硅酸盐学报

微米级SiO₂中空微球的制备及自组装光子晶体的红外性能

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吴文强 ¹^,² , 李帅 ¹^,² , 陈仕乐 ² , 郎莹 ¹ , 汪长安 ²

硅酸盐学报 | 研究论文 2024,52(6): 1996-2002

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硅酸盐学报 |研究论文 2024 , 52 (6) : 1996 -2002

微米级SiO₂中空微球的制备及自组装光子晶体的红外性能

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吴文强¹^,², 李帅¹^,², 陈仕乐², 郎莹¹, 汪长安²

作者信息

^1．景德镇陶瓷大学，材料科学与工程学院，江西景德镇 333403

^2．清华大学材料学院，新型陶瓷与精细工艺国家重点实验室，北京 100084

通讯作者:

汪长安（1969—），男，博士，教授。

作者简介:

吴文强（1998—），男，硕士研究生。

Preparation of Micrometer sized SiO₂ Hollow Microspheres and Infrared Properties of Self-Assembled Photonic Crystals

Wenqiang WU¹^,², Shuai LI¹^,², Shile CHEN², Ying LANG¹, Chang'an WANG²

Affiliations

^1.School of Materials Science and Engineering, Jingdezhen Ceramic Institute, Jingdezhen 333403, Jiangxi, China

^2.State Key Laboratory of New Ceramics and Fine Processing, School of Materials Science and Engineering, Tsinghua University, Beijing 100084, China

Corresponding Author:

WANG Chang'an (1969-), male, Ph.D., Professor. E-mail: wangca@mail.tsinghua.edu.cn

WU Wenqiang (1998-), male, Master candidate. E-mail: 2295057131@qq.com

出版时间: 2024-06-20 doi: 10.14062/j.issn.0454-5648.20240031

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摘要

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以聚苯乙烯（PS）为模板、十六烷基三甲基溴化铵（CTAB）为表面改性剂、正硅酸四乙酯（TEOS）为硅源，采用硬模板包裹法结合乙酸乙酯浸蚀的工艺，制备了微米级SiO₂中空微球，并进行垂直沉积自组装成微米级SiO₂中空微球光子晶体，研究了TEOS含量、浸蚀条件对中空微球形貌的影响，以及垂直沉积自组装溶液浓度对微米级SiO₂中空微球光子晶体红外性能的影响。结果表明：随着TEOS含量的增加，SiO₂包覆层表面由疏松变得致密，进一步增加会生成次生SiO₂颗粒，导致均匀性变差；在60 ℃乙酸乙酯中浸蚀10 min时，微米级SiO₂中空微球分散性好、球形度高，直径达到1 570 nm、壁厚达到65 nm；随着自组装溶液质量浓度的增大，微米级SiO₂中空微球的排列变得整齐、层数增多，红外反射率升高，在溶液质量浓度为0.005 g/mL时反射率最高为85%。微米级SiO₂中空微球光子晶体除实现红外辐射调控之外，还具有隔热性能好、比重小等优点，在航空航天飞行器的红外隐身涂层、建筑保温等领域具有重要的应用前景。

关键词

乙酸乙酯 / 微米级二氧化硅中空微球 / 光子晶体 / 红外发射率

Abstract

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Introduction

Micron-sized SiO₂ hollow microspheres were prepared by a hard template encapsulation method and an ethyl acetate etching process with polystyrene (PS) as a template, hexadecyltrimethylammonium bromide (CTAB) as a surface modifier, and tetraethyl orthosilicate (TEOS) as a silicon source, and vertically deposited self-assembled into micron-sized SiO₂ hollow microsphere photonic crystals. The effects of TEOS content and etching conditions on the morphology of hollow microspheres, as well as the effect of vertical deposition self-assembly solution concentration on the infrared properties of micrometer sized SiO₂ hollow microsphere photonic crystals were investigated.

Methods

For the preparation of micron-sized PS@SiO₂ microspheres, 0.15 g of polystyrene microspheres with the size of 1.5 μm were dissolved in 160 mL of deionized water and 80 mL of anhydrous ethanol. After ultrasonic dispersion, 0.03 g of CTAB was added to modify the surface of the polystyrene template under stirring. After 30 min, 3 mL of 25% ammonia water was added to prepare solution A. 0.2 mL of ethyl orthosilicate was dissolved in 5 mL of anhydrous ethanol to prepare solution B. Solution B was mixed with solution A under stirring at room temperature for 24 h. The reacted solution was filtered and washed with anhydrous ethanol and deionized water for three times. PS@SiO₂ material was obtained after drying.

For the preparation of micron-sized SiO₂ hollow microspheres, 0.5 g of PS@SiO₂ microspheres were dispersed in 20 mL of ethyl acetate, and heated at 60 ℃ for 10 min after ultrasonic dispersion. The PS template was etched off by ethyl acetate. Subsequently, the slurry was filtered and washeda with anhydrous ethanol and deionized water for three times to obtain micron-sized SiO₂ hollow microspheres.

For the preparation of micron-sized SiO₂ hollow microsphere photonic crystals, a microsphere suspension was dispersed for a certain time, and then a cleaned hydrophilic glass substrate was vertically immersed into the microsphere suspension, and dried at 60 ℃. As the mixed solvent evaporates, the microspheres self-assemble on the surface of the substrate into a photonic crystal thin film with an opal structure.

Results and discussion

Micron-sized SiO₂ hollow microspheres with a low damage rate, a good dispersibility, and a high sphericity were prepared with PS spheres as a template, CTAB as a surfactant, and TEOS as silicon source. PS template was removed via ethyl acetate etching. At TEOS content of 0.2 mL, PS@SiO₂ microspheres are tightly coated, and there are no secondary microspheres. When ethyl acetate is used for etching for 10 min, the hollow SiO₂ microspheres with the diameter of 1 570 nm and thickness of 65 nm are prepared. Moreover, micron-sized SiO₂ hollow microspheres are self-assembled into photonic crystal materials by a vertical deposition method. As the concentration of self-assembly solution increases, the arrangement of SiO₂ hollow microspheres is tightly ordered without obvious vacancies and with a hexagonal periodic structure. The number of layers increases from 6 to 16, and the reflectivity gradually increases. When the solubility of the self-assembled solution is 0.005 g/mL, the maximum reflectivity is 85%.

Conclusions

The micron-sized SiO₂ hollow microspheres with a good dispersion, a high uniformity, a less damage, and a high sphericity were prepared by a template encapsulation method and an ethyl acetate etching process. Also, micron-sized SiO₂ hollow microsphere photonic crystals with a good thermal insulation performance, a low density, and a reflectivity of 85% as infrared band hollow microsphere photonic crystals were prepared by a vertical deposition self-assembly method.

Key words

ethyl acetate / micrometer size silica hollow microspheres / photonic crystals / infrared emissivity

引用本文

吴文强, 李帅, 陈仕乐, 郎莹, 汪长安. 微米级SiO₂中空微球的制备及自组装光子晶体的红外性能. 硅酸盐学报, 2024 , 52 (6) : 1996 -2002 . DOI: 10.14062/j.issn.0454-5648.20240031

Wenqiang WU, Shuai LI, Shile CHEN, Ying LANG, Chang'an WANG. Preparation of Micrometer sized SiO₂ Hollow Microspheres and Infrared Properties of Self-Assembled Photonic Crystals[J]. Journal of the Chinese Ceramic Society, 2024 , 52 (6) : 1996 -2002 . DOI: 10.14062/j.issn.0454-5648.20240031

基金

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国家自然科学基金资助项目(52173257; 52372064)

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2024年第52卷第6期

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文章信息

doi: 10.14062/j.issn.0454-5648.20240031

接收时间：2024-01-11
首发时间：2026-10-22
出版时间：2024-06-20

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收稿日期：2024-01-11
修回日期：2024-01-30

基金

国家自然科学基金资助项目(52173257; 52372064)

作者信息

^1．景德镇陶瓷大学，材料科学与工程学院，江西景德镇 333403

^2．清华大学材料学院，新型陶瓷与精细工艺国家重点实验室，北京 100084

通讯作者:

汪长安（1969—），男，博士，教授。

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https://castjournals.cast.org.cn/joweb/gsyxb/CN/10.14062/j.issn.0454-5648.20240031

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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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