硅酸盐学报

基于新型含氯光热敏折变玻璃的全息体光栅制备和性能

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闫运浩 ¹^,² , 柴聪鹏 ¹^,² , 郭凌伟 ³ , 华有杰 ¹^,² , 徐时清 ¹^,² , 赵士龙 ¹^,²

硅酸盐学报 | 微晶玻璃专题—研究论文 2024,52(8): 2509-2516

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硅酸盐学报 |微晶玻璃专题—研究论文 2024 , 52 (8) : 2509 -2516

基于新型含氯光热敏折变玻璃的全息体光栅制备和性能

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闫运浩¹^,², 柴聪鹏¹^,², 郭凌伟³, 华有杰¹^,², 徐时清¹^,², 赵士龙¹^,²

作者信息

^1．中国计量大学光电材料与器件研究院，杭州 310018

^2．中国计量大学浙江省光电材料与器件重点实验室，杭州 310018

^3．杭州电子科技大学电子信息学院，杭州 310018

通讯作者:

赵士龙（1975—），男，博士，教授。

作者简介:

闫运浩（1999—），男，硕士研究生。

Preparation and Performance of Holographic Grating Based on Novel Chlorine-Containing Photothermal Refractive Glass

Yunhao YAN¹^,², Congpeng CHAI¹^,², Lingwei GUO³, Youjie HUA¹^,², Shiqing XU¹^,², Shilong ZHAO¹^,²

Affiliations

^1.Institute of Optoelectronic Materials and Devices, China Jiliang University, Hangzhou 310018, China

^2.Key Laboratory of Rare Earth Optoelectronic Materials and Devices of Zhejiang Province, China Jiliang University, Hangzhou 310018, China

^3.School of Electronics and Information Engineering, Hangzhou Dianzi University, Hangzhou 310018, China

Corresponding Author:

ZHAO Shilong (1975-), male, Ph.D., Professor. E-mail: zhaosl75@cjlu.edu.cn

YAN Yunhao (1999-), male, Master candidate. E-mail: 864215902@qq.com

出版时间: 2024-08-20 doi: 10.14062/j.issn.0454-5648.20240055

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摘要

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体Bragg光栅是实现半导体激光器超窄线宽激光输出的核心元件。采用高温熔融法制备了一种玻璃体系为SiO₂-Na₂O-Al₂O₃-ZnO（F^-、Cl^-）的新型含氯光热敏折变玻璃（PTR glass）。结果表明：在含氯PTR玻璃中析出了NaF纳米晶，并测得晶粒大小为5 nm，玻璃保持很高的透明度。Cl^-的引入使得PTR玻璃的等离子体吸收峰由450 nm蓝移至413 nm，为开发低吸收损耗的可见和近红外光范围元器件提供了更大可能。采用全息曝光和分步热处理工艺制得衍射效率为67.95%、半高全宽仅为0.057 nm的1.5 μm超窄线宽体Bragg光栅。

关键词

光热敏折变玻璃 / 体Bragg光栅 / 超窄线宽 / 半导体激光器

Abstract

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Introduction

With the continuous development of laser technology, ultra-narrow linewidth lasers show important application prospects in many fields. However, the output linewidth of conventional semiconductor laser chips is usually large, which cannot meet the practical application requirements. Therefore, it is of great significance to study the key technologies for preparing ultra-narrow linewidth lasers. As a new type of optical component, volume Bragg grating, with the advantages of tunable diffraction wavelength, stable laser wavelength, and narrow linewidth, has become an effective way to solve this problem. This work tried to prepare 1.5 μm volume Bragg grating (VBG) based on chlorine-containing PTR glass to meet the demand for ultra-narrow linewidth lasers in the fields of new generation of coherent laser communication, LIDAR, and high-precision fiber sensing.

Methods

The glass samples were prepared as long strips with a diameter of 5 mm and a length of 28 mm. The thermal expansion was recorded by warming the glass samples from room temperature to 800 ℃ at a rate of 10 ℃/min using a DIL 402PC/4 high-temperature thermal expansion meter from NETZSCH, Germany. The samples of chlorine-containing PTR glass before and after exposure were also tested by differential thermal analysis using a Q600SDT integrated thermal analyser from TA Instruments, USA. This is an important parameter to understand the dimensional stability of the glass during temperature change. A D2 PHASER type X-ray diffractometer from Bruker, Germany was used to analyze the changes in crystal structure of chlorine containing PTR glass before and after exposure, nucleation and precipitation heat treatment to understand the structural evolution and property changes of the material.

A Lambda 750S UV-Vis-NIR spectrophotometer from Perkin Elmer, USA was used to study the optical absorption properties of chlorine-containing PTR glass before and after exposure, nucleation and decrystallisation heat treatments, and to understand its absorption capacity at different wavelengths.

The glass powder was mixed with high purity KBr and pressed into tablets, and then scanned by infrared spectroscopy with a scanning speed of 0.158 cm/s. A Nicolet iS50 Fourier infrared spectrometer from Thermo Fisher Scientific, USA was used. The samples were then analyzed for their infrared transmittance properties. The infrared transmission properties of the samples were analyzed to understand the transmission properties of the materials in the infrared band. An in Via-Peflex type Raman spectrometer from Renishaw, UK was used. The molecular vibration and vibrational information of the samples were further analyzed through Raman spectroscopy to further understand the structure and properties of the materials.

Results and discussion

Firstly, the thermal properties of the new PTR glass were investigated. Its transition temperature (T_g) and softening temperature (T_f) were 446.2 ℃ and 499.4 ℃, respectively. These two parameters are important for glass processing and applications. The coefficient of thermal expansion was similar to that of bromine-containing PTR glass in the temperature range of 30-400 ℃, indicating that the substitution of Br^- by Cl^- has a small effect on the thermal expansion properties of PTR glass. Secondly, it was found that NaF nanocrystals were successfully precipitated from chlorine-containing PTR glass after the precipitation heat treatment by XRD (X-ray diffraction) and TEM (transmission electron microscopy) inspection. These nanocrystals were distributed as dark grey elliptical particles with a particle size of 5 nm in the glass. high-resolution transmission electron microscopy (HRTEM) further revealed the lattice structure of these nanocrystals, and the spacing of adjacent crystal planes corresponded to the (111) crystal planes of NaF crystals. In addition, the detection of absorption spectra of chlorine-containing PTR glasses showed a new broad and weak absorption peak at 413 nm, which was attributed to the absorption of plasma AgCl.

Compared with the plasma AgBr absorption peak precipitated in the conventional PTR glass, the plasma AgCl absorption peak of the chlorine-containing PTR glass blueshifted in the UV sepctrum, which supplied the possibility of developing short-wavelength VBG products. In terms of glass structure, Raman and Fourier infrared spectroscopy analyses showed that the structure of chlorine-containing PTR glasses did not change significantly after the precipitation heat treatment. Finally, the article explores the performance of chlorine-containing PTR glasses for VBG applications. The diffraction efficiency of VBG was found to be positively correlated with the refractive index modulation and grating thickness. Under the same conditions of exposure dose and heat treatment process, increasing the thickness of VBG can significantly improve its diffraction efficiency. The experimental results show that the centre wavelengths of VBGs with thicknesses of 10 mm and 16 mm are 1 549.44 nm and 1 549.48 nm, respectively, and the half-height full widths are 0.0611 nm and 0.0570 nm, respectively.

Conclusions

Novel chlorine-containing PTR glass components were designed and prepared using a two-step melting process to produce photothermally sensitive refractive glasses with a homogeneity of 10-6.325 nm UV irradiation led to a decrease in the transition temperature and the onset of precipitation of the PTR glass, and an increase in the precipitation properties, which is very favourable for the preparation of high-quality VBGs. XRD and TEM results confirmed that NaF nanocrystals of an average size of 5 nm were precipitated from the chlorine-containing PTR glass. NaF nanocrystals with an average particle size of 5 nm. Raman and FTIR spectra showed that holographic exposure and heat treatment further enhanced the glass network structure. A reflective volume Bragg grating with a centre wavelength of 1.5 μm was prepared, with a diffraction efficiency of 50% and a half-height full width of 0.0570 nm, which sets the foundation for the development of 1.5 μm ultra-narrow linewidth semiconductor lasers.

Key words

photo-thermo-refractive glass / volume Bragg grating / ultra-narrow line width / semiconductor laser

引用本文

闫运浩, 柴聪鹏, 郭凌伟, 华有杰, 徐时清, 赵士龙. 基于新型含氯光热敏折变玻璃的全息体光栅制备和性能. 硅酸盐学报, 2024 , 52 (8) : 2509 -2516 . DOI: 10.14062/j.issn.0454-5648.20240055

Yunhao YAN, Congpeng CHAI, Lingwei GUO, Youjie HUA, Shiqing XU, Shilong ZHAO. Preparation and Performance of Holographic Grating Based on Novel Chlorine-Containing Photothermal Refractive Glass[J]. Journal of the Chinese Ceramic Society, 2024 , 52 (8) : 2509 -2516 . DOI: 10.14062/j.issn.0454-5648.20240055

基金

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浙江省自然科学基金(LZ21F050001; LY23A040007)
国家自然科学基金(12174360)

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2024年第52卷第8期

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文章信息

doi: 10.14062/j.issn.0454-5648.20240055

接收时间：2024-01-22
首发时间：2026-10-22
出版时间：2024-08-20

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出版历史

收稿日期：2024-01-22
修回日期：2024-02-15

基金

浙江省自然科学基金(LZ21F050001; LY23A040007)

国家自然科学基金(12174360)

作者信息

^1．中国计量大学光电材料与器件研究院，杭州 310018

^2．中国计量大学浙江省光电材料与器件重点实验室，杭州 310018

^3．杭州电子科技大学电子信息学院，杭州 310018

通讯作者:

赵士龙（1975—），男，博士，教授。

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https://castjournals.cast.org.cn/joweb/gsyxb/CN/10.14062/j.issn.0454-5648.20240055

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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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