Fabrication, characterization and the effects of femtosecond laser ablation on Te–As–Se glasses

https://doi.org/10.1016/j.jnoncrysol.2019.119755Get rights and content

Highlights

  • Thermal and basic properties of Te–As–Se glasses were collected systematically.

  • Damage thresholds of Te–As–Se glasses was determined.

  • Femtosecond laser irradiation on the structural evolutions was studied.

Abstract

Te–As–Se (TAS) chalcogenide (ChG) glasses have broad transmission range of up to 18 μm and are suitable candidates for mid-infrared (MIR) applications. In this work, TAS glasses were synthesized via melt-quenching technique. Glass-forming domain was determined by X-ray diffraction (XRD) and differential scanning calorimeter (DSC). Optical properties and structural information were recorded. A series of glasses with compositions of TexAs40Se60-x (x == 0, 10, 20, 30, 40, 50, in mol%) was irradiated by 3 μm femtosecond (fs) laser with different powers. The morphology and structural information after laser ablation were then studied via scanning electron microscopy (SEM) and Raman technique. The laser damage threshold decreased from 29.45 mJ/cm2 to 21.93 mJ/cm2 with the increase in Te contents in the TexAs40Se60-x glasses. This study is of great importance in supercontinuum (SC) generation and infrared laser transmission based on TAS fibers in the MIR range.

Introduction

Among numerous ChG glasses, TAS glasses have been well studied for their excellent properties, such as good thermal stability for drawing fibers and optical properties [1], [2], [3], [4], [5]. In particular, the ultra-wide transmission spectra in the 2–18 μm bands can detect fingerprint region of molecules [6], [7], [8]. In 1981, Borisova et al. first reported the glass-forming domain of TAS glasses [9]. Ligero et al. discussed the crystallization kinetics of partial compositions of TAS glasses and the glass-forming ability [10]. Shiryaev et al. researched the crystallization kinetic parameters of the TexAs40Se60-x glasses (x = =0–40, in mol%) [11]. Jóvária et al. reported the atomic structure and bonding law of Te20As30Se50 glass [12]. Delaizir et al. investigated the relationship between the structures and compositions of TexAs30Se70-x (x = =0–30, in mol%) and Te2As3-xSex (x = =0–2.5, in mol%) glasses [13]. However, the above-mentioned TAS glass-forming domain is not well defined. Moreover, the performance parameters of TAS glasses are scarce and incomplete. Thus, the glass-forming ability and the corresponding thermal and optical properties of TAS glasses should be studied further.

Over the past two decades, the interaction of ultra-short and ultra-high peak power fs lasers with transparent materials has incited great interest among researchers [14]. As superior matrix materials for infrared photonic devices, ChG glasses are frequently interacted with ultrashort-pulsed lasers [15,16]. In terms of MIR applications, the SC generation of MIR needs fs lasers to pump ChG glass fibers [17]. Especially, ChG fibers usually undergo catastrophic damage while exposed to high intensity laser beams [18]. Therefore, the mechanism of interaction between fs lasers and GhG glasses should be studied investigated in detail. Usually, photoionization and avalanche ionization processes play an important role in the damage process of optical transparent materials by fs lasers. Besides, nonlinear self-focusing effect, linear heat accumulation effect, impurity and surface defect absorption, and multi-pulse ionization effect can all effect ChG glasses due to their high refractive index, low thermal conductivity, and large thermal expansion [19,20]. The dominant mechanism of fs laser-induced damage for optical materials is electronic damage, that is, high-energy electrons in the conduction bands increase rapidly in a short time due to photoelectric effect. Damage occurs when the electron concentration exceeds the affordable value of the material [18].

The fs laser damage with ChG glass in the near infrared band, which can be applied in laser micro-nano processing, have been widely studied. Messaddeq et al. first reported the laser-induced (1 kHz, 34 fs, 806 nm) periodic nanoscale structure in Ge-S-based ChG glass that can yield a calculated damage threshold of 0.12 J/cm2 when the number of pulses was 50 and can be utilized in the preparation of micro-nano gratings [21]. Romanova et al. measured the nonlinear optical coefficients after fs laser (20 Hz, 40 fs, 790 nm) interacted with As–S–Se glasses, established an ultrafast laser heating model for ChG glasses, and analyzed the damage mechanism [20]. Zhang et al. systematically studied the dominant factor of Ge–Sb–S glasses damage mechanism with different repetition frequencies by fs laser (1–1000 kHz, 216 fs, 1060 nm). The damage was mainly caused by avalanche ionization at 1 kHz, whereas thermal accumulation is a major factor at over 10 kHz [16]. In addition, optical devices based on ChG glasses are usually applied in the MIR region due to their excellent transmission characteristics. Hence, the laser damage of ChG glasses in the MIR region has received much attention in recent years. Zhang et al. investigated the damage threshold of Ge–As–S glasses after fs laser irradiation (1 kHz, 150 fs, 3 μm), Ge introduction greatly improved the laser damage resistance [22]. Xie et al. studied the effect of water peak on the ablation threshold of Ge–Sb–Se glasses (1 kHz, 150 fs, 2.86/4 μm) and found the decisive role of multi-photon ionization on the damage threshold of glass samples [23]. However, the effects of chemical compositions and glass structures on the fs laser ablation properties of ChG glasses are rarely reported.

In this work, TAS glasses were selected and prepared via melt-quenching method. The thermal, physical, and optical properties were systematically studied. Moreover, the TAS glass-forming domain was re-determined and divided into three regions according to thermal stability to determine the appropriate TAS compositions for fiber drawing. Furthermore, a series of stoichiometric TexAs40Se60-x glasses (x = =0–50, in mol%) glasses was studied in terms of fs laser ablation property at 3 μm with different powers. We analyzed the formation of damage, the change of Raman structure before and after damage, and the influence of the addition of Te on the damage resistance of TAS glasses. This study aims to provide scientific guide for the pumping scheme designs of TAS fibers.

Section snippets

Experiment

TexAsySez (x + +y + +z = =100, in mol%) glass was prepared using a conventional melt-quenching method. These glasses were labeled as TASabc (a, b, and c represent the coefficients of Te, As, and Se in the glass compositions, where a = =x/10, b = =y/10, and c = =z/10). The raw materials (Te, As, and Se) with 5 N purity were weighed and loaded into quartz ampoule (Φ=10 mm). The ampoule was sealed until it was vacuumed to ~10−5 Pa and subsequently placed into a rocking furnace. After melting and

Physical properties of glass samples

Two criteria were adopted to determine the glassy state and identify the glass-forming domain. First, naked-eye inspection was employed to examine the total or partial crystallized glasses, which usually involve phase separation or total crystallization. Second, the DSC and XRD patterns were evaluated to confirm the amorphous state. We prepared 51 samples, including 33 glassy, 11 partially glassy, and seven completely crystallization. Moreover, the glass-forming domain of TAS glasses was

Conclusions

In summary, the glass-forming domain of TAS glasses was re-determined and divided into three regions according to the XRD and DSC results. Region C (ΔT = =TcTg ≥ 150°C) shows the excellent thermal stability and is well suitable for drawing fibers. The physical properties, such as thermal parameters, density, and refractive index of the TAS glasses were measured and analyzed systematically. When MCN = =2.4, TAS glasses showed the largest molar density, the smallest molar volume, and the

Declaration of Competing Interest

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

Acknowledgements

This work was supported by the Zhejiang Provincial Natural Science Foundation of China(LY18F050004, LY18F050003), National Natural Science Foundation of China (61975156), Open Fund of the Guangdong Provincial Key Laboratory of Fiber Laser Materials and Applied Techniques (South China University of Technology), and K. C. Wong Magna Fund in Ningbo University.

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