CN105670634A - Controllable preparation method for CdSe quantum dots by organic liquid phase method - Google Patents
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- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical class [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 15
- 239000007791 liquid phase Substances 0.000 title claims abstract description 4
- 238000002360 preparation method Methods 0.000 title abstract description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000011734 sodium Substances 0.000 claims abstract description 20
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052786 argon Inorganic materials 0.000 claims abstract description 14
- 238000010992 reflux Methods 0.000 claims abstract description 14
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 8
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 8
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 8
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000005642 Oleic acid Substances 0.000 claims abstract description 8
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 8
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 8
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229940101006 anhydrous sodium sulfite Drugs 0.000 claims abstract description 7
- 235000011187 glycerol Nutrition 0.000 claims abstract description 7
- 239000002096 quantum dot Substances 0.000 claims abstract description 7
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims abstract description 7
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000002270 dispersing agent Substances 0.000 claims description 6
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 6
- 239000012154 double-distilled water Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 6
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 6
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims 1
- 238000009835 boiling Methods 0.000 claims 1
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 abstract description 11
- 239000012074 organic phase Substances 0.000 abstract description 3
- 239000012153 distilled water Substances 0.000 abstract 1
- HFQQZARZPUDIFP-UHFFFAOYSA-M sodium;2-dodecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O HFQQZARZPUDIFP-UHFFFAOYSA-M 0.000 abstract 1
- ZMBHCYHQLYEYDV-UHFFFAOYSA-N trioctylphosphine oxide Chemical compound CCCCCCCCP(=O)(CCCCCCCC)CCCCCCCC ZMBHCYHQLYEYDV-UHFFFAOYSA-N 0.000 description 5
- 239000002243 precursor Substances 0.000 description 2
- 239000011669 selenium Substances 0.000 description 2
- 101100136092 Drosophila melanogaster peng gene Proteins 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- VQNPSCRXHSIJTH-UHFFFAOYSA-N cadmium(2+);carbanide Chemical compound [CH3-].[CH3-].[Cd+2] VQNPSCRXHSIJTH-UHFFFAOYSA-N 0.000 description 1
- UJYLYGDHTIVYRI-UHFFFAOYSA-N cadmium(2+);ethane Chemical compound [Cd+2].[CH2-]C.[CH2-]C UJYLYGDHTIVYRI-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000013110 organic ligand Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- RMZAYIKUYWXQPB-UHFFFAOYSA-N trioctylphosphane Chemical compound CCCCCCCCP(CCCCCCCC)CCCCCCCC RMZAYIKUYWXQPB-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
- C09K11/881—Chalcogenides
- C09K11/883—Chalcogenides with zinc or cadmium
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
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Abstract
本发明公开了一种有机液相法可控制备CdSe量子点的方法。（1）在氩气保护下，将0.316？g硒粉和3.528g无水亚硫酸钠加入装有100mL二次蒸馏水的三口烧瓶中，回流2小时，冷却，得Na2SeSO3溶胶。（2）将20mL浓度为？0.03mol/L？的Cd(NO3)2·4H2O溶液和10mL分析纯甘油加入到三口烧瓶中混合均匀。（3）在步骤（2）所得溶液中加入6mL分析纯油酸、30mL分析纯？NMP、5mL~20mL浓度为？0.01mol/L的Na2EDTA、5mL~20mL？浓度为0.03mol/L的SDBS混合均匀。（4）置于水浴中加热，至60℃~100℃后，加入15~20mL？Na2SeSO3溶胶，在氩气保护下恒温反应回流10~60分钟，冷却。本发明制备工艺简单，最显著的特点是有机相法合成CdSe量子点，分散性好、工艺简单、易存储、无污染、可控性高。The invention discloses a method for controllable preparation of CdSe quantum dots by an organic liquid phase method. (1) Under the protection of argon, the 0.316? Add 1 g of selenium powder and 3.528 g of anhydrous sodium sulfite into a three-necked flask filled with 100 mL of twice distilled water, reflux for 2 hours, and cool to obtain Na 2 SeSO 3 sol. (2) What is the concentration of 20mL? 0.03mol/L? Cd(NO 3 ) 2 ·4H 2 O solution and 10 mL of analytically pure glycerin were added into a three-necked flask and mixed evenly. (3) Add 6 mL of analytically pure oleic acid and 30 mL of analytically pure oleic acid to the solution obtained in step (2). What is the concentration of NMP, 5mL~20mL? 0.01mol/L Na 2 EDTA, 5mL~20mL? SDBS with a concentration of 0.03mol/L was mixed evenly. (4) Put it in a water bath and heat it to 60°C~100°C, add 15~20mL? Na 2 SeSO 3 sol, reflux at constant temperature for 10-60 minutes under the protection of argon, and cool down. The preparation process of the present invention is simple, and the most notable feature is that the CdSe quantum dot is synthesized by an organic phase method, which has good dispersibility, simple process, easy storage, no pollution and high controllability.
Description
技术领域 technical field
本发明涉及一种有机液相法可控制备CdSe量子点的方法。 The invention relates to a method for the controllable preparation of CdSe quantum dots by an organic liquid phase method.
背景技术 Background technique
量子点是准零维纳米材料，三个维度尺寸均在纳米数量级内，CdSe量子点是其典型的代表。在CdSe量子点研究领域中，诸多研究工作者已经取得了较大的进展。Bawendi等人首次采用三辛基氧化膦(TOPO)作为有机配体，用二甲基镉或二乙基镉和Se的三辛基膦溶液作为镉和硒的前体，将上述前体迅速注入到剧烈搅拌的350℃的TOPO中，短时间内即有大量的CdSe量子点的晶核形成。然后通过迅速降温来阻止硒化镉量子点继续成核，再升温使其生长。这项成果意味着，它第一次解决了以往量子点制备中存在的尺寸分布过宽、表面缺陷过多而导致荧光效率低的难题，为继续深入探究硒化镉量子点的光物理与光化学性质奠定了重要的基础。Peng等对上述方法进行了改进，并在CdSe量子点的油相合成领域做了大量突出而细致的工作，为推动量子点的理论和应用研究作出了重要贡献。Biju等在Peng的研究基础上,利用TOP和TOPO的混合物作溶剂,Cd(AcO)和TOPSe作为原料,采用75℃的低温反应制备了尺寸单一的发绿光的CdSeQDs。尽管如此，CdSe量子点的制备工艺仍存在许多不足：使用有机有毒试剂（TOP和TOPO均是剧毒物质），工艺复杂，设备要求高等缺点。 Quantum dots are quasi-zero-dimensional nanomaterials, and the three dimensions are all on the order of nanometers. CdSe quantum dots are a typical representative. In the field of CdSe quantum dot research, many researchers have made great progress. For the first time, Bawendi et al. used trioctylphosphine oxide (TOPO) as an organic ligand, using trioctylphosphine solution of dimethylcadmium or diethylcadmium and Se as precursors of cadmium and selenium, and injected the above precursors rapidly In the violently stirred TOPO at 350°C, a large number of crystal nuclei of CdSe quantum dots are formed in a short time. Then the cadmium selenide quantum dots are prevented from continuing to nucleate by rapidly cooling down, and then the temperature is raised to make it grow. This achievement means that for the first time, it has solved the problem of low fluorescence efficiency caused by too wide size distribution and too many surface defects in the preparation of quantum dots in the past. Nature lays an important foundation. Peng et al. improved the above method, and did a lot of outstanding and meticulous work in the field of oil-phase synthesis of CdSe quantum dots, and made important contributions to promoting the theoretical and applied research of quantum dots. On the basis of Peng's research, Biju et al. used a mixture of TOP and TOPO as a solvent, Cd(AcO) and TOPSe as raw materials, and prepared green-emitting CdSeQDs with a single size by a low-temperature reaction at 75 °C. Nevertheless, there are still many shortcomings in the preparation process of CdSe quantum dots: the use of organic toxic reagents (TOP and TOPO are both highly toxic substances), complex processes, and high equipment requirements.
发明内容 Contents of the invention
本发明的目的是提供一种有机相法可控制备CdSe量子点的方法。 The purpose of the present invention is to provide a method for the controllable preparation of CdSe quantum dots by an organic phase method.
具体步骤为： The specific steps are:
（1）在氩气保护(无氧)条件下，将0.316g硒粉和3.528g无水亚硫酸钠加入装有100mL二次蒸馏水的三口烧瓶中，沸腾下反应回流2小时，冷却，即得浓度为0.004mol/L的Na2SeSO3溶胶。 (1) Under argon protection (oxygen-free), add 0.316g of selenium powder and 3.528g of anhydrous sodium sulfite into a three-necked flask filled with 100mL of double-distilled water, boil and reflux for 2 hours, and cool to obtain a concentration of 0.004mol/L Na 2 SeSO 3 sol.
（2）将20mL浓度为0.03mol/L的Cd(NO3)2·4H2O溶液和10mL分析纯甘油加入到三口烧瓶中混合均匀。 (2) Add 20 mL of Cd(NO 3 ) 2 ·4H 2 O solution with a concentration of 0.03 mol/L and 10 mL of analytically pure glycerin into a three-necked flask and mix well.
（3）在步骤（2）所得溶液中加入6mL分析纯油酸、30mL分析纯N-甲基吡咯烷酮溶液(NMP)、5mL~20mL浓度为0.01mol/L的乙二胺四乙酸二钠溶液(Na2EDTA)和5mL~20mL浓度为0.03mol/L的十二烷基苯磺酸钠溶液(SDBS)，混合均匀，得到溶液A。 (3) Add 6 mL of analytically pure oleic acid, 30 mL of analytically pure N-methylpyrrolidone solution (NMP), and 5 mL to 20 mL of 0.01 mol/L disodium edetate solution ( Na 2 EDTA) and 5mL~20mL sodium dodecylbenzenesulfonate solution (SDBS) with a concentration of 0.03mol/L, mix well to obtain solution A.
（4）将步骤（3）所得A溶液置于水浴中加热，待温度升至60℃~100℃后，缓慢加入15~20mL步骤（1）所得浓度为0.004mol/L的Na2SeSO3溶胶，在氩气保护(无氧)条件下恒温反应回流10~60分钟，冷却，即得CdSe量子点，对其进行离心沉淀分离后用分散剂分散，其粒径分布在1.7nm~700nm。 (4) Heat the A solution obtained in step (3) in a water bath. After the temperature rises to 60°C~100°C, slowly add 15~20mL of Na 2 SeSO 3 sol with a concentration of 0.004mol/L obtained in step (1) , under argon protection (oxygen-free) conditions, constant temperature reaction and reflux for 10-60 minutes, cooling to obtain CdSe quantum dots, which are separated by centrifugal precipitation and dispersed with a dispersant, and the particle size distribution is 1.7nm-700nm.
本发明与其他相关技术相比，最显著的特点是有机相法合成CdSe量子点，制备方法简单，具有分散性好，量子点尺寸可控，易存储，毒性小、无污染等优点。 Compared with other related technologies, the present invention has the most notable features of synthesizing CdSe quantum dots by organic phase method, simple preparation method, good dispersibility, controllable size of quantum dots, easy storage, low toxicity and no pollution.
具体实施方式 detailed description
实施例1： Example 1:
（1）在氩气保护(无氧)条件下，将0.316g硒粉和3.528g无水亚硫酸钠加入装有100mL二次蒸馏水的三口烧瓶中，沸腾下反应回流2小时，冷却，即得浓度为0.004mol/L的Na2SeSO3溶胶。 (1) Under argon protection (oxygen-free), add 0.316g of selenium powder and 3.528g of anhydrous sodium sulfite into a three-necked flask filled with 100mL of double-distilled water, boil and reflux for 2 hours, and cool to obtain a concentration of 0.004mol/L Na 2 SeSO 3 sol.
（2）将20mL浓度为0.03mol/L的Cd(NO3)2·4H2O溶液和10mL分析纯甘油加入到三口烧瓶中混合均匀。 (2) Add 20 mL of Cd(NO 3 ) 2 ·4H 2 O solution with a concentration of 0.03 mol/L and 10 mL of analytically pure glycerin into a three-necked flask and mix well.
（3）在步骤（2）所得溶液中加入6mL分析纯油酸、30mL分析纯N-甲基吡咯烷酮溶液(NMP)、10mL浓度为0.01mol/L的乙二胺四乙酸二钠溶液(Na2EDTA)和10mL浓度为0.03mol/L的十二烷基苯磺酸钠溶液(SDBS)，混合均匀，得到溶液A。 (3) Add 6 mL of analytically pure oleic acid, 30 mL of analytically pure N-methylpyrrolidone solution (NMP), and 10 mL of 0.01 mol/L disodium edetate solution (Na 2 EDTA) and 10 mL of sodium dodecylbenzenesulfonate solution (SDBS) with a concentration of 0.03 mol/L, mixed uniformly to obtain solution A.
（4）将步骤（3）所得A溶液置于水浴中加热，待温度升至100℃后，缓慢加入20mL步骤（1）所得浓度为0.004mol/L的Na2SeSO3溶胶，在氩气保护(无氧)条件下恒温反应回流30分钟，冷却，即得CdSe量子点，对其进行离心沉淀分离后用分散剂分散，其粒径分布在1.7nm~2.3nm。 (4) Heat the A solution obtained in step (3) in a water bath. After the temperature rises to 100°C, slowly add 20 mL of Na 2 SeSO 3 sol with a concentration of 0.004 mol/L obtained in step (1) and protect it under argon Under the condition of constant temperature (without oxygen), reflux at constant temperature for 30 minutes, and cool to obtain CdSe quantum dots, which are separated by centrifugal precipitation and dispersed with dispersant, and the particle size distribution is between 1.7nm and 2.3nm.
实施例2： Example 2:
（1）在氩气保护(无氧)条件下，将0.316g硒粉和3.528g无水亚硫酸钠加入装有100mL二次蒸馏水的三口烧瓶中，沸腾下反应回流2小时，冷却，即得浓度为0.004mol/L的Na2SeSO3溶胶。 (1) Under argon protection (oxygen-free), add 0.316g of selenium powder and 3.528g of anhydrous sodium sulfite into a three-necked flask filled with 100mL of double-distilled water, boil and reflux for 2 hours, and cool to obtain a concentration of 0.004mol/L Na 2 SeSO 3 sol.
（2）将20mL浓度为0.03mol/L的Cd(NO3)2·4H2O溶液和10mL分析纯甘油加入到三口烧瓶中混合均匀。 (2) Add 20 mL of Cd(NO 3 ) 2 ·4H 2 O solution with a concentration of 0.03 mol/L and 10 mL of analytically pure glycerin into a three-necked flask and mix well.
（3）在步骤（2）所得溶液中加入6mL分析纯油酸、30mL分析纯N-甲基吡咯烷酮溶液(NMP)、5mL浓度为0.01mol/L的乙二胺四乙酸二钠溶液(Na2EDTA)和15mL浓度为0.03mol/L的十二烷基苯磺酸钠溶液(SDBS)，混合均匀，得到溶液A。 (3) Add 6 mL of analytically pure oleic acid, 30 mL of analytically pure N-methylpyrrolidone solution (NMP), and 5 mL of 0.01 mol/L disodium edetate solution (Na 2 EDTA) and 15 mL of sodium dodecylbenzene sulfonate solution (SDBS) with a concentration of 0.03 mol/L, mixed uniformly to obtain solution A.
（4）将步骤（3）所得A溶液置于水浴中加热，待温度升至90℃后，缓慢加入20mL步骤（1）所得浓度为0.004mol/L的Na2SeSO3溶胶，在氩气保护(无氧)条件下恒温反应回流50分钟，冷却，即得CdSe量子点，对其进行离心沉淀分离后用分散剂分散，其粒径分布在10nm~550nm。 (4) Heat the A solution obtained in step (3) in a water bath. After the temperature rises to 90°C, slowly add 20 mL of Na 2 SeSO 3 sol with a concentration of 0.004 mol/L obtained in step (1) and protect it under argon Under (oxygen-free) conditions, constant temperature reaction and reflux for 50 minutes, cooling to obtain CdSe quantum dots, which are separated by centrifugal precipitation and dispersed with dispersant, and the particle size distribution is 10nm~550nm.
实施例3： Example 3:
（1）在氩气保护(无氧)条件下，将0.316g硒粉和3.528g无水亚硫酸钠加入装有100mL二次蒸馏水的三口烧瓶中，沸腾下反应回流2小时，冷却，即得浓度为0.004mol/L的Na2SeSO3溶胶。 (1) Under argon protection (oxygen-free), add 0.316g of selenium powder and 3.528g of anhydrous sodium sulfite into a three-necked flask filled with 100mL of double-distilled water, boil and reflux for 2 hours, and cool to obtain a concentration of 0.004mol/L Na 2 SeSO 3 sol.
（2）将20mL浓度为0.03mol/L的Cd(NO3)2·4H2O溶液和10mL分析纯甘油加入到三口烧瓶中混合均匀。 (2) Add 20 mL of Cd(NO 3 ) 2 ·4H 2 O solution with a concentration of 0.03 mol/L and 10 mL of analytically pure glycerin into a three-necked flask and mix well.
（3）在步骤（2）所得溶液中加入6mL分析纯油酸、30mL分析纯N-甲基吡咯烷酮溶液(NMP)、20mL浓度为0.01mol/L的乙二胺四乙酸二钠溶液(Na2EDTA)、5mL浓度为0.03mol/L的十二烷基苯磺酸钠溶液(SDBS)混合均匀，得到溶液A。 (3) Add 6 mL of analytically pure oleic acid, 30 mL of analytically pure N-methylpyrrolidone solution (NMP), and 20 mL of 0.01 mol/L disodium edetate solution (Na 2 EDTA), 5 mL of sodium dodecylbenzenesulfonate solution (SDBS) with a concentration of 0.03 mol/L were mixed uniformly to obtain solution A.
（4）将步骤（3）所得A溶液置于水浴中加热，待温度升至60℃后，缓慢加入20mL步骤（1）所得浓度为0.004mol/L的Na2SeSO3溶胶，在氩气保护(无氧)条件下恒温反应回流30分钟，冷却，即得CdSe量子点，对其进行离心沉淀分离后用分散剂分散，其粒径分布在8nm~700nm。 (4) Heat the A solution obtained in step (3) in a water bath. After the temperature rises to 60°C, slowly add 20 mL of Na 2 SeSO 3 sol with a concentration of 0.004 mol/L obtained in step (1), and protect it under argon Under the condition of (oxygen-free) constant temperature reaction and reflux for 30 minutes, cooling to obtain CdSe quantum dots, which are separated by centrifugal precipitation and dispersed with dispersant, and the particle size distribution is 8nm~700nm.
实施例4： Example 4:
（1）在氩气保护(无氧)条件下，将0.316g硒粉和3.528g无水亚硫酸钠加入装有100mL二次蒸馏水的三口烧瓶中，沸腾下反应回流2小时，冷却，即得浓度为0.004mol/L的Na2SeSO3溶胶。 (1) Under argon protection (oxygen-free), add 0.316g of selenium powder and 3.528g of anhydrous sodium sulfite into a three-necked flask filled with 100mL of double-distilled water, boil and reflux for 2 hours, and cool to obtain a concentration of 0.004mol/L Na 2 SeSO 3 sol.
（2）将20mL浓度为0.03mol/L的Cd(NO3)2·4H2O溶液和10mL分析纯甘油加入到三口烧瓶中混合均匀。 (2) Add 20 mL of Cd(NO 3 ) 2 ·4H 2 O solution with a concentration of 0.03 mol/L and 10 mL of analytically pure glycerin into a three-necked flask and mix well.
（3）在步骤（2）所得溶液中加入6mL分析纯油酸、30mL分析纯N-甲基吡咯烷酮溶液(NMP)、20mL浓度为0.01mol/L的乙二胺四乙酸二钠溶液(Na2EDTA)和20mL浓度为0.03mol/L的十二烷基苯磺酸钠溶液(SDBS)，混合均匀，得到溶液A。 (3) Add 6 mL of analytically pure oleic acid, 30 mL of analytically pure N-methylpyrrolidone solution (NMP), and 20 mL of 0.01 mol/L disodium edetate solution (Na 2 EDTA) and 20 mL of sodium dodecylbenzenesulfonate solution (SDBS) with a concentration of 0.03 mol/L, mixed uniformly to obtain solution A.
（4）将步骤（3）所得A溶液置于水浴中加热，待温度升至100℃后，缓慢加入20mL步骤（1）所得浓度为0.004mol/L的Na2SeSO3溶胶，在氩气保护(无氧)条件下恒温反应回流10分钟，冷却，即得CdSe量子点，对其进行离心沉淀分离后用分散剂分散，其粒径分布在100nm~400nm。 (4) Heat the A solution obtained in step (3) in a water bath. After the temperature rises to 100°C, slowly add 20 mL of Na 2 SeSO 3 sol with a concentration of 0.004 mol/L obtained in step (1) and protect it under argon Under (oxygen-free) condition, constant temperature reaction and reflux for 10 minutes, cooling to obtain CdSe quantum dots, which are separated by centrifugal precipitation and dispersed with dispersant, and the particle size distribution is 100nm~400nm.
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