Photocontrolled Aggregation Induced Emission of Hexathiobenzene Hexapyridine in Organic Phase

{ "defaultlang": "zh", "titlegroup": { "articletitle": [ { "lang": "zh", "data": [ { "name": "text", "data": "六硫苯六吡啶在有机相中的光控聚集诱导发光行为" } ] }, { "lang": "en", "data": [ { "name": "text", "data": "Photocontrolled Aggregation Induced Emission of Hexathiobenzene Hexapyridine in Organic Phase" } ] } ] }, "contribgroup": { "author": [ { "name": [ { "lang": "zh", "surname": "周", "givenname": "璐璐", "prefix": "" }, { "lang": "en", "surname": "ZHOU", "givenname": "Lu-lu", "namestyle": "eastern", "prefix": "" } ], "stringName": [], "aff": [], "role": [ "first-author" ], "bio": [ { "lang": "zh", "text": [ "周璐璐(1996－)，女，安徽马鞍山人，博士研究生，2018年于北京化工大学获得学士学位，主要从事物理发光材料的研究。E-mail: 18110440017@fudan.edu.cn" ], "graphic": [ { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21348545&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21348540&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21348545&type=" } ], "data": [ [ { "name": "text", "data": "周璐璐" }, { "name": "text", "data": "(1996－)，女，安徽马鞍山人，博士研究生，2018年于北京化工大学获得学士学位，主要从事物理发光材料的研究。E-mail: " }, { "name": "text", "data": "18110440017@fudan.edu.cn" } ] ] } ], "email": "18110440017@fudan.edu.cn", "deceased": false }, { "name": [ { "lang": "zh", "surname": "吴", "givenname": "斌", "prefix": "" }, { "lang": "en", "surname": "WU", "givenname": "Bin", "namestyle": "eastern", "prefix": "" } ], "stringName": [], "aff": [], "role": [], "deceased": false }, { "name": [ { "lang": "zh", "surname": "李", "givenname": "安泽", "prefix": "" }, { "lang": "en", "surname": "LI", "givenname": "An-ze", "namestyle": "eastern", "prefix": "" } ], "stringName": [], "aff": [], "role": [], "deceased": false }, { "name": [ { "lang": "zh", "surname": "罗", "givenname": "梦恺", "prefix": "" }, { "lang": "en", "surname": "LUO", "givenname": "Meng-kai", "namestyle": "eastern", "prefix": "" } ], "stringName": [], "aff": [], "role": [], "deceased": false }, { "name": [ { "lang": "zh", "surname": "朱", "givenname": "亮亮", "prefix": "" }, { "lang": "en", "surname": "ZHU", "givenname": "Liang-liang", "namestyle": "eastern", "prefix": "" } ], "stringName": [], "aff": [], "role": [ "corresp", "corresp" ], "corresp": [ { "rid": "cor1", "lang": "zh", "text": "朱亮亮(1982－)，男，浙江舟山人， 2005年本科毕业于浙江大学化学系， 2011年在华东理工大学应用化学专业获得博士学位。在相继完成新加坡南洋理工大学和美国哥伦比亚大学的博士后工作之后，于2015年起任复旦大学高分子科学系和聚合物分子工程国家重点实验室研究员，独立课题组负责人。入选第十二批国家海外高层次青年人才以及2017年国家重点研发计划青年科学家项目研究骨干，也曾获多项国家和地方项目资助。担任《中国化学快报》第二届和第三届青年编委会有机高分子材料专业委员会副主任、《中国科学：化学》第三届青年编委及国际期刊Dyes and Pigments编委。主要从事功能自组装发光材料化学的研究。在PNAS, Nat. Commun., Sci. Adv., JACS, Angewandte Chemie, Adv. Mater., Chem. Sci.等期刊发表科技论文近百篇。指导的博士生/博士后已有多人先后取得高校教职。", "data": [ { "name": "text", "data": "朱亮亮(1982－)，男，浙江舟山人， 2005年本科毕业于浙江大学化学系， 2011年在华东理工大学应用化学专业获得博士学位。在相继完成新加坡南洋理工大学和美国哥伦比亚大学的博士后工作之后，于2015年起任复旦大学高分子科学系和聚合物分子工程国家重点实验室研究员，独立课题组负责人。入选第十二批国家海外高层次青年人才以及2017年国家重点研发计划青年科学家项目研究骨干，也曾获多项国家和地方项目资助。担任《中国化学快报》第二届和第三届青年编委会有机高分子材料专业委员会副主任、《中国科学：化学》第三届青年编委及国际期刊Dyes and Pigments编委。主要从事功能自组装发光材料化学的研究。在PNAS, Nat. Commun., Sci. Adv., JACS, Angewandte Chemie, Adv. Mater., Chem. Sci.等期刊发表科技论文近百篇。指导的博士生/博士后已有多人先后取得高校教职。" } ] }, { "rid": "cor2", "lang": "en", "text": "E-mail: zhuliangliang@fudan.edu.cn", "data": [ { "name": "text", "data": "E-mail: zhuliangliang@fudan.edu.cn" } ] } ], "bio": [ { "lang": "zh", "text": [ "朱亮亮(1982－)，男，浙江舟山人，博士，研究员，2011年于华东理工大学获得博士学位，主要从事功能自组装发光材料化学的研究。E-mail: zhuliangliang@fudan.edu.cn" ], "graphic": [ { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21348556&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21348552&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21348556&type=" } ], "data": [ [ { "name": "text", "data": "朱亮亮" }, { "name": "text", "data": "(1982－)，男，浙江舟山人，博士，研究员，2011年于华东理工大学获得博士学位，主要从事功能自组装发光材料化学的研究。E-mail: " }, { "name": "text", "data": "zhuliangliang@fudan.edu.cn" } ] ] } ], "email": "zhuliangliang@fudan.edu.cn", "deceased": false } ], "aff": [ { "id": "aff1", "intro": [ { "lang": "zh", "text": "复旦大学 高分子科学系， 聚合物分子工程国家重点实验室， 上海 　 200438", "data": [ { "name": "text", "data": "复旦大学 高分子科学系， 聚合物分子工程国家重点实验室， 上海 　 200438" } ] }, { "lang": "en", "text": "State Key Laboratory of Molecular Engineering of Polymers, Department of Macromolecular Science, Fudan University, Shanghai 200438, China", "data": [ { "name": "text", "data": "State Key Laboratory of Molecular Engineering of Polymers, Department of Macromolecular Science, Fudan University, Shanghai 200438, China" } ] } ] } ] }, "abstracts": [ { "lang": "zh", "data": [ { "name": "p", "data": [ { "name": "text", "data": "以六硫苯作为母核，采用多步合成法制得了一种在有机溶剂中具有光控聚集诱导发光(AIE)行为的衍生物六硫苯六吡啶(6SB6Py)。该化合物在无外加能量参与的前提下，可均匀分散于有机溶剂DMF和DMSO中，在此状态下几乎不发光。施加365 nm光照后，两个有机相体系的发光强度均增强5～10倍。其中，6SB6Py的DMF溶液在500 nm处为单峰发射，而6SB6Py的DMSO溶液在420 nm和500 nm处均有发射峰。体系光照前后的核磁对比图几乎无变化，说明365 nm光照并没有使得体系发生传统的光化学反应。动态光散射数据表明，随着光照时间的增加，6SB6Py在溶液中的聚集状态也在不断改变。这说明外加光导致6SB6Py有机溶液发光增强的原因是一种新颖的机制——光激发分子重组，而非光化学反应。" } ] } ] }, { "lang": "en", "data": [ { "name": "p", "data": [ { "name": "text", "data": "A derivative of hexathiobenzene, named hexathiobenzene hexapyridine(6SB6Py) that can exhibit a photocontrolled aggregation-induced emission(AIE) behavior in organic phase, was prepared by a multi-step synthesis method. This compound can be dispersed in organic solvents DMF and DMSO with barely glows. However, the emission intensity is enhanced by 5 to 10 times after 365 nm irradiation. Among them, the DMF solution of 6SB6Py shows a single peak emission at 500 nm, whereas the DMSO solution of 6SB6Py has double emission peaks at both 420 nm and 500 nm. The almost unchanged " }, { "name": "sup", "data": [ { "name": "text", "data": "1" } ] }, { "name": "text", "data": "H NMR signal before and after irradiation indicates that 365 nm light has not caused a traditional photochemical reaction of this system. Dynamic light scattering data also show the aggregation size of 6SB6Py in the solution is changed with the increase of irradiation time. It suggested that the effect of photoinduced molecular realignment caused the enhanced emission of 6SB6Py by external light in organic solutions, instead of a photochemical reaction." } ] } ] } ], "keyword": [ { "lang": "zh", "data": [ [ { "name": "text", "data": "聚集诱导发光" } ], [ { "name": "text", "data": "有机溶剂" } ], [ { "name": "text", "data": "分散态" } ], [ { "name": "text", "data": "聚集态" } ], [ { "name": "text", "data": "光激发分子重组" } ] ] }, { "lang": "en", "data": [ [ { "name": "text", "data": "aggregation-induced luminescence" } ], [ { "name": "text", "data": "organic solvents" } ], [ { "name": "text", "data": "dispersed state" } ], [ { "name": "text", "data": "aggregated state" } ], [ { "name": "text", "data": "photoinduced molecular realignment" } ] ] } ], "highlights": [], "body": [ { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "1　引言" } ], "level": "1", "id": "s1" } }, { "name": "p", "data": [ { "name": "text", "data": "随着科学技术的快速发展，荧光材料这一类特殊材料越来越多地走进人们的视野，并且在生活、医学、电子信息技术等方面有着非常广泛的应用" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "blockXref", "data": { "data": [ { "name": "xref", "data": { "text": "1", "type": "bibr", "rid": "R1", "data": [ { "name": "text", "data": "1" } ] } }, { "name": "text", "data": "-" }, { "name": "xref", "data": { "text": "6", "type": "bibr", "rid": "R6", "data": [ { "name": "text", "data": "6" } ] } } ], "rid": [ "R1", "R2", "R3", "R4", "R5", "R6" ], "text": "1-6", "type": "bibr" } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。但是传统荧光材料，如罗丹明、香豆素等都存在着一个共同弊端——聚集荧光猝灭(ACQ)" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "blockXref", "data": { "data": [ { "name": "xref", "data": { "text": "7", "type": "bibr", "rid": "R7", "data": [ { "name": "text", "data": "7" } ] } }, { "name": "text", "data": "-" }, { "name": "xref", "data": { "text": "9", "type": "bibr", "rid": "R9", "data": [ { "name": "text", "data": "9" } ] } } ], "rid": [ "R7", "R8", "R9" ], "text": "7-9", "type": "bibr" } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。这主要是因为荧光分子一般都具有平面的稠环结构，导致它们很难通过发生分子内运动来消耗能量，所以当在良溶剂中呈分散状态时，分子会通过辐射跃迁发出荧光来达到消耗能量的目的，此时会发出较强荧光。而当它们处于聚集状态时(如处于不良溶剂或固体状态下)，各分子之间相互碰撞从而导致能量转移，分子无需辐射跃迁便消耗了能量，此时则表现为荧光猝灭的现象。也正是由于传统荧光分子的这一特性，导致其应用范围大大受限。直到唐本忠等" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "10", "type": "bibr", "rid": "R10", "data": [ { "name": "text", "data": "10" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "发现了一类具有聚集诱导发光(AIE)性能的荧光材料，才成功解决了传统荧光材料的这一弊端。这种材料只有在聚集状态下才会有较强荧光，其机理解释目前被广为接受的仍是唐本忠等" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "2", "type": "bibr", "rid": "R2", "data": [ { "name": "text", "data": "2" } ] } }, { "name": "text", "data": "," }, { "name": "blockXref", "data": { "data": [ { "name": "xref", "data": { "text": "10", "type": "bibr", "rid": "R10", "data": [ { "name": "text", "data": "10" } ] } }, { "name": "text", "data": "-" }, { "name": "xref", "data": { "text": "12", "type": "bibr", "rid": "R12", "data": [ { "name": "text", "data": "12" } ] } } ], "rid": [ "R10", "R11", "R12" ], "text": "10-12", "type": "bibr" } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "提出的分子内运动受限模型(RIM)。这类AIE材料目前也在不同领域得到了广泛应用" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "blockXref", "data": { "data": [ { "name": "xref", "data": { "text": "13", "type": "bibr", "rid": "R13", "data": [ { "name": "text", "data": "13" } ] } }, { "name": "text", "data": "-" }, { "name": "xref", "data": { "text": "17", "type": "bibr", "rid": "R17", "data": [ { "name": "text", "data": "17" } ] } } ], "rid": [ "R13", "R14", "R15", "R16", "R17" ], "text": "13-17", "type": "bibr" } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。" } ] }, { "name": "p", "data": [ { "name": "text", "data": "本课题组基于一类以六硫苯为母核的系列衍生物，对其AIE性能进行研究。我们此前对以六硫苯为母核的3种衍生物乙酰胺、酰胺和N-甲基甲酰胺在不同配比的DMF/H" }, { "name": "sub", "data": [ { "name": "text", "data": "2" } ] }, { "name": "text", "data": "O中的发光性能进行了实验(其中DMF为良溶剂，H" }, { "name": "sub", "data": [ { "name": "text", "data": "2" } ] }, { "name": "text", "data": "O为不良溶剂)" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "18", "type": "bibr", "rid": "R18", "data": [ { "name": "text", "data": "18" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "，结果发现3种衍生物都会随着H" }, { "name": "sub", "data": [ { "name": "text", "data": "2" } ] }, { "name": "text", "data": "O含量的提高而呈现出发光增强的趋势，说明了这类结构的AIE通性。之后我们合成了一种以六硫苯为母核的水溶性衍生物——羧酸钠" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "19", "type": "bibr", "rid": "R19", "data": [ { "name": "text", "data": "19" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "，并对其水溶液的发光性能进行实验与测试，发现当对其施加光照时，溶液光强迅速升高，而当光照撤出时，溶液光强恢复初始状态。我们首次论证了这个现象背后的光激发分子重组机理，这种重组导致了AIE性质开关式的变化。我们利用这一特殊性能成功实现了闪动荧光，增强了荧光探针的可视化效果，对今后生物荧光标记具有推动作用。" } ] }, { "name": "p", "data": [ { "name": "text", "data": "为了进一步拓展这种光控AIE性质的适用范围，本文以结构修饰拓展出发，合成了一种以六硫苯为母核的六吡啶衍生物(6SB6Py)，并分别对其在DMF和DMSO中的光控发光性能进行了研究与实验。实验结果表明，6SB6Py在有机溶剂中也能通过引入光照来激发分子重组，从而达到控制光强和AIE性质的目的。" } ] } ] }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "2　实验" } ], "level": "1", "id": "s2" } }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "2.1　原料" } ], "level": "2", "id": "s2a" } }, { "name": "p", "data": [ { "name": "text", "data": "实验中使用的化学试剂主要有：对巯基苯甲酸乙酯、六氟苯、无水乙醇、乙酸乙酯(EA)、氨基吡啶、2-(7-氮杂苯并三氮唑)-N，N，N′，N′-四甲基脲六氟磷酸酯(HATU)、N，N-二异丙基乙胺(DIPEA)、碘甲烷(CH" }, { "name": "sub", "data": [ { "name": "text", "data": "3" } ] }, { "name": "text", "data": "I)。" } ] } ] }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "2.2　合成" } ], "level": "2", "id": "s2b" } }, { "name": "p", "data": [ { "name": "text", "data": "按10∶1的化学计量比准确称取对巯基苯甲酸乙酯和六氟苯溶于适量DMF(保证原料全部溶解)中，并按与六氟苯化学计量比25∶1加入无水K" }, { "name": "sub", "data": [ { "name": "text", "data": "2" } ] }, { "name": "text", "data": "CO" }, { "name": "sub", "data": [ { "name": "text", "data": "3" } ] }, { "name": "text", "data": "，置于70 ℃ Ar体系下，搅拌反应48 h。再加入过量水沉淀，过滤出沉淀后，用无水乙醇反复冲洗，得到产物1。随后将得到的纯净产物1完全溶解于适量THF中，按照一定比例滴加提前配置好的NaOH水溶液，整个体系在50 ℃水浴条件下搅拌反应10 h。再加入过量稀盐酸沉淀，过滤出沉淀后，用去离子水、乙酸乙酯和无水乙醇反复冲洗，得到产物2，为黄色粉末状固体。将得到的产物2与按一定化学计量比称取好的氨基吡啶溶解于适量的DMF中，再加入已经计算好量的HATU和DIPEA，随后将整个体系置于室温，Ar体系下，搅拌过夜反应。之后于80 ℃旋干得到淡黄色粉末状固体。用去离子水反复冲洗该沉淀，最终得到6SB6Py(见" }, { "name": "xref", "data": { "text": "图1", "type": "fig", "rid": "F1", "data": [ { "name": "text", "data": "图1" } ] } }, { "name": "text", "data": ")，产率为58.3%。" } ] }, { "name": "fig", "data": { "id": "F1", "caption": [ { "lang": "zh", "label": [ { "name": "text", "data": "图1" } ], "title": [ { "name": "text", "data": "6SB6Py合成示意图" } ] }, { "lang": "en", "label": [ { "name": "text", "data": "Fig.1" } ], "title": [ { "name": "text", "data": "Synthesis diagram of 6SB6Py" } ] } ], "subcaption": [], "note": [], "graphics": [ { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21348561&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21348571&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21348567&type=" } ] } } ] }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "2.3　测试仪器" } ], "level": "2", "id": "s2c" } }, { "name": "p", "data": [ { "name": "text", "data": "核磁共振使用Bruker AVANCEⅢHD 400MHz型核磁共振仪检测，用TMS作为内标，以氘代DMSO和氘代DMF为测试溶剂，" }, { "name": "sup", "data": [ { "name": "text", "data": "1" } ] }, { "name": "text", "data": "H NMR的共振频率为400 MHz；基质辅助激光解吸-串联飞行时间质谱测试(MALDI-TOF-MS)采用ABSCIEX 5800型质谱仪，样品溶解在四氢呋喃中，然后滴在测试板上蒸干溶剂进行测试；紫外-可见吸收光谱(UV/Vis)采用岛津1800型分光光度计测试；荧光发射光谱和寿命测试采用爱丁堡FLS1000荧光光谱仪；粒径测试采用Nano-Zeta Potential Analyzer ZS-90。" } ] } ] } ] }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "3　结果与讨论" } ], "level": "1", "id": "s3" } }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "3.1　结构表征" } ], "level": "2", "id": "s3a" } }, { "name": "p", "data": [ { "name": "xref", "data": { "text": "图2", "type": "fig", "rid": "F2", "data": [ { "name": "text", "data": "图2" } ] } }, { "name": "text", "data": "为最终产物6SB6Py的核磁共振氢谱图，经分析该分子为轴对称结构，应共有5种化学环境的氢，而核磁谱图中仅有4个对应的质子峰。这是由于苯环上的两种氢因为吡啶等基团的引入而发生了化学位移，导致其化学位移相近，呈现出一个质子峰。其中分子中各化学环境的氢与质子峰的对应关系如图所示。同时，对谱图进行积分，发现找到的各个质子峰的谱图峰面积之比与理论峰面积之比基本一致，为" }, { "name": "italic", "data": [ { "name": "text", "data": "S" } ] }, { "name": "sub", "data": [ { "name": "text", "data": "a，b" } ] }, { "name": "text", "data": "∶" }, { "name": "italic", "data": [ { "name": "text", "data": "S" } ] }, { "name": "sub", "data": [ { "name": "text", "data": "c" } ] }, { "name": "text", "data": "∶" }, { "name": "italic", "data": [ { "name": "text", "data": "S" } ] }, { "name": "sub", "data": [ { "name": "text", "data": "d" } ] }, { "name": "text", "data": "∶" }, { "name": "italic", "data": [ { "name": "text", "data": "S" } ] }, { "name": "sub", "data": [ { "name": "text", "data": "e" } ] }, { "name": "text", "data": "＝4∶1∶2∶2。这说明实验中合成的6SB6Py较为纯净，可投入后续测试。" } ] }, { "name": "fig", "data": { "id": "F2", "caption": [ { "lang": "zh", "label": [ { "name": "text", "data": "图2" } ], "title": [ { "name": "text", "data": "6SB6Py的核磁共振氢谱图(DMSO-" }, { "name": "italic", "data": [ { "name": "text", "data": "d" } ] }, { "name": "sub", "data": [ { "name": "text", "data": "6" } ] }, { "name": "text", "data": ")" } ] }, { "lang": "en", "label": [ { "name": "text", "data": "Fig.2" } ], "title": [ { "name": "sup", "data": [ { "name": "text", "data": "1" } ] }, { "name": "text", "data": "H NMR spectrum of 6SB6Py(in DMSO-" }, { "name": "italic", "data": [ { "name": "text", "data": "d" } ] }, { "name": "sub", "data": [ { "name": "text", "data": "6" } ] }, { "name": "text", "data": ")" } ] } ], "subcaption": [], "note": [], "graphics": [ { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21348576&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21348587&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21348581&type=" } ] } }, { "name": "p", "data": [ { "name": "xref", "data": { "text": "图3", "type": "fig", "rid": "F3", "data": [ { "name": "text", "data": "图3" } ] } }, { "name": "text", "data": "为产物6SB6Py的质谱图，对其分子式进行分析可知，它的分子量为1 447。从" }, { "name": "xref", "data": { "text": "图3", "type": "fig", "rid": "F3", "data": [ { "name": "text", "data": "图3" } ] } }, { "name": "text", "data": "的MALDI-TOF图中可以清晰地看到分子离子峰1 447.55，这也再次说明合成的准确性与可信度。质谱图中分子峰1 217.46经解析，为6SB6Py在核心苯环处断裂一处C—S键得到的碎片峰。" } ] }, { "name": "fig", "data": { "id": "F3", "caption": [ { "lang": "zh", "label": [ { "name": "text", "data": "图3" } ], "title": [ { "name": "text", "data": "6SB6Py的质谱图" } ] }, { "lang": "en", "label": [ { "name": "text", "data": "Fig.3" } ], "title": [ { "name": "text", "data": "Mass spectrum of 6SB6Py" } ] } ], "subcaption": [], "note": [], "graphics": [ { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21348592&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21348601&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21348597&type=" } ] } } ] }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "3.2　发光性质" } ], "level": "2", "id": "s3b" } }, { "name": "p", "data": [ { "name": "text", "data": "实验中研究6SB6Py的AIE性能采用的方法是将其溶解在良溶剂中，通过外加光照来调节其聚集行为，从而调节其发光行为。由于6SB6Py为脂溶性化合物，分别用DMF和DMSO作为溶剂来研究其在分散态下的光控行为。在两溶液浓度都为10" }, { "name": "sup", "data": [ { "name": "text", "data": "－5" } ] }, { "name": "text", "data": " mol/L的条件下，向两体系分别施加365 nm光照30 min，并对光照前后的发射光谱均进行了测试，得到测试结果如" }, { "name": "xref", "data": { "text": "图4(a)", "type": "fig", "rid": "F4", "data": [ { "name": "text", "data": "图4(a)" } ] } }, { "name": "text", "data": "和" }, { "name": "xref", "data": { "text": "图4(b)", "type": "fig", "rid": "F4", "data": [ { "name": "text", "data": "图4(b)" } ] } }, { "name": "text", "data": "。" }, { "name": "xref", "data": { "text": "图4(a)", "type": "fig", "rid": "F4", "data": [ { "name": "text", "data": "图4(a)" } ] } }, { "name": "text", "data": "为6SB6Py在DMF中光照前后的发射谱图，从图中可以看到当6SB6Py在DMF中均匀分散时，溶液几乎不发光。而在365 nm光照射30 min后，溶液光强迅速提升，表现为在波长500 nm处有一个强发射峰。" }, { "name": "xref", "data": { "text": "图4(b)", "type": "fig", "rid": "F4", "data": [ { "name": "text", "data": "图4(b)" } ] } }, { "name": "text", "data": "为6SB6Py在DMSO中光照前后的发射谱图，同样表现为在分散状态下几乎不发光，而当施加365 nm光照30 min后，溶液光强增大。光照后的发射光谱不仅在波长500 nm处升起一个强发射峰，同时在波长为420 nm处有一个新发射峰。此外，分别对两种溶液光照后的发光寿命进行了检测，实验数据如" }, { "name": "xref", "data": { "text": "图4(c)～(e)", "type": "fig", "rid": "F4", "data": [ { "name": "text", "data": "图4(c)～(e)" } ] } }, { "name": "text", "data": "。从寿命图中可以看到6SB6Py的DMF溶液在365 nm光照半小时后，在波长500 nm处的寿命约为8.93 μs，即光照后溶液发磷光。6SB6Py的DMSO溶液在365 nm光照半小时后，同样是在500 nm处有磷光峰，寿命约为173.1 μs。而在420 nm处寿命约为5.35 ns，即为荧光峰。从TEM图(" }, { "name": "xref", "data": { "text": "图4(f)～(g)", "type": "fig", "rid": "F4", "data": [ { "name": "text", "data": "图4(f)～(g)" } ] } }, { "name": "text", "data": ")中可以看出，在保证6SB6Py的DMF溶液和DMSO溶液浓度均为10" }, { "name": "sup", "data": [ { "name": "text", "data": "－5" } ] }, { "name": "text", "data": " mol/L的前提下，二者的聚集状态有所不同。6SB6Py在DMF溶液中多以片状或不规则形状呈现，而在DMSO溶液中则多聚集为椭圆形态。这说明6SB6Py在两种溶液中所呈现出来的不同光学性质，可能与其在两溶液中的不同聚集形貌相关。" } ] }, { "name": "fig", "data": { "id": "F4", "caption": [ { "lang": "zh", "label": [ { "name": "text", "data": "图4" } ], "title": [ { "name": "text", "data": "6SB6Py的DMF溶液(a)和DMSO溶液(b)光照前后的发射谱图；6SB6Py的DMF溶液(c)和DMSO溶液((d)～ (e))在光照后的寿命曲线；6SB6Py的DMF溶液(f)和DMSO溶液(g)的TEM图片(浓度：10" }, { "name": "sup", "data": [ { "name": "text", "data": "－5" } ] }, { "name": "text", "data": " mol/L)。" } ] }, { "lang": "en", "label": [ { "name": "text", "data": "Fig.4" } ], "title": [ { "name": "text", "data": "Emission spectra of 6SB6Py before and after illumination in DMF(a) and DMSO(b). Lifetime curves of 6SB6Py after illumination in DMF(c) and DMSO((d)－(e)). TEM images of 6SB6Py in DMF(f) and DMSO(g)(Concentration: 10" }, { "name": "sup", "data": [ { "name": "text", "data": "－5" } ] }, { "name": "text", "data": " mol/L)．" } ] } ], "subcaption": [], "note": [], "graphics": [ { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21348606&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21348615&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21348611&type=" } ] } }, { "name": "p", "data": [ { "name": "text", "data": "这种通过外加光照使得溶液光强迅速提升的现象，推测可能的原因有两种：第一种是光照使得体系内发生光化学反应，从而使得光强变化" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "blockXref", "data": { "data": [ { "name": "xref", "data": { "text": "20", "type": "bibr", "rid": "R20", "data": [ { "name": "text", "data": "20" } ] } }, { "name": "text", "data": "-" }, { "name": "xref", "data": { "text": "21", "type": "bibr", "rid": "R21", "data": [ { "name": "text", "data": "21" } ] } } ], "rid": [ "R20", "R21" ], "text": "20-21", "type": "bibr" } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "；第二种则是施加光照后，分子由初始的均匀分散状态变成能量更为稳定的聚集态，即发生了聚集诱导发光行为，从而导致发光增强" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "blockXref", "data": { "data": [ { "name": "xref", "data": { "text": "18", "type": "bibr", "rid": "R18", "data": [ { "name": "text", "data": "18" } ] } }, { "name": "text", "data": "-" }, { "name": "xref", "data": { "text": "19", "type": "bibr", "rid": "R19", "data": [ { "name": "text", "data": "19" } ] } } ], "rid": [ "R18", "R19" ], "text": "18-19", "type": "bibr" } }, { "name": "text", "data": "," }, { "name": "xref", "data": { "text": "22", "type": "bibr", "rid": "R22", "data": [ { "name": "text", "data": "22" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。为了进一步验证6SB6Py在溶液中的光控发光行为是由哪种原因导致的，首先对其在DMF溶液中光照前后的核磁共振氢谱进行了测试，测试结果如" }, { "name": "xref", "data": { "text": "图5", "type": "fig", "rid": "F5", "data": [ { "name": "text", "data": "图5" } ] } }, { "name": "text", "data": "所示。从图中的核磁共振氢谱图可以发现，6SB6Py的DMF溶液在365 nm光下照射30 min前后，各特征峰位置以及峰形几乎没有变化，这说明在光照半小时后，6SB6Py并没有发生化学变化，即排除了发光增强是因为体系内发生了光化学反应的原因。结合我们此前的相关文献推断" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "18", "type": "bibr", "rid": "R18", "data": [ { "name": "text", "data": "18" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "，通过外加光照改变了6SB6Py的激发态构型，从而改变了其在溶液中的聚集排布状态。这个过程显示了6SB6Py是一种具有光控AIE特性的分子。" } ] }, { "name": "fig", "data": { "id": "F5", "caption": [ { "lang": "zh", "label": [ { "name": "text", "data": "图5" } ], "title": [ { "name": "text", "data": "6SB6Py在光照前后的" }, { "name": "sup", "data": [ { "name": "text", "data": "1" } ] }, { "name": "text", "data": "H NMR(DMF-" }, { "name": "italic", "data": [ { "name": "text", "data": "d" } ] }, { "name": "sub", "data": [ { "name": "text", "data": "6" } ] }, { "name": "text", "data": ")" } ] }, { "lang": "en", "label": [ { "name": "text", "data": "Fig.5" } ], "title": [ { "name": "sup", "data": [ { "name": "text", "data": "1" } ] }, { "name": "text", "data": "H NMR of 6SB6Py in DMF-" }, { "name": "italic", "data": [ { "name": "text", "data": "d" } ] }, { "name": "sub", "data": [ { "name": "text", "data": "6" } ] }, { "name": "text", "data": " before and after illumination" } ] } ], "subcaption": [], "note": [], "graphics": [ { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21348620&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21348630&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21348625&type=" } ] } }, { "name": "p", "data": [ { "name": "text", "data": "对于6SB6Py的DMSO溶液，又对其光照前后的粒径进行了测试，得到的测试结果如" }, { "name": "xref", "data": { "text": "图6", "type": "fig", "rid": "F6", "data": [ { "name": "text", "data": "图6" } ] } }, { "name": "text", "data": "及" }, { "name": "xref", "data": { "text": "表1", "type": "table", "rid": "T1", "data": [ { "name": "text", "data": "表1" } ] } }, { "name": "text", "data": "所示。对6SB6Py的DMSO溶液不断地施加365 nm光照，分别对光照前和光照后1，3，5，10，20 min的粒径进行了测试。从测试结果可以看到，随光照时间不断增加，6SB6Py在DMSO中的粒径呈现出较大幅度的变化，表现为其强度平均值、数量平均值和体积平均值都在随着光照时间的变化而大幅度改变。这是由于光照不仅使得6SB6Py在DMSO中呈现聚集程度的改变，也使得其聚集状态在不断地发生改变。根据之前的相关文献推测" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "23", "type": "bibr", "rid": "R23", "data": [ { "name": "text", "data": "23" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "，光照的引入可能会使得6SB6Py存在球形、棒状等各种聚集形态的转变，这些变化能够引起分子荧光-磷光比例分布的变化，从而出现双发射特性。" } ] }, { "name": "fig", "data": { "id": "F6", "caption": [ { "lang": "zh", "label": [ { "name": "text", "data": "图6" } ], "title": [ { "name": "text", "data": "6SB6Py在DMSO溶液中光照前后的粒径变化图" } ] }, { "lang": "en", "label": [ { "name": "text", "data": "Fig.6" } ], "title": [ { "name": "text", "data": "Grain size change diagram of 6SB6Py before and after illumination in DMSO" } ] } ], "subcaption": [], "note": [], "graphics": [ { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21348635&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21348644&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21348639&type=" } ] } }, { "name": "table", "data": { "id": "T1", "caption": [ { "lang": "zh", "label": [ { "name": "text", "data": "表1" } ], "title": [ { "name": "text", "data": "6SB6Py在DMSO溶液中光照前后的粒径变化数据" } ] }, { "lang": "en", "label": [ { "name": "text", "data": "Tab.1" } ], "title": [ { "name": "text", "data": "DLS(dynamic light scattering) data of 6SB6Py in DMSO before and after illumination" } ] } ], "note": [], "table": [ { "head": [ [ { "colspan": "1", "rowspan": "1", "align": "center", "style": "border-top:1px solid #000;border-bottom:1px solid #000;", "data": [ { "name": "text", "data": "序号" } ] }, { "colspan": "1", 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"http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21348653&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21348649&type=" } } }, { "name": "p", "data": [ { "name": "text", "data": "通过以上实验数据，我们可以进一步证实，6SB6Py在DMF和DMSO中所呈现出的光照发光增强的现象是由于光激发分子重组的结果，即为光控聚集诱导发光的一种形式，与光化学反应无关。" } ] } ] } ] }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "4　结论" } ], "level": "1", "id": "s4" } }, { "name": "p", "data": [ { "name": "text", "data": "本文采用多步合成法合成了一种以六硫苯作为母核的衍生物六硫苯六吡啶(6SB6Py)，其可以很好地溶解于有机溶剂DMF和DMSO中。通过发射光谱可得，6SB6Py在有机溶剂中呈均匀分散状态时，几乎不发光或发光极其微弱；但当施加外部光照，如365 nm光照半小时后，溶液光强会迅速提升。其中，以DMF为溶液时，体系在365 nm光照半小时后，升起一个磷光峰，位置在500 nm处。而以DMSO为溶液的体系中，在365 nm光照半小时后，同时升起两个峰，分别为420 nm处的荧光峰和500 nm处的磷光峰。通过光照前后的核磁共振氢谱图以及DLS数据，证明这种外加光照使得体系光强迅速提升的内部原因是光激发分子重组，即证明6SB6Py具有光控AIE的特性。同时，分子的聚集状态也在随着光照时间的改变而不断变化。该结果对于今后研究在有机溶剂中的AIE现象，提供了重要的理论基础。" } ] } ] } ], "footnote": [], "reflist": { "title": [ { "name": "text", "data": 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