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Ultrastable Amorphous SbSe Film Kai Zhang, Yang Li, Quan Huang, Bihan Wang, Xuerong Zheng, Yang Ren, and Wenge Yang J. Phys. Chem. B, Just Accepted Manuscript • DOI: 10.1021/acs.jpcb.7b03408 • Publication Date (Web): 09 Aug 2017 Downloaded from http://pubs.acs.org on August 10, 2017

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The Journal of Physical Chemistry

Ultrastable Amorphous Sb2Se3 Film Kai Zhang1, Yang Li2, Quan Huang1, Bihan Wang, Xuerong Zheng3, Yang Ren4, Wenge Yang1,5,* 1

Center for High Pressure Science and Technology Advanced Research (HPSTAR), Shanghai 201203, China 2

Wuhan National Laboratory for Optoelectronics and School of Optical and Electronic

Information, Huazhong University of Science and Technology (HUST), Wuhan 430074, China 3

School of Materials Science and Engineering, Key Laboratory of Advanced Ceramics and

Machining Technology of Ministry of Education, Tianjin University, Tianjin 300072, China 4

X-Ray Science Division, Advanced Photon Source, Argonne National Laboratory, Argonne, IL 60439, USA

5

High Pressure Synergetic Consortium (HPSynC), Geophysical Laboratory, Carnegie Institution of Washington, Argonne, IL 60439, USA

ACS Paragon Plus Environment


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Abstract Increasing the thermostability of amorphous materials has been a long journey to improve their properties. The metastable nature of chalcogenide glasses limits their practical applications as an amorphous semiconductor in photovoltaic performance. Here, we report the formation and physical properties of ultrastable amorphous Sb2Se3 with an enhanced thermal stability compared to ordinary amorphous Sb2Se3 (∆Tx= 17 K). By in situ high temperature-high energy synchrotron X-ray diffraction, the difference in structure relaxation between ordinary and ultrastable amorphous Sb2Se3 was manifested by local structure evolution. Ultrastable amorphous Sb2Se3 showed the smallest surface roughness and highest refractive index, the mechanism behind was further discussed in terms of fast molecular mobility and molecular orientation during vapor deposition. Formation of ultrastable amorphous Sb2Se3 demonstrated a promising avenue to obtain novel functional amorphous semiconductor with modulated structure and property.


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INTRODUCTION Glass has its unique mechanical, optical, chemical, magnetic properties comparing to crystalline solids1-4. As glass is in its thermodynamic metastable state, it will transform to crystalline phase above the glass transition temperature (Tg). The most common method for preparing a glass is to quench the material from its high temperature liquid state quickly5. Thus, glass can be deemed as a frozen liquid, which locates at any metastable state in the potential energy landscape (PEL) depending on thermal history condition and cooling rate6. With aids of suitable temperature and/or pressure conditions, it may relax towards more stable state7 or even transform to crystalline counterpart8. In consequence, pursuing the lower energy state of glass is important to enhance the thermal stability in practical applications9-11. The most widely-used method is annealing the glass at the temperature of slightly lower than Tg to access into the relative stable state9. However, much closer to the thermodynamic equilibrium state, much more time it takes in the annealing process. Recent study indicated that if reaching 70% reduction of the β relaxation intensity by annealing an ordinary glass, it may take ~3500 years7. Fortunately, it has been reported that an ultrastable glass can be prepared by physical vapor deposition (PVD) method10, 12-17. A relative lower deposition rate and suitable substrate temperature (Tsub ≈ 0.85Tg) in PVD deposition can be helpful for obtaining ultrastable glass18. The mechanism leading to this exceptional stability was ascribed to the fast mobility of atoms at the surface of glass during deposition, in which atom can readily self-regulate configuration to reach a lower energy state before buried by the next arriving atoms. Therefore, ultrastable glass shows higher packing density, lower thermal capacity, higher modulus and distinct surface-initiated transformation mechanism and so on. Using PVD method, glasses with more diverse structures and properties can be achieved without any post-treatment19-20. Such highly stable glass provides a reliable model to access into the long-sought “ideal glass” to investigate the fundamental scientific questions in glass formation and property. Up to now, much work has been done about the stability and structure of the ultrastable organic glass and metallic glass, and quite different ultrastable behaviors between them were found13-14. In polymer glass and Zr-based metallic glass, it is considered that the high kinetic stability is due to the high-thermodynamics-energy state; but in ultrastable molecular glass, the ultrastability is reported to connect with a low-thermodynamic-energy state10, 12, 21. So, it is not clear on the relationship between the thermodynamics energy state and the kinetic ultrastable state. As an important branch of glass, the ultrastable chalcogenide glass has yet to be found. Spontaneously, whether the ultrastable chalcogenide glass can be prepared by PVD? How about its stability and some related physical properties? In this work, we choose the amorphous Sb2Se3 as a model to investigate the ultrastability in the chalcogenide glass. It is worth noting that crystalline Sb2Se3 is a novel non-cubic photoelectric material with an optimal solar bandgap of 1.1 eV, non-toxic and low-cost, which has received much attentions in the field of photovoltaic2. The obtained Sb2Se3 glass showed



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extraordinary thermal stability with enhanced crystallization temperature, remarkable low surface roughness and high refractive index. The structure relaxation difference between ordinary glass and ultrastable glass was probed by in situ high energy X-ray diffraction. EXPERIMENTAL METHODS A series of Sb2Se3 films from amorphous to crystalline at different substrate temperatures were prepared by using thermal evaporation method. The substrate temperature was the only variable for all depositions. The pristine Sb2Se3 bulk sample was heated to evaporate onto an oxide glass substrate with a constant deposition rate of 5 Å/s. The film thickness was about 500 nm checked by a scanning electron microscopy (SEM). The morphology and structure of film was characterized by SEM, transmission electron microscopy (TEM) and X-ray diffraction (XRD). The chemical composition of the film was ascertained by energy dispersive spectrometer (EDS) equipped with the SEM. The thermodynamic properties of as-prepared Sb2Se3 glass were measured by using NETZSCH differential scanning calorimetry (DSC) 200F3. The heating rate was 20 K/min under high-purity N2 gas protection. The amorphous sample was scraped from the substrate and compacted into powder for DSC measurement with a mass of about 15 mg. All samples were confirmed to be pure without containing any impurity from substrate by SEM-EDS analysis. The refractive index of amorphous Sb2Se3 was tested by using ellipsometry (J.A. WOOLLAM Co. Inc) with the wavelength range from 280 to 2500 nm. The refractive index was obtained by analyzing the phase difference and amplitude ratio between the incident and reflected polarized light, utilizing the Tauc-Lorentz model that was a widely used model for the amorphous semiconductor. In situ high energy X-ray diffraction (λ = 0.1174 Å) at 11-ID-C station at the Advanced Photon Source of Argonne National Laboratory was performed from room temperature up to 573 K with a Linkam heating system, with acquisition time 20 s, heating rate 4 K/min between 298 K and 443 K, 1 K/min between 443 K and 523 K, and 4 K/min between 523 K and 573 K. These three temperature ranges correspond to the amorphous state, crystallization process, and crystalline state, respectively. RESULTS AND DISCUSSION Figure 1a shows the SEM image of the amorphous Sb2Se3 film prepared at room temperature (ordinary sample). A granular morphology with the particle size of about dozens of nanometers is observed that are typical characteristics of films obtained through PVD. As shown in the inset of Figure 1a, an explicit TEM image further confirms the benign amorphous structure without any indication of crystallinity. Figure 1b represents several typical XRD curves measured by Cu Kα X-ray diffractometer. With the substrate temperature between room temperature and 413 K, we can obtain amorphous films. When the substrate kept at 433 K, some sharp diffraction peaks were present that confirmed the crystalline nature of Sb2Se3 film.


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Figure 1 Characterization of the as-deposited samples. (a) SEM image of amorphous Sb2Se3 film prepared at room temperature. Inset: the TEM selected-area electron diffraction pattern indicating a pure amorphous phase; (b) Several representative XRD profiles of amorphous and crystalline films obtained with different substrate temperatures. Figure 2a displayed the DSC heat flow curves for deposited amorphous and crystalline Sb2Se3. As shown in Figure 2a, the distinct exothermic crystalline peak (Tx) can be seen clearly, however, we cannot find the glass transition peak (Tg). The absence of Tg has also been reported in amorphous Ge2Sb2Te522, Al-based23-24, and Ce-based metallic glass8, amorphous Cu50Zr50 film25, which is believed to be the small temperature difference between Tg and Tx due to very similar structural rearrangement scale during glass transition and crystallization. Therefore, Tg was easily obscured by the strong Tx during DSC scanning. Considering the indiscernible Tg during heating, we adopt the onset temperature of crystallization (Tx) to evaluate the thermal stability of amorphous Sb2Se3 as used in References24-25. From Figure 2b, Tx is very sensitive to the substrate temperature (Tsub). Tx shows the highest value (469 K) when the Tsub is at 373 K, i.e., the highest thermal stable film can be formed with substrate temperature at 373 K. This implies that ultrastable amorphous Sb2Se3 can be obtained by optimizing the substrate temperature. The ordinary amorphous Sb2Se3 showed the onset temperature of crystallization, Tx = 452 K. Therefore, there is an enhanced onset temperature of crystallization for ultrastable amorphous Sb2Se3 with respect to ordinary amorphous Sb2Se3, ∆Tx = Tx, ultrastable – Tx, ordinary = 17 K. The remarkably enhanced Tx can be considered as direct evidence of the high thermal stability25. During deposition, much enthalpy is frozen in amorphous film due to equivalent high cooling rate for vapor deposition. Therefore, a prominent enthalpy release can be observed on DSC curve during upscan, as the black arrow shown in the inset of Figure 2c. The corresponding onset temperature of enthalpy release was termed as Tr. With increasing substrate temperature, Tr gradually increased to a



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highest value and then decreased, as shown in Figure 2c. The difference between Tr and Tx reaches the lowest value (25 K) as shown in Figure 2d, which implies the frozen enthalpy reaches minimum in ultrastable amorphous Sb2Se3.

Figure 2 Thermal stability of vapor-deposited Sb2Se3 as indicated by the onset temperature of crystallization from DSC: (a) Heat flow curves of amorphous Sb2Se3 prepared at different substrate temperatures (b) Onset temperature of crystallization Tx plotted as a function of Tsub, the dash line is a guide to the eye for showing the change trend of temperature. (c) Onset temperature of enthalpy release Tr plotted as a function of Tsub, inset: heat flow curves for ordinary and ultrastable amorphous Sb2Se3, the black arrow showing the onset temperature of enthalpy release, i.e., Tr, (d) The temperature difference between Tr and Tx. As a photovoltaic material, the surface roughness is an important microstructural parameter for its performance. We have conducted the surface roughness measurements on different amorphous films using the atomic force microscopy (AFM). Two typical AFM pictures corresponding to ordinary amorphous Sb2Se3 (298K), ultrastable-amorphous Sb2Se3 (373 K) are shown in Figure 3a. For the ordinary amorphous Sb2Se3, a large amount of island particles was uniformly distributed on surface with a size of dozens of nanometers. For ultrastable amorphous Sb2Se3, a smooth surface morphology can be seen with the lowest surface roughness of 3.05 Å (Figure 3b) that was close to the threshold value of AFM measurement (1 Å), which is consistent with atomic scale smooth surface (1.18 Å) in ultrastable CuZr metallic glass25. Figure 3b summarizes the RMS surface roughness for all films measured. Clearly, the ultrastable amorphous Sb2Se3 has the smallest surface roughness among the deposited films. During deposition, fast-moving molecules formed more regular packing, which reduced the dangling bonds that readily results in


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unstable state of molecule. Thus, the efficient combination between molecules in the ultrastable amorphous Sb2Se3 finally produced the lowest surface roughness. By varying the substrate temperature, one can obtain ultrastable film with smooth surface that could be of technological interest for such as solar cell device fabrication with enhancing interface cohesion with electrode. Sb2Se3 has been considered as a promising photovoltaic absorber because of the optimal solar bandgap2. Here, we compared the optical properties of Sb2Se3 films by ellipsometer from 280 to 2500 nm from which the refractive index n of film can be extracted as shown in Figure 3c. In the whole wavelength range, n showed a similar value for different amorphous films, which may originate from a very subtle structure difference. By a careful analysis on the maximum refractive index nmax, we found that with increasing substrate temperature nmax shows a consistent change with the mentioned above thermal ability as shown in Figure 3d, i.e., the highest nmax corresponding to the ultrastable amorphous state. For the vapor deposited ultrastable molecule glass, an important feature is the molecule orientation and the resulting higher density of glass19, 26-30. During deposition process, these small molecules can adjust the configuration to satisfy the lowest energy state. Chalcogenide amorphous Sb2Se3 contains fundamental structure unit connected by strong covalent bonds. Thus, to some extent there exists certain ordered molecule orientation in ultrastable amorphous Sb2Se3 to minimize the free volume, which resulted in increased density. The refractive index of glass is closely related to its density13, 31. Therefore, it is reasonable for ultrastable amorphous Sb2Se3 showing the highest refractive index.

Figure 3 Surface morphology and optical properties of Sb2Se3 films. (a) Atomic Force Microscopy of surface morphology of Sb2Se3 films prepared at two typical temperature 298 K, 373 K. (b) Surface roughness plotted as a function of substrate temperature, the dashed line is for eye-guidance. (c) Refractive index of different



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films (d) nmax plotted as a function of substrate temperature. Even though the extraordinary stability and diverse physical properties of ultrastable glass, the structure origin behind remains unknown because the delicate structure difference for the different nonequilibrium glassy states were difficult to distinguish. Here, we utilized high-energy synchrotron X-ray diffraction to reveal the structure relaxation behavior of ordinary and ultrastable amorphous Sb2Se3 during in situ heating and further understand the correlation between structure and optical property. The large q range up to 28 Å-1 can be achieved using high energy XRD located at 11ID-C station, Advanced Photon Source, Argonne National Laboratory. Figure 4 shows high energy XRD patterns for ordinary and ultrastable amorphous Sb2Se3 during in situ heating from room temperature to crystallization temperature.

Figure 4 In situ high energy synchrotron X-ray diffraction patterns for (a) Ordinary amorphous Sb2Se3 and (b) Ultrastable amorphous Sb2Se3. An iterative optimization method32 was used to get the structure factor S(q) and the pair distribution function g(r) from the pristine intensity data. Figure 5a, b show some representative results of S(q) with temperature interval of about 10 K, for ordinary and ultrastable amorphous Sb2Se3, respectively. To detect the subtle structural changes during in situ heating, the difference curve, ∆S(q), for each temperature was obtained by subtracting the S(q) at T = 304.6 K (initial temperature of in situ heating), as shown in Figure 5c, d, respectively. For ordinary amorphous Sb2Se3, abrupt structural changes occurred around 357.3 K that is evidenced by appearances of new peaks in the ∆S(q) curve (red arrow shown in Figure 5c). The structural transition temperature showed high consistency with the onset temperature of enthalpy release. This indicates that the structural change occurs when relaxation initiates in the ordinary


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amorphous Sb2Se3. In contrast, no distinct structural change can be found in the ultrastable amorphous Sb2Se3 during annealing.

Figure 5 In situ X-ray diffraction data, structure factor for (a) Ordinary amorphous Sb2Se3 (b) Ultrastable amorphous Sb2Se3, (c, d) are the respective difference plots, ∆S(q), obtained by substracting the diffraction pattern at T = 304.6 K. To see the real-space structure insight at atomic level, the pair distribution functions, g(r), were obtained by Fourier transformation of S(q). By the deliberative data processing, we extract the position of the first peak of g(r), r1, and the coordination number for the nearest neighbor atoms, CN, shown in Figure 6. As shown in Figure 6a, a subtle transition point at around 350 K obtained from the change trend in r1 of ordinary amorphous Sb2Se3 can be found, which is consistent with the onset temperature of enthalpy release in the corresponding DSC curve as indicated by the black arrow in inset of Figure 2c. This indicated that structure relaxation in ordinary amorphous Sb2Se3 occurred in short-range order scale associated with local atomic rearrangement. Further, the evolution behavior of CN also indicated an enhancement when the relaxation is activated, as shown in Figure 6c. It indicated that the structure transition from loose packing to dense packing occurred in ordinary amorphous Sb2Se3, which is consistent with local structure evolution behaviors in Au-based metallic glass at the onset temperature of relaxation33. In contrast, a monotonous change in r1 and CN of ultrastable amorphous Sb2Se3 was demonstrated as indicated in Figure 6 b, d. It has been suggested that atomic rearrangement in metallic glass during relaxation occurs in higher free volume region34 and originates from short-range collective rearrangements of large solvent atoms35. Chalcogenide glass has open network structure that easily forms more free volume/cavity. Therefore, the transition point of r1 and CN is mainly due to densification process along with the



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annihilation of free volume. For ultrastable amorphous Sb2Se3, the dense structure packing has already formed during deposition with minimum free volume, a featureless change was shown during annealing. This also clearly manifested higher structure stability in ultrastable amorphous Sb2Se3 compared to the ordinary amorphous Sb2Se3 during annealing relaxation.

Figure 6 Local structural evolution during in situ heating, position of the first peak, r1, of g(r) for (a) Ordinary amorphous Sb2Se3 and (b) Ultrastable amorphous Sb2Se3, respectively, (c, d) are the respective coordination number, CN. Meanwhile, noting that the coordination number of ultrastable amorphous Sb2Se3 is distinctly smaller than that of ordinary amorphous Sb2Se3 shown in Figure 6c, d. To date, there is no report on the coordination number of ultrastable glass. Our results imply that the ultrastable glass is not always simultaneously coupled with the occurrence of the densest atomic packing because the densest atomic packing is not always corresponding to the most stable glass state. Especially for chalcogenide glass, a large amount of inter- and intra-molecule interactions may result in strong repulsive force for the densest molecule packing. Amorphous Sb2Se3 displayed the similar short range order of crystalline counterpart, consisting of one-dimensional ribboned crystal structure. Tang et al, has found a preferred oriented Sb2Se3 ribbon vertically on the substrate in the crystalline Sb2Se3 when deposited at the substrate temperature of 573 K2. Enhanced molecule orientation have also been verified in ultrastable organic glasses19, 26, the longer the molecule length is, the larger the anisotropic of the orientation becomes27. Thus, it can be speculated that there is an enhanced molecule orientation at short-range order scale within ultrastable amorphous Sb2Se3, which further resulted in a lower CN. Ultrastable glass may be related to a special hidden topological network structure associated with enhanced molecule orientation36-37.


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Therefore, our method provides a promising route to tune the optical property in chalcogenide amorphous semiconductor that has been widely applied in optical fiber and photovoltaic fields. In summary, ultrastable amorphous Sb2Se3 was obtained with physical vapor deposition method by optimizing the substrate temperature. The amorphous Sb2Se3 film prepared at 373 K shows the highest crystallization temperature and minimum temperature gap between Tr and Tx. In situ high energy synchrotron X-ray diffraction revealed the local structure difference between ordinary and ultrastable amorphous Sb2Se3 during relaxation, i.e., a distinct atomic rearrangement at the onset temperature of relaxation in ordinary glass, in contrast, a monotonous structure change was shown in ultrastable glass. Ultrastable glass shows high quality amorphous films with the lowest surface roughness and the highest refractive index, which provides a promising route to tune the structure and property of amorphous semiconductor by changing the substrate temperature.

AUTHOR INFORMATION Corresponding Author * E-mail: [email protected] Notes: the authors declare no competing financial interest. ACKNOWLEDGMENTS This work was supported by the National Nature Science Foundation of China under Grants No. U1530402 and 51527801 and China Postdoctoral Science Foundation (Grant No. 2016M600909). REFERENCES 1. Wang, G.; Zhao, D. Q.; Bai, H. Y.; Pan, M. X.; Xia, A. L.; Han, B. S.; Xi, X. K.; Wu, Y.; Wang, W. H. Nanoscale Periodic Morphologies on the Fracture Surface of Brittle Metallic Glasses. Phys. Rev. Lett. 2007, 98 (23), 235501. 2. Zhou, Y.; Wang, L.; Chen, S.; Qin, S.; Liu, X.; Chen, J.; Xue, D.-J.; Luo, M.; Cao, Y.; Cheng, Y.; Sargent, E. H.; Tang, J. Thin-film Sb2Se3 Photovoltaics with Oriented One-dimensional Ribbons and Benign Grain Boundaries. Nat.

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Ultrastable Amorphous Sb2Se3 Film - The Journal of Physical

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