发光可调控CDs@MOFs复合荧光材料制备及其在高显色白光LED中的应用

何俊坚; 洪卓宝; 余林梁; 胡广齐; 刘晓瑭

doi:10.37188/CJL.20210122

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发光可调控CDs@MOFs复合荧光材料制备及其在高显色白光LED中的应用

材料合成及性能 | 更新时间：2021-07-22

- 发光可调控CDs@MOFs复合荧光材料制备及其在高显色白光LED中的应用增强出版
- Preparation of Controllable Luminescence CDs@MOFs Fluorescent Composites and Their Application in High Color Rendering White LED
- 发光学报 2021年 42卷第7期 (2021)
- 作者机构：
  
  华南农业大学　材料与能源学院,广东,广州,510642;广东技术师范大学　光电工程学院,广东,广州,510665;华南农业大学材料与能源学院　生物基材料与能源教育部重点实验室,广东,广州,510642
- 作者简介：
- 基金信息：
- DOI：10.37188/CJL.20210122 中图分类号： O482.31;TN312.8
- 纸质出版日期：2021-07-01，
  
  收稿日期：2021-04-06，
  
  修回日期：2021-04-20，
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引用本文
何俊坚, 洪卓宝, 余林梁, 等. 发光可调控CDs@MOFs复合荧光材料制备及其在高显色白光LED中的应用[J]. 发光学报, 2021, 42(7):984-996.

Jun-jian HE, Zhuo-bao HONG, Lin-liang YU, et al. Preparation of Controllable Luminescence CDs@MOFs Fluorescent Composites and Their Application in High Color Rendering White LED[J]. Chinese Journal of Luminescence, 2021, 42(7):984-996.
何俊坚, 洪卓宝, 余林梁, 等. 发光可调控CDs@MOFs复合荧光材料制备及其在高显色白光LED中的应用[J]. 发光学报, 2021, 42(7):984-996. DOI： 10.37188/CJL.20210122.

Jun-jian HE, Zhuo-bao HONG, Lin-liang YU, et al. Preparation of Controllable Luminescence CDs@MOFs Fluorescent Composites and Their Application in High Color Rendering White LED[J]. Chinese Journal of Luminescence, 2021, 42(7):984-996. DOI： 10.37188/CJL.20210122.

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China" } ] } ] }, { "id": "aff2", "intro": [ { "lang": "zh", "label": "2", "text": "广东技术师范大学　光电工程学院，广东　广州　 510665", "data": [ { "name": "text", "data": "广东技术师范大学　光电工程学院，广东　广州　 510665" } ] }, { "lang": "en", "label": "2", "text": "College of Photoelectric Engineering, Guangdong Polytechnic Normal University, Guangzhou 510665, China", "data": [ { "name": "text", "data": "College of Photoelectric Engineering, Guangdong Polytechnic Normal University, Guangzhou 510665, China" } ] } ] }, { "id": "aff3", "intro": [ { "lang": "zh", "label": "3", "text": "华南农业大学材料与能源学院　生物基材料与能源教育部重点实验室，广东　广州　 510642", "data": [ { "name": "text", "data": "华南农业大学材料与能源学院　生物基材料与能源教育部重点实验室，广东　广州　 510642" } ] }, { "lang": "en", "label": "3", "text": "Key Laboratory for Biobased Materials and Energy of Ministry of Education, College of Materials and Energy, South China Agricultural University, Guangzhou 510642, China", "data": [ { "name": "text", "data": "Key Laboratory for Biobased Materials and Energy of Ministry of Education, College of Materials and Energy, South China Agricultural University, Guangzhou 510642, China" } ] } ] } ] }, "abstracts": [ { "lang": "zh", "data": [ { "name": "p", "data": [ { "name": "text", "data": "选用中性红和硫脲作为原料，制备出一种540 nm波长发射的新型黄光碳点(CDs)水溶液，具有激发依赖特性。选择Al-MOFs和Zn-MOFs分别作为CDs的载体基质，得到CDs@Al-MOFs和CDs@Zn-MOFs两种复合荧光材料，都显示出非激发依赖特性。而CDs@Al-MOFs和CDs@Zn-MOFs的最佳发射峰分别位于555 nm 和612 nm，与CDs水溶液540 nm的发射波长相比，都出现不同程度的红移。通过对黄光CDs及其复合荧光材料进行TEM、XRD、FT-IR、XPS、UV-Vis和FL等系列表征，证明其发光机理是由CDs的表面态发光转变为分子态发光占主导地位。通过调整两种复合荧光材料的配比可获得不同发光性能的白光LED器件，当CDs@Al-MOFs与CDs@Zn-MOFs的质量比为1∶0.65时，器件的色温为3 968 K、显色指数达82.4，表明该碳点基复合荧光材料在白光LED领域具有广阔的发展前景和应用价值。" } ] } ] }, { "lang": "en", "data": [ { "name": "p", "data": [ { "name": "text", "data": "In this paper, neutral red and thiourea were chosen as the raw materials to prepare a novel yellow light carbon dots(CDs) aqueous solution emitting at 540 nm with excitation-dependent fluorescence property. CDs@Al-MOFs and CDs@Zn-MOFs composite fluorescent materials were prepared by Al-MOFs and Zn-MOFs as the support matrices for CDs, respectively, and both of them shown excitation-independent fluorescence property. The optimal emission peaks of CDs@Al-MOFs and CDs@Zn-MOFs were at 555 nm and 612 nm, respectively. Both composites appeared red-shifted to different degrees compared to the emission wavelength at 540 nm of CDs aqueous solution. Through a series of characterizations including TEM, XRD, FT-IR, XPS, UV-Vis and FL on yellow light CDs and their composite fluorescent materials, it was proven that the luminescence mechanism was dominated by the transition of the surface state luminescence of CDs to molecular state luminescence. White light LED devices with different luminescent properties can be obtained by adjusting the ratio of two kinds of composite fluorescent materials. When the mass ratio of CDs@Al-MOFs and CDs@Zn-MOFs is 1∶0.65, the color temperature of the white light LED is 3 968 K and the color rendering index is as high as 82.4, indicating that the CDs@MOFs composite fluorescent material has broad development prospects and application value in the field of white LED." } ] } ] } ], "keyword": [ { "lang": "zh", "data": [ [ { "name": "text", "data": "黄色发光碳点" } ], [ { "name": "text", "data": "有机金属框架" } ], [ { "name": "text", "data": "固态照明" } ], [ { "name": "text", "data": "白光LED" } ] ] }, { "lang": "en", "data": [ [ { "name": "text", "data": "yellow emissive carbon dots" } ], [ { "name": "text", "data": "metal-organic framework" } ], [ { "name": "text", "data": "solid lighting" } ], [ { "name": "text", "data": "white light-emitting diodes" } ] ] } ], "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": "碳点(Carbon dots,CDs)由于其出色而独特的性质而备受关注。继Xu等" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "1", "type": "bibr", "rid": "R1", "data": [ { "name": "text", "data": "1" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "开创性报告碳点之后，各种碳源" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "blockXref", "data": { "data": [ { "name": "xref", "data": { "text": "2", "type": "bibr", "rid": "R2", "data": [ { "name": "text", "data": "2" } ] } }, { "name": "text", "data": "-" }, { "name": "xref", "data": { "text": "3", "type": "bibr", "rid": "R3", "data": [ { "name": "text", "data": "3" } ] } } ], "rid": [ "R2", "R3" ], "text": "2-3", "type": "bibr" } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "都被发现可以用于制备CDs，其低毒性" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "4", "type": "bibr", "rid": "R4", "data": [ { "name": "text", "data": "4" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "、低成本" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "5", "type": "bibr", "rid": "R5", "data": [ { "name": "text", "data": "5" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "和良好的生物相容性" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "blockXref", "data": { "data": [ { "name": "xref", "data": { "text": "6", "type": "bibr", "rid": "R6", "data": [ { "name": "text", "data": "6" } ] } }, { "name": "text", "data": "-" }, { "name": "xref", "data": { "text": "7", "type": "bibr", "rid": "R7", "data": [ { "name": "text", "data": "7" } ] } } ], "rid": [ "R6", "R7" ], "text": "6-7", "type": "bibr" } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "广受生物医学领域的关注和研究" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "blockXref", "data": { "data": [ { "name": "xref", "data": { "text": "8", "type": "bibr", "rid": "R8", "data": [ { "name": "text", "data": "8" } ] } }, { "name": "text", "data": "-" }, { "name": "xref", "data": { "text": "9", "type": "bibr", "rid": "R9", "data": [ { "name": "text", "data": "9" } ] } } ], "rid": [ "R8", "R9" ], "text": "8-9", "type": "bibr" } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。同时，还具有优异光稳定性" }, { "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": "、宽发射" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "11", "type": "bibr", "rid": "R11", "data": [ { "name": "text", "data": "11" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "和荧光不发生闪烁" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "12", "type": "bibr", "rid": "R12", "data": [ { "name": "text", "data": "12" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "等突出优点，也深受发光器件及其他领域的青睐" }, { "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": "14", "type": "bibr", "rid": "R14", "data": [ { "name": "text", "data": "14" } ] } } ], "rid": [ "R13", "R14" ], "text": "13-14", "type": "bibr" } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。因此，碳点是一种具有广泛应用前景的新型荧光材料，但是对碳点的发光机理还没有统一的解释，最被广泛接受的CDs荧光机理解释有三种。(1)由碳核结构决定的量子限域效应和共轭π键结构荧光效应。当纳米材料的尺寸逐渐减小至玻尔半径时，其准连续电子能级变为离散分布的形式，碳点的尺寸影响共轭结构的大小，共轭程度增加，最高占据分子轨道与最低未占据轨道之间能带变窄，即π-π" }, { "name": "sup", "data": [ { "name": "text", "data": "*" } ] }, { "name": "text", "data": "电子能级变窄，导致荧光红移" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "blockXref", "data": { "data": [ { "name": "xref", "data": { "text": "15", "type": "bibr", "rid": "R15", "data": [ { "name": "text", "data": "15" } ] } }, { "name": "text", "data": "-" }, { "name": "xref", "data": { "text": "16", "type": "bibr", "rid": "R16", "data": [ { "name": "text", "data": "16" } ] } } ], "rid": [ "R15", "R16" ], "text": "15-16", "type": "bibr" } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。(2)由表面的化学基团决定表面态理论。大部分碳点的表面会存在大量的表面基团，例如羰基、羧基、环氧基等含氧基团，不同的官能团具有不同的能级，也会有不同的发射缺陷，表面官能团是影响表面能级和带隙的重要因素，碳点的荧光效率可以通过表面钝化来提高" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "blockXref", "data": { "data": [ { "name": "xref", "data": { "text": "17", "type": "bibr", "rid": "R17", "data": [ { "name": "text", "data": "17" } ] } }, { "name": "text", "data": "-" }, { "name": "xref", "data": { "text": "18", "type": "bibr", "rid": "R18", "data": [ { "name": "text", "data": "18" } ] } } ], "rid": [ "R17", "R18" ], "text": "17-18", "type": "bibr" } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。(3)由荧光分子团决定的分子态理论。分子态发光不同于表面态发光，区别在于分子态发光具有相对独立的荧光中心——发色团，发色团可以键连在碳点表面或者碳链的内部，独立发射荧光，通常具有较高的量子产率，而且表现出不明显的激发依赖或非激发依赖特性" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "blockXref", "data": { "data": [ { "name": "xref", "data": { "text": "19", "type": "bibr", "rid": "R19", "data": [ { "name": "text", "data": "19" } ] } }, { "name": "text", "data": "-" }, { "name": "xref", "data": { "text": "22", "type": "bibr", "rid": "R22", "data": [ { "name": "text", "data": "22" } ] } } ], "rid": [ "R19", "R20", "R21", "R22" ], "text": "19-22", "type": "bibr" } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。因为发光机理尚未明确，目前被报道的CDs多是蓝色和绿色发光" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "blockXref", "data": { "data": [ { "name": "xref", "data": { "text": "23", "type": "bibr", "rid": "R23", "data": [ { "name": "text", "data": "23" } ] } }, { "name": "text", "data": "-" }, { "name": "xref", "data": { "text": "25", "type": "bibr", "rid": "R25", "data": [ { "name": "text", "data": "25" } ] } } ], "rid": [ "R23", "R24", "R25" ], "text": "23-25", "type": "bibr" } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "，对于黄色和红色发光的碳点仍然较为稀缺。同时，聚集诱导猝灭效应导致碳点变成固体时荧光猝灭，只能依靠载体来实现碳点的固体发光。现有的技术以制备出长波长发射的碳点为前提，再选择载体实现固体发光，进一步进行发光器件等应用测试" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "14", "type": "bibr", "rid": "R14", "data": [ { "name": "text", "data": "14" } ] } }, { "name": "text", "data": "," }, { "name": "xref", "data": { "text": "26", "type": "bibr", "rid": "R26", "data": [ { "name": "text", "data": "26" } ] } }, { "name": "text", "data": "," }, { "name": "xref", "data": { "text": "27", "type": "bibr", "rid": "R27", "data": [ { "name": "text", "data": "27" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。这样的技术较为依赖于碳点发光条件，严重影响碳点在发光领域的应用发展，亟待开发新途径来减弱对碳点发光的依赖同时实现长波长固体发光。有机金属框架(Metal-organic framework,MOFs)是一种由过渡金属或稀土金属离子和含氧、氮等有机配体形成的多孔吸附材料，具有巨大的比表面积、丰富的孔道结构和功能基团等优点" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "blockXref", "data": { "data": [ { "name": "xref", "data": { "text": "28", "type": "bibr", "rid": "R28", "data": [ { "name": "text", "data": "28" } ] } }, { "name": "text", "data": "-" }, { "name": "xref", "data": { "text": "29", "type": "bibr", "rid": "R29", "data": [ { "name": "text", "data": "29" } ] } } ], "rid": [ "R28", "R29" ], "text": "28-29", "type": "bibr" } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。利用MOFs材料作为载体的碳点基荧光材料大多被应用于传感器" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "30", "type": "bibr", "rid": "R30", "data": [ { "name": "text", "data": "30" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "、药物输送" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "31", "type": "bibr", "rid": "R31", "data": [ { "name": "text", "data": "31" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "、探针" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "32", "type": "bibr", "rid": "R32", "data": [ { "name": "text", "data": "32" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "和荧光防伪" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "33", "type": "bibr", "rid": "R33", "data": [ { "name": "text", "data": "33" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "等领域。应用于LED领域的碳点基MOFs材料较为少见，而且多是短波长发射" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "34", "type": "bibr", "rid": "R34", "data": [ { "name": "text", "data": "34" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。Wang等" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "35", "type": "bibr", "rid": "R35", "data": [ { "name": "text", "data": "35" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "用蓝色发光碳点和黄色发光Zr-MOF材料复合成CDs/Zr-MOF纳米复合材料，借助黄色发光Zr-MOF填补长波长发光，致使复合材料在365 nm激发下发出白光，沉积在紫外LED芯片上得到WLED，具有82的显色指数和1.7 lm·W" }, { "name": "sup", "data": [ { "name": "text", "data": "-1" } ] }, { "name": "text", "data": "的发光效率。缺少良好光热稳定性和具有长波长发射的碳点基MOFs材料，是阻碍该材料在LED领域应用发展的主要难题。" } ] }, { "name": "p", "data": [ { "name": "text", "data": "本工作中，我们实现了以单一碳点制备出不同发射波长的碳点基固体发光材料。首先，选择中性红和硫脲作为原料，采用溶剂热法在乙醇溶液中制备了黄色发光的CDs，选择MOFs材料作为碳点载体基质，分别制备了CDs@Al-MOFs复合荧光材料和CDs@Zn-MOFs复合荧光材料，表征了它们的组成、结构和发光性能，并探讨了其在白光LED领域的应用前景。" } ] } ] }, { "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": "实验原料包括:中性红(分析纯，上海麦克林生化科技有限公司)，无水乙醇(分析纯，广东光华科技股份有限公司)，硫脲(分析纯，天津市科密欧化学试剂厂)，乙酸乙酯(分析纯，天津市富宇精细化工有限公司)，无水醋酸锌(分析纯，上海麦克林生化科技有限公司)，氯化铝(分析纯，广州化学试剂厂),N,N-二甲基甲酰胺(分析纯，天津市永大化学试剂有限公司)，对苯二甲酸(分析纯，阿拉丁试剂)，有机硅胶A胶(深圳市展望隆科有限公司)，固化剂B胶(深圳市展望隆科有限公司)。" } ] } ] }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "2.2　样品制备" } ], "level": "2", "id": "s2b" } }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "2.2.1　黄光CDs制备" } ], "level": "3", "id": "s2b1" } }, { "name": "p", "data": [ { "name": "text", "data": "采用溶剂热法合成CDs溶液，典型的制备方法如下:称取0.05 g中性红溶解在20 mL无水乙醇中，称取0.1 g硫脲溶解在15 mL无水乙醇中，在常温下，将两种溶液混合并磁力搅拌30 min。然后把溶液转移至50 mL的聚四氟乙烯反应釜中，放入烘箱200 ℃下反应4 h。反应结束后冷却至室温，将反应液转移至分液漏斗中，加入30 mL乙酸乙酯和20 mL去离子水，振荡，静置分层。取上层溶液在60 ℃水浴下真空旋蒸，蒸干溶液得到固体，再加入30 mL去离子水超声溶解固体;然后将溶液转移至500 u的透析袋子中透析72 h，透析后的溶液真空旋蒸，蒸干得到固体;最后再加入10 mL去离子水得到CDs水溶液，室温保存。" } ] } ] }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "2.2.2　Zn-MOFs和Al-MOFs材料制备" } ], "level": "3", "id": "s2b2" } }, { "name": "p", "data": [ { "name": "text", "data": "采用溶剂热法制备Zn-MOFs材料，典型的制备方法如下:称取1.8 g的醋酸锌溶解在10 mL的N,N-二甲基酰胺中得到溶液A，称取1.7 g的对苯二甲酸溶解在20 mL的N,N-二甲基酰胺中得到溶液B。边搅拌边将溶液A慢慢滴加到溶液B中，滴加完后再搅拌30 min，随后把混合液转移至50 mL的聚四氟乙烯反应釜中，放入烘箱在150 ℃下反应72 h，用离心机7 000 r/min离心5 min得到固体，用N,N-二甲基酰胺和乙醇洗涤分别洗涤三次，固体放进烘箱60 ℃烘干后得到Zn-MOFs白色粉末。用相同方法制备Al-MOFs，只需将醋酸锌换成氯化铝。" } ] } ] }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "2.2.3　CDs@MOFs复合荧光材料制备" } ], "level": "3", "id": "s2b3" } }, { "name": "p", "data": [ { "name": "text", "data": "称取0.5 g的 Zn-MOFs白色粉末分散在30 mL去离子水中，移取0.5 mL CDs水溶液加入Zn-MOFs的分散液中，常温下搅拌反应3 h，离心，去离子水洗涤3次，烘箱中60 ℃烘干，得到CDs@Zn-MOFs复合荧光材料。采用相同的方法制备CDs@Al-MOFs复合荧光材料。" } ] } ] }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "2.2.4　LED器件封装" } ], "level": "3", "id": "s2b4" } }, { "name": "p", "data": [ { "name": "text", "data": "将2 g有机硅胶A胶和0.5 gCDs@Al-MOFs复合荧光粉搅拌均匀后，加入8 g固化剂B胶，再次充分混合均匀，放进真空干燥箱中脱泡，待用。把脱泡后的混合荧光粉胶水适量涂覆在InGaN(450 nm)蓝光芯片上，放入烘箱60 ℃烘烤2 h进行固化，固化完成后降温冷却至常温，得到封装好的①号白光LED器件。将CDs@Al-MOFs和CDs@Zn-MOFs按照质量比为1∶0.65混合制备荧光粉，再按照上述制备方法封装得到②号白光LED器件。蓝光LED芯片的工作电压固定为2.7 V。" } ] } ] } ] }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "2.3　样品表征" } ], "level": "2", "id": "s2c" } }, { "name": "p", "data": [ { "name": "text", "data": "通过JEM-2100F透射电子显微镜(TEM，日本JEOL)在200 kV的工作电压下观察CDs及CDs@MOFs复合荧光材料的形貌和尺寸。通过XD-2X型X射线粉末衍射仪(XRD)对固体样品进行结构表征。采用傅里叶变换红外光谱(FT-IR,Nicolet IS 10)和X射线光电子能谱(XPS,Escalab 250Xi)对CDs及CDs@MOFs复合荧光材料的结构进行表征。CDs及CDs@MOFs复合荧光材料的荧光光谱和紫外-可见吸收光谱分别用RF-5301PC型荧光分光光度计(FL)和UV-2550型紫外-可见吸收光谱仪(UV-Vis)进行测量。利用OHSP-350UV型紫外光谱照度计测定白光LED光源。" } ] } ] } ] }, { "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　CDs形貌和结构表征" } ], "level": "2", "id": "s3a" } }, { "name": "p", "data": [ { "name": "text", "data": "TEM和HRTEM对CDs的形貌表征结果如" }, { "name": "xref", "data": { "text": "图1", "type": "fig", "rid": "F1", "data": [ { "name": "text", "data": "图1" } ] } }, { "name": "text", "data": "所示。由" }, { "name": "xref", "data": { "text": "图1(a)", "type": "fig", "rid": "F1", "data": [ { "name": "text", "data": "图1(a)" } ] } }, { "name": "text", "data": "可见，CDs为类球体微粒，在乙醇溶液中有很好的分散性，计算得到CDs的晶格条纹间距约为0.21 nm。通过统计100个以上纳米粒子得到CDs的尺寸分布图(" }, { "name": "xref", "data": { "text": "图1(b)", "type": "fig", "rid": "F1", "data": [ { "name": "text", "data": "图1(b)" } ] } }, { "name": "text", "data": ")，可以看到CDs的平均粒径约为4.50 nm，分布范围为2.3~7.2 nm。" } ] }, { "name": "fig", "data": { "id": "F1", "caption": [ { "lang": "zh", "label": [ { "name": "text", "data": "图1" } ], "title": [ { "name": "text", "data": "CDs的TEM和HRTEM图像(a)及粒径分布图(b)" } ] }, { "lang": "en", "label": [ { "name": "text", "data": "Fig.1" } ], "title": [ { "name": "text", "data": "TEM and HRTEM images(a) and size normal distribution histogram(b) of CDs" } ] } ], "subcaption": [], "note": [], "graphics": [ { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352123&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352130&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352127&type=" } ] } }, { "name": "p", "data": [ { "name": "text", "data": "CDs的FR-IT光谱如" }, { "name": "xref", "data": { "text": "图2(a)", "type": "fig", "rid": "F2", "data": [ { "name": "text", "data": "图2(a)" } ] } }, { "name": "text", "data": "所示，可以观察到在3 430 cm" }, { "name": "sup", "data": [ { "name": "text", "data": "-1" } ] }, { "name": "text", "data": "的宽吸收峰，归属于O—H和N—H的伸缩振动" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "blockXref", "data": { "data": [ { "name": "xref", "data": { "text": "36", "type": "bibr", "rid": "R36", "data": [ { "name": "text", "data": "36" } ] } }, { "name": "text", "data": "-" }, { "name": "xref", "data": { "text": "37", "type": "bibr", "rid": "R37", "data": [ { "name": "text", "data": "37" } ] } } ], "rid": [ "R36", "R37" ], "text": "36-37", "type": "bibr" } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。而2 923 cm" }, { "name": "sup", "data": [ { "name": "text", "data": "-1" } ] }, { "name": "text", "data": "和1 640 cm" }, { "name": "sup", "data": [ { "name": "text", "data": "-1" } ] }, { "name": "text", "data": "分别归属于C—H和C" }, { "name": "inlineformula", "data": [ { "name": "math", "data": { "graphicsData": { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352134&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352139&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352136&type=" } } } ] }, { "name": "text", "data": "O/C" }, { "name": "inlineformula", "data": [ { "name": "math", "data": { "graphicsData": { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352141&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352144&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352143&type=" } } } ] }, { "name": "text", "data": "C的伸缩振动" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "blockXref", "data": { "data": [ { "name": "xref", "data": { "text": "38", "type": "bibr", "rid": "R38", "data": [ { "name": "text", "data": "38" } ] } }, { "name": "text", "data": "-" }, { "name": "xref", "data": { "text": "39", "type": "bibr", "rid": "R39", "data": [ { "name": "text", "data": "39" } ] } } ], "rid": [ "R38", "R39" ], "text": "38-39", "type": "bibr" } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。在1 319 cm" }, { "name": "sup", "data": [ { "name": "text", "data": "-1" } ] }, { "name": "text", "data": "和1 200 cm" }, { "name": "sup", "data": [ { "name": "text", "data": "-1" } ] }, { "name": "text", "data": "处吸收峰分别是C—N和C—S/C—O的伸缩振动的特征峰" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "blockXref", "data": { "data": [ { "name": "xref", "data": { "text": "40", "type": "bibr", "rid": "R40", "data": [ { "name": "text", "data": "40" } ] } }, { "name": "text", "data": "-" }, { "name": "xref", "data": { "text": "41", "type": "bibr", "rid": "R41", "data": [ { "name": "text", "data": "41" } ] } } ], "rid": [ "R40", "R41" ], "text": "40-41", "type": "bibr" } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。而在1 375 cm" }, { "name": "sup", "data": [ { "name": "text", "data": "-1" } ] }, { "name": "text", "data": "和890 cm" }, { "name": "sup", "data": [ { "name": "text", "data": "-1" } ] }, { "name": "text", "data": "的特征峰分别归属于C—H的剪切振动和弯曲振动" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "42", "type": "bibr", "rid": "R42", "data": [ { "name": "text", "data": "42" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。有趣的是，在2 055 cm" }, { "name": "sup", "data": [ { "name": "text", "data": "-1" } ] }, { "name": "text", "data": "处的吸收峰归属于—SCN的伸缩振动" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "43", "type": "bibr", "rid": "R43", "data": [ { "name": "text", "data": "43" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。证明N元素和S元素掺杂进所制备的CDs中，在碳化过程中形成了硫氰基、氨基和酰胺等官能团。" } ] }, { "name": "fig", "data": { "id": "F2", "caption": [ { "lang": "zh", "label": [ { "name": "text", "data": "图2" } ], "title": [ { "name": "text", "data": "CDs的FR-IT谱图(a)、XPS总谱(b)、XPS C" }, { "name": "sub", "data": [ { "name": "text", "data": "1s" } ] }, { "name": "text", "data": "高分辨能谱(c)、XPS O" }, { "name": "sub", "data": [ { "name": "text", "data": "1s" } ] }, { "name": "text", "data": "高分辨能谱(d)、XPS N" }, { "name": "sub", "data": [ { "name": "text", "data": "1s" } ] }, { "name": "text", "data": "高分辨能谱(e)和XPS S" }, { "name": "sub", "data": [ { "name": "text", "data": "2p" } ] }, { "name": "text", "data": "高分辨能谱(f)。" } ] }, { "lang": "en", "label": [ { "name": "text", "data": "Fig.2" } ], "title": [ { "name": "text", "data": "FT-IR spectra(a) and full survey XPS spectrum(b) of CDs. High-resolution XPS spectra of C" }, { "name": "sub", "data": [ { "name": "text", "data": "1s" } ] }, { "name": "text", "data": "(c), O" }, { "name": "sub", "data": [ { "name": "text", "data": "1s" } ] }, { "name": "text", "data": "(d), N" }, { "name": "sub", "data": [ { "name": "text", "data": "1s" } ] }, { "name": "text", "data": "(e) and S" }, { "name": "sub", "data": [ { "name": "text", "data": "2p" } ] }, { "name": "text", "data": "(f) of the CDs." } ] } ], "subcaption": [], "note": [], "graphics": [ { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352146&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352150&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352148&type=" } ] } }, { "name": "p", "data": [ { "name": "text", "data": "CDs的XPS能谱分析总谱如" }, { "name": "xref", "data": { "text": "图2(b)", "type": "fig", "rid": "F2", "data": [ { "name": "text", "data": "图2(b)" } ] } }, { "name": "text", "data": "所示。结果显示，在163.5,284.8,399.3,532.0 eV处出现4个特征峰，分别对应于S" }, { "name": "sub", "data": [ { "name": "text", "data": "2p" } ] }, { "name": "text", "data": "、C" }, { "name": "sub", "data": [ { "name": "text", "data": "1s" } ] }, { "name": "text", "data": "、N" }, { "name": "sub", "data": [ { "name": "text", "data": "1s" } ] }, { "name": "text", "data": "和" }, { "name": "inlineformula", "data": [ { "name": "math", "data": { "graphicsData": { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352152&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352156&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352154&type=" } } } ] }, { "name": "text", "data": "，证实该方法制备得到的CDs主要由C、O、N和S 4种元素组成，其含量分别是77.6%、14.1%、6.2%和2.1%。C" }, { "name": "sub", "data": [ { "name": "text", "data": "1s" } ] }, { "name": "text", "data": "高分辨能谱(" }, { "name": "xref", "data": { "text": "图2(c)", "type": "fig", "rid": "F2", "data": [ { "name": "text", "data": "图2(c)" } ] } }, { "name": "text", "data": ")可以分为284.7,286.0,287.1,288.5 eV 4个特征峰，分别对应于C—C/C" }, { "name": "inlineformula", "data": [ { "name": "math", "data": { "graphicsData": { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352158&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352162&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352160&type=" } } } ] }, { "name": "text", "data": "C、C—N/C—O、C—S和C" }, { "name": "inlineformula", "data": [ { "name": "math", "data": { "graphicsData": { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352164&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352168&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352166&type=" } } } ] }, { "name": "text", "data": "O键" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "46", "type": "bibr", "rid": "R46", "data": [ { "name": "text", "data": "46" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。O" }, { "name": "sub", "data": [ { "name": "text", "data": "1s" } ] }, { "name": "text", "data": "高分辨能谱(" }, { "name": "xref", "data": { "text": "图2(d)", "type": "fig", "rid": "F2", "data": [ { "name": "text", "data": "图2(d)" } ] } }, { "name": "text", "data": ")显示了532.0,532.9 eV两个特征峰，分别归属于C—O和C" }, { "name": "inlineformula", "data": [ { "name": "math", "data": { "graphicsData": { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352170&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352177&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352174&type=" } } } ] }, { "name": "text", "data": "O键" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "47", "type": "bibr", "rid": "R47", "data": [ { "name": "text", "data": "47" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。N" }, { "name": "sub", "data": [ { "name": "text", "data": "1s" } ] }, { "name": "text", "data": "高分辨能谱(" }, { "name": "xref", "data": { "text": "图2(e)", "type": "fig", "rid": "F2", "data": [ { "name": "text", "data": "图2(e)" } ] } }, { "name": "text", "data": ")主要分为399.1,400.1 eV两个特征峰，分别归属于C—N和N—H键;而在406.8 eV显示了一个弱π-π" }, { "name": "sup", "data": [ { "name": "text", "data": "*" } ] }, { "name": "text", "data": "卫星特征峰，来自于—CO—N—CO—键" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "48", "type": "bibr", "rid": "R48", "data": [ { "name": "text", "data": "48" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。S" }, { "name": "sub", "data": [ { "name": "text", "data": "2p" } ] }, { "name": "text", "data": "的高分辨能谱(" }, { "name": "xref", "data": { "text": "图2(f)", "type": "fig", "rid": "F2", "data": [ { "name": "text", "data": "图2(f)" } ] } }, { "name": "text", "data": ")主要被分为两个特征峰，分别为C—S—C(163.3 eV)和C—SO" }, { "name": "sub", "data": [ { "name": "italic", "data": [ { "name": "text", "data": "X" } ] } ] }, { "name": "text", "data": "(169.0 eV)键" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "49", "type": "bibr", "rid": "R49", "data": [ { "name": "text", "data": "49" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。XPS测定结果进一步证实CDs中掺杂了S元素和N元素，且与上述FR-IT测试结果相符合。" } ] } ] }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "3.2　CDs@MOFs复合荧光材料形貌和结构表征" } ], "level": "2", "id": "s3b" } }, { "name": "p", "data": [ { "name": "text", "data": "CDs@Al-MOFs和CDs@Zn-MOFs两种复合荧光材料的TEM和HRTEM图像分别如" }, { "name": "xref", "data": { "text": "图3(a)和3(d)", "type": "fig", "rid": "F3", "data": [ { "name": "text", "data": "图3(a)和3(d)" } ] } }, { "name": "text", "data": "所示，可以清楚地观察到Al-MOFs和Zn-MOFs的表面上分布着许多纳米粒子，经过测量计算，晶格条纹间隔均约为0.21 nm，与上述的CDs晶格条纹一致。与其相对应的X射线能量色散谱图(Energy dispersive spectroscopy,EDS)分别见" }, { "name": "xref", "data": { "text": "图3(b)", "type": "fig", "rid": "F3", "data": [ { "name": "text", "data": "图3(b)" } ] } }, { "name": "text", "data": "和" }, { "name": "xref", "data": { "text": "图3(e)", "type": "fig", "rid": "F3", "data": [ { "name": "text", "data": "图3(e)" } ] } }, { "name": "text", "data": "，两者都显示了在0.277,0.392,0.525,2.310 keV 4个特征峰" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "blockXref", "data": { "data": [ { "name": "xref", "data": { "text": "50", "type": "bibr", "rid": "R50", "data": [ { "name": "text", "data": "50" } ] } }, { "name": "text", "data": "-" }, { "name": "xref", "data": { "text": "51", "type": "bibr", "rid": "R51", "data": [ { "name": "text", "data": "51" } ] } } ], "rid": [ "R50", "R51" ], "text": "50-51", "type": "bibr" } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "，分别对应于C、N、O和S元素的Kα" }, { "name": "sub", "data": [ { "name": "text", "data": "1" } ] }, { "name": "text", "data": "。" }, { "name": "xref", "data": { "text": "图3(b)", "type": "fig", "rid": "F3", "data": [ { "name": "text", "data": "图3(b)" } ] } }, { "name": "text", "data": "中的1.486 keV特征峰归属于Al元素的Kα" }, { "name": "sub", "data": [ { "name": "text", "data": "1" } ] }, { "name": "text", "data": "，而" }, { "name": "xref", "data": { "text": "图3(e)", "type": "fig", "rid": "F3", "data": [ { "name": "text", "data": "图3(e)" } ] } }, { "name": "text", "data": "中的1.012,8.637,9.570 keV 3个峰分别归属于Zn元素的Lα" }, { "name": "sub", "data": [ { "name": "text", "data": "1" } ] }, { "name": "text", "data": "、Kα" }, { "name": "sub", "data": [ { "name": "text", "data": "1" } ] }, { "name": "text", "data": "和Kβ" }, { "name": "sub", "data": [ { "name": "text", "data": "1" } ] }, { "name": "text", "data": "。" }, { "name": "xref", "data": { "text": "图3(b)", "type": "fig", "rid": "F3", "data": [ { "name": "text", "data": "图3(b)" } ] } }, { "name": "text", "data": "和" }, { "name": "xref", "data": { "text": "图3(e)", "type": "fig", "rid": "F3", "data": [ { "name": "text", "data": "图3(e)" } ] } }, { "name": "text", "data": "中在8.046 keV和8.904 keV的峰都来自于铜网上的Cu元素，对应于Cu的Kα" }, { "name": "sub", "data": [ { "name": "text", "data": "1" } ] }, { "name": "text", "data": "和Kβ" }, { "name": "sub", "data": [ { "name": "text", "data": "1" } ] }, { "name": "text", "data": "，而" }, { "name": "xref", "data": { "text": "图3(b)", "type": "fig", "rid": "F3", "data": [ { "name": "text", "data": "图3(b)" } ] } }, { "name": "text", "data": "中0.928 keV的峰来自于铜网上Cu元素的Lα" }, { "name": "sub", "data": [ { "name": "text", "data": "1" } ] }, { "name": "text", "data": "。TEM和EDS表征都证实了S、N掺杂的黄光CDs成功地负载在Al-MOFs和Zn-MOFs材料上。" } ] }, { "name": "fig", "data": { "id": "F3", "caption": [ { "lang": "zh", "label": [ { "name": "text", "data": "图3" } ], "title": [ { "name": "text", "data": "CDs@Al-MOFs的TEM和HRTEM图像(a)、EDS谱图(b)和FT-IR谱图(c);CDs@Zn-MOFs的TEM和HRTEM图像(d)、EDS谱图(e)和FT-IR谱图(f)。" } ] }, { "lang": "en", "label": [ { "name": "text", "data": "Fig.3" } ], "title": [ { "name": "text", "data": "TEM image and HRTEM image(a), EDS spectra(b) and FT-IR spectra(c) of CDs@Al-MOFs. TEM image and HRTEM image (d), EDS spectra(e) and FT-IR spectra(f) of CDs@Zn-MOFs." } ] } ], "subcaption": [], "note": [], "graphics": [ { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352180&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352185&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352183&type=" } ] } }, { "name": "p", "data": [ { "name": "text", "data": "利用FT-IR对MOFs材料和CDs-MOFs复合荧光材料的结构组成进行了表征。" }, { "name": "xref", "data": { "text": "图3(c)", "type": "fig", "rid": "F3", "data": [ { "name": "text", "data": "图3(c)" } ] } }, { "name": "text", "data": "为Al-MOFs与CDs复合前和复合后的FT-IR光谱，对比二者后可以发现，复合后位于1 290 cm" }, { "name": "sup", "data": [ { "name": "text", "data": "-1" } ] }, { "name": "text", "data": "和1 025 cm" }, { "name": "sup", "data": [ { "name": "text", "data": "-1" } ] }, { "name": "text", "data": "的红外吸收峰都明显增强，分别对应于C—N和C—O/C—S的伸缩振动" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "46", "type": "bibr", "rid": "R46", "data": [ { "name": "text", "data": "46" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": ";C—H的剪切振动红外吸收峰(1 380 cm" }, { "name": "sup", "data": [ { "name": "text", "data": "-1" } ] }, { "name": "text", "data": ")和弯曲振动吸收峰(997 cm" }, { "name": "sup", "data": [ { "name": "text", "data": "-1" } ] }, { "name": "text", "data": ")都有明显的增强" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "52", "type": "bibr", "rid": "R52", "data": [ { "name": "text", "data": "52" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "，这些特征峰的红外吸收增强归因于CDs的C—O、C—S、C—H和C—N键。而位于2 534 cm" }, { "name": "sup", "data": [ { "name": "text", "data": "-1" } ] }, { "name": "text", "data": "的吸收峰对应于S—H的特征吸收峰是新出现的，是由于Al-MOFs材料结构中存在大量稳定且规整分布的金属位点，提供了充足的活性中心" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "53", "type": "bibr", "rid": "R53", "data": [ { "name": "text", "data": "53" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "，将SCN催化生成S—H键" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "blockXref", "data": { "data": [ { "name": "xref", "data": { "text": "54", "type": "bibr", "rid": "R54", "data": [ { "name": "text", "data": "54" } ] } }, { "name": "text", "data": "-" }, { "name": "xref", "data": { "text": "55", "type": "bibr", "rid": "R55", "data": [ { "name": "text", "data": "55" } ] } } ], "rid": [ "R54", "R55" ], "text": "54-55", "type": "bibr" } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。同时，还注意到Al-MOFs材料原本位于1 673 cm" }, { "name": "sup", "data": [ { "name": "text", "data": "-1" } ] }, { "name": "text", "data": "的红外吸收峰，与黄光CDs复合后，位移到1 697 cm" }, { "name": "sup", "data": [ { "name": "text", "data": "-1" } ] }, { "name": "text", "data": "。这是因为在复合前，1 673 cm" }, { "name": "sup", "data": [ { "name": "text", "data": "-1" } ] }, { "name": "text", "data": "的特征峰归属于羧基中C" }, { "name": "inlineformula", "data": [ { "name": "math", "data": { "graphicsData": { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352186&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352188&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352187&type=" } } } ] }, { "name": "text", "data": "O;复合后，来自CDs的C" }, { "name": "inlineformula", "data": [ { "name": "math", "data": { "graphicsData": { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352189&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352191&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352190&type=" } } } ] }, { "name": "text", "data": "C键和表面电负性较强的表面基团，如氨基和羟基，由于静电场作用，对C" }, { "name": "inlineformula", "data": [ { "name": "math", "data": { "graphicsData": { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352192&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352196&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352194&type=" } } } ] }, { "name": "text", "data": "O产生诱导效应，诱导电子云由氧原子向双键的中间移动，导致振动频率增强，吸收谱带向高波数移动" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "56", "type": "bibr", "rid": "R56", "data": [ { "name": "text", "data": "56" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。FT-IR的测试结果也进一步证实CDs成功地与Al-MOFs成键复合在一起。" }, { "name": "xref", "data": { "text": "图3(f)", "type": "fig", "rid": "F3", "data": [ { "name": "text", "data": "图3(f)" } ] } }, { "name": "text", "data": "是Zn-MOFs与CDs复合前后的FT-IR光谱，对比二者后可以观察到，CDs@Zn-MOFs复合荧光材料于1 652 cm" }, { "name": "sup", "data": [ { "name": "text", "data": "-1" } ] }, { "name": "text", "data": "新出现一个红外吸收峰，归属于C" }, { "name": "inlineformula", "data": [ { "name": "math", "data": { "graphicsData": { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352198&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352203&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352200&type=" } } } ] }, { "name": "text", "data": "O和C" }, { "name": "inlineformula", "data": [ { "name": "math", "data": { "graphicsData": { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352206&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352213&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352209&type=" } } } ] }, { "name": "text", "data": "C的伸缩振动" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "57", "type": "bibr", "rid": "R57", "data": [ { "name": "text", "data": "57" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。位于1 300 cm" }, { "name": "sup", "data": [ { "name": "text", "data": "-1" } ] }, { "name": "text", "data": "和1 145 cm" }, { "name": "sup", "data": [ { "name": "text", "data": "-1" } ] }, { "name": "text", "data": "的特征峰分别归属于C—N和C—O的伸缩振动" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "58", "type": "bibr", "rid": "R58", "data": [ { "name": "text", "data": "58" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "，其红外吸收峰均有明显增强。同时，位于1 375 cm" }, { "name": "sup", "data": [ { "name": "text", "data": "-1" } ] }, { "name": "text", "data": "和854 cm" }, { "name": "sup", "data": [ { "name": "text", "data": "-1" } ] }, { "name": "text", "data": "的特征峰的红外吸收也有所增强，分别归属于C—H的剪切振动和弯曲振动" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "59", "type": "bibr", "rid": "R59", "data": [ { "name": "text", "data": "59" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。FT-IR表征结果同样进一步证明了CDs成功地与Zn-MOFs材料成键复合在一起。" } ] }, { "name": "p", "data": [ { "name": "text", "data": "利用XRD对MOFs材料和MOFs复合荧光材料进行了结构表征，如" }, { "name": "xref", "data": { "text": "图4", "type": "fig", "rid": "F4", "data": [ { "name": "text", "data": "图4" } ] } }, { "name": "text", "data": "所示。可以观察到Al-MOFs和CDs@Al-MOFs的XRD谱(" }, { "name": "xref", "data": { "text": "图4(a)", "type": "fig", "rid": "F4", "data": [ { "name": "text", "data": "图4(a)" } ] } }, { "name": "text", "data": ")基本一致，Zn-MOFs和CDs@Zn-MOFs的XRD谱(" }, { "name": "xref", "data": { "text": "图4(b)", "type": "fig", "rid": "F4", "data": [ { "name": "text", "data": "图4(b)" } ] } }, { "name": "text", "data": ")也基本一致，表明Al-MOFs和Zn-MOFs分别与CDs复合后，依然保持Al-MOFs和Zn-MOFs的晶型结构。" } ] }, { "name": "fig", "data": { "id": "F4", "caption": [ { "lang": "zh", "label": [ { "name": "text", "data": "图4" } ], "title": [ { "name": "text", "data": "(a)Al-MOFs和CDs@Al-MOFs的XRD谱;(b)Zn-MOFs和CDs@Zn-MOFs的XRD谱。" } ] }, { "lang": "en", "label": [ { "name": "text", "data": "Fig.4" } ], "title": [ { "name": "text", "data": "(a)XRD spectra of Al-MOFs and CDs@Al-MOFs. (b)XRD spectra of Zn-MOFs and CDs@Zn-MOFs." } ] } ], "subcaption": [], "note": [], "graphics": [ { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352216&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352221&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352218&type=" } ] } } ] }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "3.3　CDs及CDs@MOFs复合荧光材料光学性能" } ], "level": "2", "id": "s3c" } }, { "name": "p", "data": [ { "name": "text", "data": "CDs水溶液及CDs@MOFs固体复合荧光材料的归一化UV-Vis谱如" }, { "name": "xref", "data": { "text": "图5", "type": "fig", "rid": "F5", "data": [ { "name": "text", "data": "图5" } ] } }, { "name": "text", "data": "所示。" }, { "name": "xref", "data": { "text": "图5(a)", "type": "fig", "rid": "F5", "data": [ { "name": "text", "data": "图5(a)" } ] } }, { "name": "text", "data": "是CDs、Al-MOFs及CDs@Al-MOFs的归一化UV-Vis谱，CDs水溶液显示了两个吸收带，分别为278 nm吸收带和低能区400~570 nm的宽吸收带，后者的最高峰位于460 nm。278 nm吸收带归属于C" }, { "name": "inlineformula", "data": [ { "name": "math", "data": { "graphicsData": { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352223&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352227&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352225&type=" } } } ] }, { "name": "text", "data": "C键的π→π" }, { "name": "sup", "data": [ { "name": "text", "data": "*" } ] }, { "name": "text", "data": "跃迁，而400~570 nm的宽带吸收归属于C" }, { "name": "inlineformula", "data": [ { "name": "math", "data": { "graphicsData": { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352230&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352236&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352233&type=" } } } ] }, { "name": "text", "data": "O键的n→π" }, { "name": "sup", "data": [ { "name": "text", "data": "*" } ] }, { "name": "text", "data": "跃迁" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "blockXref", "data": { "data": [ { "name": "xref", "data": { "text": "60", "type": "bibr", "rid": "R60", "data": [ { "name": "text", "data": "60" } ] } }, { "name": "text", "data": "-" }, { "name": "xref", "data": { "text": "61", "type": "bibr", "rid": "R61", "data": [ { "name": "text", "data": "61" } ] } } ], "rid": [ "R60", "R61" ], "text": "60-61", "type": "bibr" } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。Al-MOFs材料的归一化UV-Vis谱显示了两个特征吸收峰，分别位于248 nm和290 nm，对应于苯环中C" }, { "name": "inlineformula", "data": [ { "name": "math", "data": { "graphicsData": { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352238&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352244&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352242&type=" } } } ] }, { "name": "text", "data": "C键的π→π" }, { "name": "sup", "data": [ { "name": "text", "data": "*" } ] }, { "name": "text", "data": "和羧基中C" }, { "name": "inlineformula", "data": [ { "name": "math", "data": { "graphicsData": { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352250&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352259&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352255&type=" } } } ] }, { "name": "text", "data": "O键的n→π" }, { "name": "sup", "data": [ { "name": "text", "data": "*" } ] }, { "name": "text", "data": "跃迁" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "blockXref", "data": { "data": [ { "name": "xref", "data": { "text": "62", "type": "bibr", "rid": "R62", "data": [ { "name": "text", "data": "62" } ] } }, { "name": "text", "data": "-" }, { "name": "xref", "data": { "text": "63", "type": "bibr", "rid": "R63", "data": [ { "name": "text", "data": "63" } ] } } ], "rid": [ "R62", "R63" ], "text": "62-63", "type": "bibr" } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。CDs@Al-MOFs的归一化UV-Vis谱中不但保留Al-MOFs的248 nm和290 nm两个吸收带，而且还显示出一个从紫外区(350 nm)延伸至低能区域(700 nm)的宽吸收峰，最大吸收峰位于480 nm，与CDs低能区的紫外吸收相比，最大吸收峰明显出现红移现象，这是因为CDs与Al-MOFs键合后生成了新的π-π共轭的生色团。" }, { "name": "xref", "data": { "text": "图5(b)", "type": "fig", "rid": "F5", "data": [ { "name": "text", "data": "图5(b)" } ] } }, { "name": "text", "data": "是CDs、Zn-MOFs及CDs@Zn-MOFs的归一化UV-Vis谱，也可以明显观察到CDs@Zn-MOFs保留了Zn-MOFs的C" }, { "name": "inlineformula", "data": [ { "name": "math", "data": { "graphicsData": { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352265&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352272&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352268&type=" } } } ] }, { "name": "text", "data": "C键的π→π" }, { "name": "sup", "data": [ { "name": "text", "data": "*" } ] }, { "name": "text", "data": "(231 nm)和C" }, { "name": "inlineformula", "data": [ { "name": "math", "data": { "graphicsData": { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352276&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352285&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352280&type=" } } } ] }, { "name": "text", "data": "O键的n→π" }, { "name": "sup", "data": [ { "name": "text", "data": "*" } ] }, { "name": "text", "data": "跃迁(292 nm)，同时，在低能区域显示了一个非对称宽吸收带，从400 nm一直延伸到650 nm，于540 nm达到最高峰。与CDs低能区的紫外吸收带相比，吸收峰的红移现象更为显著，这种现象归因于CDs与Zn-MOFs复合后生成了新的π-π共轭的生色团。CDs@Zn-MOFs在低能区的紫外吸收红移现象比CDs@Al-MOFs更为显著，其原因在于CDs与Zn-MOFs复合生成生色团的π-π共轭程度更大。" } ] }, { "name": "fig", "data": { "id": "F5", "caption": [ { "lang": "zh", "label": [ { "name": "text", "data": "图5" } ], "title": [ { "name": "text", "data": "(a)CDs、Al-MOFs和CDs@Al-MOFs的归一化UV-Vis谱;(b)CDs、Zn-MOFs和CDs@Zn-MOFs的归一化UV-Vis谱。" } ] }, { "lang": "en", "label": [ { "name": "text", "data": "Fig.5" } ], "title": [ { "name": "text", "data": "(a)Normalized UV-Vis absorption of CDs, Al-MOFs and CDs@Al-MOFs. (b)Normalized UV-Vis absorption of CDs, Zn-MOFs and CDs@Zn-MOFs." } ] } ], "subcaption": [], "note": [], "graphics": [ { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352289&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352298&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352294&type=" } ] } }, { "name": "p", "data": [ { "name": "text", "data": "利用荧光光谱进一步研究了CDs、CDs@Al-MOFs和CDs@Zn-MOFs的光学性质。" }, { "name": "xref", "data": { "text": "图6(a)", "type": "fig", "rid": "F6", "data": [ { "name": "text", "data": "图6(a)" } ] } }, { "name": "text", "data": "是CDs水溶液的荧光光谱，可以看到CDs水溶液用365 nm的波长激发可以发射黄色荧光(" }, { "name": "xref", "data": { "text": "图6(a)", "type": "fig", "rid": "F6", "data": [ { "name": "text", "data": "图6(a)" } ] } }, { "name": "text", "data": "插图)。CDs水溶液的激发谱出现了位于300 nm和420 nm的两个宽激发峰，其荧光强度和发射波长随激发波长从340 nm到560 nm的变化而改变，用420 nm的波长激发，最大发射峰位于540 nm，荧光量子产率为24.47%，其余波长激发得到的发射强度都相对较低;并且发射波长随着激发波长的增加而发生红移，显示出激发依赖特性。" }, { "name": "xref", "data": { "text": "图6(b)", "type": "fig", "rid": "F6", "data": [ { "name": "text", "data": "图6(b)" } ] } }, { "name": "text", "data": "为CDs@Al-MOFs的荧光光谱，可以看到在365 nm波长激发下可以发射黄色荧光(" }, { "name": "xref", "data": { "text": "图6(b)", "type": "fig", "rid": "F6", "data": [ { "name": "text", "data": "图6(b)" } ] } }, { "name": "text", "data": "插图)。在340~510 nm的不同激发波长激发下，发射峰波长均位于555 nm处，显示出非激发依赖行为，用480 nm波长激发得到最强发射峰，荧光量子产率为6.71%。" }, { "name": "xref", "data": { "text": "图6(c)", "type": "fig", "rid": "F6", "data": [ { "name": "text", "data": "图6(c)" } ] } }, { "name": "text", "data": "为CDs@Zn-MOFs的荧光光谱，可以看到在365 nm紫外光激发下可以发射红色荧光(" }, { "name": "xref", "data": { "text": "图6(c)", "type": "fig", "rid": "F6", "data": [ { "name": "text", "data": "图6(c)" } ] } }, { "name": "text", "data": "插图)。在440 nm到580 nm不同波长的激发下，发射峰的最大峰值均位于612 nm，同样显示出非激发依赖行为，在560 nm的最优激发下得到612 nm波长的宽带发射，其发射强度最大，荧光量子产率为3.64%。由" }, { "name": "xref", "data": { "text": "图6", "type": "fig", "rid": "F6", "data": [ { "name": "text", "data": "图6" } ] } }, { "name": "text", "data": "可见，CDs与MOFs键合为CDs@MOFs，两种复合荧光材料的发射峰与CDs水溶液的发射峰相比，均发生了不同程度的红移;并且激发性能由CDs水溶液的激发依赖特性都变为复合荧光材料的非激发依赖特性，这是因为CDs@MOFs复合荧光材料生成了新的生色团，产生了新的分子态发光。" } ] }, { "name": "fig", "data": { "id": "F6", "caption": [ { "lang": "zh", "label": [ { "name": "text", "data": "图6" } ], "title": [ { "name": "text", "data": "CDs水溶液(a)、CDs@Al-MOFs(b)和CDs@Zn-MOFs(c)的激发谱和在不同激发波长下的发射谱，插图分别是在自然光照下和365 nm紫外光激发下的照片。" } ] }, { "lang": "en", "label": [ { "name": "text", "data": "Fig.6" } ], "title": [ { "name": "text", "data": "Excitation and emission spectra under different excitation of CDs(a), CDs@Al-MOFs(b) and CDs@Zn-MOFs(c). Photos of CDs(inset of (a)), CDs@Al-MOFs(inset of (b)) and CDs@Zn-MOFs(inset of (c)) under the sunlight and UV light." } ] } ], "subcaption": [], "note": [], "graphics": [ { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352303&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352313&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352308&type=" } ] } } ] }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "3.4　发光机理分析" } ], "level": "2", "id": "s3d" } }, { "name": "p", "data": [ { "name": "text", "data": "通过FT-IR和XPS对结构表征分析，可以知道CDs存在着硫氰基、氨基和酰胺等表面官能团。从荧光光谱可知，CDs的发光存在激发依赖行为，当激发光谱波长小于460 nm时，主要是540 nm左右的黄色发光。从紫外吸收光谱可知CDs在400~570 nm的宽吸收带归属于C" }, { "name": "inlineformula", "data": [ { "name": "math", "data": { "graphicsData": { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352318&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352329&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352324&type=" } } } ] }, { "name": "text", "data": "O键，并且吸收带位置基本与CDs水溶液位于420 nm的宽激发峰(350~530 nm)重合。综合上述结果与分析，CDs的发光主要来自于C" }, { "name": "inlineformula", "data": [ { "name": "math", "data": { "graphicsData": { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352333&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352345&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352339&type=" } } } ] }, { "name": "text", "data": "O基团的表面态发光" }, { "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": "。Al-MOFs和Zn-MOFs材料体色都为白色且无荧光，而所制备的CDs@Al-MOFs和CDs@Zn-MOFs的体色分别为米黄色和粉红色，与白色的MOFs原料相比都有明显的变化。伴随其发光性质的改变，在低能区域的紫外吸收带出现显著红移，可以推断CDs@MOFs复合荧光材料产生了新的π-π共轭生色团。CDs@MOFs复合荧光材料的发射波长与CDs水溶液的高强度发射波长相比，都明显发生了红移，并且激发依赖特性消失。所以CDs@MOFs复合荧光材料主要依靠生色团发光，由原来碳点溶液的表面态发光转变为分子态发光" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "blockXref", "data": { "data": [ { "name": "xref", "data": { "text": "19", "type": "bibr", "rid": "R19", "data": [ { "name": "text", "data": "19" } ] } }, { "name": "text", "data": "-" }, { "name": "xref", "data": { "text": "20", "type": "bibr", "rid": "R20", "data": [ { "name": "text", "data": "20" } ] } } ], "rid": [ "R19", "R20" ], "text": "19-20", "type": "bibr" } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。CDs@Al-MOFs和CDs@Zn-MOFs的发射波长红移程度不同可能是由于两种不同金属MOFs的结构不同导致的。Zn" }, { "name": "sup", "data": [ { "name": "text", "data": "2+" } ] }, { "name": "text", "data": "常见的配位数是4，与有机团结合形成Zn-MOFs时空间构型更趋向于四面体构型" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "64", "type": "bibr", "rid": "R64", "data": [ { "name": "text", "data": "64" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": ";而Al" }, { "name": "sup", "data": [ { "name": "text", "data": "3+" } ] }, { "name": "text", "data": "常见的配位数是6，在形成Al-MOFs时更有利于形成八面体构型" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "65", "type": "bibr", "rid": "R65", "data": [ { "name": "text", "data": "65" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "。当CDs与Zn-MOFs成键复合时，更容易受到MOFs上的共轭基团影响，使复合荧光材料生成π-π共轭程度更大的生色团，从而使低能区紫外吸收红移程度更显著。" } ] } ] }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "3.5　CDs@MOFs复合荧光材料的白光LED应用" } ], "level": "2", "id": "s3e" } }, { "name": "p", "data": [ { "name": "text", "data": "基于CDs@Al-MOFs和CDs@Zn-MOFs良好的发射黄光和红光的性能，我们设计和封装了LED器件，期望它们能作为白光LED，其发光性能如" }, { "name": "xref", "data": { "text": "图7", "type": "fig", "rid": "F7", "data": [ { "name": "text", "data": "图7" } ] } }, { "name": "text", "data": "所示。" } ] }, { "name": "fig", "data": { "id": "F7", "caption": [ { "lang": "zh", "label": [ { "name": "text", "data": "图7" } ], "title": [ { "name": "text", "data": "(a)①号白光LED光谱;(b)②号白光LED光谱;(c)①号白光LED、②号白光LED和YAG基白光LED的CIE坐标、色温和显色指数;(d)~(e)不同颜色的电池和水果分别在②号白光LED光源和自然光照射下的照片。" } ] }, { "lang": "en", "label": [ { "name": "text", "data": "Fig.7" } ], "title": [ { "name": "text", "data": "Spectrum of ①WLED(a) and ②WLED(b). (c)CIE, CT and CRI of ①WLED, ②WLED and YAG-WLED. (d)-(e)Photographs of batteries and fruits with different colors under ②WLED light source and daylight, respectively." } ] } ], "subcaption": [], "note": [], "graphics": [ { "print": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352350&type=", "small": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352360&type=", "big": "http://html.publish.founderss.cn/rc-pub/api/common/picture?pictureId=21352356&type=" } ] } }, { "name": "p", "data": [ { "name": "xref", "data": { "text": "图7(a)", "type": "fig", "rid": "F7", "data": [ { "name": "text", "data": "图7(a)" } ] } }, { "name": "text", "data": "是将CDs@Al-MOFs黄色荧光粉涂覆在蓝光芯片上封装的①号白光LED发射谱，可以看到在480~725 nm范围有较宽的发射峰，最强发射峰位于555 nm，与商用YAG粉制得的LED光谱高度(左侧光谱插图)一致，仅是725 nm以后的红光部分发射稍低，因此CDs@Al-MOFs复合荧光材料是极好的白光LED用黄色荧光粉。由其在正常工作状态下的照片(右侧插图)可见，该器件可发射偏冷色调的白光。由" }, { "name": "xref", "data": { "text": "图6(c)", "type": "fig", "rid": "F6", "data": [ { "name": "text", "data": "图6(c)" } ] } }, { "name": "text", "data": "可见，CDs@Zn-MOFs在不同波长激发下均可发射红光，由于激发谱图以及在440 nm和460 nm激发时的发射强度较低，所以当蓝光芯片用450 nm激发时其发射强度也较低，因此其较强的红光发射应归因于能量传递。而560 nm为最优激发波长，该波长与CDs@Al-MOFs在555 nm的发射波长几乎完全吻合，因此CDs@Al-MOFs的发射波长可作为CDs@Zn-MOFs的激发波长进行能量传递，增强CDs@Zn-MOFs的红光发射。因此，我们将其作为红光源与黄光源CDs@Al-MOFs以不同比例混合制成混合荧光粉，通过调节混合比进而调控发光的冷暖性能。在①号器件的基础上，添加65%的CDs@Zn-MOFs制成混合荧光粉涂覆于蓝光芯片上，封装成②号白光LED器件，其光谱见" }, { "name": "xref", "data": { "text": "图7(b)", "type": "fig", "rid": "F7", "data": [ { "name": "text", "data": "图7(b)" } ] } }, { "name": "text", "data": "。由图可见，该器件在480~800 nm范围内发射的半峰宽明显增大，绿光和红光发射明显变宽，特别是红光发射增加显著，以600~800 nm下光谱的积分面积计，比①号器件的红光发射增加228%，比YAG器件的红光发射增加65%，因此器件的暖色调增加。由7(b)的插图可见，②号白光LED器件在正常工作时呈现暖色调的白光。" }, { "name": "xref", "data": { "text": "图7(c)", "type": "fig", "rid": "F7", "data": [ { "name": "text", "data": "图7(c)" } ] } }, { "name": "text", "data": "为基于两种复合荧光材料的白光LED器件和商用YAG器件的国际照明委员会标准色彩空间色坐标图，可以看到①号白光LED器件的色坐标(Chromaticity coordinate,CIE)为(0.32,0.34)、色温(Color temperature,CT)为6 070 K、显色指数(Color render index,CRI)为72.7，对应a点;而②号白光LED器件的色坐标为(0.37,0.33)、色温为3 968 K、显色指数为82.4，对应b点。c点为市售YAG制白光LED的相关数据，色坐标为(0.33,0.34)、色温为5 606 K、显色指数为73.1。根据《建筑照明设计标准》GB50034-2013的规定" }, { "name": "sup", "data": [ { "name": "text", "data": "[" }, { "name": "xref", "data": { "text": "66", "type": "bibr", "rid": "R66", "data": [ { "name": "text", "data": "66" } ] } }, { "name": "text", "data": "]" } ] }, { "name": "text", "data": "，室内照明光源色表按相关色温分为三组:相关色温" }, { "name": "text", "data": "<" }, { "name": "text", "data": "3 300 K为暖色，3 000~5 300 K为中间色，" }, { "name": "text", "data": ">" }, { "name": "text", "data": "5 300 K为冷色，同时规定长期工作或停留的房间或场所选用LED光源时，其色温不宜高于4 000 K，显色指数(" }, { "name": "italic", "data": [ { "name": "text", "data": "Ra" } ] }, { "name": "text", "data": ")不应小于80，特殊显色指数" }, { "name": "italic", "data": [ { "name": "text", "data": "R" } ] }, { "name": "text", "data": "9应大于零。因此，②号白光LED器件有潜力用作长期使用的白光LED照明光源。将不同颜色的电池和水果分别暴露在②号白光LED光源和自然光照射下进行拍照对比，照片分别见" }, { "name": "xref", "data": { "text": "图7(d)、(e)", "type": "fig", "rid": "F7", "data": [ { "name": "text", "data": "图7(d)、(e)" } ] } }, { "name": "text", "data": "。结果显示，在②号白光LED光源的照射下拍照能达到颜色鲜艳饱满的效果，证明该基于CDs的复合荧光粉在固态照明领域具有巨大的应用潜力。" } ] } ] } ] }, { "name": "sec", "data": [ { "name": "sectitle", "data": { "title": [ { "name": "text", "data": "4　结论" } ], "level": "1", "id": "s4" } }, { "name": "p", "data": [ { "name": "text", "data": "我们制备了掺杂了N和S元素的黄色发光CDs，表现出明显激发依赖特性，最强发射峰是用420 nm激发时出现在540 nm。将CDs分别与Al-MOFs和Zn-MOFs材料复合，制备了不同载体基质的CDs@MOFs复合荧光材料，其发射波长与CDs水溶液的发射相比发生了不同程度的红移，CDs@Al-MOFs为发射波长位于555 nm的黄色荧光复合荧光材料，CDs@Zn-MOFs为发射波长位于612 nm的红色荧光复合荧光材料，它们均表现出非激发依赖行为。红移的原因是由于复合荧光材料产生了新的π-π共轭生色团，由依靠CDs表面态发光转变成依靠分子态发光。通过一种简单新颖的方式制备了基于CDs的长波发光固体材料，有效抑制了CDs的聚集诱导荧光猝灭。应用所制备的CDs@Al-MOFs复合荧光材料制备成①号白光LED器件，色温为6 070 K，显色指数为72.7。应用所制备的CDs@Al-MOFs和CDs@Zn-MOFs复合荧光材料(混合质量比为1∶0.65)制备成②号白光LED器件，其色温小于4 000 K，显色指数达82.4，符合GB50034-2013中规定的LED照明光源指标，表明其CDs@MOFs复合荧光材料在LED照明领域具有广阔的应用前景。" } ] }, { "name": "p", "data": [ { "name": "text", "data": "本文专家审稿意见及作者回复内容的下载地址:http://cjl.lightpublishing.cn/thesisDetails#10.37188/CJL.20210122." } ] } ] } ], "footnote": [], "reflist": { "title": [ { "name": "text", "data": "参考文献:" } ], "data": [ { "id": "R1", "label": "[1]", "citation": [ { "lang": "en", "text": [ { "name": "text", "data": "XU X Y" }, { "name": "text", "data": ", " }, { "name": "text", "data": "RAY R" }, { "name": "text", "data": ", " }, { "name": "text", "data": "GU Y L" }, { "name": "text", "data": ", " }, { "name": "text", "data": "et al" }, { "name": "text", "data": ". 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