胡伟,尹勇明,郝霞,孟鸿.基于仿生蛾眼结构制备减反射微晶玻璃[J].表面技术,2024,53(18):183-191.
HU Wei,YIN Yongming,HAO Xia,MENG Hong.Preparation of Antireflective Glass-ceramic Based on Biomimetic Moth Eye Structure[J].Surface Technology,2024,53(18):183-191 |
| 基于仿生蛾眼结构制备减反射微晶玻璃 |
| Preparation of Antireflective Glass-ceramic Based on Biomimetic Moth Eye Structure |
| 投稿时间：2023-09-21 修订日期：2024-02-23 |
| DOI：10.16490/j.cnki.issn.1001-3660.2024.18.016 |
| 中文关键词: 微晶玻璃 湿法刻蚀 蛾眼结构 晶粒大小 透过率 晶化工艺 |
| 英文关键词:glass-ceramic wet etching moth eye structure grain size transmittance crystallization process |
| 基金项目:国家自然科学基金(51873002);广东省基础与应用基础研究基金(2020B1515120029) |
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| Author | Institution |
| HU Wei | School of Advanced Materials, Peking University Shenzhen Graduate School, Guangdong Shenzhen 518000, China |
| YIN Yongming | Shenzhen MSU-BIT University, Guangdong Shenzhen 518000, China |
| HAO Xia | Hainan Holdings Special Glass Technology Co., Ltd., Hainan Chengmai 571925, China |
| MENG Hong | School of Advanced Materials, Peking University Shenzhen Graduate School, Guangdong Shenzhen 518000, China |
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| 中文摘要: |
| 目的 采用湿法刻蚀制备减反射微晶玻璃，分析晶化时间对透过率、反射率和形貌的影响。方法 通过熔融法制备得到基础玻璃，调整晶化时间制备得到一系列不同晶粒尺寸(12.2～27.4 nm)的微晶玻璃，将制备得到的基础玻璃及不同晶粒尺寸的微晶玻璃放置在配制好的5%(质量分数)HF、2%(质量分数)SiO2、1.5%(质量分数)BaSO4、2%(质量分数)羧甲基纤维素钠、89.5%(质量分数)H2O的刻蚀液中，在25 ℃条件下，以40 kHz的超声频率双面蚀刻60 min，通过分光光度计测试刻蚀前后样品的透过率和反射率，利用扫描电子显微镜对刻蚀前后样品的表面和断面形貌进行表征。结果 基础玻璃在500 ℃核化230 min，665 ℃晶化135 min后，制备得到微晶玻璃的晶粒尺寸约为25.1 nm，进一步经过湿法刻蚀后，刻蚀深度约为150 nm，蛾眼玻璃透过率最高为98.02%。结论 微晶玻璃经过湿法刻蚀后增透效果明显，对X射线衍射(XRD)、掠入射X射线衍射(GIXRD)、扫描电子显微镜(SEM)的测试结果进行分析可知，微晶玻璃中存在晶体相和残余玻璃相，经过酸蚀处理后，表面能形成以透锂长石晶体和二硅酸锂晶体均匀分布的蛾眼结构，晶体尺寸为12.2～27.4 nm的微晶玻璃进行湿法刻蚀后透过率分布在95.99%～98.02%。 |
| 英文摘要: |
| The high transparency and low reflection performance of the moth eye structure is of great significance for industries such as photovoltaic and display screens. The work aims to develop a simple and rapid method for preparing moth eye glass based on glass-ceramic (GC). Antireflective GC was prepared by wet etching, and the effect of crystallization time on transmittance, reflectance, and morphology were analyzed. Basic glass was prepared by melting method, and a series of GCs with different grain sizes (12.2-27.4 nm) were prepared by adjusting the crystallization time. As the crystallization process time increased, the crystal size in GC also increased. When the crystallization time was 180 min, the average crystal size reached 27.4 nm. Continuing to increase the time might lead to excessive crystallization and cause glass opacity. The prepared basic glass and GCs with different grain sizes were placed in a prepared etching solution of 5wt.% HF, 2wt.% SiO2, 1.5wt.% BaSO4, 2wt.% carboxymethyl cellulose sodium, and 89.5wt.% H2O. The etching was carried out on both sides at 40 kHz ultrasonic frequency for 60 min at 25 ℃. The transmittance and reflectance of the sample before and after etching were measured by spectrophotometer, and the surface and cross-sectional morphology of the sample before and after etching were characterized by scanning electron microscope. After nucleating the basic glass at 500 ℃ for 230 min and crystallizing at 665 ℃ for 135 min, the grain size of the GC prepared was about 25.1 nm. After further wet etching, the etching depth was about 150 nm, and the highest transmittance of the moth eye glass was 98.02%. The lowest reflectance was 1.82%. The sum of the transmittance, reflectance, and absorption of glass was 100%, and the absorption of glass was considered constant. As the transmittance increased, the reflectance decreased. The results showed that after wet etching, the GC formed a moth eye structure on the glass surface, greatly improving the glass transmittance and reducing its reflectance. After wet etching, the antireflective effect of GC was significant. Analysis of the test results of X-ray diffraction (XRD), grazing incidence X-ray diffraction (GIXRD), and scanning electron microscopy (SEM) showed that there were crystal phases and residual glass phases in GC. After acid etching treatment, a moth eye structure with uniformly distributed petalite and lithium disilicate crystals could be formed on the surface. The transmittance of GC with a crystal size distribution of 12.2-27.4 nm after wet etching ranged from 95.99% to 98.02%. As the crystallization time increased, the crystal size of the microcrystalline phase in the GC gradually increased, the crystal phase content gradually increased, and the glass phase content gradually decreased. Under the same etching conditions, the longer the crystallization time of the GC substrate, the deeper it was etched, resulting in an increase in the thickness of the final moth eye structure film layer. The antireflective surface modification of transparent materials has always attracted much attention, and the research on the structure of surface facial mask based on different methods has been ongoing. There is a theoretical threshold for the transmittance of each material, so in the absence of significant differences in the performance of various methods in enhancing transparency, future research directions will focus on large-scale, low-cost, and easy processing. |
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