CN107425130A - Preparation method of inorganic quantum dot light-emitting diode device - Google Patents
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- 239000002096 quantum dot Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000243 solution Substances 0.000 claims abstract description 27
- 239000000758 substrate Substances 0.000 claims abstract description 27
- 239000011521 glass Substances 0.000 claims abstract description 20
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000011259 mixed solution Substances 0.000 claims abstract description 5
- 238000004140 cleaning Methods 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000001704 evaporation Methods 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- 230000008020 evaporation Effects 0.000 claims description 16
- 239000002105 nanoparticle Substances 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 8
- 230000004048 modification Effects 0.000 claims description 5
- 238000012986 modification Methods 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000007740 vapor deposition Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 12
- 238000002347 injection Methods 0.000 abstract description 8
- 239000007924 injection Substances 0.000 abstract description 8
- 238000005036 potential barrier Methods 0.000 abstract 1
- 239000010409 thin film Substances 0.000 abstract 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 48
- 239000011787 zinc oxide Substances 0.000 description 24
- 230000000052 comparative effect Effects 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 3
- 230000004888 barrier function Effects 0.000 description 3
- 238000006862 quantum yield reaction Methods 0.000 description 3
- NZJMPGDMLIPDBR-UHFFFAOYSA-M tetramethylazanium;hydroxide;hydrate Chemical compound O.[OH-].C[N+](C)(C)C NZJMPGDMLIPDBR-UHFFFAOYSA-M 0.000 description 3
- 239000004246 zinc acetate Substances 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- MYXKPFMQWULLOH-UHFFFAOYSA-M tetramethylazanium;hydroxide;pentahydrate Chemical compound O.O.O.O.O.[OH-].C[N+](C)(C)C MYXKPFMQWULLOH-UHFFFAOYSA-M 0.000 description 2
- YZYKBQUWMPUVEN-UHFFFAOYSA-N zafuleptine Chemical compound OC(=O)CCCCCC(C(C)C)NCC1=CC=C(F)C=C1 YZYKBQUWMPUVEN-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000005525 hole transport Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000002186 photoelectron spectrum Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
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- 238000005215 recombination Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- -1 tetramethylammonium hydroxide pentahydrate ethanol Chemical compound 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
本发明提供一种高效无机量子点发光二极管器件的制备方法，制备步骤如下：将ITO透明导电玻璃基片清洗后烘干；将PEIE用乙醇稀释到浓度为0.05‑0.1wt%，然后将PEIE溶液涂在基片上形成10 nm左右的薄膜；接着将PEIE掺入ZnO 溶液中，掺杂浓度为0.05‑0.1 wt%，然后将ZnO:PEIE的混合溶液涂在基片上；随后涂上溶解在甲苯中的无机量子点；最后将基片置于真空腔内，依次蒸镀CBP,CBP:MoO3,MoO3,Al，即得量子点发光二极管器件。本发明采用PEIE/ZnO:PEIE作为电子注入层，降低了电子的注入势垒，提高了电子的注入效率，从而大大提高了器件的整体效率。
The invention provides a method for preparing a high-efficiency inorganic quantum dot light-emitting diode device. The preparation steps are as follows: cleaning and drying the ITO transparent conductive glass substrate; Coated on the substrate to form a thin film of about 10 nm; then PEIE was mixed into the ZnO solution at a doping concentration of 0.05‑0.1 wt%, and then the mixed solution of ZnO:PEIE was coated on the substrate; then coated with a solution dissolved in toluene Inorganic quantum dots; finally, place the substrate in a vacuum chamber and vapor-deposit CBP, CBP:MoO 3 , MoO 3 , Al in sequence to obtain a quantum dot light-emitting diode device. The invention adopts PEIE/ZnO:PEIE as the electron injection layer, which reduces the electron injection potential barrier, improves the electron injection efficiency, and thus greatly improves the overall efficiency of the device.
Description
技术领域technical field
本发明涉及半导体器件领域，具体涉及一种无机量子点发光二极管器件的制备方法。The invention relates to the field of semiconductor devices, in particular to a method for preparing an inorganic quantum dot light-emitting diode device.
背景技术Background technique
在平面型发光半导体器件中，各层之间的能极差很大，特别是电极和有机、无机界面之间的能极差， 这导致电子和空穴很难注入到发光层，激子复合效率较低。由于器件的界面势垒较大，电子从氧化铟锡（ITO）注入到电子传输层、从电子传输层注入到发光层更困难，这使得器件的工作电压很大，效率很低。因此，在器件的制备过程中常常需要通过在电子传输层和电极之间使用界面修饰层降低电子注入势垒，平衡电子和空穴，从而实现低电压、高效率、长寿命器件的制作。In planar light-emitting semiconductor devices, the energy gap between layers is very large, especially between the electrodes and the organic and inorganic interfaces, which makes it difficult for electrons and holes to inject into the light-emitting layer, and excitons recombine less efficient. Due to the large interface barrier of the device, it is more difficult for electrons to be injected from indium tin oxide (ITO) to the electron transport layer, and from the electron transport layer to the light-emitting layer, which makes the operating voltage of the device very high and the efficiency is very low. Therefore, in the process of device preparation, it is often necessary to use an interface modification layer between the electron transport layer and the electrode to reduce the electron injection barrier and balance electrons and holes, so as to achieve low voltage, high efficiency, and long-life devices.
发明内容Contents of the invention
要解决的技术问题：针对现有技术的不足，本发明的目的是提供一种无机量子点发光二极管器件的制备方法，该制备方法工艺方便易行，使得发光器件的电子注入效率提高，从而使得器件效率提高。Technical problem to be solved: In view of the deficiencies in the prior art, the purpose of the present invention is to provide a method for preparing an inorganic quantum dot light-emitting diode device. Device efficiency is improved.
技术方案：一种无机量子点发光二极管器件的制备方法，包括以下步骤：Technical solution: a method for preparing an inorganic quantum dot light-emitting diode device, comprising the following steps:
第一步：将ITO透明导电玻璃基片进行标准化清洗后烘干；Step 1: Standardize cleaning and drying of the ITO transparent conductive glass substrate;
第二步：以乙醇为溶剂，配置PEIE溶液，然后将ITO透明导电玻璃基片上涂PEIE溶液，形成PEIE界面修饰层；The second step: using ethanol as a solvent, configure PEIE solution, and then coat the PEIE solution on the ITO transparent conductive glass substrate to form a PEIE interface modification layer;
第三步：将PEIE掺入ZnO纳米粒子溶液中，然后将ZnO：PEIE的混合溶液涂在经过第二步处理的ITO透明导电玻璃基片上，形成ZnO：PEIE电子传输层；The third step: mixing PEIE into the ZnO nanoparticle solution, and then coating the mixed solution of ZnO:PEIE on the ITO transparent conductive glass substrate treated in the second step to form a ZnO:PEIE electron transport layer;
第四步：将经过第三步处理的ITO透明导电玻璃基片上，涂抹溶解了无机量子点甲苯溶液，形成无机量子点发光层；The fourth step: apply the dissolved inorganic quantum dot toluene solution on the ITO transparent conductive glass substrate treated in the third step to form an inorganic quantum dot light-emitting layer;
第五步：在第四步处理的ITO透明导电玻璃基片置于真空腔内，依次蒸镀CBP，CBP:MoO3，MoO3和Al，其中CBP: MoO3采用双源蒸镀的方法，即得无机量子点发光二极管。The fifth step: the ITO transparent conductive glass substrate processed in the fourth step is placed in a vacuum chamber, and CBP, CBP:MoO 3 , MoO 3 and Al are sequentially evaporated, wherein CBP: MoO 3 adopts a dual-source evaporation method, That is, the inorganic quantum dot light-emitting diode is obtained.
进一步的，所述的一种无机量子点发光二极管器件的制备方法，所述第二步中PEIE乙醇溶液的浓度为0.1wt% 左右，PEIE界面修饰层的厚度为10 nm左右。Further, in the preparation method of an inorganic quantum dot light-emitting diode device, the concentration of the PEIE ethanol solution in the second step is about 0.1 wt%, and the thickness of the PEIE interface modification layer is about 10 nm.
进一步的，所述的一种无机量子点发光二极管器件的制备方法，所述第三步中将PEIE掺入ZnO纳米粒子溶液中，其中ZnO纳米粒子的直径为8-15nm，其掺杂浓度为0.05-0.1wt%，形成ZnO：PEIE电子传输层的厚度为60 nm左右。Further, in the preparation method of an inorganic quantum dot light-emitting diode device, in the third step, PEIE is mixed into the ZnO nanoparticle solution, wherein the diameter of the ZnO nanoparticle is 8-15nm, and its doping concentration is 0.05-0.1wt%, the thickness of ZnO: PEIE electron transport layer is about 60 nm.
进一步的，所述的一种无机量子点发光二极管器件的制备方法，所述第四步中无机量子点为CdSeZnS, CdSeCdS/ZnS, ZnCdS/ZnS，无机量子点薄膜层的厚度为25 nm左右。Further, in the preparation method of an inorganic quantum dot light-emitting diode device, in the fourth step, the inorganic quantum dots are CdSeZnS, CdSeCdS/ZnS, ZnCdS/ZnS, and the thickness of the inorganic quantum dot film layer is about 25 nm.
进一步的，所述的一种无机量子点发光二极管器件的制备方法，所述第五步中CBP: MoO3，以CBP为主体材料，MoO3为客体材料，MoO3的掺杂浓度为10 wt%。Further, in the preparation method of an inorganic quantum dot light-emitting diode device, in the fifth step, CBP: MoO 3 , with CBP as the host material, MoO 3 as the guest material, and the doping concentration of MoO 3 is 10 wt %.
进一步的，所述的一种无机量子点发光二极管器件的制备方法，所述第五步中蒸镀CBP，CBP: MoO3，MoO3和Al形成薄膜层的厚度分别为15nm，30nm，8nm和100nm，CBP蒸镀速率为4Å/s，CBP: MoO3 蒸镀速率为2Å/s，MoO3的蒸镀速率为0.5 Å/s，Al蒸镀速率为6 Å/s。Further, the preparation method of described a kind of inorganic quantum dot light-emitting diode device, vapor deposition CBP in the described 5th step, CBP: MoO 3 , the thickness of MoO 3 and Al formation film layer is respectively 15nm, 30nm, 8nm and 100nm, the evaporation rate of CBP is 4 Å/s, the evaporation rate of CBP: MoO 3 is 2 Å/s, the evaporation rate of MoO 3 is 0.5 Å/s, and the evaporation rate of Al is 6 Å/s.
有益效果：本发明的本发明提供的一种无机量子点发光二极管器件的制备方法，该制备方法具有以下优点：Beneficial effects: The present invention provides a method for preparing an inorganic quantum dot light-emitting diode device, which has the following advantages:
1. 本发明制作工艺简单便捷，制备难度低，本发明采用PEIE/ZnO:PEIE作为电子注入层，降低了电子的注入势垒；1. The manufacturing process of the present invention is simple and convenient, and the preparation difficulty is low. The present invention uses PEIE/ZnO:PEIE as the electron injection layer, which reduces the electron injection barrier;
2. 本发明采用PEIE/ZnO:PEIE电子传输层，CBP: MoO3空穴传输层，两者的结合，有效的控制了载流子的传输和复合速率，使得器件的性能大大的提高；2. The present invention adopts PEIE/ZnO: PEIE electron transport layer, CBP: MoO 3 hole transport layer, the combination of the two effectively controls the transmission and recombination rate of carriers, so that the performance of the device is greatly improved;
3. 本发明采用PEIE/ZnO:PEIE制备的传输层具有良好的电荷注入和传输能力，使得器件外量子产率高，器件性能更加稳定。3. The transport layer prepared by PEIE/ZnO:PEIE in the present invention has good charge injection and transport capabilities, so that the external quantum yield of the device is high and the device performance is more stable.
附图说明Description of drawings
图1 为ZnO纳米粒子合成方法制备的ZnO纳米粒子的TEM图；Fig. 1 is the TEM picture of the ZnO nanoparticle prepared by ZnO nanoparticle synthesis method;
图2 为PEIE的化学结构式；Fig. 2 is the chemical structural formula of PEIE;
图3为将实施例1中第三步处理后的导电玻璃基片和对比例1中第二步处理后的导电玻璃基片于光电子能谱仪（XPS）真空腔内，抽真空至2.0×10-8Pa，用HeI作紫外光源（21.2 eV）测得的紫外光电子能谱图。从图中可以看出，对比例1中ZnO功函数为4.1 eV，实施例1中ZnO:PEIE的功函数为3.7 eV，功函数的提高有利于电子从ITO透明导电玻璃基片注入到电子传输层；Figure 3 shows that the conductive glass substrate processed in the third step in Example 1 and the conductive glass substrate processed in the second step in Comparative Example 1 were placed in the vacuum chamber of a photoelectron spectrometer (XPS) and vacuumed to 2.0× 10 -8 Pa, UV photoelectron spectrum measured with HeI as UV light source (21.2 eV). As can be seen from the figure, the work function of ZnO in Comparative Example 1 is 4.1 eV, and the work function of ZnO:PEIE in Example 1 is 3.7 eV, and the improvement of work function is conducive to the injection of electrons from the ITO transparent conductive glass substrate to the electron transport. Floor;
图4为将实施例1中第三步处理后的导电玻璃基片和对比例1中第二步处理后的导电玻璃基片置于原子力显微镜（AFM）下。从图中可以看出，在相同测试范围下，实施例1制成的薄膜比仅使用对比例1制成的薄膜粗糙度（RMS）小；FIG. 4 shows that the conductive glass substrate treated in the third step in Example 1 and the conductive glass substrate treated in the second step in Comparative Example 1 were placed under an atomic force microscope (AFM). It can be seen from the figure that under the same test range, the roughness (RMS) of the film made in Example 1 is smaller than that of the film made only in Comparative Example 1;
图5 为实施例1制备得到的无机量子点发光二极管器件与对比例1制备得到的发光二极管器件的亮度与电压关系图。从图中可以看出，在相同电压条件下实施例1制成的发光二极管器件比仅使用对比例1制成的发光二极管器件亮度高；5 is a graph showing the relationship between brightness and voltage of the inorganic quantum dot light-emitting diode device prepared in Example 1 and the light-emitting diode device prepared in Comparative Example 1. It can be seen from the figure that under the same voltage conditions, the light-emitting diode device made in Example 1 has higher brightness than the light-emitting diode device made only in Comparative Example 1;
图6 为实施例1制备得到的无机量子点发光二极管器件与对比例1制备得到的发光二极管器件的电流密度与电压关系图。从图中可以看出，在相同电压条件下实施例1制成的无机量子点发光二极管器件比仅使用对比例1制成的发光二极管器件的电流密度高；6 is a graph showing the relationship between current density and voltage of the inorganic quantum dot light-emitting diode device prepared in Example 1 and the light-emitting diode device prepared in Comparative Example 1. As can be seen from the figure, under the same voltage conditions, the inorganic quantum dot light-emitting diode device made in Example 1 has a higher current density than the light-emitting diode device made only in Comparative Example 1;
图7为实施例1制备得到的无机量子点发光二极管器件与对比例1制备得到的发光二极管器件的电流效率与外量子产率关系图。从图中可以看出，在相同电流密度条件下实施例1制成的无机量子点发光二极管器件比仅使用对比例1制成的发光二极管器件外量子产率高。7 is a graph showing the relationship between the current efficiency and the external quantum yield of the inorganic quantum dot light-emitting diode device prepared in Example 1 and the light-emitting diode device prepared in Comparative Example 1. It can be seen from the figure that the external quantum yield of the inorganic quantum dot light-emitting diode device made in Example 1 is higher than that of the light-emitting diode device made only in Comparative Example 1 under the same current density condition.
具体实施方式detailed description
以下实施例中使用的ITO透明导电玻璃基片购自Lumitec公司，PEIE，醋酸锌，四甲基氢氧化铵水合物购自Sigma Aldrich公司，CBP、MoO3和Al 均购自Lumitec公司，无机量子点ZnCdS/ZnS在北京聚邦公司购买。The ITO transparent conductive glass substrate used in the following examples was purchased from Lumitec Company, PEIE, zinc acetate, tetramethylammonium hydroxide hydrate were purchased from Sigma Aldrich Company, CBP, MoO 3 and Al were purchased from Lumitec Company, inorganic quantum Point ZnCdS/ZnS can be purchased from Beijing Jubang Company.
实施例1Example 1
一种无机量子点发光二极管器件的制备，该方法的制备步骤如下：A preparation of an inorganic quantum dot light-emitting diode device, the preparation steps of the method are as follows:
第一步：将ITO透明导电玻璃基片先在去离子水中冲洗，接着用去离子水、丙酮、乙醇反复清洗三次，在洁净的环境下烘烤至完全去除水分；Step 1: Rinse the ITO transparent conductive glass substrate in deionized water first, then wash it repeatedly with deionized water, acetone, and ethanol three times, and bake it in a clean environment until the water is completely removed;
第二步：PEIE用乙醇稀释到浓度为0.1 wt%，然后在ITO透明导电玻璃基片上涂PEIE溶液，形成10 nm左右的PEIE薄膜层；The second step: PEIE is diluted with ethanol to a concentration of 0.1 wt%, and then coated with PEIE solution on the ITO transparent conductive glass substrate to form a PEIE film layer of about 10 nm;
第三步：将PEIE掺入ZnO 纳米粒子溶液中，掺杂浓度为0.1 wt%，然后将ZnO:PEIE的混合溶液涂在基片上，形成ZnO：PEIE薄膜层的厚度在60 nm，其中，ZnO 纳米粒子溶液制备采用常见的工艺，由醋酸锌和四甲基氢氧化铵水合物混合反应制得，ZnO 纳米粒子大小在8-15 nm；The third step: PEIE was mixed into the ZnO nanoparticle solution with a doping concentration of 0.1 wt%, and then the mixed solution of ZnO:PEIE was coated on the substrate to form a ZnO:PEIE film layer with a thickness of 60 nm, wherein ZnO The nanoparticle solution is prepared by a common process, which is prepared by the mixed reaction of zinc acetate and tetramethylammonium hydroxide hydrate, and the size of ZnO nanoparticles is 8-15 nm;
第四步：随后涂上溶解在甲苯中的无机量子点ZnCdS/ZnS，无机量子点薄膜层厚度在25nm左右；Step 4: Then apply inorganic quantum dots ZnCdS/ZnS dissolved in toluene, and the thickness of the inorganic quantum dot film layer is about 25nm;
第五步：将基片置于真空腔内5 ×10-4 Pa，依次蒸镀CBP (15 nm)，CBP：MoO3 (30 nm)，MoO3 (8 nm)，Al (100 nm)，其中CBP：MoO3采用双源蒸镀的方法，以CBP为主体材料，MoO3为客体材料，MoO3的掺杂浓度为10 wt%，CBP蒸镀速率为4Å/s，CBP: MoO3 蒸镀速率为2Å/s，MoO3的蒸镀速率为0.5 Å/s，Al蒸镀速率为6 Å/s。Step 5: Place the substrate in a vacuum chamber at 5 × 10 -4 Pa, and sequentially evaporate CBP (15 nm), CBP: MoO 3 (30 nm), MoO 3 (8 nm), Al (100 nm), Among them, CBP: MoO 3 adopts a dual-source evaporation method, with CBP as the host material and MoO 3 as the guest material, the doping concentration of MoO 3 is 10 wt%, the CBP evaporation rate is 4 Å/s, and the CBP: MoO 3 evaporation The plating rate is 2 Å/s, the evaporation rate of MoO 3 is 0.5 Å/s, and the evaporation rate of Al is 6 Å/s.
实施例2Example 2
实施例2与实施例1的区别为第二步中乙醇溶液的浓度为0.05 wt%，形成5 nm左右的PEIE薄膜层。The difference between Example 2 and Example 1 is that the concentration of the ethanol solution in the second step is 0.05 wt%, and a PEIE film layer of about 5 nm is formed.
实施例3Example 3
实施例3与实施例1的区别为第三步中ZnO:PEIE的混合溶液的浓度为0.05 wt%，薄膜层厚度为50 nm。The difference between Example 3 and Example 1 is that the concentration of the mixed solution of ZnO:PEIE in the third step is 0.05 wt%, and the thickness of the film layer is 50 nm.
实施例4 ZnO 纳米粒子溶液合成过程Embodiment 4 ZnO nanoparticle solution synthesis process
（1）称量：首先称量3 mmol（0.658g）二水合醋酸锌溶解在30 ml二甲亚砜中，三颈烧瓶中磁子搅拌至完全溶解。称量3 mmol（0.55g）五水合四甲基氢氧化铵溶解在6ml无水乙醇中，待五水合四甲基氢氧化铵完全溶解；(1) Weighing: First weigh 3 mmol (0.658 g) of zinc acetate dihydrate and dissolve it in 30 ml of dimethyl sulfoxide, and stir with a magnet in a three-necked flask until it is completely dissolved. Weigh 3 mmol (0.55g) of tetramethylammonium hydroxide pentahydrate and dissolve it in 6ml of absolute ethanol until the tetramethylammonium hydroxide pentahydrate is completely dissolved;
（2）水浴反应：然后将五水合四甲基氢氧化铵乙醇溶液滴加到二水合醋酸锌的二甲亚砜溶液中。30℃水浴加热，反应2小时；(2) Water bath reaction: Then add tetramethylammonium hydroxide pentahydrate ethanol solution dropwise to the dimethyl sulfoxide solution of zinc acetate dihydrate. Heating in a water bath at 30°C, reacting for 2 hours;
（3）离心提纯：待反应结束，向反应液中加入乙酸乙酯沉淀至澄清的反应液变浑浊，用离心机3000rpm离心3分钟，去除上清液；(3) Centrifugal purification: After the reaction is completed, add ethyl acetate to the reaction solution to precipitate until the clear reaction solution becomes turbid, centrifuge at 3000rpm for 3 minutes, and remove the supernatant;
（4）第二次提纯：将上述所得沉淀溶解在甲醇中，静置，待浑浊后，同样3000 rpm离心3分钟，去掉上清液，向沉淀中加入1 ml正丁醇溶剂，使氧化锌纳米粒子自行溶解，得到澄清透明的氧化锌纳米粒子溶液。(4) The second purification: Dissolve the precipitate obtained above in methanol, let it stand, and after it becomes turbid, centrifuge at 3000 rpm for 3 minutes, remove the supernatant, and add 1 ml of n-butanol solvent to the precipitate to make zinc oxide The nanoparticles dissolve by themselves, and a clear and transparent zinc oxide nanoparticle solution is obtained.
对比例1Comparative example 1
一种无机量子点发光二极管器件的制备，该方法的制备步骤如下：A preparation of an inorganic quantum dot light-emitting diode device, the preparation steps of the method are as follows:
第一步：将ITO透明导电玻璃基片先在去离子水中冲洗，接着用去离子水、丙酮、乙醇反复清洗三次，在洁净的环境下烘烤至完全去除水分；Step 1: Rinse the ITO transparent conductive glass substrate in deionized water first, then wash it repeatedly with deionized water, acetone, and ethanol three times, and bake it in a clean environment until the water is completely removed;
第二步：将ZnO纳米粒子溶液涂在基片上，厚度为60 nm，其中，ZnO纳米粒子溶液制备采用常见的工艺，由醋酸锌和四甲基氢氧化铵水合物混合反应制得，粒子大小在8-15 nm；Step 2: Coat the ZnO nanoparticle solution on the substrate with a thickness of 60 nm. Among them, the ZnO nanoparticle solution is prepared by a common process, which is prepared by the mixed reaction of zinc acetate and tetramethylammonium hydroxide hydrate. The particle size is at 8-15 nm;
第四步：随后涂上溶解在甲苯中的无机量子点ZnCdS/ZnS，无机量子点薄膜层厚度在25nm 左右；Step 4: Then apply inorganic quantum dots ZnCdS/ZnS dissolved in toluene, and the thickness of the inorganic quantum dot film layer is about 25nm;
第五步：将基片置于真空腔内5 x 10-4 Pa，依次蒸镀CBP (15 nm)，CBP: MoO3 (30nm)，MoO3 (8 nm)，Al (100 nm)，其中CBP: MoO3采用双源蒸镀的方法，以CBP为主体材料，MoO3为客体材料，MoO3的掺杂浓度为10 wt%，CBP蒸镀速率为4Å/s，CBP: MoO3蒸镀速率为2Å/s，MoO3的蒸镀速率为0.5 Å/s，Al蒸镀速率为6 Å/s。Step 5: Place the substrate in a vacuum chamber at 5 x 10 -4 Pa, and sequentially evaporate CBP (15 nm), CBP: MoO 3 (30 nm), MoO 3 (8 nm), Al (100 nm), where CBP: MoO 3 adopts a dual-source evaporation method, with CBP as the host material and MoO 3 as the guest material, the doping concentration of MoO 3 is 10 wt%, the CBP evaporation rate is 4Å/s, and the CBP: MoO 3 evaporation The rate is 2 Å/s, the evaporation rate of MoO 3 is 0.5 Å/s, and the evaporation rate of Al is 6 Å/s.
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