CN111206414A - 基于稀土掺杂上转换纳米材料的荧光纤维及其制备方法 - Google Patents
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Abstract
本发明公开了一种基于稀土掺杂上转换纳米材料的荧光纤维，将聚多巴胺改性纤维首先浸渍在GPTMS修饰YF3:Yb,Er纳米晶胶体溶液中30‑60min，取出后用乙醇反复冲洗，再次浸渍在PEI修饰YF3:Yb,Er纳米晶胶体溶液中30‑60min；重复上述组装过程，即可制备得到基于稀土掺杂上转换纳米材料的荧光纤维。本发明赋予纤维上转换荧光性能，在防伪纺织品领域有重要的应用价值。
Description
技术领域
本发明涉及基于稀土掺杂上转换纳米材料的荧光纤维及其制备方法，属纤维材料领域。
背景技术
稀土掺杂上转换纳米材料(upconversion nanoparticles，UCNPs)由于其生物体毒性低、背景荧光弱、灵敏度高、化学稳定性高、光稳定性好、光穿透能力强、Stokes位移大等优点，成为了新一代荧光纳米材料(功能材料,2017,48(05):5028-5036)，在免疫分析、生物标记、生物传感、生物成像、药物载体、光动力治疗、光热治疗、光导开关、信息存储、食品安全检测、光催化以及太阳能电池等领域有着广泛的研究和应用(化学进展,2016,28(11):1615-1625)。
UCNPs在纺织领域的研究和应用也有少量文献报道。中国发明专利CN201410701957.9一种荧光沙柳再生纤维素纤维及其制备方法将UCNPs添加到纺丝液中，通过高效共混、湿法纺丝技术制备得到具有优异荧光性能的纤维。但是共混纺丝法只适用于合成纤维，其应用范围受到限制。此外，UCNPs在纺丝液中团聚的难题也很难解决(化学进展,2017,29(08):892-901)。
中国发明专利CN201710836604.3利用MoO3:Yb,Er/Tm之间的静电作用作为成膜推动力，将纤维依次浸渍在带正电的MoO3:Yb,Er/Tm胶体溶液和带负电的MoO3:Yb,Er/Tm胶体溶液中，根据需要决定纤维表面MoO3:Yb,Er/Tm组装的层数，从而赋予纤维上转换荧光性能。但是基于静电引力或者氢键作用的弱超分子相互作用导致多层膜的稳定性不高，构筑基元间缺乏较为牢固的结合力，导致多层膜在较为严苛的条件下(如高离子强度、强酸、强碱、氧化还原剂等)会遭到破坏，从而限制了静电层层自组装技术的进一步应用(ChemicalSociety Reviews,2018,47(13):5061-5098)。
发明内容
本发明针对上述不足，提供一种基于稀土掺杂上转换纳米材料的荧光纤维。
本发明通过下述技术方案予以实现：(1)将平均粒径1-20nm的无表面配体YF3:Yb,Er纳米晶与PEI混合，匀速搅拌12-24h后，使用乙醇反复清洗、离心、真空干燥，得到PEI修饰YF3:Yb,Er纳米晶；(2)将平均粒径80-100nm的无表面配体YF3:Yb,Er纳米晶与GPTMS混合，匀速搅拌12-24h后，使用乙醇反复清洗、离心、真空干燥，得到GPTMS修饰YF3:Yb,Er纳米晶；(3)配制1wt％-5wt％的多巴胺Tris-HCl缓冲液，调节pH值至8.5，将纤维浸渍在上述缓冲液中12-24h，浴比1:50，使用乙醇反复清洗、离心、真空干燥，制备得到聚多巴胺改性纤维；(4)将PEI修饰YF3:Yb,Er纳米晶和GPTMS修饰YF3:Yb,Er纳米晶分别配制成质量分数0.1％-1％的胶体溶液，然后将上述聚多巴胺改性纤维首先浸渍在GPTMS修饰YF3:Yb,Er纳米晶胶体溶液中30-60min，取出后用乙醇反复冲洗，再次浸渍在PEI修饰YF3:Yb,Er纳米晶胶体溶液中30-60min；重复上述组装过程，最终制备得到基于稀土掺杂上转换纳米材料的荧光纤维。
无表面基团/无表面配体的UCNPs为现有技术，市场上也有南京先丰纳米材料科技有限公司等出售相关产品。目前去除UCNPs表面的配体/基团的方法主要有以下三种：(1)超声法：该方法需要掌握好超声的时间和强度，超声时间过短不能完全去除UCNPs表面的配体/基团，超声时间过长容易造成UCNPs团聚。(2)四氟硼酸亚硝鎓NOBF4处理，可参见中国发明专利CN201410701945.6。(3)酸处理(pH＝4)，可参见中国发明专利CN201310153965.X。
与现有技术相比，本发明的优点在于：(1)聚多巴胺改性纤维和GPTMS修饰YF3:Yb,Er纳米晶，GPTMS修饰YF3:Yb,Er纳米晶和PEI修饰YF3:Yb,Er纳米晶之间均通过共价键结合。相比于常规的静电引力和氢键作用力，共价键结合大大提高了YF3:Yb,Er纳米晶多层膜的稳定性和吸附牢度。(2)分别选用平均粒径不同的YF3:Yb,Er纳米晶进行层层自组装，YF3:Yb,Er纳米晶之间穿插交互排列，进一步提高了YF3:Yb,Er纳米晶之间的附着牢度。
具体实施方式
下面结合具体实施方式，进一步阐述本发明。
实施例1
(1)将平均粒径5nm的无表面配体YF3:Yb,Er纳米晶与PEI混合，匀速搅拌12h后，使用乙醇反复清洗、离心、真空干燥，得到PEI修饰YF3:Yb,Er纳米晶；(2)将平均粒径80nm的无表面配体YF3:Yb,Er纳米晶与GPTMS混合，匀速搅拌12h后，使用乙醇反复清洗、离心、真空干燥，得到GPTMS修饰YF3:Yb,Er纳米晶；(3)配制1wt％的多巴胺Tris-HCl缓冲液，调节pH值至8.5，将纤维浸渍在上述缓冲液中12h，浴比1:50，使用乙醇反复清洗、离心、真空干燥，制备得到聚多巴胺改性纤维；(4)将上述聚多巴胺改性纤维首先浸渍在质量分数0.1％的GPTMS修饰YF3:Yb,Er纳米晶胶体溶液中30min，取出后用乙醇反复冲洗，再次浸渍在质量分数0.1％的PEI修饰YF3:Yb,Er纳米晶胶体溶液中30min，最终制备得到基于稀土掺杂上转换纳米材料的荧光纤维。
实施例2
(1)将平均粒径10nm的无表面配体YF3:Yb,Er纳米晶与PEI混合，匀速搅拌18h后，使用乙醇反复清洗、离心、真空干燥，得到PEI修饰YF3:Yb,Er纳米晶。(2)将平均粒径90nm的无表面配体YF3:Yb,Er纳米晶与GPTMS混合，匀速搅拌18h后，使用乙醇反复清洗、离心、真空干燥，得到GPTMS修饰YF3:Yb,Er纳米晶。(3)配制3wt％的多巴胺Tris-HCl缓冲液，调节pH值至8.5，将纤维浸渍在上述缓冲液中18h，浴比1:50，使用乙醇反复清洗、离心、真空干燥，制备得到聚多巴胺改性纤维。(4)将PEI修饰YF3:Yb,Er纳米晶和GPTMS修饰YF3:Yb,Er纳米晶分别配制成质量分数0.5％的胶体溶液，然后将上述聚多巴胺改性纤维首先浸渍在GPTMS修饰YF3:Yb,Er纳米晶胶体溶液中45min，取出后用乙醇反复冲洗，再次浸渍在PEI修饰YF3:Yb,Er纳米晶胶体溶液中45min；重复3次上述聚多巴胺改性纤维在GPTMS修饰YF3:Yb,Er纳米晶/PEI修饰YF3:Yb,Er纳米晶中的组装过程，最终制备得到基于稀土掺杂上转换纳米材料的荧光纤维。
实施例3
(1)将平均粒径20nm的无表面配体YF3:Yb,Er纳米晶与PEI混合，匀速搅拌24h后，使用乙醇反复清洗、离心、真空干燥，得到PEI修饰YF3:Yb,Er纳米晶；(2)将平均粒径100nm的无表面配体YF3:Yb,Er纳米晶与GPTMS混合，匀速搅拌24h后，使用乙醇反复清洗、离心、真空干燥，得到GPTMS修饰YF3:Yb,Er纳米晶；(3)配制5wt％的多巴胺Tris-HCl缓冲液，调节pH值至8.5，将纤维浸渍在上述缓冲液中24h，浴比1:50，使用乙醇反复清洗、离心、真空干燥，制备得到聚多巴胺改性纤维；(4)将上述聚多巴胺改性纤维首先浸渍在质量分数1％的GPTMS修饰YF3:Yb,Er纳米晶胶体溶液中60min，取出后用乙醇反复冲洗，再次浸渍在质量分数1％的PEI修饰YF3:Yb,Er纳米晶胶体溶液中60min；重复5次上述聚多巴胺改性纤维在GPTMS修饰YF3:Yb,Er纳米晶/PEI修饰YF3:Yb,Er纳米晶中的组装过程，最终制备得到基于稀土掺杂上转换纳米材料的荧光纤维。
显然，本发明的上述实施例仅仅是为清楚地说明本发明所作的举例，而并非是对本发明的实施方式的限定。对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无法对所有的实施方式予以穷举。凡是属于本发明的技术方案所引申出的显而易见的变化或变动仍处于本发明的保护范围之列。
Claims (4)
1.一种基于稀土掺杂上转换纳米材料的荧光纤维的制备方法，其特征在于：
S1，将YF3:Yb,Er纳米晶与PEI混合，匀速搅拌12-24h后，使用乙醇反复清洗、离心、真空干燥，得到PEI修饰YF3:Yb,Er纳米晶；
S2，将YF3:Yb,Er纳米晶与GPTMS混合，匀速搅拌12-24h后，使用乙醇反复清洗、离心、真空干燥，得到GPTMS修饰YF3:Yb,Er纳米晶；
S3，配制1wt％-5wt％的多巴胺Tris-HCl缓冲液，调节pH值至8.5，将纤维浸渍在上述缓冲液中12-24h，浴比1:50，使用乙醇反复清洗、离心、真空干燥，制备得到聚多巴胺改性纤维；
S4，将PEI修饰YF3:Yb,Er纳米晶和GPTMS修饰YF3:Yb,Er纳米晶分别配制成质量分数0.1％-1％的胶体溶液，然后将上述聚多巴胺改性纤维首先浸渍在GPTMS修饰YF3:Yb,Er纳米晶胶体溶液中30-60min，取出后用乙醇反复冲洗，再次浸渍在PEI修饰YF3:Yb,Er纳米晶胶体溶液中30-60min；重复上述组装过程，最终制备得到基于稀土掺杂上转换纳米材料的荧光纤维。
2.根据权利要求1所述的基于稀土掺杂上转换纳米材料的荧光纤维的制备方法，其特征在于，所述S1中YF3:Yb,Er纳米晶无表面配体，平均粒径1-20nm。
3.根据权利要求1所述的基于稀土掺杂上转换纳米材料的荧光纤维的制备方法，其特征在于，所述S2中YF3:Yb,Er纳米晶无表面配体，平均粒径80-100nm。
4.按权利要求1制备方法得到的基于稀土掺杂上转换纳米材料的荧光纤维。
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