CN101104801A - CdTeS量子点的制备 - Google Patents
CdTeS量子点的制备 Download PDFInfo
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- CN101104801A CN101104801A CNA2006100147711A CN200610014771A CN101104801A CN 101104801 A CN101104801 A CN 101104801A CN A2006100147711 A CNA2006100147711 A CN A2006100147711A CN 200610014771 A CN200610014771 A CN 200610014771A CN 101104801 A CN101104801 A CN 101104801A
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- 239000002096 quantum dot Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title description 16
- 238000000034 method Methods 0.000 claims abstract description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- 239000007787 solid Substances 0.000 claims description 8
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 239000000047 product Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000006073 displacement reaction Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 230000001476 alcoholic effect Effects 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims 1
- 239000013557 residual solvent Substances 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 4
- 229910052793 cadmium Inorganic materials 0.000 abstract description 3
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 abstract description 3
- 239000002360 explosive Substances 0.000 abstract description 3
- 238000006862 quantum yield reaction Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 abstract 1
- CXKCTMHTOKXKQT-UHFFFAOYSA-N cadmium oxide Inorganic materials [Cd]=O CXKCTMHTOKXKQT-UHFFFAOYSA-N 0.000 abstract 1
- CFEAAQFZALKQPA-UHFFFAOYSA-N cadmium(2+);oxygen(2-) Chemical compound [O-2].[Cd+2] CFEAAQFZALKQPA-UHFFFAOYSA-N 0.000 abstract 1
- 239000011258 core-shell material Substances 0.000 abstract 1
- 229910004613 CdTe Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910005543 GaSe Inorganic materials 0.000 description 2
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002159 nanocrystal Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- -1 BaS Inorganic materials 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 229910000530 Gallium indium arsenide Inorganic materials 0.000 description 1
- 229910000673 Indium arsenide Inorganic materials 0.000 description 1
- 229910004411 SrTe Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
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- 230000002209 hydrophobic effect Effects 0.000 description 1
- RPQDHPTXJYYUPQ-UHFFFAOYSA-N indium arsenide Chemical compound [In]#[As] RPQDHPTXJYYUPQ-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000004054 semiconductor nanocrystal Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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Abstract
本发明公开了一种制备CdTeS量子点的方法。本方法是用氧化镉或醋酸镉等无机物做原料，在一定的温度条件下制备CdTeS量子点。该方法既避免了核/壳型量子点的制备繁杂，又克服了采用Cd(CH3)2等有机镉的易燃易爆及价格昂贵的缺陷。本发明的方法操作简便，重复性好，安全易行，成本低廉。本发明得到的CdTeS量子点荧光强度高，半峰宽窄，量子产率高，稳定性好，发射波长更长(红外及近红外部份(λ＝620－728nm))。
Description
技术领域
本发明涉及一种CdTeS量子点的制备方法
背景技术
量子点(quantum dots，QDs)又可称为半导体纳米晶体(semicondutor nanocrystal)，是一种由II-VI族或III-V族元素组成的的纳米晶粒。量子点的超微尺寸导致了一种量子尺度效应，赋予了其独特的光学和电子学性质。量子点由于其大小不同(或组成不同)即可发出不同颜色的荧光，而且可用单一波长的光去激发多种不同颜色的量子点。近年来，量子点由于其独特的光致发光性质越来越受到人们的重视，1998年开始应用于生命科学研究，随后，其研究应用范围涉及物理、化学、材料、生物等多学科，已成为一门新兴的交叉学科。
常见的量子点发光材料多为II-IV族或III-V族的元素组成，发光范围覆盖可见光及红外区域。其中II-IV族的元素包括MgS，MgSe，GaS，GaSe，GaSe，SrTe，BaS，ZnS，CdS，CdSe，CdTe等，III-V族的元素包括GaAs，InGaAs，InP，InAs等。研究比较多的是CdS、CdSe、CdTe、ZnS、InGaN/GaN等。
量子点材料的制备方法很多，可以分为物理和化学两类制备方法。物理制备方法常常需要大型的仪器设备、高阵控等比较苛刻的条件，并且制备出的纳米颗粒粒径分布宽，不易控制。而化学制备方法则具有化学方法的优点是：量子点尺寸可以小至2～10nm，平均尺寸分布大约在5％～10％的范围内，量子点的组分易于控制，可获得高密度的量子点阵列，制备价格较为低廉等。
目前，常见的化学制备方法，主要采取核/壳型量子点的制备工艺，采用Cd(CH3)2等有机镉的易燃易爆及价格昂贵原料，工艺复杂，不安全，难操作。
本发明方法既避免了核/壳型量子点的制备繁杂，，又克服了采用Cd(CH3)2等有机镉的易燃易爆及价格昂贵的缺陷。
发明内容
本发明针对以往量子点合成的不足，提出了一种合成疏水性CdTeS量子点的方法。本方法操作简便，安全，易行，再现性好，成本低廉。
本发明提出的具体技术方案是：一种CdTeS量子点的制备方法，采用如下步骤：
(a)准确称量Te和S加入反应器A中，再加入OA和TOP制得储备液。
(b)准确称量CdO加到反应器B中，先后加入OA、TOA和TOP，输入Ar气置换净瓶中空气，搅拌下加热至260-330℃，滴加上述储备液，维持该温度10秒至5分钟，去掉加热装置，待温度降到100-30℃时，将反应液倒入盛有甲醇或乙醇的容器C中。
(c)将得到的产物倾去上清液，固体用氯仿溶解后，再加入甲醇或乙醇，离心沉降2-20min，倾去上清液，剩余的固体用真空泵抽净挥发性物质，得到固体量子点产物。将该CdTeS量子点产物溶于溶剂，可得到发射波长为600-728nm的量子点溶液。
采用本发明方法制备的CdTeS量子点荧光强度高，半峰宽窄，量子产率高，稳定性好，发射波长更长(红外及近红外部份(λ＝620-728nm))。
具体实施方式
CdTeS量子点制备分为三部分：(a)Te和S储备液的制备；(b)CdTeS量子点的合成；(c)后处理。
(a)Te和S储备液的制备
在25ml圆底烧瓶中(反应器A)加入5mgTe粉和320mgS粉，移入5mlOA和1mlTOP，溶解后得到TeS储备液。
(b)CdTeS量子点的合成
在100ml四口瓶中(反应器B)装搅拌，温度计和氩气保护装置，准确称量CdO 400mg，加入20ml OA、5ml TOA及20ml TOP，通Ar置换净空气，搅拌下加热升温。当反应器B温度达到260-300℃，滴加储备液A，维持260℃反应30秒钟，去掉加热装置，待温度降到100℃时，将反应液倒入盛有50ml甲醇的100ml三角瓶中(反应器C)，密封后避光保存。
(c)后处理
将C中的上清液倾去，加入10ml氯仿溶解至均匀透明，加入20ml甲醇离心沉降5分钟后，倾去上层清液，余下的固体用真空泵抽干挥发物后，得到固体CdTeS量子点。
Claims (1)
1.一种制备CdTeS量子点的方法，其特征在于采用下述步骤：
(a)在反应器A中准确称量Te和S，加入OA和TOP制成储备液。
(b)准确称量CdO加入反应器B中，先后加入OA、TOA和TOP，通入隋性气体(Ar)置换净空气，搅拌下加热升温，当反应温度达到265-330℃时，滴加上述储备液，维持温度反应10秒到15分钟，去掉加热装置，待温度降低到100-30℃，将反应液倒入盛有甲醇或乙醇的容器C中。
将得到的产物倾去上清液，固体用氯仿溶解后，再加甲醇，离心2-20min，倾去上清液，剩余固体用真空泵抽净残余溶剂，可得到波长600-728nm的量子点固体。
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2006100147711A CN101104801A (zh) | 2006-07-13 | 2006-07-13 | CdTeS量子点的制备 |
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| CNA2006100147711A CN101104801A (zh) | 2006-07-13 | 2006-07-13 | CdTeS量子点的制备 |
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| CN101104801A true CN101104801A (zh) | 2008-01-16 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106318372A (zh) * | 2015-09-15 | 2017-01-11 | 中国科学院遗传与发育生物学研究所 | 一种荧光纳米颗粒及其合成方法、应用 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106318372A (zh) * | 2015-09-15 | 2017-01-11 | 中国科学院遗传与发育生物学研究所 | 一种荧光纳米颗粒及其合成方法、应用 |
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