Page 68 - 精细化工2020年第2期

第 37 卷第 2 期 精 细 化 工 Vol.37, No.2
202 0 年 2 月 FINE CHEMICALS Feb. 2020

功能材料
掺杂上转换纳米粒子的温敏性发光

水凝胶的制备及性能

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张 伟，廖正芳，阿尔普丁·艾尼娃尔，左 芳
（西南民族大学 化学与环境保护工程学院，四川 成都 610041）

摘要：采用水热法，以聚乙烯亚胺（PEI）为表面改性剂，合成了水分散性较好的上转换纳米粒子（UC@PEI NPs）。
考察了溶剂组成、反应时间、PEI 分子量与加入量对 UC@PEI NPs 发光强度的影响，并进行了表征。结果显示：
V(H 2 O)∶V(EG)=1∶1，PEI（M w = 10000）加入量为 1.2 g，并于 200 ℃反应 8 h 为最优合成条件。随后在 UC@PEI
NPs、聚 N-异丙基丙烯酰胺（PNIPAM）存在下，丙烯酰胺、N,N'-亚甲基双丙烯酰胺发生自由基聚合，制备复
合水凝胶，采用 SEM、拉伸试验机、发光光谱仪进行形貌、机械强度和发光温度响应性的表征。结果表明：该
互穿网络结构复合水凝胶反复脱水溶胀后，材料保持完好，平均脱水率和溶胀率为 81.18%和 61.38%；应力作用
下的应变量达到 251.10%，机械强度为 22.92 kPa；在 980 nm 近红外光激发下，当温度从 20 ℃升至 48 ℃时，
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540 nm 处（Er , S 3/2 → I 15/2 ）的发光强度减少 42.64%，而当温度下降，发光强度可逆回升。说明该复合水凝胶
具有可逆的上转换发光温度响应性，材料稳定性和拉伸性良好，并且有一定的机械强度。
关键词：水热法；上转换纳米粒子；PNIPAM；发光温度响应性；水凝胶；功能材料
中图分类号：TQ427 文献标识码：A 文章编号：1003-5214 (2020) 02-0270-08

Preparation and properties of a luminescent thermo-sensitive

hydrogel doped with upconversion nanoparticles

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Zhang Wei, Liao Zhengfang, A Erpuding·Ai Niwaer, Zuo Fang
（College of Chemistry and Environmental Protection Engineering, Southwest Minzu University, Chengdu 610041,
Sichuan ,China）

Abstract: Water-dispersive upconversion nanoparticles (UC@PEI NPs) were synthesized by hydrothermal
method using polyethyleneimine (PEI) as surface modification agent. The effects of solvent components,
reaction time, relative molecular mass (M w) of PEI and addition dosage of PEI on the luminescence
intensity were investigated. The sample was characterized. The results showed that the optimal synthesis
conditions were as follows: V(H 2O)∶V(EG)=1∶1, PEI (M w=10000) dosage 1.2 g, reaction temperature
200 ℃, and reaction time 8 h. Subsequently, a composite hydrogel was prepared from acrylamide and
N,N'-methylenebisacrylamide by free radical polymerization in the presence of UC@PEI NPs and
poly(N-isopropylacrylamide) (PNIPAM). The morphology, mechanical strength and luminescent thermo-
sensitive of composite hydrogel were characterized by SEM, tensile testing machine and luminescence
spectrometer. It was found that the composite hydrogel with interpenetrating network structure still
remained intact after repeated dehydration and swelling, and the average dehydration ratio and swelling
ratio were 81.18% and 61.38%, respectively. The strain under stress was 251.10%, and the mechanical
strength was 22.92 kPa. Under the excitation of 980 nm NIR laser, the luminescence intensity of composite
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hydrogel at 540 nm (Er , S 3/2→ I 15/2) was decreased by 42.64% when the temperature rised from 20 ℃ to
48 ℃. While the luminescence intensity could be reversibly recovered when the temperature dropped. The
results indicated that the composite hydrogel had a reversible upconversion luminescent thermo-sensitive

收稿日期：2019-07-08; 定用日期：2019-08-27; DOI: 10.13550/j.jxhg.20190657
基金项目：西南民族大学研究生创新型科研项目（CX2018SZ127）
作者简介：张 伟（1994─），男，硕士生，E-mail：polymerzw@163.com。联系人：左 芳（1980─），女，研究员，E-mail：
polymerzf@swun.cn。