CN106186045A - A kind of preparation method of flower shape zinc oxide nano-particle cluster - Google Patents
A kind of preparation method of flower shape zinc oxide nano-particle cluster Download PDFInfo
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 36
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title description 9
- 238000000034 method Methods 0.000 claims abstract description 24
- 150000003751 zinc Chemical class 0.000 claims abstract description 23
- 238000003756 stirring Methods 0.000 claims abstract description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 45
- 239000012266 salt solution Substances 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 15
- 239000012153 distilled water Substances 0.000 claims description 14
- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical compound C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 230000001376 precipitating effect Effects 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 13
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 4
- 239000011701 zinc Substances 0.000 abstract description 4
- 229910052725 zinc Inorganic materials 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N glycerol group Chemical group OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 5
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 239000002073 nanorod Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004246 zinc acetate Substances 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- 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
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/50—Agglomerated particles
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Description
技术领域technical field
本发明涉及一种纳米氧化锌的制备方法，具体是一种花状氧化锌纳米颗粒团簇的制备方法。The invention relates to a preparation method of nano-zinc oxide, in particular to a preparation method of flower-shaped zinc oxide nano-particle clusters.
背景技术Background technique
氧化锌在室温下的禁带宽度约为3.37eV，具有良好的导热、导电、压电、光电特性，而且化学性质稳定，因此在太阳能电池、锂离子电池、紫外激光发射器、气体传感器、场发射器件等多个领域得到广泛应用。此外，氧化锌具有原材料资源丰富，价格低廉，绿色环保等优点，可以进行大规模生产。氧化锌纳米材料的性能取决于其形貌和尺寸，因此合成不同形貌和尺寸的氧化锌纳米材料来研究其新的性能并找到相应的应用领域已成为新的研究方向。大量文献报道了用不同的方法制备出各种不同形貌的纳米氧化锌，如纳米颗粒、纳米线、纳米棒、纳米带、纳米管、纳米片等，常用的制备方法有水热法、溶胶凝胶法、微乳液法和沉淀法等。Zinc oxide has a band gap of about 3.37eV at room temperature, has good thermal conductivity, electrical conductivity, piezoelectricity, photoelectricity, and stable chemical properties, so it is widely used in solar cells, lithium-ion batteries, ultraviolet laser emitters, gas sensors, field It has been widely used in many fields such as transmitting devices. In addition, zinc oxide has the advantages of abundant raw material resources, low price, environmental protection, etc., and can be mass-produced. The performance of ZnO nanomaterials depends on their shape and size, so it has become a new research direction to synthesize ZnO nanomaterials with different shapes and sizes to study their new properties and find corresponding application fields. A large number of literatures have reported the preparation of nano-zinc oxide with various shapes by different methods, such as nanoparticles, nanowires, nanorods, nanobelts, nanotubes, nanosheets, etc. The commonly used preparation methods include hydrothermal method, sol Gel method, microemulsion method and precipitation method, etc.
文献“张现利.ZnO纳米材料的制备及性能研究[D].安徽:安徽大学,2009.”报道了一种花瓣状氧化锌的制备方法，即采用直接沉淀法在醋酸锌和氢氧化钠摩尔比为1:2、温度为80℃到100℃、溶剂为丙三醇的条件下反应24h。该方法反应时间较长，而且用丙三醇做溶剂，成本高，在实际生产中有一定的局限性。The literature "Zhang Xianli. Preparation and performance research of ZnO nanomaterials [D]. Anhui: Anhui University, 2009." reported a preparation method of petal-shaped zinc oxide, that is, using the direct precipitation method at the molar ratio of zinc acetate and sodium hydroxide The ratio is 1:2, the temperature is 80°C to 100°C, and the solvent is glycerol for 24 hours. The method has a long reaction time and uses glycerol as a solvent, which has high cost and has certain limitations in actual production.
文献“谢志强.氧化锌纳米棒的水热法制备及其光催化性能的研究[D].南宁:广西大学，2012.”采用分析纯氧化锌作为锌源，氢氧化钠为矿化剂，以盐酸调控反应溶液的碱度，用水热合成方法在60℃，18h的反应条件下制备出了许多纳米颗粒聚集在一起的花状氧化锌。该水热合成法对设备要求高，危险系数大，有一定的操作难度。The literature "Xie Zhiqiang. Preparation of zinc oxide nanorods by hydrothermal method and its photocatalytic performance [D]. Nanning: Guangxi University, 2012." uses analytically pure zinc oxide as the zinc source and sodium hydroxide as the mineralizer. Hydrochloric acid regulates the alkalinity of the reaction solution, and a flower-shaped zinc oxide with many nanoparticles aggregated together is prepared by hydrothermal synthesis method under the reaction conditions of 60° C. and 18 hours. The hydrothermal synthesis method has high requirements on equipment, high risk factor and certain difficulty in operation.
发明内容Contents of the invention
本发明的目的是克服上述现有技术的不足，提供一种花状氧化锌纳米颗粒团簇的制备方法，工艺流程简单，操作方便，反应过程中无添加剂、模板，保证了产品纯度，而且反应温度低，反应时间短，成本和能耗低，可以大规模工业化生产The purpose of the present invention is to overcome above-mentioned deficiencies in the prior art, provide a kind of preparation method of flower-like zinc oxide nano particle cluster, technological process is simple, easy to operate, there is no additive, template in the reaction process, has guaranteed product purity, and reaction temperature Low, short reaction time, low cost and energy consumption, large-scale industrial production
为了达到上述目的，本发明采取的技术方案为：In order to achieve the above object, the technical scheme that the present invention takes is:
一种制备花状氧化锌纳米颗粒团簇的方法，包括以下步骤：A method for preparing flower-shaped zinc oxide nanoparticle clusters, comprising the following steps:
1)将沉淀剂加入到锌盐溶液中，搅拌0.5-1h；其中，锌盐溶液的摩尔浓度为0.001-0.004mol/L，沉淀剂与锌盐的摩尔比为1:10；1) adding the precipitant to the zinc salt solution and stirring for 0.5-1h; wherein the molar concentration of the zinc salt solution is 0.001-0.004mol/L, and the molar ratio of the precipitant to the zinc salt is 1:10;
2)将步骤1)搅拌后的溶液加热至90-100℃，搅拌4-6h后降至室温、洗涤、干燥，得到花状氧化锌纳米颗粒团簇。2) The solution stirred in step 1) is heated to 90-100° C., stirred for 4-6 hours, then lowered to room temperature, washed and dried to obtain flower-shaped zinc oxide nanoparticle clusters.
本发明进一步的改进在于，所述锌盐溶液是通过将六水合硝酸锌溶于水中制得。A further improvement of the present invention is that the zinc salt solution is prepared by dissolving zinc nitrate hexahydrate in water.
本发明进一步的改进在于，所述沉淀剂为氢氧化钠。A further improvement of the present invention is that the precipitation agent is sodium hydroxide.
本发明进一步的改进在于，所述步骤1)中搅拌是在室温下进行的。A further improvement of the present invention lies in that the stirring in the step 1) is carried out at room temperature.
本发明进一步的改进在于，降温采用自然降至室温。A further improvement of the present invention is that the temperature is naturally lowered to room temperature.
本发明进一步的改进在于，洗涤采用蒸馏水清洗至pH值为7，再用无水乙醇清洗3次。A further improvement of the present invention is that the washing is performed with distilled water until the pH value is 7, and then washed with absolute ethanol for 3 times.
本发明进一步的改进在于，干燥是在恒温干燥箱中进行。A further improvement of the present invention is that the drying is carried out in a constant temperature drying oven.
本发明进一步的改进在于，干燥的温度为60-80℃，时间为10-12h。The further improvement of the present invention lies in that the drying temperature is 60-80° C. and the drying time is 10-12 hours.
与现有技术相比，本发明具有的有益效果：本发明以锌盐和沉淀剂为原料，采用直接沉淀法在90-100℃下反应4-6h，合成了形貌可控的花状氧化锌纳米颗粒团簇。氧化锌纳米颗粒分布均匀，尺寸为20-40纳米，可广泛应用于催化、生物医药、传感器、电磁吸收、光致发光、气敏及压敏电阻等领域。本发明与现有技术相比，具有方法简便，成本低的优点，仅仅通过沉淀法即可制得花状氧化锌纳米颗粒团簇，工艺流程简单，操作方便，反应过程中无添加剂、模板，并保证了产品纯度，而且反应温度低，反应时间短，成本和能耗低，环境友好，可以大规模工业化生产。Compared with the prior art, the present invention has beneficial effects: the present invention uses zinc salt and precipitating agent as raw materials, adopts direct precipitation method to react at 90-100°C for 4-6h, and synthesizes a flower-like oxide with controllable morphology. Zinc nanoparticle clusters. Zinc oxide nanoparticles are evenly distributed and the size is 20-40 nanometers, which can be widely used in the fields of catalysis, biomedicine, sensors, electromagnetic absorption, photoluminescence, gas sensors and piezoresistors. Compared with the prior art, the present invention has the advantages of simple method and low cost, flower-shaped zinc oxide nanoparticle clusters can be prepared only by precipitation method, simple process flow, convenient operation, no additives and templates in the reaction process, The product purity is guaranteed, and the reaction temperature is low, the reaction time is short, the cost and energy consumption are low, the environment is friendly, and large-scale industrial production is possible.
进一步，沉淀剂为氢氧化钠，是因为氢氧化钠具有较强的碱性，可以作为碱源。Further, the precipitating agent is sodium hydroxide, because sodium hydroxide has strong alkalinity and can be used as an alkali source.
附图说明Description of drawings
图1为本发明实施例1中氧化锌的XRD图；Fig. 1 is the XRD pattern of zinc oxide in the embodiment of the present invention 1;
图2为本发明实施例1中不同放大倍数下氧化锌的SEM图。其中，图2(a)放大倍数为30000，图2(b)方法倍数为110000。Fig. 2 is an SEM image of zinc oxide at different magnifications in Example 1 of the present invention. Among them, Figure 2(a) has a magnification of 30,000, and Figure 2(b) has a magnification of 110,000.
具体实施方式detailed description
下面结合附图与实施例对本发明做进一步详细说明。The present invention will be described in further detail below in conjunction with the accompanying drawings and embodiments.
实施例1Example 1
称取0.1188g六水合硝酸锌溶解于400mL蒸馏水中，加入0.1600g氢氧化钠到上述锌盐溶液中，室温下混合搅拌0.5h。然后加热上述溶液至95℃，反应5h。反应结束待自然降至室温，产物用蒸馏水清洗至pH值为7，再用无水乙醇清洗3次，60℃的恒温干燥箱中干燥10h，即可得到白色氧化锌粉体。Weigh 0.1188g of zinc nitrate hexahydrate and dissolve it in 400mL of distilled water, add 0.1600g of sodium hydroxide to the above zinc salt solution, mix and stir at room temperature for 0.5h. Then the above solution was heated to 95°C and reacted for 5h. After the reaction was completed, the product was cooled down to room temperature naturally, and the product was washed with distilled water until the pH value was 7, then washed three times with absolute ethanol, and dried in a constant temperature drying oven at 60°C for 10 hours to obtain white zinc oxide powder.
参见图1，从图1可以看出制备的纳米氧化锌为纤锌矿型，且纯度高，无杂质峰。Referring to Fig. 1, it can be seen from Fig. 1 that the prepared nano-zinc oxide is wurtzite type, and has high purity and no impurity peak.
参见图2，从图2(a)可以看出制备出的氧化锌纳米颗粒自组装成了一种花状团簇，从图2(b)可以看出氧化锌纳米颗粒分布均匀，尺寸为20-40纳米。Referring to Figure 2, it can be seen from Figure 2(a) that the prepared zinc oxide nanoparticles self-assemble into a flower-like cluster, and from Figure 2(b) it can be seen that the zinc oxide nanoparticles are evenly distributed and the size is 20- 40 nm.
实施例2Example 2
称取0.2380g六水合硝酸锌溶解于400mL蒸馏水中，加入0.3200g氢氧化钠到上述锌盐溶液中，室温下混合搅拌0.8h。然后加热上述溶液至95℃，反应6h。反应结束待自然降至室温，产物用蒸馏水清洗至pH值为7，再用无水乙醇清洗3次，70℃的恒温干燥箱中干燥11h，即可得到白色氧化锌粉体。Weigh 0.2380g of zinc nitrate hexahydrate and dissolve it in 400mL of distilled water, add 0.3200g of sodium hydroxide to the above zinc salt solution, mix and stir at room temperature for 0.8h. Then the above solution was heated to 95°C and reacted for 6h. After the reaction was completed, the product was cooled down to room temperature naturally, and the product was washed with distilled water until the pH value was 7, then washed three times with absolute ethanol, and dried in a constant temperature drying oven at 70°C for 11 hours to obtain white zinc oxide powder.
实施例3Example 3
称取0.2975g六水合硝酸锌溶解于400mL蒸馏水中，加入0.3999g氢氧化钠到上述锌盐溶液中，室温下混合搅拌1h。然后加热上述溶液至90℃，反应6h。反应结束待自然降至室温，产物用蒸馏水清洗至pH值为7，再用无水乙醇清洗3次，70℃的恒温干燥箱中干燥12h，即可得到白色氧化锌粉体。Weigh 0.2975g of zinc nitrate hexahydrate and dissolve it in 400mL of distilled water, add 0.3999g of sodium hydroxide to the above zinc salt solution, and mix and stir for 1 hour at room temperature. Then the above solution was heated to 90°C and reacted for 6h. After the reaction was completed, the product was cooled down to room temperature naturally, and the product was washed with distilled water until the pH value was 7, then washed three times with absolute ethanol, and dried in a constant temperature drying oven at 70°C for 12 hours to obtain white zinc oxide powder.
实施例4Example 4
称取0.3572g六水合硝酸锌溶解于400mL蒸馏水中，加入0.4800g氢氧化钠到上述锌盐溶液中，室温下混合搅拌0.8h。然后加热上述溶液至100℃，反应5h。反应结束待自然降至室温，产物用蒸馏水清洗至pH值为7，再用无水乙醇清洗3次，80℃的恒温干燥箱中干燥10h，即可得到白色氧化锌粉体。Weigh 0.3572g of zinc nitrate hexahydrate and dissolve it in 400mL of distilled water, add 0.4800g of sodium hydroxide to the above zinc salt solution, and mix and stir at room temperature for 0.8h. Then the above solution was heated to 100°C and reacted for 5h. After the reaction was completed, the product was cooled down to room temperature naturally, and the product was washed with distilled water until the pH value was 7, then washed with absolute ethanol three times, and dried in a constant temperature drying oven at 80°C for 10 hours to obtain white zinc oxide powder.
实施例5Example 5
称取0.4760g六水合硝酸锌溶解于400mL蒸馏水中，加入0.6400g氢氧化钠到上述锌盐溶液中，室温下混合搅拌1h。然后加热上述溶液至100℃，反应4h。反应结束待自然降至室温，产物用蒸馏水清洗至pH值为7，再用无水乙醇清洗3次，80℃的恒温干燥箱中干燥12h，即可得到白色氧化锌粉体。Weigh 0.4760g of zinc nitrate hexahydrate and dissolve it in 400mL of distilled water, add 0.6400g of sodium hydroxide to the above zinc salt solution, and mix and stir for 1 hour at room temperature. Then the above solution was heated to 100°C and reacted for 4h. After the reaction was completed, the product was cooled to room temperature naturally, and the product was washed with distilled water until the pH value was 7, then washed three times with absolute ethanol, and dried in a constant temperature drying oven at 80°C for 12 hours to obtain white zinc oxide powder.
实施例6Example 6
1)将六水合硝酸锌溶于水中制得锌盐溶液，将氢氧化钠加入到锌盐溶液中，室温下搅拌0.5h，得到水溶性锌盐溶液；其中，锌盐溶液的摩尔浓度为0.001mol/L，氢氧化钠与六水合硝酸锌的摩尔比为1:10；1) Dissolving zinc nitrate hexahydrate in water to prepare a zinc salt solution, adding sodium hydroxide to the zinc salt solution, stirring at room temperature for 0.5h, to obtain a water-soluble zinc salt solution; wherein, the molar concentration of the zinc salt solution is 0.001 mol/L, the mol ratio of sodium hydroxide to zinc nitrate hexahydrate is 1:10;
2)将步骤1)所得溶液加热至100℃，搅拌4h后，自然降温至室温，采用蒸馏水清洗至pH值为7，再用无水乙醇清洗3次，于恒温干燥箱中，在60℃干燥12h，得到花状氧化锌纳米颗粒团簇。2) Heat the solution obtained in step 1) to 100°C, stir for 4 hours, then cool down to room temperature naturally, wash with distilled water until the pH value is 7, then wash with absolute ethanol for 3 times, and dry at 60°C in a constant temperature drying oven After 12 hours, the flower-shaped ZnO nanoparticle clusters were obtained.
实施例7Example 7
1)将六水合硝酸锌溶于水中制得锌盐溶液，将氢氧化钠加入到锌盐溶液中，室温下搅拌1h，得到水溶性锌盐溶液；其中，锌盐溶液的摩尔浓度为0.004mol/L，氢氧化钠与六水合硝酸锌的摩尔比为1:10；1) Dissolving zinc nitrate hexahydrate in water to prepare a zinc salt solution, adding sodium hydroxide to the zinc salt solution, stirring at room temperature for 1 hour, to obtain a water-soluble zinc salt solution; wherein, the molar concentration of the zinc salt solution is 0.004mol /L, the mol ratio of sodium hydroxide to zinc nitrate hexahydrate is 1:10;
2)将步骤1)所得溶液加热至90℃，搅拌6h后，自然降温至室温，采用蒸馏水清洗至pH值为7，再用无水乙醇清洗3次，于恒温干燥箱中，在80℃干燥10h，得到花状氧化锌纳米颗粒团簇。2) Heat the solution obtained in step 1) to 90°C, stir for 6 hours, then cool down to room temperature naturally, wash with distilled water until the pH value is 7, then wash with absolute ethanol for 3 times, and dry at 80°C in a constant temperature drying oven After 10 h, flower-shaped ZnO nanoparticle clusters were obtained.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107089677A (en) * | 2017-06-07 | 2017-08-25 | 首都医科大学宣武医院 | Preparation method of zinc oxide nanoparticles based on silk fibroin biological template regulation |
| CN109928421A (en) * | 2019-02-28 | 2019-06-25 | 江苏赛清科技有限公司 | With flower-like micro/nano structure Zinc oxide powder and its preparation method and application |
| CN111170356A (en) * | 2020-02-11 | 2020-05-19 | 江南大学 | Preparation method of shape-controllable nano zinc oxide |
| US20220113270A1 (en) * | 2020-10-08 | 2022-04-14 | City University Of Hong Kong | Method for fabricating zinc oxide nanostructures and gas sensors |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101613121A (en) * | 2009-07-16 | 2009-12-30 | 聊城大学 | A kind of preparation method of ellipsoidal zinc oxide |
| CN102101693A (en) * | 2010-12-29 | 2011-06-22 | 安徽理工大学 | Preparation method and application of double-function micro-nano hierarchical structural zinc oxide power |
-
2016
- 2016-07-26 CN CN201610596102.3A patent/CN106186045A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101613121A (en) * | 2009-07-16 | 2009-12-30 | 聊城大学 | A kind of preparation method of ellipsoidal zinc oxide |
| CN102101693A (en) * | 2010-12-29 | 2011-06-22 | 安徽理工大学 | Preparation method and application of double-function micro-nano hierarchical structural zinc oxide power |
Non-Patent Citations (2)
| Title |
|---|
| YONGJIANG SUN ET AL.: "Facile synthesis of flower-like 3D ZnO superstructures via solution route", 《CRYSTENGCOMM》 * |
| 汪苇等: "片状纳米氧化锌的合成和形貌控制", 《大连工业大学学报》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107089677A (en) * | 2017-06-07 | 2017-08-25 | 首都医科大学宣武医院 | Preparation method of zinc oxide nanoparticles based on silk fibroin biological template regulation |
| CN107089677B (en) * | 2017-06-07 | 2018-07-10 | 首都医科大学宣武医院 | Preparation method of zinc oxide nanoparticles based on silk fibroin biological template regulation |
| CN109928421A (en) * | 2019-02-28 | 2019-06-25 | 江苏赛清科技有限公司 | With flower-like micro/nano structure Zinc oxide powder and its preparation method and application |
| CN111170356A (en) * | 2020-02-11 | 2020-05-19 | 江南大学 | Preparation method of shape-controllable nano zinc oxide |
| CN111170356B (en) * | 2020-02-11 | 2021-04-20 | 江南大学 | A kind of preparation method of nanometer zinc oxide with controllable morphology |
| US20220113270A1 (en) * | 2020-10-08 | 2022-04-14 | City University Of Hong Kong | Method for fabricating zinc oxide nanostructures and gas sensors |
| US11639910B2 (en) * | 2020-10-08 | 2023-05-02 | City University Of Hong Kong | Method for fabricating zinc oxide nanostructures and gas sensors |
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