二氧化钒-荧光增白剂-有机聚合物三层多功能复合薄膜

高迎; 秦成远; 聂永; 呼啸; 徐慧妍; 苗金玲; 蒋绪川

doi:10.13801/j.cnki.fhclxb.20211027.003

二氧化钒-荧光增白剂-有机聚合物三层多功能复合薄膜

doi: 10.13801/j.cnki.fhclxb.20211027.003

高迎^1,,
秦成远¹,
聂永^1, ,,
呼啸¹,
徐慧妍¹,
苗金玲²,
蒋绪川^1, ,

1.
济南大学　智能材料与工程研究院，济南 250002
2.
济南大学　化学化工学院，济南 250002

基金项目: 济南大学和山东莘纳智能新材料有限公司资助项目

详细信息

通讯作者:
聂永，博士，教授，硕士生导师，研究方向为有机-无机复合功能材料　E-mail：chm_niey@ujn.edu.cn

蒋绪川，博士，教授，博士生导师，研究方向为光、热、电、磁等外界刺激响应型无机功能材料和隔热节能玻璃的工程化E-mail：ism_jiangxc@ujn.edu.cn

中图分类号: TB332
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出版历程
- 收稿日期: 2021-08-03
- 修回日期: 2021-09-17
- 录用日期: 2021-10-13
- 网络出版日期: 2021-10-28
- 刊出日期: 2022-08-31

Three-layer multifunctional vanadium dioxide-fluorescent brightener-organic polymer composite films

1.
Institute for Smart Materials & Engineering, University of Jinan, Jinan 250002, China
2.
School of Chemistry and Chemical Engineering, University of Jinan, Jinan 250002, China

摘要

摘要: 二氧化钒(VO₂)是一种典型的热致变色材料，用于智能窗可有效降低建筑能耗。然而，VO₂智能玻璃的颜色和稳定性问题限制了其大规模应用。本文报道一种VO₂基三层荧光复合膜，包括VO₂@SiO₂热致变色层、荧光增白剂分子层和有机聚合物层。VO₂@SiO₂层可根据外界温度变化，调控太阳光的摄入量，起到冬暖夏凉的作用，其核壳结构有利于提高VO₂的稳定性；荧光分子层在太阳光照射下，吸收紫外光，发射蓝色荧光，从而改善VO₂涂层固有的棕黄色；有机聚合物层作为最上层，能有效保护下层的VO₂@SiO₂层和中间的荧光分子层，增加复合薄膜的稳定性。与纯VO₂膜相比，这种复合膜不但保持了较高的可见光透过率和太阳光调制能力，而且在太阳光下颜色可逆地从棕黄色变为蓝色，同时稳定性和紫外阻隔能力明显提升，有利于VO₂基智能窗的推广和应用。
- 二氧化钒 /
- 复合薄膜 /
- 智能玻璃 /
- 荧光增白剂 /
- 聚合物
Abstract: Vanadium dioxide (VO₂) is a typical thermochromic material that can be used for smart windows, which can effectively reduce the building energy consumption. However, the issues of the yellow brown color and instabi-lity of VO₂ based smart glass restrict its wide application. Herein, a series of VO₂ based three-layer fluorescent composite films has been reported. The composite films consist of VO₂@SiO₂ based thermochromic layer, fluorescent brightener layer and organic polymer layer. The VO₂@SiO₂ layer can control the sunlight intake with the change of external temperature, regulating the indoor temperature, with the core-shell structure improving the stability of the film. The fluorescent brightener layer absorbs ultraviolet irradiation and emit blue fluorescence, thus improving the color of VO₂ coating. As the top layer, the organic polymer layer can effectively protect the lower layers and increase the stability of the whole composite film. Compared with the pure VO₂ films, these composite films not only maintain high visible light transmittance and solar modulation ability, but also reversibly change color from yellow-brown to blue under sunlight. Meanwhile, the stability and the UV blocking property are also significantly improved. The properties of this type of composite films are beneficial to the promotion and application of VO₂-based smart windows.
- vanadium dioxide /
- composite films /
- smart windows /
- fluorescent brightener /
- polymer

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图 1 4, 4-双(2-甲氧基苯乙烯基)联苯(CBS-127)、4, 4-双(2-磺酰苯乙烯基钠)联苯(CBS-X)和KH550的结构式

Figure 1. Structures of 4, 4-bis(2-methoxy styrene) biphenyl (CBS-127), 4, 4-bis(2-sulfonyl styrene sodium) biphenyl (CBS-X) and KH550

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图 2 VO₂@SiO₂-KH550-二苯乙烯基联苯类荧光增白剂(CBS)-polymer薄膜的制备示意图

Figure 2. Schematic diagram of the preparation of VO₂@SiO₂-KH550-stilbenyl biphenyl fluorescent brightener (CBS)-polymer composite film

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图 3 用于制备复合膜的VO₂(M)纳米粒子的XRD图谱(a)和DSC曲线(b)

Figure 3. XRD pattern (a) and DSC curves (b) of VO₂(M) nanoparticles for composite films

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图 4 VO₂(M)纳米粒子的SEM图像

Figure 4. SEM images of VO₂(M) nanoparticles

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图 5 VO₂(M)纳米粒子的TEM图像

Figure 5. TEM images of VO₂(M) nanoparticles

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图 6 改性后纳米粒子的XRD图谱 (a)、TGA曲线 (b)、FTIR图谱 (c)、FTIR图谱中VO₂-KH550和VO₂@SiO₂-KH550部分图谱放大 (d)

Figure 6. XRD patterns(a), TGA curves (b), FTIR spectra (c) and magnified images of part of the FTIR spectra of VO₂-KH550 and VO₂@SiO₂-KH550 particles (d)

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图 7 VO₂@SiO₂ ((a)~(c)) 和VO₂@SiO₂-KH550 ((d)~(e)) 的TEM图像

Figure 7. TEM images of VO₂@SiO₂ ((a)-(c)) and VO₂@SiO₂-KH550 particles ((d)-(e))

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图 8 VO₂@SiO₂ ((a)~(c)) 和VO₂@SiO₂-KH550 ((d)~(e)) 的SEM图像

Figure 8. SEM images of VO₂@SiO₂ ((a)-(c)) and VO₂@SiO₂-KH550 particles ((d)-(e))

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图 9 (a) 每张照片从左到右依次为VO₂、VO₂-KH550、VO₂@SiO₂和VO₂@SiO₂-KH550纳米颗粒分散在0.5 mol/L H₂SO₄溶液中不同时间的变化情况；(b) 不同时间悬浮液在570 nm处的透射率；(c) 经过30 min 0.5 mol/L H₂SO₄浸泡后VO₂-KH550、VO₂@SiO₂和VO₂@SiO₂-KH550纳米颗粒的XRD图谱

Figure 9. (a) In each picture, from left to right: VO₂, VO₂-KH550, VO₂@SiO₂ and VO₂@SiO₂-KH550 particles being dispersed in 0.5 mol/L H₂SO₄against time; (b) Transmission spectra of different suspensions at 570 nm; (c) XRD patterns of VO₂-KH550, VO₂@SiO₂ and VO₂@SiO₂-KH550 particles after being immersed in 0.5 mol/L H₂SO₄ for 30 min

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图 10 (a) 纳米颗粒分散在0.1 mol/L H₂O₂溶液中不同时间的变化情况，每张照片从左到右依次为VO₂、VO₂-KH550、VO₂@SiO₂和VO₂@SiO₂-KH550；(b) 悬浮液在不同时间570 nm处的透射率；(c) 0.1 mol/L H₂O₂浸泡30 min后VO₂-KH550、VO₂@SiO₂和VO₂@SiO₂-KH550纳米颗粒的XRD图谱

Figure 10. (a) In each picture, from left to right: VO₂, VO₂-KH550, VO₂@SiO₂ and VO₂@SiO₂-KH550 particles being dispersed in 0.1 mol/L H₂O₂against time; (b) Transmission spectra of different suspensions at 570 nm; (c) XRD patterns of VO₂-KH550, VO₂@SiO₂ and VO₂@SiO₂-KH550 particles after being immersed in 0.1 mol/L H₂O₂ for 30 min

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图 11 在空气中不同温度加热时VO₂(a)、VO₂-KH550 (b)、VO₂@SiO₂ (c)和VO₂@SiO₂-KH550 (d) 纳米粒子的XRD图谱

Figure 11. XRD patterns of VO₂(a), VO₂-KH550 (b), VO₂@SiO₂ (c) and VO₂@SiO₂-KH550 (d) after being heated at different temperatures in the air

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图 12 VO₂-CBS、VO₂@SiO₂-KH550-CBS复合薄膜 ((a)、(c)) 和VO₂@SiO₂-KH550-CBS-polymer复合薄膜 ((b)、(d)) 在20℃和90℃的紫外-可见-近红外透射光谱

Figure 12. UV-Vis-NIR spectra of composite films of VO₂-CBS, VO₂@SiO₂-KH550-CBS ((a), (c)) and VO₂@SiO₂-KH550-CBS-polymer ((b), (d)) at 20℃ and 90℃

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图 13 VO₂、VO₂@SiO₂薄膜和VO₂-CBS、VO₂@SiO₂-KH550、VO₂@SiO₂-KH550-CBS-PMMA复合薄膜在室内自然光、365 nm紫外灯及室外太阳光下的照片

Figure 13. Pictures of films of VO₂, VO₂@SiO₂and composite films of VO₂-CBS, VO₂@SiO₂-KH550 and VO₂@SiO₂-KH550-CBS-PMMA under indoor natural light, UV light of 365 nm and outdoor sunlight

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图 15 VO₂-CBS、VO₂@SiO₂-KH550-CBS和VO₂@SiO₂-KH550-CBS-PMMA薄膜湿热老化48 h在室内自然光、365 nm紫外灯及室外太阳光下的照片

Figure 15. Pictures of films of VO₂-CBS, VO₂@SiO₂-KH550-CBS and VO₂@SiO₂-KH550-CBS-PMMA under indoor natural light, UV light of 365 nm and outdoor sunlight after damp heat test for 48 h

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图 14 VO₂-CBS ((a)、(d))、VO₂@SiO₂-KH550-CBS ((b)、(e)) 和VO₂@SiO₂-KH550-CBS-PMMA薄膜 ((c)、(f)) 湿热老化48 h的透射光谱

Figure 14. Transmission spectra of films of VO₂-CBS ((a), (d)), VO₂@SiO₂-KH550-CBS ((b), (e)) and VO₂@SiO₂-KH550-CBS-PMMA ((c), (f)) after damp heat test for 48 h

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图 16 VO₂-CBS-127、VO₂@SiO₂-KH550-CBS-127和VO₂@SiO₂-KH550-CBS-127-PMMA薄膜最初(左)及紫外老化24 h(右)在室内自然光、365 nm紫外灯及室外太阳光下的照片

Figure 16. Pictures of films of VO₂-CBS-127, VO₂@SiO₂-KH550-CBS-127 and VO₂@SiO₂-KH550-CBS-127-PMMA under indoor natural light, UV light of 365 nm and outdoor sunlight after UV irradiation for 24 h

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图 17 VO₂-CBS-127、VO₂@SiO₂-KH550-CBS-127和VO₂@SiO₂-KH550-CBS-127-PMMA薄膜紫外老化前后的荧光光谱(最大激发波长λ_ex= 365 nm)

Figure 17. Fluorescence emission spectra of films of VO₂-CBS-127, VO₂@SiO₂-KH550-CBS-127 and VO₂@SiO₂-KH550-CBS-127-PMMA before and after UV irradiation for 24 h (Maximum excitation wavelength λ_ex= 365 nm)

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图 18 VO₂-CBS-127 (a)、VO₂@SiO₂-KH550-CBS-127 (b) 和VO₂@SiO₂-KH550-CBS-127-PMMA (c) 复合薄膜在0.5 mol/L H₂SO₄溶液浸泡24 h前后的照片及透射光谱

Figure 18. Pictures and transmission spectra of films of VO₂-CBS-127 (a), VO₂@SiO₂-KH550-CBS-127 (b) and VO₂@SiO₂-KH550-CBS-127-PMMA (c) after being immersed in 0.5 mol/L H₂SO₄ for 24 h

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表 1 VO₂-CBS, VO₂@SiO₂-KH550-CBS和VO₂@SiO₂-KH550-CBS-polymer复合薄膜的光学性质

Table 1. Optical property of composite films of VO₂-CBS, VO₂@SiO₂-KH550-CBS and VO₂@SiO₂-KH550-CBS-polymer

Film	T_lum/%		T_sol/%		ΔT_sol/%
Film	20℃	90℃	20℃	90℃	ΔT_sol/%
VO₂-CBS-127	68.80	69.30	71.62	65.11	6.51
VO₂@SiO₂-KH550-CBS-127	77.86	76.91	79.26	71.84	7.42
VO₂@SiO₂-KH550-CBS-127-PVB	78.94	78.97	80.24	72.55	7.69
VO₂@SiO₂-KH550-CBS-127-PVA	79.68	79.63	80.31	72.62	7.69
VO₂@SiO₂-KH550-CBS-127-PMMA	78.30	78.87	80.04	72.65	7.39
VO₂-CBS-X	73.42	73.09	75.36	68.66	6.70
VO₂@SiO₂-KH550-CBS-X	78.71	78.80	79.32	71.44	7.88
VO₂@SiO₂-KH550-CBS-127-PVB	78.23	78.85	79.16	71.74	7.42
VO₂@SiO₂-KH550-CBS-127-PVA	78.32	78.79	79.06	71.38	7.68
VO₂@SiO₂-KH550-CBS-127-PMMA	78.87	78.65	79.34	72.00	7.34
Notes: T_lum—Visible transmittance; T_sol—Solar transmittance; ΔT_sol—Solar modularity.

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表 2 湿热实验前后VO₂基复合薄膜的光学性质对比

Table 2. Comparison of the optical property of VO₂-based composite films before and after the damp heating test

Films	T_lum/%		T_sol/%		ΔT_sol/%
Films	20℃	90℃	20℃	90℃	ΔT_sol/%
VO₂-CBS-127	73.24	73.83	76.89	70.00	6.89
After damp heating test	71.54	71.27	76.59	73.57	3.02
VO₂@SiO₂-KH550-CBS-127	75.96	75.77	77.78	68.62	9.16
After damp heating test	72.95	73.40	77.02	69.49	7.53
VO₂@SiO₂-KH550-CBS-127-PMMA	74.07	74.70	76.32	67.86	8.46
After damp heating test	72.82	73.15	76.21	67.73	8.48
VO₂-CBS-X	72.86	72.44	74.84	67.73	7.11
After damp heating test	74.21	74.92	75.97	73.27	2.70
VO₂@SiO₂-KH550-CBS-X	77.15	76.61	78.48	69.39	9.09
After damp heating test	77.41	77.61	79.89	72.18	7.71
VO₂@SiO₂-KH550-CBS-127-PMMA	78.99	77.64	79.73	70.08	9.65
After damp heating test	78.59	76.79	80.58	71.08	9.50

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