CN106129142A - A kind of preparation method of vulcanized lead quantum dot - Google Patents
A kind of preparation method of vulcanized lead quantum dot Download PDFInfo
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- 239000002096 quantum dot Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- XCAUINMIESBTBL-UHFFFAOYSA-N lead(ii) sulfide Chemical compound [Pb]=S XCAUINMIESBTBL-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229940056932 lead sulfide Drugs 0.000 claims abstract description 14
- 229910052981 lead sulfide Inorganic materials 0.000 claims abstract description 14
- 239000000243 solution Substances 0.000 claims description 47
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 30
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 27
- 239000001509 sodium citrate Substances 0.000 claims description 27
- 239000000126 substance Substances 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 17
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 15
- 239000011259 mixed solution Substances 0.000 claims description 15
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 12
- 229940046892 lead acetate Drugs 0.000 claims description 12
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 239000000654 additive Substances 0.000 claims description 3
- 239000012752 auxiliary agent Substances 0.000 claims description 3
- 239000000376 reactant Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 5
- 238000001228 spectrum Methods 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000001816 cooling Methods 0.000 description 5
- IZFHEQBZOYJLPK-SSDOTTSWSA-N (R)-dihydrolipoic acid Chemical compound OC(=O)CCCC[C@@H](S)CCS IZFHEQBZOYJLPK-SSDOTTSWSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- WQABCVAJNWAXTE-UHFFFAOYSA-N dimercaprol Chemical compound OCC(S)CS WQABCVAJNWAXTE-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 238000002866 fluorescence resonance energy transfer Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229940035024 thioglycerol Drugs 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000090 biomarker Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
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Abstract
本发明公开了一种硫化铅量子点的制备方法。使用水浴加热法制备出具有良好单分散性，尺寸约为3~5 nm的硫化铅量子点。硫化铅量子点材料可减少透射光及长波长入射光的能量损失，改善太阳电池在整个太阳光谱范围内的利用效率，进一步提高太阳能电池的光电转换效率。此方法简单，易于操作，成本低，可大面积制作生产。
The invention discloses a preparation method of lead sulfide quantum dots. Lead sulfide quantum dots with good monodispersity and a size of about 3-5 nm were prepared by water bath heating method. Lead sulfide quantum dot materials can reduce the energy loss of transmitted light and long-wavelength incident light, improve the utilization efficiency of solar cells in the entire solar spectrum range, and further improve the photoelectric conversion efficiency of solar cells. This method is simple, easy to operate, low in cost, and can be produced in a large area.
Description
技术领域technical field
本发明涉及太阳能电池技术领域，尤其涉及一种硫化铅量子点的制备方法。The invention relates to the technical field of solar cells, in particular to a preparation method of lead sulfide quantum dots.
背景技术Background technique
目前，在化石燃料日趋减少、温室效应不断的加剧的情况下，太阳能已成为人类使用能源的重要组成部分。太阳能由于清洁无污染、储量丰富。太阳能是清洁无污染的可再生能源，而且储量丰富且不受地域限制，被用于替代即将枯竭的化石能源，且能解决中国面临的低碳经济的冲击。在各类新型太阳电池中，量子点与上转换发光材料相结合在太阳能电池领域以低成本、制作工艺简单、相对较高的光电转换效率而成为研究热点。At present, in the case of decreasing fossil fuels and increasing greenhouse effect, solar energy has become an important part of energy used by human beings. Solar energy is clean and pollution-free and has abundant reserves. Solar energy is a clean and non-polluting renewable energy with abundant reserves and no geographical restrictions. It is used to replace the fossil energy that is about to be exhausted, and can solve the impact of China's low-carbon economy. Among all kinds of new solar cells, the combination of quantum dots and up-conversion luminescent materials has become a research hotspot in the field of solar cells due to its low cost, simple manufacturing process, and relatively high photoelectric conversion efficiency.
量子点(QDs)，又可称为纳米晶，一般由II—VI族或IV－VI族元素组成的纳米颗粒，粒径一般介于1~10 nm之间。当量子点的尺寸小于其有效Bohr半径时，量子限制效应(quantum confinement effect)十分明显，表现出独特的随着本身尺寸大小而该改变的物理化学性能、光电性能和磁学性能。量子点材料的主要应用领域为太阳能电池、生物标记和生物传感器等。例如应用多种尺寸量子点材料可提高整个太阳光谱范围内的效率，减少了透过及短波长范围内的能量损失，这意味着太阳能电池的光电转换效率能够得到大幅度的提高。此外，量子点作为荧光共振能量转移(Fluorescence resonant energy transfer,FRET)的供体或给体，与上转换发光材料相结合在生物医学、传感器、太阳能电池等方面有很大的应用潜力。Quantum dots (QDs), also known as nanocrystals, are generally nanoparticles composed of II-VI or IV-VI elements, and the particle size is generally between 1 and 10 nm. When the size of the quantum dot is smaller than its effective Bohr radius, the quantum confinement effect (quantum confinement effect) is very obvious, showing unique physical and chemical properties, photoelectric properties and magnetic properties that change with the size of the quantum dot itself. The main application fields of quantum dot materials are solar cells, biomarkers and biosensors. For example, the application of quantum dot materials of various sizes can improve the efficiency in the entire solar spectrum and reduce the energy loss in the transmission and short wavelength ranges, which means that the photoelectric conversion efficiency of solar cells can be greatly improved. In addition, as the donor or donor of fluorescence resonance energy transfer (FRET), quantum dots have great application potential in biomedicine, sensors, solar cells, etc. in combination with upconversion luminescent materials.
作为IV－VI族半导体中的重要化合物，硫化铅由于较小的能带间隙(0.41 eV，300K)和较大的激子半径(18 nm)，纳米尺度的PbS能带从近红外蓝移到可见光区域，呈现出独特的光学性质和电学性质。传统上采用有机金属路线法合成PbS纳米材料，此方法常使用有毒性原料，并且需要高温和高沸点等反应条件。目前，已有研究者报道采用湿化学方法合成不同形貌的PbS纳米材料，例如纳米棒、纳米片、树状结构等，但采用湿化学方法合成PbS量子点却鲜有报道。Bakueva研究小组首次报道了采用表面活性剂一硫代丙三醇(TGL)和二硫代丙三醇(DTG)的混合物在水溶液中制备出尺寸均匀、直径约为4 nm ± 1 nm的PbS量子点。Deng等采用表面活性剂二氢硫辛酸(DHLA)在室温和水溶液条件下成功合成水溶性的PbS量子点。虽然通过使用表面活性剂一硫代丙三醇(TGL)和二硫代丙三醇或者二氢硫辛酸(DHLA)能在水溶液条件下制备出PbS量子点，但是此类稳定剂价格昂贵，而且有毒性，不适合规模化生产。因此，迫切需要寻找一种价格低廉制备PbS量子点的制备方法。As an important compound in IV-VI semiconductors, due to the small energy band gap (0.41 eV, 300K) and large exciton radius (18 nm), the energy band of PbS at the nanoscale is blue-shifted from near-infrared to In the visible light region, it exhibits unique optical and electrical properties. Traditionally, PbS nanomaterials are synthesized by organometallic routes, which often use toxic raw materials and require reaction conditions such as high temperature and high boiling point. At present, researchers have reported the synthesis of PbS nanomaterials with different morphologies, such as nanorods, nanosheets, tree structures, etc., by wet chemical methods, but there are few reports on the synthesis of PbS quantum dots by wet chemical methods. Bakueva's research group reported for the first time that PbS quantum particles with a uniform size and a diameter of about 4 nm ± 1 nm were prepared in aqueous solution using a mixture of surfactants-thioglycerol (TGL) and dithioglycerol (DTG). point. Deng et al. successfully synthesized water-soluble PbS quantum dots using the surfactant dihydrolipoic acid (DHLA) at room temperature and in aqueous solution. Although PbS quantum dots can be prepared under aqueous conditions by using surfactants-thioglycerol (TGL) and dithioglycerol or dihydrolipoic acid (DHLA), such stabilizers are expensive, and Toxic, not suitable for large-scale production. Therefore, there is an urgent need to find a low-cost preparation method for PbS quantum dots.
发明内容Contents of the invention
本发明的目的在于针对现有技术上的不足，提供一种硫化铅量子点的制备方法。The object of the present invention is to provide a preparation method of lead sulfide quantum dots aiming at the deficiencies in the prior art.
一种硫化铅量子点的制备方法，包括如下步骤：A preparation method of lead sulfide quantum dots, comprising the steps of:
a. 按照物质的量准备助剂：十六烷基三甲基溴化铵 20~ 30份、十二烷基硫酸钠20~30份、柠檬酸钠 40~ 60份；a. Prepare additives according to the amount of substances: 20~30 parts of cetyltrimethylammonium bromide, 20~30 parts of sodium lauryl sulfate, 40~60 parts of sodium citrate;
b. 将上述混合助剂加入水浴温度为50℃~70℃去离子水中，持续高速搅拌3~5 min使之完全溶解，配置成混合溶液；b. Add the above-mentioned mixing aids into deionized water at a water bath temperature of 50°C~70°C, stir continuously at high speed for 3~5 minutes to completely dissolve, and prepare a mixed solution;
c. 加数滴稀硝酸溶液于上述混合溶液中，将pH值调节到3~5，然后向该溶液中加入柠檬酸钠，柠檬酸钠物质的量为乙酸铅的2~4倍，溶液持续高速搅拌1~2 min，直至变为浅黄色溶液；c. Add a few drops of dilute nitric acid solution to the above mixed solution, adjust the pH value to 3~5, then add sodium citrate to the solution, the amount of sodium citrate is 2~4 times that of lead acetate, the solution lasts Stir at high speed for 1-2 min until it turns into a light yellow solution;
d. 继续缓慢加入柠檬酸钠，柠檬酸钠物质的量为硫脲的2~4倍，溶液持续高速搅拌3~5min，溶液颜色由橙黄色慢慢变为棕褐色；d. Continue to slowly add sodium citrate, the amount of sodium citrate is 2 to 4 times that of thiourea, the solution continues to stir at high speed for 3 to 5 minutes, and the color of the solution changes from orange yellow to brown;
e. 将上述所得混合溶液，室温冷却后，经过离心处理，依次用去离子水、无水乙醇各清洗三次，将得到的硫化铅保存于无水乙醇。e. After cooling the mixed solution obtained above at room temperature, after centrifugation, wash with deionized water and absolute ethanol three times respectively, and store the obtained lead sulfide in absolute ethanol.
所述的柠檬酸钠的物质的量为十六烷基三甲基溴化铵、十二烷基硫酸钠二者物质的量之和。The amount of the sodium citrate is the sum of the amounts of cetyltrimethylammonium bromide and sodium lauryl sulfate.
所述的乙酸铅溶液和硫脲溶液所含物质的量相等。The amounts of substances contained in the lead acetate solution and the thiourea solution are equal.
所述的制备出的硫化铅量子点的直径尺寸为3~5 nm。The diameter of the prepared lead sulfide quantum dots is 3-5 nm.
所述的助剂以物质的量计：十六烷基三甲基溴化铵25份、十二烷基硫酸钠25份、柠檬酸钠50份；The auxiliary agent is based on the amount of substance: 25 parts of cetyltrimethylammonium bromide, 25 parts of sodium lauryl sulfate, and 50 parts of sodium citrate;
所述的乙酸铅溶液和硫脲溶液所含物质的量都为柠檬酸钠物质的量2.5倍。The amount of substances contained in the lead acetate solution and the thiourea solution is 2.5 times that of sodium citrate.
所述的制备步骤从硫脲溶液加入那一刻时间算起，反应物加入完之后时间控制在3~5分钟。反应时间要严格控制，时间过长，则制备不出量子点。The preparation steps are calculated from the moment when the thiourea solution is added, and the time after the addition of the reactants is controlled within 3 to 5 minutes. The reaction time should be strictly controlled, if the time is too long, quantum dots cannot be prepared.
所述步骤b中将上述混合助剂加入水浴温度为60℃去离子水中。In the step b, the above-mentioned mixing aid is added into deionized water with a water bath temperature of 60°C.
本发明的有益效果：Beneficial effects of the present invention:
反应温度较低，反应条件温和；无需使用高沸点溶剂；制备方法安全无毒，实验重复性好；所得硫化铅量子点具有良好单分散性。The reaction temperature is low and the reaction conditions are mild; no high-boiling solvent is needed; the preparation method is safe and non-toxic, and the experiment repeatability is good; the obtained lead sulfide quantum dots have good monodispersity.
附图说明Description of drawings
下面将结合附图及实施例对本发明作进一步说明，附图中：The present invention will be further described below in conjunction with accompanying drawing and embodiment, in the accompanying drawing:
图1是所制备的PbS量子点透射电镜图；Fig. 1 is prepared PbS quantum dot transmission electron microscope picture;
图2是所制备的PbS量子XRD图谱。Fig. 2 is the quantum XRD spectrum of the prepared PbS.
具体实施方式detailed description
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合附图及实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅用以解释本发明，并不用于限定本发明。In order to make the object, technical solution and advantages of the present invention clearer, the present invention will be further described in detail below in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described here are only used to explain the present invention, not to limit the present invention.
一种硫化铅量子点的制备方法，包括如下步骤：A preparation method of lead sulfide quantum dots, comprising the steps of:
a. 按照物质的量准备助剂：十六烷基三甲基溴化铵 20~30份、十二烷基硫酸钠20~30份、柠檬酸钠 40~60份；a. Prepare additives according to the amount of substances: 20-30 parts of cetyltrimethylammonium bromide, 20-30 parts of sodium lauryl sulfate, 40-60 parts of sodium citrate;
b. 将上述混合助剂加入温度为50℃~70℃水，持续高速搅拌3~5 min使之完全溶解,配置成混合溶液；b. Add the above-mentioned mixing aids into water at a temperature of 50°C~70°C, and continue to stir at high speed for 3~5 minutes to completely dissolve it, and prepare a mixed solution;
c. 加数滴稀硝酸溶液于上述混合溶液中，将pH值调节到3~5，然后向该溶液中加入柠檬酸钠，柠檬酸钠物质的量为乙酸铅的2~4倍，溶液持续高速搅拌1~2 min，直至变为浅黄色溶液；c. Add a few drops of dilute nitric acid solution to the above mixed solution, adjust the pH value to 3~5, then add sodium citrate to the solution, the amount of sodium citrate is 2~4 times that of lead acetate, the solution lasts Stir at high speed for 1-2 min until it turns into a light yellow solution;
d. 继续缓慢加入柠檬酸钠，柠檬酸钠物质的量为硫脲的2~4倍，溶液持续高速搅拌3~5min，溶液颜色由橙黄色慢慢变为棕褐色；d. Continue to slowly add sodium citrate, the amount of sodium citrate is 2 to 4 times that of thiourea, the solution continues to stir at high speed for 3 to 5 minutes, and the color of the solution changes from orange yellow to brown;
e. 将上述所得混合溶液，室温冷却后，经过离心处理，依次用去离子水、无水乙醇各清洗三次，将得到的硫化铅保存于无水乙醇。e. After cooling the mixed solution obtained above at room temperature, after centrifugation, wash with deionized water and absolute ethanol three times respectively, and store the obtained lead sulfide in absolute ethanol.
所述的柠檬酸钠的物质的量为十六烷基三甲基溴化铵、十二烷基硫酸钠二者物质的量之和。The amount of the sodium citrate is the sum of the amounts of cetyltrimethylammonium bromide and sodium lauryl sulfate.
所述乙酸铅溶液和硫脲溶液所含物质的量相等。The amounts of substances contained in the lead acetate solution and the thiourea solution are equal.
制备出的硫化铅量子点的直径尺寸为3~5 nm。The diameter of the prepared lead sulfide quantum dots is 3-5 nm.
所述助剂以物质的量计：十六烷基三甲基溴化铵25份、十二烷基硫酸钠25份、柠檬酸钠50份；The auxiliary agent is calculated by the amount of substance: 25 parts of cetyltrimethylammonium bromide, 25 parts of sodium lauryl sulfate, and 50 parts of sodium citrate;
所述乙酸铅溶液和硫脲溶液所含物质的量都为柠檬酸钠物质的量2.5倍。The amount of substances contained in the lead acetate solution and the thiourea solution is 2.5 times that of sodium citrate.
所述的制备步骤从硫脲溶液加入那一刻时间算起，反应物加入完之后时间控制在3~5分钟。反应时间要严格控制，时间过长，则制备不出量子点。The preparation steps are calculated from the moment when the thiourea solution is added, and the time after the addition of the reactants is controlled within 3 to 5 minutes. The reaction time should be strictly controlled, if the time is too long, quantum dots cannot be prepared.
所述步骤b中将上述混合助剂加入水浴温度为60℃去离子水中。In the step b, the above-mentioned mixing aid is added into deionized water with a water bath temperature of 60°C.
实施例1Example 1
1）分别称量十六烷基三甲基溴化铵18.2 mg (0.05 mmol)、十二烷基硫酸钠14.4 mg(0.05 mmol)、柠檬酸钠 29.4 mg (0.1 mmol)，加入到50 mL水温为60℃的烧杯中，持续高速搅拌3~5 min使之完全溶解；1) Weigh 18.2 mg (0.05 mmol) of cetyltrimethylammonium bromide, 14.4 mg (0.05 mmol) of sodium lauryl sulfate and 29.4 mg (0.1 mmol) of sodium citrate respectively, and add them to 50 mL of water In a beaker at 60°C, stir continuously at high speed for 3-5 minutes to dissolve completely;
2）加数滴稀硝酸溶液于上述混合溶液中，并用pH计调节pH值到4，然后加入5 mL 0.05mol/L乙酸铅溶液并持续高速搅拌2min，此时溶液变为浅黄色；2) Add a few drops of dilute nitric acid solution to the above mixed solution, and adjust the pH value to 4 with a pH meter, then add 5 mL of 0.05mol/L lead acetate solution and continue stirring at high speed for 2 minutes, at this time the solution turns light yellow;
3）缓慢加入10 mL 浓度为0.025 mol/L的硫脲溶液并持续高速搅拌4 min，溶液颜色由橙黄色慢慢变为棕褐色。3) Slowly add 10 mL of thiourea solution with a concentration of 0.025 mol/L and continue to stir at high speed for 4 min, the color of the solution gradually changes from orange to brown.
4）将上述所得混合溶液，室温冷却后，经过离心处理，依次用去离子水、无水乙醇各清洗三次，将得到的硫化铅保存于无水乙醇。4) After cooling the mixed solution obtained above at room temperature, centrifuge, wash with deionized water and absolute ethanol three times respectively, and store the obtained lead sulfide in absolute ethanol.
实施例2Example 2
1） 分别称量十六烷基三甲基溴化铵36.4mg (0.1 mmol)、十二烷基硫酸钠28.8mg(0.1 mmol)、柠檬酸钠58.8 mg (0.2 mmol)，加入到100 mL水温为70℃的烧杯中，持续高速搅拌3~5 min使之完全溶解；1) Weigh 36.4 mg (0.1 mmol) of cetyltrimethylammonium bromide, 28.8 mg (0.1 mmol) of sodium lauryl sulfate, and 58.8 mg (0.2 mmol) of sodium citrate, respectively, and add them to 100 mL of water In a beaker at 70°C, stir continuously at high speed for 3-5 minutes to dissolve completely;
2）加数滴稀硝酸溶液于上述混合溶液中，并用pH计调节pH值到5，然后加入40ml 0.05mol/L硫脲溶液并持续高速搅拌2 min；2) Add a few drops of dilute nitric acid solution to the above mixed solution, and adjust the pH value to 5 with a pH meter, then add 40ml of 0.05mol/L thiourea solution and continue stirring at high speed for 2 minutes;
3）缓慢加入80 mL 浓度为0.025 mol/L的乙酸铅溶液并持续高速搅拌3min，溶液颜色由浅黄色、橙黄色慢慢变为棕褐色，这意味着PbS量子点的生成；3) Slowly add 80 mL of lead acetate solution with a concentration of 0.025 mol/L and continue to stir at high speed for 3 minutes, the color of the solution gradually changes from light yellow or orange to brown, which means the formation of PbS quantum dots;
4）将上述所得混合溶液，室温冷却后，经过离心处理，依次用去离子水、无水乙醇各清洗三次，将得到的硫化铅保存于无水乙醇。4) After cooling the mixed solution obtained above at room temperature, centrifuge, wash with deionized water and absolute ethanol three times respectively, and store the obtained lead sulfide in absolute ethanol.
实施例3Example 3
1） 分别称量十六烷基三甲基溴化铵29.12 mg (0.08 mmol)、十二烷基硫酸钠34.56mg (0.12 mmol)、柠檬酸钠 58.8 mg (0.2 mmol)，加入到300mL水温为70℃的烧杯中，持续高速搅拌3~5 min使之完全溶解；1) Weigh 29.12 mg (0.08 mmol) of cetyltrimethylammonium bromide, 34.56 mg (0.12 mmol) of sodium lauryl sulfate, and 58.8 mg (0.2 mmol) of sodium citrate respectively, and add them to 300 mL of water at a temperature of In a beaker at 70°C, stir continuously at high speed for 3-5 minutes to dissolve completely;
2）加数滴稀硝酸溶液于上述混合溶液中，并用pH计调节pH值到5，然后加入80 ml 0.05mol/L硫脲溶液并持续高速搅拌2 min；2) Add a few drops of dilute nitric acid solution to the above mixed solution, and adjust the pH value to 5 with a pH meter, then add 80 ml of 0.05mol/L thiourea solution and continue stirring at high speed for 2 min;
3）缓慢加入160 mL 浓度为0.025 mol/L的乙酸铅溶液并持续高速搅拌3min，溶液颜色由浅黄色、橙黄色慢慢变为棕褐色，这意味着PbS量子点的生成；3) Slowly add 160 mL of lead acetate solution with a concentration of 0.025 mol/L and continue to stir at high speed for 3 minutes, the color of the solution gradually changes from light yellow or orange to brown, which means the formation of PbS quantum dots;
4）将上述所得混合溶液，室温冷却后，经过离心处理，依次用去离子水、无水乙醇各清洗三次，将得到的硫化铅保存于无水乙醇。4) After cooling the mixed solution obtained above at room temperature, centrifuge, wash with deionized water and absolute ethanol three times respectively, and store the obtained lead sulfide in absolute ethanol.
应当理解的是，对本领域普通技术人员来说，可以根据上述说明加以改进或变换，而所有这些改进和变换都应属于本发明所附权利要求的保护范围。It should be understood that those skilled in the art can make improvements or changes based on the above description, and all these improvements and changes should fall within the protection scope of the appended claims of the present invention.
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| CN101117237A (en) * | 2007-07-17 | 2008-02-06 | 浙江大学 | A method for preparing hexagonal star-shaped lead sulfide nanocrystals |
| CN104297306A (en) * | 2014-09-30 | 2015-01-21 | 江南大学 | Multifunctional photoelectrochemical sensor based on G-tetrahedron/hemin |
| CN105304338A (en) * | 2015-09-21 | 2016-02-03 | 河南师范大学 | Counter electrode for quantum-dot sensitized solar cell and manufacturing method thereof |
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| CN101117237A (en) * | 2007-07-17 | 2008-02-06 | 浙江大学 | A method for preparing hexagonal star-shaped lead sulfide nanocrystals |
| CN104297306A (en) * | 2014-09-30 | 2015-01-21 | 江南大学 | Multifunctional photoelectrochemical sensor based on G-tetrahedron/hemin |
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