硅酸盐学报

低散射中长波As₂Se₃玻璃的制备与性能

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方沁楠 ¹^,² , 王煜泽 ¹^,² , 樊智超 ¹^,² , 王雨杨 ¹^,² , 朱合盼 ¹^,² , 白胜闯 ¹^,² , 刘永兴 ¹^,² , 王训四 ¹^,²

硅酸盐学报 | 研究论文 2024,52(9): 3012-3018

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硅酸盐学报 |研究论文 2024 , 52 (9) : 3012 -3018

低散射中长波As₂Se₃玻璃的制备与性能

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方沁楠¹^,², 王煜泽¹^,², 樊智超¹^,², 王雨杨¹^,², 朱合盼¹^,², 白胜闯¹^,², 刘永兴¹^,², 王训四¹^,²

作者信息

^1．宁波大学信息科学与工程学院，高等技术研究院，红外材料与器件实验室，浙江宁波 315211

^2．浙江省光电探测材料及器件重点实验室，浙江宁波 315211

通讯作者:

王训四（1979—），男，博士，研究员。

作者简介:

方沁楠（2000—），男，硕士研究生。

Preparation and Performance of Low-Scattering Mid-to-Long Wave Infrared As₂Se₃ Glass

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

Corresponding Author:

WANG Xunsi (1979-), male, Ph.D., Professor. E-mail: wangxunsi@nbu.edu.cn

FANG Qinnan (2000-), male, Master candidate. E-mail: 741774613@qq.com

出版时间: 2024-09-20 doi: 10.14062/j.issn.0454-5648.20230822

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摘要

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颗粒引发的散射是影响玻璃透光性的关键因素之一。在红外硫系玻璃的基础组分中，通常包含单质S或Se。通过在石英安瓿瓶内使用还原金属（Al或Mg）进行提纯，容易引入微米级的金属氧化物颗粒（Al₂O₃、MgO）或硅杂质。为了深入探究滤网在微米级颗粒滤除方面的效能，通过在主动蒸馏过程中装载不同孔径的过滤网，对比研究了玻璃的光谱和透光率变化情况。研究结果表明，使用10 μm孔径滤网过滤后，玻璃的光学透过率接近不考虑任何散射损失的理论透过率——62%；同时，玻璃内的氧杂质（O—H、H₂O、Se—O）和异相杂质含量也有了显著下降。在玻璃内部散射降低的前提下，2~20 mm厚度不同的样品之间的透过率差不超过2%，而制备超低散射的As₂Se₃玻璃需要更小滤网孔径的过滤网。本研究为进一步降低硫系玻璃内部散射，以及制备超低损耗的硫系光纤提供了一种新技术。

关键词

硫系玻璃 / 颗粒散射 / 异相杂质 / 超低损耗 / 三硫化二砷

Abstract

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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.

Key words

chalcogenide glass / particle scattering / heterogeneous impurities / ultra-low loss / arsenic trisulfide

引用本文

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

基金

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国家自然科学基金(U22A2085; 62205163; 61875097; 61627815; 61705091)
浙江省万人计划
宁波市自然科学基金(202003N4101)
宁波市领军和拔尖人才培养工程
王宽诚幸福基金课题

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2024年第52卷第9期

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文章信息

doi: 10.14062/j.issn.0454-5648.20230822

接收时间：2023-10-26
首发时间：2026-10-22
出版时间：2024-09-20

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收稿日期：2023-10-26
修回日期：2023-12-01

基金

国家自然科学基金(U22A2085; 62205163; 61875097; 61627815; 61705091)

浙江省万人计划

宁波市自然科学基金(202003N4101)

宁波市领军和拔尖人才培养工程

王宽诚幸福基金课题

作者信息

^1．宁波大学信息科学与工程学院，高等技术研究院，红外材料与器件实验室，浙江宁波 315211

^2．浙江省光电探测材料及器件重点实验室，浙江宁波 315211

通讯作者:

王训四（1979—），男，博士，研究员。

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https://castjournals.cast.org.cn/joweb/gsyxb/CN/10.14062/j.issn.0454-5648.20230822

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2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 total species (%)	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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