高可见光透过、高紫外截止镀膜玻璃的制备

doi:10.15541/jim20160600

摘要/Abstract

摘要：

为了提高镀膜玻璃的可见光透过率, 本研究通过反胶束溶液刻蚀法制备出一种新型玻璃基板, 即表面多孔玻璃。玻璃表面形成了蜂窝状的多孔膜层, 减小了对可见光的反射率, 从而使可见光平均透过率提高了7%。通过一系列射频磁控溅射实验, 探索了可见光平均透过率高, 紫外阻隔率最高的最佳工艺条件。在此条件下, 分别在制备的表面多孔玻璃和普通玻璃上镀CeO₂/TiO₂防紫外线膜, 并采用紫外-可见分光光度计、SEM、XRD、XPS等测试手段对样品进行了分析表征。结果表明, 在相同的镀膜条件下, 当镀膜后表面多孔玻璃与镀膜普通玻璃的紫外光阻隔率均为99%时, 表面多孔玻璃镀膜后的可见光平均透过率为85%, 而普通玻璃镀膜后的可见光平均透过率仅为79%。此外, 玻璃表面上的孔结构还提高了薄膜与基板的接触面积, 使膜基结合力提高2倍左右。

关键词: 多孔玻璃, 透过率, CeO₂/TiO₂薄膜, 磁控溅射

Abstract:

A glass with a honeycomb surface was prepared by a reverse micellar solution etching technology. The honeycomb surface might reduce the light reflection and increase the average transmittance of visible light by nearly 7%. The chemical etching technology is environment friendly for unuse of HF or fluosilicate. To compare the visible light transmittance of the coated glass, CeO₂/TiO₂ films were deposited on the honeycomb surface glass and raw glass by radio frequency magnetron sputtering. A series of optimization experiments were carried out to obtain a coated glass with high visible transmittance and high UV cut-off. The samples were characterized by UV-Vis spectrophotometer, SEM, XRD, and XPS. When the UV cut-off ratios were 99% for both the honeycomb surface glass and the raw glass, the average transmittance of visible light was 85% for the coated honeycomb surface glass, and only 79% for the coated raw glass prepared under the same coating conditions. In addition, the porous structure on the glass surface also improved the contact area between the film and the substrate. Therefore, the binding force between film and substrate was increased by about 2 times.

Key words: porous glass, transmittance, CeO₂/TiO₂ coating, magnetron sputtering

中图分类号:

TQ174

王红燕, 张浩, 姜宏, 汪国庆, 熊春荣. 高可见光透过、高紫外截止镀膜玻璃的制备[J]. 无机材料学报, 2017, 32(7): 758-764.

WANG Hong-Yan, ZHANG Hao, JIANG Hong, WANG Guo-Qing, XIONG Chun-Rong. Preparation of Coating Glass with High Visible Transmittance and High UV Cut-off[J]. Journal of Inorganic Materials, 2017, 32(7): 758-764.

图/表 12

图1 表面多孔玻璃的(a)表面和(b)断面的SEM照片

Fig. 1 Top view (a) and cross section (b) SEM images of the porous glass

图2 表面多孔玻璃(a)与玻璃原片(b)的透过率曲线

Fig. 2 Transmittances of the honeycomb surface glass (a) and the raw glass (b)

图3 阳光下玻璃原片(a)和表面多孔玻璃(b)的数码照片

Fig. 3 Digital photos of the raw glass (a) and the honeycomb surface glass (b) under sunlight

图4 不同功率对CeO2/TiO2薄膜透过性能的影响

Fig. 4 Influence on sputtering powers on the transmittance of the CeO2-TiO2 films

图5 不同CeO2/TiO2溅射功率时薄膜的XPS图谱

Fig. 5 XPS spectra of the CeO2/TiO2 films deposited under different sputtering powers

表1 不同镀膜功率对CeO2/TiO2薄膜透过率及组成的影响

Table 1 Effect of relative sputtering powers on properties and compositions of CeO2/TiO2 films

	A1	A2	A3	A4	A5	A6
Power (TiO₂)/W	140	140	140	140	140	140
Power (CeO₂)/W	80	100	120	140	160	180
Transmittance of visible/%	79.9	77.9	76.9	75.3	72.5	67.8
UV cut-off ratios/%	96.8	97.2	99.1	98.4	95.3	89.5
(Ce/Ti)/%	42	46	50	55	62	65
[Ce³⁺/(Ce³⁺+Ce⁴⁺)]/%	68	70	72	69	64	61
[Ti³⁺ /(Ti³⁺+ Ti⁴⁺)]/%	57	59	64	58	56	55
Thickness of the film/nm	540	550	570	580	587	595

图6 不同溅射功率制备的CeO2/TiO2薄膜的XRD图谱

Fig. 6 XRD patterns of the CeO2/TiO2 films deposited under different sputtering powers

图7 不同溅射时间制备的CeO2/TiO2薄膜的SEM照片

Fig.7 SEM images of CeO2/TiO2 thin films sputtered for different time

表2 镀膜时间对CeO2/TiO2薄膜透过率的影响

Table 2 Influence of sputtering time on the transmittance of the CeO2/TiO2 thin-films

Samples	B1	B2	B3	B4	B5
Sputtering time/min	10	20	30	40	50
Transmittance of visible/%	86.4	82.5	80.6	79.5	70.1
UV cut-off ratio/%	79.8	82.2	88.5	96.6	99.2
Thickness of the film/nm	127	235	352	456	554

图8 溅射时间对CeO2/TiO2薄膜透过率的影响

Fig. 8 Influence on sputtering times on the transmittance of CeO2/TiO2 thin films

表3 表面多孔镀膜玻璃与原片镀膜玻璃的透过率

Table 3 Transmittances of the CeO2/TiO2 coated honeycomb surface glass and raw glass

Samples	Transmittance of visible/%	UV cut-off ratio/%	Thickness of the film /nm
Coated raw glass	79.8	99.1	435
Coated honeycomb surface glass	84.7	99.7	410

图9 (a)玻璃原片和(b)表面多孔玻璃基板上薄膜的结合力测试

Fig. 9 Cohesion results of the thin films on (a) the raw glass and (b) the honeycomb surface glass substrates by scratching test

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