higher symmetry, the lattice vibration in fluorite SnO2 demonstrated better coordination and subdued internal damping phenomenon than those in rutile phase, which resulted in weakened phonon scattering and enhanced carrier mobility and therefore increased conductivity. As shown in our measurements, the electrical conductivity of fluorite SnO2 was one magnitude higher than that of rutile phase. The coordination number of Sn4+ was increased from 6 to 8 while the packing density of oxygen network was increased simultaneously as the transformation occurred. A more difficult situation for Sn4+’s migration through the crystalline structure was created after the transformation.28 At room temperature this phase transition kinetics process was slow,29 there was no sufficient energy to overcome the kinetic barrier to 12 ACS Paragon Plus Environment

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order cations inside a close oxygen network. Our experimental results show that the combined non-hydrostatic pressure and heating can realized the transition from rutile phase to cubic fluorite phase at 12.0 GPa, 500 K, and the fluorite phase can remain to ambient. According to our experiment investigation, one thing should be noticed. Haines et al. carried out DAC high pressure experiment on bulk SnO2.17 The laser heating was utilized for accelerating the dynamic process and reducing the stress during the phase transition, the fluorite structure was found not being retained in the sample when released to ambient condition. Fast sample cooling accompanied by laser heating method may be a factor of not remaining the fluorite structure to ambient. Liu et al. also conducted a laser heating experiment and found the fluorite structure of SnO2 at 25 GPa.24 But in quenched sample the cube fluorite phase was not remained. One et al. carried out high temperature and high pressure study on SnO2 by multi anvils equipment. In their experiment, the sample cooling was conducted by cutting off the electric power supply.21 Finally, the fluorite structure was not retained too. Compared to above mentioned reports, in our experiment, the sample was heated and cooled slowly and got the high-pressure fluorite structure SnO2 after temperature and pressure dropping down to ambient. Slowly heating and cooling made in our work may the possible formation of new types of interfaces, which interfaces act as high energy barriers to block the back transformation pathway, allowing an effective harvest of high



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pressure metastable phases under ambient conditions.30,31 Slowly heating and cooling may be, we believe, an important factor for getting the different results. CONCLUSIONS In conclusion, bulk SnO2 was subjected to in-situ XRD and resistivity measurements under high pressure (up to 26.7 GPa) and high temperature (up to 500 K). An irreversible phase transformation from rutile SnO2 to its fluorite phase was discovered at a significantly reduced pressure 12.0 GPa (compared to 18.2 GPa under uniaxial compression without heating) and 500 K. In-situ impedance measurement shows that the electrical resistivity value of fluorite phase is about 10 times higher than that of the rutile phase and can be quenched to ambient after the sample was compressed and heated to 12.0 GPa and 500 K, respectively. Uniaxial compression combined with evenly heating and cooling was proved essential preserving SnO2’s fluorite phase to ambient condition. These results provide a valuable approach to capture a pressure induced phase with better physical property for new applications. ASSOCIATED CONTENT

Supporting Information. Pressure dependence of activation energy.

AUTHOR INFORMATION

*To whom correspondence should be addressed. Yang Gao, E-mail: [email protected]


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Yonghao Han, E-mail: [email protected] Tel: +86-(0)431-516-8878-601 Notes The authors declare no competing financial interests.

ACKNOWLEDGMENT

This work is supported by the National Natural Science Foundation of China (Grant Nos. 11674404, 11774126) and Program for Chang Jiang Scholars and Innovative Research Team in University (No. IRT_15R23). Angle-dispersive XRD measurement was performed at the BL15U1 beamline, Shanghai Synchrotron Radiation Facility (SSRF) and the BL4W2 beamline, Beijing Synchrotron Radiation Facility (BSRF).

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The Fluorite Phase Transition in SnO2 under Uniaxial Compression

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