WO2021082960A1 - 一种溶质非完全溶解方式超声辅助制备氧化锌量子点的方法 - Google Patents
一种溶质非完全溶解方式超声辅助制备氧化锌量子点的方法 Download PDFInfo
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 238000000034 method Methods 0.000 title claims abstract description 45
- 238000004090 dissolution Methods 0.000 title claims abstract description 26
- 239000002096 quantum dot Substances 0.000 claims abstract description 23
- 239000011787 zinc oxide Substances 0.000 claims abstract description 20
- 239000003960 organic solvent Substances 0.000 claims abstract description 14
- 239000002244 precipitate Substances 0.000 claims abstract description 14
- 239000000725 suspension Substances 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 9
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 9
- 239000011701 zinc Substances 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 238000000137 annealing Methods 0.000 claims abstract description 7
- 239000012454 non-polar solvent Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 239000002243 precursor Substances 0.000 claims abstract description 6
- 239000003513 alkali Substances 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims abstract description 4
- 230000035484 reaction time Effects 0.000 claims abstract description 4
- 239000006228 supernatant Substances 0.000 claims abstract description 4
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- 230000001476 alcoholic effect Effects 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 7
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 6
- 239000002585 base Substances 0.000 claims description 5
- YZYKBQUWMPUVEN-UHFFFAOYSA-N zafuleptine Chemical compound OC(=O)CCCCCC(C(C)C)NCC1=CC=C(F)C=C1 YZYKBQUWMPUVEN-UHFFFAOYSA-N 0.000 claims description 5
- PQVSTLUFSYVLTO-UHFFFAOYSA-N ethyl n-ethoxycarbonylcarbamate Chemical group CCOC(=O)NC(=O)OCC PQVSTLUFSYVLTO-UHFFFAOYSA-N 0.000 claims description 4
- GLXDVVHUTZTUQK-UHFFFAOYSA-M lithium hydroxide monohydrate Substances [Li+].O.[OH-] GLXDVVHUTZTUQK-UHFFFAOYSA-M 0.000 claims description 4
- 229940040692 lithium hydroxide monohydrate Drugs 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 150000003751 zinc Chemical class 0.000 claims description 4
- 239000003495 polar organic solvent Substances 0.000 claims description 3
- 238000006862 quantum yield reaction Methods 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 239000013049 sediment Substances 0.000 claims description 2
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 claims 2
- 229940050176 methyl chloride Drugs 0.000 claims 1
- 238000005119 centrifugation Methods 0.000 abstract 1
- 238000001556 precipitation Methods 0.000 abstract 1
- 230000003068 static effect Effects 0.000 abstract 1
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 238000002604 ultrasonography Methods 0.000 description 4
- 239000003446 ligand Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000010899 nucleation Methods 0.000 description 3
- 230000006911 nucleation Effects 0.000 description 3
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
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- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- MARUHZGHZWCEQU-UHFFFAOYSA-N 5-phenyl-2h-tetrazole Chemical class C1=CC=CC=C1C1=NNN=N1 MARUHZGHZWCEQU-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- FRLJSGOEGLARCA-UHFFFAOYSA-N cadmium sulfide Chemical class [S-2].[Cd+2] FRLJSGOEGLARCA-UHFFFAOYSA-N 0.000 description 1
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical class [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000011217 control strategy Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
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- 238000010586 diagram Methods 0.000 description 1
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- 230000000694 effects Effects 0.000 description 1
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- 238000005265 energy consumption Methods 0.000 description 1
- 238000000024 high-resolution transmission electron micrograph Methods 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- XCAUINMIESBTBL-UHFFFAOYSA-N lead(ii) sulfide Chemical compound [Pb]=S XCAUINMIESBTBL-UHFFFAOYSA-N 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
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- 238000010992 reflux Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 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
- C09K11/54—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing zinc or cadmium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Definitions
- the invention belongs to the field of semiconductor nano materials, and specifically relates to a method for preparing zinc oxide quantum dots.
- Quantum dot refers to a functional nanomaterial whose semiconductor particle size is small enough to be between 1-20 nm on a three-dimensional scale.
- Quantum dots are generally spherical or quasi-spherical, and are usually composed of group IV, II-VI or III-V elements. The size effect of quantum dots causes them to have optoelectronic properties that are usually not available in macroscopic bulk materials. By applying a certain light pressure or electric field to quantum dots, they will emit light of specific wavelengths or frequencies.
- Common quantum dot materials include cadmium sulfide quantum dots, cadmium selenide quantum dots, cadmium telluride quantum dots, lead sulfide quantum dots and so on.
- zinc oxide (ZnO) quantum dots Compared with general quantum dots, zinc oxide (ZnO) quantum dots have the advantages of non-toxic, harmless, and environmentally friendly. At the same time, zinc oxide has a wide band gap (3.2eV) and strong exciton binding energy (60meV), which is a semiconductor material with important application value. It is currently used in many areas, such as photocatalysis, sensors, solar cells, biomedicine, ceramic materials, rubber industry, etc.
- the current methods for preparing zinc oxide quantum dots are mainly sol-gel method and hydrothermal synthesis method.
- the specific treatment methods of this kind of method include high temperature treatment, reflux high-power stirring, etc., and the energy consumption and cost are relatively high.
- the preparation of the precursor part particularly emphasizes the need to completely dissolve the solute and prepare a completely transparent and clear solution before the quantum dots can be prepared. This leads to a longer preparation process time, limits its promotion and application, and also hinders the study of the nucleation mechanism in the field of quantum dots.
- the technical problem to be solved by the present invention is to provide a method for preparing zinc oxide quantum dots assisted by ultrasound in a solute incomplete dissolution mode.
- the technical solution adopted by the present invention includes the following preparation methods:
- Step 1 Place the zinc-containing inorganic salt in an alcoholic organic solvent in an ultrasonic environment to form a ZnO precursor suspension A;
- Step 2 Fully dissolve the strong base in an alcoholic organic solvent in a stirring environment to obtain a clear solution B;
- Step 3 In an ultrasonic environment, add the clear solution B obtained in step 2 dropwise to the suspension A obtained in step 1, and allow it to fully react in an ultrasonic environment.
- the reaction time is 10-40 min to obtain solution C ;
- Step 4 Add the solution C after the reaction in step 3 to the non-polar solvent, leave it to settle, centrifuge at a certain speed, remove the supernatant to obtain the initial precipitate, and then add the alcoholic organic solvent, and ultrasonic Disperse the sediment in the environment;
- Step 5 Repeat step 4 more than twice to obtain pure ZnO quantum dot precipitate
- Step 6 Place the ZnO quantum dot precipitate obtained in Step 5 in a vacuum dryer for annealing treatment to obtain ZnO powder.
- the method for preparing zinc oxide quantum dots by ultrasonic-assisted solute incomplete dissolution is characterized in that: in steps 1 and 3, the ultrasonic power of the ultrasonic wave is 200-500W, the ultrasonic time is 10-40min, and the ultrasonic temperature is 40-70°C.
- the method for preparing zinc oxide quantum dots with the aid of ultrasonic-assisted solute dissolution is characterized in that: in steps 1 and 2, the alcoholic organic solvent is absolute ethanol, and its purity is chromatographic purity.
- the method for preparing zinc oxide quantum dots by ultrasonic-assisted solute incomplete dissolution is characterized in that: in step 1, the concentration of zinc salt in suspension A is 0.01-0.4 mol/L, and the The zinc-containing inorganic salt is zinc acetate dihydrate.
- the method for preparing zinc oxide quantum dots by ultrasonic-assisted solute incomplete dissolution is characterized in that: in step 2, the strong base is lithium hydroxide monohydrate, and its molar solution concentration in the solution is 0.2- 0.5mol/L.
- the method for preparing zinc oxide quantum dots by ultrasonic-assisted solute incomplete dissolution is characterized in that: in step 1, the amount ratio of the zinc salt of the zinc-containing inorganic salt to the alkali substance is 1:0.2-1: 1.
- step 3 the clear solution B obtained in step 2 is added dropwise to the suspension described in step 1 through a constant pressure separatory funnel.
- Solution C is obtained from solution A.
- the method for preparing zinc oxide quantum dots by ultrasonic-assisted solute incomplete dissolution is characterized in that: in step 4, the non-polar organic solvent is: n-heptane, n-hexane, toluene, methylene chloride, chloroform In one of them, the volume ratio of the alcohol organic solvent to the non-polar solvent is 1:2-1:4.
- the method for preparing zinc oxide quantum dots by ultrasonic-assisted solute dissolution is characterized in that: in step 4, the centrifugal speed is 2000-6000 r/min, and the centrifugal time is 10-20 min.
- the method for preparing zinc oxide quantum dots by ultrasonic-assisted solute incomplete dissolution is characterized in that: in step 6, the annealing temperature is 50-100° C., and the equipment used is a vacuum drying oven.
- the method for preparing zinc oxide quantum dots with the aid of ultrasonic-assisted solute dissolution is characterized in that the ultrasonic environment is composed of an ultrasonic generating device with a water circulation constant temperature system.
- the method for preparing zinc oxide quantum dots by ultrasonic-assisted solute incomplete dissolution is characterized in that steps 1, 2 and 3 are carried out in a mixed environment composed of an ultrasonic environment and a stirring environment, respectively.
- the ultrasonic-assisted preparation method can promote the growth and nucleation of quantum dots.
- the method is safe, non-toxic, and environmentally friendly.
- the prepared quantum dots have the advantages of good particle uniformity, high quantum yield, and good luminescence performance.
- Figure 1 is a TEM image of zinc oxide quantum dots prepared by the method of the present invention.
- Figure 2 is an HRTEM image of zinc oxide quantum dots prepared by the method of the present invention.
- Figure 3 is an XRD pattern of zinc oxide quantum dots prepared by the method of the present invention.
- Figure 4 is an electron diffraction pattern of zinc oxide quantum dots prepared by the method of the present invention.
- Fig. 5 is a diagram showing the luminescence of zinc oxide quantum prepared by the method of the present invention.
- Step 1 Weigh 1.6 g of zinc acetate dihydrate, add it to 50 mL of absolute ethanol (its purity is chromatographically pure), and mix for 20 minutes in an ultrasonic environment to form a ZnO precursor suspension A. During this period, the ultrasonic power of the ultrasonic generator is controlled to be 300W and the ultrasonic temperature is 40°C, so that the zinc acetate dihydrate and the absolute ethanol are fully mixed.
- Step 2 Weigh 0.38 g of lithium hydroxide monohydrate, add it to 25 mL of absolute ethanol (its purity is chromatographically pure), and stir at room temperature for 30 minutes to form a colorless and transparent lye, and a clear solution B is obtained.
- Step 3 In an ultrasonic environment, add the clear solution B obtained in step 2 dropwise to the suspension A obtained in step 1, and allow it to fully react in an ultrasonic environment, and the reaction time is 20 minutes to obtain solution C. During this period, the ultrasonic power of the ultrasonic generator is controlled to be 300 W and the ultrasonic temperature is 40° C., so that the clear solution B and the suspension A are fully reacted.
- Step 4 Add the solution C after the reaction in Step 3 to the non-polar solvent according to the volume ratio of 1:2, and let it settle for 20 minutes. After the precipitate is completely precipitated, the liquid is centrifuged at a speed of 4000 r/min, and then the supernatant liquid is removed to obtain the initial precipitate. Subsequently, 10 mL of anhydrous ethanol solution was added, and it was re-dispersed in anhydrous ethanol by sonicating for 2 minutes to form a colorless transparent liquid.
- Step 5 Repeat the process of step 4 three times to obtain a pure ZnO quantum dot precipitate, which is recorded as liquid D.
- Step 6 Place the ZnO quantum dot precipitate obtained in Step 5 in a vacuum dryer for annealing treatment to obtain ZnO powder.
- the annealing temperature is 50-100°C, and the equipment used is a vacuum drying oven.
- the zinc oxide quantum dots with a particle size of 1-10 nm, a fluorescence range of 370-690 nm, and a quantum yield >50% can be obtained by using the above method.
- the concentration of the zinc acetate dihydrate is 0.01-0.4 mol/L, so as to appropriately scale up when the optimal concentration is obtained.
- the strong base is lithium hydroxide monohydrate, and the molar solution concentration in the solution is 0.2-0.5 mol/L, so as to obtain the optimum concentration. enlarge.
- the ratio of the amount of the zinc salt of the zinc-containing inorganic salt to the alkali substance is 1:0.2-1:1, so as to appropriately scale up when the optimal ratio is obtained.
- step 3 the clear solution B obtained in step 2 is added dropwise to the suspension A of step 1 through a constant pressure separatory funnel to obtain solution C.
- the dropwise addition is to ensure product uniformity and ensure The nucleation and growth process of the quantum dot reaction makes the reaction product more uniform.
- the non-polar organic solvent is one of n-heptane, n-hexane, toluene, dichloromethane, and chloroform.
- the quantum dots prepared by the above reaction have no ligands on the surface, so the product can be obtained by changing the polarity system of the solution. Compared with the addition of long-chain ligands (such as oleic acid) during the synthesis process, the operation is easier, and the modification of the ligands usually leads to changes in the surface groups of the quantum dots, which is not conducive to subsequent operations.
- the ultrasonic environment is constituted by an ultrasonic generator with a water circulation constant temperature system.
- Ultrasound has significant advantages over traditional magnetic and mechanical stirring methods.
- the frequency of the ultrasound is very large, which can more fully mix the products evenly and ensure the experimental results.
- the temperature control method with its own water circulation is used, so that the ultrasonic generator device can be prepared for temperature control and heat preservation.
- step 1 step 2, and step 3 they are carried out in a mixed environment composed of an ultrasonic environment and a stirring environment, respectively, so that the solution is fully dissolved and reacted.
- the liquid D is dripped onto the XRD sample stage, and after drying, the test result with the XRD equipment is shown in FIG. 3.
- Each diffraction peak corresponds to the ZnO standard card 36-1451. It can be seen that the sample peak has no large peak shift, indicating that the ZnO precursor has been completely converted into ZnO quantum dots, and the XRD diffraction peaks are strong and the peak shape is sharper. It shows that the crystallinity of the sample is better.
- the liquid D was dropped onto the carbon mesh support net, and after drying, the results of testing with a transmission electron microscope are shown in Figure 1.
- Figure 1 There is no obvious agglomeration among the particles, and the particles are uniform in shape (spherical), and the distribution is relatively uniform.
- Figure 2 it can be seen (Figure 2) that the prepared sample has clear lattice fringes, indicating that its crystallization is in good condition.
- the average particle size of the prepared sample is 4nm.
- the prepared ZnO quantum dots have a hexagonal wurtzite structure, and there are no other polycrystalline or amorphous structures.
- the volume ratio of the alcoholic organic solvent to the non-polar solvent is in the range of 1:2-1:4; in steps 1 and 3, the ultrasonic power is 200-500W, and the ultrasonic time is 10-40min, the ultrasonic temperature is in the range of 40-70°C; in step 4, the centrifugal speed is 2000-6000r/min, and the centrifugal time is in the range of 10-20min. Both can achieve the effects of the present invention.
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Abstract
Description
Claims (10)
- 一种溶质非完全溶解方式超声辅助制备氧化锌量子点的方法,所述氧化锌量子点的粒径范围为1-10nm、荧光范围为370-690nm、量子产率>50%,其特征在于,制备方法如下:步骤1:在超声波环境中将含锌无机盐置于醇类有机溶剂中,形成ZnO前驱体悬浊液A;步骤2:将强碱在搅拌环境中充分溶解在醇类有机溶剂中,获得澄清溶液B;步骤3:在超声波环境中,将步骤2所得的澄清溶液B逐滴加入步骤1所得的悬浊液A中,并任其在超声波环境下实现充分反应,反应时间为10-40min,获得溶液C;步骤4:将步骤3反应后的溶液C加入到非极性溶剂中,静置沉淀,在一定速度下离心后,移去上清液,获得初始沉淀物,随后加入醇类有机溶剂,在超声环境中分散该沉淀物;步骤5:重复步骤4两次以上,可得到纯净的ZnO量子点沉淀物;步骤6:将步骤5得到的ZnO量子点沉淀物置于真空干燥机中进行退火处理,得到ZnO粉末。
- 根据权利要求1所述的溶质非完全溶解方式超声辅助制备氧化锌量子点的方法,其特征在于:在步骤1、3中,所述超声波的超声功率为200-500W、超声时间为10-40min、超声温度为40-70℃。
- 根据权利要求1所述的溶质非完全溶解方式超声辅助制备氧化锌量子点的方法,其特征在于:在步骤1、2中,所述醇类有机溶剂为无水乙醇,其纯度为色谱纯。
- 根据权利要求1所述的溶质非完全溶解方式超声辅助制备氧化锌量子点的方法,其特征在于:在步骤1中,所述的悬浊液A中含锌无机盐的浓度为0.01-0.4mol/L,所采用的含锌无机盐为二水合醋酸锌。
- 根据权利要求1所述的溶质非完全溶解方式超声辅助制备氧化锌量子点的方法,其特征在于:在步骤2中,所述的强碱为一水氢氧化锂,其在溶液中的摩尔溶液浓度为0.2-0.5mol/L。
- 根据权利要求1所述的溶质非完全溶解方式超声辅助制备氧化锌量子点的方法,其特征在于:在步骤1中,所述含锌无机盐的锌盐与碱的物质的量比为1:0.2-1:1。
- 根据权利要求1所述的溶质非完全溶解方式超声辅助制备氧化锌量子点的方法,其特征在于:在步骤3中,通过恒压分液漏斗将步骤2所得的澄清溶液B逐滴加入步骤1所述悬浊液A中获得溶液C。
- 根据权利要求1所述的溶质非完全溶解方式超声辅助制备氧化锌量子点的方法,其特征在于:在步骤4中,所述非极性有机溶剂为:正庚烷、正己烷、甲苯、二氯甲烷、氯仿中的其中一种,所用醇类有机溶剂与该非极性溶剂的体积比为1:2-1:4。
- 根据权利要求1所述的溶质非完全溶解方式超声辅助制备氧化锌量子点的方法,其特征在于:在步骤4中,离心速度为2000-6000r/min、离心时间为10-20min。
- 根据权利要求1所述的溶质非完全溶解方式超声辅助制备氧化锌量子点的方法,其特征在在于:在步骤6,所述退火温度为50-100℃,所使用的设备为真空干燥箱。
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