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Preparation and Performance of Low-Scattering Mid-to-Long Wave Infrared As2Se3 Glass
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Qinnan FANG1, 2, Yuze WANG1, 2, Zhichao FAN1, 2, Yuyang WANG1, 2, Hepan ZHU1, 2, Shengchuang BAI1, 2, Yongxing LIU1, 2, Xunsi WANG1, 2
Journal of the Chinese Ceramic Society | 2024, 52(9) : 3012 - 3018
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Journal of the Chinese Ceramic Society | 2024, 52(9): 3012-3018
• Research Article •
Preparation and Performance of Low-Scattering Mid-to-Long Wave Infrared As2Se3 Glass
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Qinnan FANG1, 2, Yuze WANG1, 2, Zhichao FAN1, 2, Yuyang WANG1, 2, Hepan ZHU1, 2, Shengchuang BAI1, 2, Yongxing LIU1, 2, Xunsi WANG1, 2
Affiliations
  • 1Laboratory of Infrared Materials and Devices, Research Institute of Advanced Technology, College of Information, Ningbo University, Ningbo 315211, Zhejiang, China
  • 2Zhejiang Key Laboratory of Photoelectric Materials and Devices, Ningbo 315211, Zhejiang, China
  • FANG Qinnan (2000-), male, Master candidate. E-mail:

About Author:

FANG Qinnan (2000-), male, Master candidate. E-mail:

Published: 2024-09-20 doi: 10.14062/j.issn.0454-5648.20230822
Outline
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Introduction

Chalcogenide glasses are primarily composed of elements from group VI of the periodic table, such as sulfur, selenium, and tellurium, and may include other non-oxide elements like germanium and arsenic. These glasses exhibit properties such as high refractive index (2-3.5), low phonon energy (<350 cm-1), and tunable performance. As the most popular chalcogenide glasses, As-Se and As-S glasses are widely used in the fields of mid- and far-infrared imaging, supercontinuum generation, infrared laser power transmission, etc. However, the soluble impurity absorption and insoluble particle impurities inside the glass lead to a lot of trouble. In particular, particle-induced scattering is one of the key factors for the decrease of the glass transmittance. Such particles may be sourced from various conditions, such as the original presence of raw materials and introduction during glass preparation. So, it is urgent to find the real source and remove these impurities. For example, Nguyen et al. prepared As2Se3 fiber with the lowest loss below 1 dB/m, but found that there are a large number of submicron particles-Al2SiO3-inside the fiber, which enhances the scattering loss of the glass. To address this challenge, this work investigated the optical properties of glass by adding deoxidizers and filter sheets to the dynamic distillation process.

Methods

The glass was prepared using three-stage quartz ampoules. Filters with apertures of 250 μm, 160 μm, 100 μm and 10 μm were added to the multi-stage dynamic distillation process for removing particulate impurities from the glass. Metal Al as a deoxidizer was loaded in the ampoule during the distillation process for removing oxide impurities such as H2O, O—H, etc. After the glass was ground and polished, the particles inside the glass samples were observed using a Dino Capture infrared camera and analyzed in the context of scattering theory to determine how the particles affect the transmittance of the glass; Then, transmittance maps were plotted to analyze the relationship between particles and transmittance of the glass prepared with different filter apertures.

The glass prepared using the same filter aperture was ground into thin slices of different thicknesses ranging from 2-20 mm to research the relationship between glass thickness, transmittance and cut-off wavelength. At the same time, As2Se3 glass with the highest purity in this study was loaded on the newly constructed CO2 laser experimental platform for testing, and the relationship between the content of particles inside the glass and the CO2 laser damage threshold of the glass was investigated.

Results and discussion

High-purity, low-scattering As2Se3 glasses were prepared by adding filters as well as deoxidizers to the multistage dynamic distillation process. The transmittance of the glass samples obtained with a 250 μm pore size filter was only 43 % at 10.6 μm, while the transmittance obtained with a 160 μm pore size filter was increased to 57 %. When the pore size of the filter was further reduced to 100 μm, the transmittance reached to 59 %, and finally, the transmittance reached the highest level of 62 % at a pore size of 10 μm.

Additionally, the content of oxygen impurities (O—H, H2O, Se—O) and heterogeneous impurities inside the glass was significantly reduced after purification. The difference in transmittance between samples with different thicknesses (from 2 to 20 mm) was not more than 2 %, suggesting that the glass has a high degree of homogeneity and reduced internal particle scattering.

Excluding the influence of external factors, the resistance of glass to laser damage is related to the glass component and the concentration of inclusions, under the premise of determining the glass component, it is necessary to improve the laser threshold by reducing the internal particles of the glass. The absorption of heat by particulate impurities within the glass affects its laser threshold, so the increase of the glass purity also increases the CO2 laser damage threshold of the glass, specifically to 32.83 kW cm-2 (Spot diameter of 0.025 cm).

Conclusions

The results of this study showed that the optical transmittance of the glass after filtration with a 10 μm pore size screen was close to the theoretical transmittance - 62.22 % - without taking into account any scattering losses. Meanwhile, the content of oxygen impurities (O—H, H2O, Se—O) and heterogeneous impurities inside the glass has been significantly reduced. The difference in transmittance between samples with different thicknesses from 2 to 20 mm is not more than 2% with the reduced scattering inside the glass, while the preparation of ultra-low-scattering As2Se3 glass requires filters with smaller filter apertures. In summary, this study provides a new technique to further reduce the internal scattering of sulfur-based glass and to prepare ultra-low-loss sulfur-based optical fibers.

chalcogenide glass  /  particle scattering  /  heterogeneous impurities  /  ultra-low loss  /  arsenic trisulfide
方沁楠, 王煜泽, 樊智超, 王雨杨, 朱合盼, 白胜闯, 刘永兴, 王训四. 低散射中长波As2Se3玻璃的制备与性能. 硅酸盐学报, 2024 , 52 (9) : 3012 -3018 . DOI: 10.14062/j.issn.0454-5648.20230822
Qinnan FANG, Yuze WANG, Zhichao FAN, Yuyang WANG, Hepan ZHU, Shengchuang BAI, Yongxing LIU, Xunsi WANG. Preparation and Performance of Low-Scattering Mid-to-Long Wave Infrared As2Se3 Glass[J]. Journal of the Chinese Ceramic Society, 2024 , 52 (9) : 3012 -3018 . DOI: 10.14062/j.issn.0454-5648.20230822
Year 2024 volume 52 Issue 9
13
2
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Article Info
doi: 10.14062/j.issn.0454-5648.20230822
  • Receive Date:2023-10-26
  • Online Date:2026-10-22
  • Published:2024-09-20
Article Data
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History
  • Received:2023-10-26
  • Revised:2023-12-01
Funding
Affiliations
    1Laboratory of Infrared Materials and Devices, Research Institute of Advanced Technology, College of Information, Ningbo University, Ningbo 315211, Zhejiang, China
    2Zhejiang Key Laboratory of Photoelectric Materials and Devices, Ningbo 315211, Zhejiang, China

Corresponding:

WANG Xunsi (1979-), male, Ph.D., Professor. E-mail:
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表12种不同金属材料的力学参数
科
Family
属数
Number of
genus
种数
Number of
species
占总种数比例
Percentage of
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属
Genus
种数
Number of
species
占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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