CN102134091B - Method for preparing micro structural zinc oxide by hydrothermal method - Google Patents
Method for preparing micro structural zinc oxide by hydrothermal method Download PDFInfo
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- CN102134091B CN102134091B CN 201110024679 CN201110024679A CN102134091B CN 102134091 B CN102134091 B CN 102134091B CN 201110024679 CN201110024679 CN 201110024679 CN 201110024679 A CN201110024679 A CN 201110024679A CN 102134091 B CN102134091 B CN 102134091B
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- zinc oxide
- distilled water
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- acetate dihydrate
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 172
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 86
- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000001027 hydrothermal synthesis Methods 0.000 title claims abstract description 28
- YZYKBQUWMPUVEN-UHFFFAOYSA-N zafuleptine Chemical compound OC(=O)CCCCCC(C(C)C)NCC1=CC=C(F)C=C1 YZYKBQUWMPUVEN-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000000126 substance Substances 0.000 claims abstract description 17
- 241000257465 Echinoidea Species 0.000 claims abstract description 16
- 239000007787 solid Substances 0.000 claims abstract description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 124
- 238000003756 stirring Methods 0.000 claims description 54
- 239000012153 distilled water Substances 0.000 claims description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 48
- 238000002360 preparation method Methods 0.000 claims description 30
- 239000007864 aqueous solution Substances 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 14
- 238000001338 self-assembly Methods 0.000 claims description 11
- 238000007789 sealing Methods 0.000 claims description 8
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 6
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 abstract description 17
- 238000006243 chemical reaction Methods 0.000 abstract description 11
- 239000013078 crystal Substances 0.000 abstract description 2
- 239000000446 fuel Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract 1
- 239000007800 oxidant agent Substances 0.000 abstract 1
- 230000001590 oxidative effect Effects 0.000 abstract 1
- 229920006316 polyvinylpyrrolidine Polymers 0.000 abstract 1
- 239000000376 reactant Substances 0.000 abstract 1
- 239000011701 zinc Substances 0.000 abstract 1
- 229910052725 zinc Inorganic materials 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 description 12
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000011805 ball Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- -1 nanometer sheet Substances 0.000 description 1
- 239000002063 nanoring Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
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Abstract
一种水热法制备微米结构氧化锌，以聚乙烯吡咯烷酮K-30为模板、二水醋酸锌为锌源、H2O2为氧化剂，通过控制反应物浓度、水热生长时间和反应温度制备成海胆状、锥状、六棱柱自组装实心球状和糖葫芦状四种微米结构的氧化锌材料。本发明具有方法简单、成本低、条件温和以及对环境无污染等优点。本发明制备的微米氧化锌材料纯度较高，晶体结构规整，材料形貌的可控性好，生产周期短，在燃料电池、光电转换材料以及化学传感器等方面有着巨大的应用前景。A hydrothermal method for preparing micron-structured zinc oxide, using polyvinylpyrrolidone K-30 as a template, zinc acetate dihydrate as a zinc source, and H2O2 as an oxidant, by controlling the concentration of reactants, hydrothermal growth time and reaction temperature . Zinc oxide materials with four micron structures in the shape of sea urchins, cones, hexagonal self-assembled solid spheres and candied haws. The invention has the advantages of simple method, low cost, mild conditions, no pollution to the environment and the like. The micron zinc oxide material prepared by the invention has high purity, regular crystal structure, good controllability of material appearance and short production cycle, and has great application prospects in fuel cells, photoelectric conversion materials, chemical sensors and the like.
Description
Technical field
The invention belongs to semi-conductor micron field of material preparation, be specifically related to the preparation method of a kind of micron zinc oxide material, particularly a kind of method that adopts the emulsion assisting alcohol-hydrothermal method to prepare four kinds of special appearance zinc oxide.
Background technology
Zinc oxide is a kind of important semiconductor material with wide forbidden band, bandwidth can reach the wurtzite crystal structure of 3.37eV, have good chemical property, thermostability, optical property and electrical properties, can under high-density, produce near ultraviolet room-temperature exciton laser, thereby have a wide range of applications in fields such as gas sensor, piezoelectric, catalyzer, solar cell, biological medicines.The research Showed Very Brisk of the preparation of zinc oxide micrometer nano structured unit and assembling and application.Because nano zinc oxide material at room temperature has the exciton bind energy up to 60meV, can be used for making the short-wavelength light electrical part, such as ultraviolet laser, high frequency filter, ultraviolet light detector and photodiode etc., make luminescent device and can obtain the higher gain of light, make zinc oxide have huge potential using value aspect the optical storage density increasing substantially.
The nanostructures such as nanometer ball, nano wire, nano belt, nanometer sheet, nano-rings, nanometer rod of zinc oxide have been prepared at present.Its preparation method who relates to comprises sol-gel method, hydrolysis method, antiphase emulsifiable method, the precipitator method, electrochemical deposition method and chemical vapour deposition (CVD) etc.Yet in the preparation process of micron zinc oxide material, ubiquity the shortcomings such as process is loaded down with trivial details, experiment condition is harsh, temperature of reaction is high, poor repeatability, apparatus expensive.Therefore, the preparation of relevant micron zinc oxide material and method thereof are probed into and are still the focus that present people pay close attention to.
Summary of the invention
Technical problem to be solved by this invention is to overcome above-mentioned preparation method's shortcoming, provides that a kind of safety simple to operate, cost are low, the gentle easy control of reaction conditions and repeatability is high, the preparation method of product pattern and the micrometer structure zinc oxide that size is controlled, crystalline structure is regular, monodispersity is good.
Solving the problems of the technologies described above the technical scheme that adopts is: be 30% H with massfraction
2O
2Add in the distilled water, stirring at room 5 minutes, add PVP K-30, stirring at room 10 minutes, add zinc acetate dihydrate, stirring at room 20 minutes, adding amount of substance concentration is the NaOH aqueous solution of 5mol/L, PVP K-30 and zinc acetate dihydrate, massfraction are 30% H
2O
2, distilled water, NaOH mass ratio be 1: 0.3658～36.58: 8.333～166.7: 466.7～625: 0.1667～25, stirring at room, after producing white opacity, continues solution to stir 5 minutes, white opacity solution is poured in the hydrothermal reaction kettle that liner is tetrafluoroethylene, the sealing hydrothermal reaction kettle, it is that 80～200 ℃ baking oven reacted 0.5～24 hour that hydrothermal reaction kettle is put into temperature, centrifugation, precipitation is alternately washed 3 times with distilled water, dehydrated alcohol successively, 60 ℃ of vacuum-drying 24 hours is prepared into micrometer structure zinc oxide.
In the inventive method, PVP K-30 and zinc acetate dihydrate, massfraction are 30% H
2O
2, distilled water, NaOH mass ratio be 1: 0.3658～10.98: 8.333～166.7: 466.7～625: 3.333～25, be prepared into a micron sea urchin shape zinc oxide, grow many zinc oxide micron rods from the center of ball, the diameter of sea urchin shape ball is 30～100 μ m, and the length of rod is that 15～50 μ m, diameter are 0.3～2 μ m.Wherein, PVP K-30 and zinc acetate dihydrate, massfraction are 30% H
2O
2, distilled water, NaOH mass ratio the best be 1: 3.658: 41.67: 591.7: 6.667.
In the inventive method, PVP K-30 and zinc acetate dihydrate, massfraction are 30% H
2O
2, distilled water, NaOH mass ratio be 1: 18.29: 8.333～166.7: 466.7～625: 3.333～25, be prepared into a micron taper zinc oxide, the length of cone is that 15～80 μ m, diameter are 0.5～10 μ m.Wherein, PVP K-30 and zinc acetate dihydrate, massfraction are 30% H
2O
2, distilled water, NaOH mass ratio the best be 1: 18.29: 41.67: 591.7: 6.667.
In the inventive method, PVP K-30 and zinc acetate dihydrate, massfraction are 30% H
2O
2, distilled water, NaOH mass ratio be 1: 29.27～36.58: 8.333～166.7: 466.7～625: 3.333～25, be prepared into the solid spherical zinc oxide of micron six prismatic self-assemblies, the diameter of solid sphere is 80～120 μ m, and the length of six prisms is that 40～60 μ m, diameter are 2～5 μ m.Wherein, PVP K-30 and zinc acetate dihydrate, massfraction are 30% H
2O
2, distilled water, NaOH mass ratio the best be 1: 29.27: 41.67: 591.7: 6.667.
In the inventive method, PVP K-30 and zinc acetate dihydrate, massfraction are 30% H
2O
2, distilled water, NaOH mass ratio be 1: 0.3658～18.29: 8.333～166.7: 466.7～625: 0.1667～1.667, be prepared into a micron sugarcoated haws on a stick shape zinc oxide, insert a taper zinc oxide in the middle of the flower shape zinc oxide ball, the diameter of ball is 3～20 μ m, and the length of cone is that 10～50 μ m, diameter are 0.5～10 μ m.Wherein, PVP K-30 and zinc acetate dihydrate, massfraction are 30% H
2O
2, distilled water, NaOH mass ratio the best be 1: 3.658: 41.67: 616.7: 1.667.
The present invention adopts hydrothermal method to be prepared into solid spherical, the taper of sea urchin shape, six prismatic self-assemblies, sugarcoated haws on a stick shape micrometer structure zinc oxide, has that method is simple, cost is low, an advantage such as mild condition and environmentally safe.The micron zinc oxide material purity of the present invention's preparation is higher, and crystalline structure is regular, and the controllability of material pattern is good, and is with short production cycle, at aspects such as fuel cell, photoelectric conversion material and chemical sensors huge application prospect arranged.
Description of drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the micron sea urchin shape zinc oxide of the embodiment of the invention 1 preparation.
Fig. 2 is the scanning electron microscope (SEM) photograph of the micron sea urchin shape zinc oxide of the embodiment of the invention 2 preparations.
Fig. 3 is the scanning electron microscope (SEM) photograph of the micron sea urchin shape zinc oxide of the embodiment of the invention 3 preparations.
Fig. 4 is the scanning electron microscope (SEM) photograph of the micron taper zinc oxide of the embodiment of the invention 4 preparations.
Fig. 5 is the scanning electron microscope (SEM) photograph of the micron taper zinc oxide of the embodiment of the invention 5 preparations.
Fig. 6 is the scanning electron microscope (SEM) photograph of the micron taper zinc oxide of the embodiment of the invention 6 preparations.
Fig. 7 is the scanning electron microscope (SEM) photograph of the solid spherical zinc oxide of micron six prismatic self-assemblies of the embodiment of the invention 7 preparations.
Fig. 8 is the scanning electron microscope (SEM) photograph of the solid spherical zinc oxide of micron six prismatic self-assemblies of the embodiment of the invention 8 preparations.
Fig. 9 is the scanning electron microscope (SEM) photograph of the solid spherical zinc oxide of micron six prismatic self-assemblies of the embodiment of the invention 9 preparations.
Figure 10 is the scanning electron microscope (SEM) photograph of the micron sugarcoated haws on a stick shape zinc oxide of the embodiment of the invention 10 preparations.
Figure 11 is the scanning electron microscope (SEM) photograph of the micron sugarcoated haws on a stick shape zinc oxide of the embodiment of the invention 11 preparations.
Figure 12 is the scanning electron microscope (SEM) photograph of the micron sugarcoated haws on a stick shape zinc oxide of the embodiment of the invention 12 preparations.
Embodiment
The present invention is described in more detail below in conjunction with drawings and Examples, but the invention is not restricted to these embodiment.
Embodiment 1
Take preparation micron sea urchin shape zinc oxide material as example, its concrete preparation method is as follows:
Be 30% H with massfraction
2O
25g joins in the 71g distilled water, stirring at room 5 minutes, add PVP K-30 0.12g, stirring at room 10 minutes, add zinc acetate dihydrate 0.439g, stirring at room 20 minutes, adding 4mL amount of substance concentration is the NaOH aqueous solution of 5mol/L, PVP K-30 and zinc acetate dihydrate, massfraction are 30% H
2O
2, distilled water, NaOH mass ratio be 1: 3.658: 41.67: 591.7: 6.667, stirring at room, after producing white opacity, continues solution to stir 5 minutes, white opacity solution is poured in the hydrothermal reaction kettle that liner is tetrafluoroethylene, the sealing hydrothermal reaction kettle, it is 180 ℃ baking oven reaction 24 hours that hydrothermal reaction kettle is put into temperature, centrifugation, precipitation is alternately washed 3 times with distilled water, dehydrated alcohol successively, 60 ℃ of vacuum-drying 24 hours.Products therefrom characterizes with Quanta 200 type environmental scanning electronic microscopes, the results are shown in Figure 1.
As seen from Figure 1, products therefrom is a micron sea urchin shape zinc oxide, grows many zinc oxide micron rods from the center of ball, and the diameter of sea urchin shape ball is 60～100 μ m, and the length of rod is that 30～50 μ m, diameter are 1.5～2 μ m.
Embodiment 2
In embodiment 1, be 30% H with massfraction
2O
21g joins in the 56g distilled water, stirring at room 5 minutes, add PVP K-30 0.12g, stirring at room 10 minutes, add zinc acetate dihydrate 0.0439g, stirring at room 20 minutes, adding 2mL amount of substance concentration is the NaOH aqueous solution of 5mol/L, PVP K-30 and zinc acetate dihydrate, massfraction are 30% H
2O
2, distilled water, NaOH mass ratio be 1: 0.3658: 8.333: 466.7: 3.333, other steps were identical with corresponding embodiment, are prepared into micrometer structure zinc oxide.Products therefrom characterizes with Quanta 200 type environmental scanning electronic microscopes, the results are shown in Figure 2.
As seen from Figure 2, products therefrom is a micron sea urchin shape zinc oxide, grows many zinc oxide micron rods from the center of ball, and the diameter of sea urchin shape ball is 40～80 μ m, and the length of rod is that 20～40 μ m, diameter are 1～1.5 μ m.
Embodiment 3
In embodiment 1, be 30% H with massfraction
2O
216g joins in the 60g distilled water, stirring at room 5 minutes, add PVP K-30 0.096g, stirring at room 10 minutes, add zinc acetate dihydrate 1.054g, stirring at room 20 minutes, adding 12mL amount of substance concentration is the NaOH aqueous solution of 5mol/L, PVP K-30 and zinc acetate dihydrate, massfraction are 30% H
2O
2, distilled water, NaOH mass ratio be 1: 10.98: 166.7: 625: 25, other steps were identical with corresponding embodiment, are prepared into micrometer structure zinc oxide.Products therefrom characterizes with Quanta 200 type environmental scanning electronic microscopes, the results are shown in Figure 3.
As seen from Figure 3, products therefrom is a micron sea urchin shape zinc oxide, grows many zinc oxide micron rods from the center of ball, and the diameter of sea urchin shape ball is 30～60 μ m, and the length of rod is that 15～30 μ m, diameter are 0.3～1 μ m.
Embodiment 4
Take preparation micron taper zinc oxide material as example, its concrete preparation method is as follows:
Be 30% H with massfraction
2O
25g joins in the 71g distilled water, stirring at room 5 minutes, add PVP K-30 0.12g, stirring at room 10 minutes, add zinc acetate dihydrate 2.195g, stirring at room 20 minutes, adding 4mL amount of substance concentration is the NaOH aqueous solution of 5mol/L, PVP K-30 and zinc acetate dihydrate, massfraction are 30% H
2O
2, distilled water, NaOH mass ratio be 1: 18.29: 41.67: 591.7: 6.667, stirring at room, after producing white opacity, continues solution to stir 5 minutes, white opacity solution is poured in the hydrothermal reaction kettle that liner is tetrafluoroethylene, the sealing hydrothermal reaction kettle, it is 180 ℃ baking oven reaction 24 hours that hydrothermal reaction kettle is put into temperature, centrifugation, precipitation is alternately washed 3 times with distilled water, dehydrated alcohol successively, 60 ℃ of vacuum-drying 24 hours.Products therefrom characterizes with Quanta 200 type environmental scanning electronic microscopes, the results are shown in Figure 4.
As seen from Figure 4, products therefrom is a micron taper zinc oxide, and the length of cone is that 15～30 μ m, diameter are 0.5～1 μ m.
Embodiment 5
In embodiment 4, be 30% H with massfraction
2O
21g joins in the 56g distilled water, stirring at room 5 minutes, add PVP K-30 0.12g, stirring at room 10 minutes, add zinc acetate dihydrate 2.195g, stirring at room 20 minutes, adding 2mL amount of substance concentration is the NaOH aqueous solution of 5mo1/L, PVP K-30 and zinc acetate dihydrate, massfraction are 30% H
2O
2, distilled water, NaOH mass ratio be 1: 18.29: 8.333: 466.7: 3.333, other steps were identical with corresponding embodiment, are prepared into micrometer structure zinc oxide.Products therefrom characterizes with Quanta 200 type environmental scanning electronic microscopes, the results are shown in Figure 5.
As seen from Figure 5, products therefrom is a micron taper zinc oxide, and the length of cone is that 50～80 μ m, diameter are 5～10 μ m.
Embodiment 6
In embodiment 4, be 30% H with massfraction
2O
216g joins in the 60g distilled water, stirring at room 5 minutes, add PVP K-30 0.096g, stirring at room 10 minutes, add zinc acetate dihydrate 1.756g, stirring at room 20 minutes, adding 12mL amount of substance concentration is the NaOH aqueous solution of 5mol/L, PVP K-30 and zinc acetate dihydrate, massfraction are 30% H
2O
2, distilled water, NaOH mass ratio be 1: 18.29: 166.7: 625: 25, other steps were identical with corresponding embodiment, are prepared into micrometer structure zinc oxide.Products therefrom characterizes with Quanta 200 type environmental scanning electronic microscopes, the results are shown in Figure 6.
As seen from Figure 6, products therefrom is a micron taper zinc oxide, and the length of cone is that 30～60 μ m, diameter are 3～10 μ m.
Embodiment 7
Take the solid spherical zinc oxide material of preparation micron six prismatic self-assemblies as example, its concrete preparation method is as follows:
Be 30% H with massfraction
2O
25g joins in the 71g distilled water, stirring at room 5 minutes, add PVP K-30 0.12g, stirring at room 10 minutes, add zinc acetate dihydrate 3.512g, stirring at room 20 minutes, adding 4mL amount of substance concentration is the NaOH aqueous solution of 5mol/L, PVP K-30 and zinc acetate dihydrate, massfraction are 30% H
20
2, distilled water, Na0H mass ratio be 1: 29.27: 41.67: 591.7: 6.667, stirring at room, after producing white opacity, continues solution to stir 5 minutes, white opacity solution is poured in the hydrothermal reaction kettle that liner is tetrafluoroethylene, the sealing hydrothermal reaction kettle, it is 180 ℃ baking oven reaction 24 hours that hydrothermal reaction kettle is put into temperature, centrifugation, precipitation is alternately washed 3 times with distilled water, dehydrated alcohol successively, 60 ℃ of vacuum-drying 24 hours.Products therefrom characterizes with Quanta 200 type environmental scanning electronic microscopes, the results are shown in Figure 7.
As seen from Figure 7, products therefrom is the solid spherical zinc oxide of micron six prismatic self-assemblies, and the diameter of solid sphere is 100～120 μ m, and the length of six prisms is that 40～60 μ m, diameter are 3～5 μ m.
Embodiment 8
In embodiment 7, be 30% H with massfraction
2O
21g joins in the 56g distilled water, stirring at room 5 minutes, add PVP K-30 0.12g, stirring at room 10 minutes, add zinc acetate dihydrate 3.512g, stirring at room 20 minutes, adding 2mL amount of substance concentration is the NaOH aqueous solution of 5mol/L, PVP K-30 and zinc acetate dihydrate, massfraction are 30% H
2O
2, distilled water, NaOH mass ratio be 1: 29.27: 8.333: 466.7: 3.333, other steps were identical with corresponding embodiment, are prepared into micrometer structure zinc oxide.Products therefrom characterizes with Quanta 200 type environmental scanning electronic microscopes, the results are shown in Figure 8.
As seen from Figure 8, products therefrom is the solid spherical zinc oxide of micron six prismatic self-assemblies, and the diameter of solid sphere is 80～100 μ m, and the length of six prisms is that 40～50 μ m, diameter are 3～4 μ m.
Embodiment 9
In embodiment 7, be 30% H with massfraction
2O
216g adds in the 60g distilled water, stirring at room 5 minutes, add PVP K-30 0.096g, stirring at room 10 minutes, add zinc acetate dihydrate 3.512g, stirring at room 20 minutes, adding 12mL amount of substance concentration is the NaOH aqueous solution of 5mol/L, PVP K-30 and zinc acetate dihydrate, massfraction are 30% H
2O
2, distilled water, NaOH mass ratio be 1: 36.58: 166.7: 625: 25, other steps were identical with corresponding embodiment, are prepared into micrometer structure zinc oxide.Products therefrom characterizes with Quanta 200 type environmental scanning electronic microscopes, the results are shown in Figure 9.
As seen from Figure 9, products therefrom is the solid spherical zinc oxide of micron six prismatic self-assemblies, and the diameter of solid sphere is 90～110 μ m, and the length of six prisms is that 45～55 μ m, diameter are 2～4 μ m.
Embodiment 10
Take preparation micron sugarcoated haws on a stick shape zinc oxide material as example, its concrete preparation method is as follows:
Be 30% H with massfraction
2O
25g joins in the 74g distilled water, stirring at room 5 minutes, add PVP K-30 0.12g, stirring at room 10 minutes, add zinc acetate dihydrate 0.439g, stirring at room 20 minutes, adding 1mL amount of substance concentration is the NaOH aqueous solution of 5mol/L, PVP K-30 and zinc acetate dihydrate, massfraction are 30% H
2O
2, distilled water, NaOH mass ratio be 1: 3.658: 41.67: 616.7: 1.667, stirring at room, after producing white opacity, continues solution to stir 5 minutes, white opacity solution is poured in the hydrothermal reaction kettle that liner is tetrafluoroethylene, the sealing hydrothermal reaction kettle, it is 180 ℃ baking oven reaction 24 hours that hydrothermal reaction kettle is put into temperature, centrifugation, precipitation is alternately washed 3 times with distilled water, dehydrated alcohol successively, 60 ℃ of vacuum-drying 24 hours.Products therefrom characterizes with Quanta 200 type environmental scanning electronic microscopes, the results are shown in Figure 10.
As seen from Figure 10, products therefrom is a micron sugarcoated haws on a stick shape zinc oxide, inserts a taper zinc oxide in the middle of the flower shape zinc oxide ball, and the diameter of ball is 3～6 μ m, and the length of cone is that 10～20 μ m, diameter are 0.5～1.5 μ m.
Embodiment 11
In embodiment 10, be 30% H with massfraction
2O
21g joins in the 56g distilled water, stirring at room 5 minutes, add PVP K-30 0.12g, stirring at room 10 minutes, add zinc acetate dihydrate 0.0439g, stirring at room 20 minutes, adding 0.1mL amount of substance concentration is the NaOH aqueous solution of 5mol/L, PVP K-30 and zinc acetate dihydrate, massfraction are 30% H
2O
2, distilled water, NaOH mass ratio be 1: 0.3658: 8.333: 466.7: 0.1667, other steps were identical with corresponding embodiment, are prepared into micrometer structure zinc oxide.Products therefrom characterizes with Quanta 200 type environmental scanning electronic microscopes, the results are shown in Figure 11.
As seen from Figure 10, products therefrom is a micron sugarcoated haws on a stick shape zinc oxide, inserts a taper zinc oxide in the middle of the flower shape zinc oxide ball, and the diameter of ball is 5～10 μ m, and the length of cone is that 20～30 μ m, diameter are 2～5 μ m.
Embodiment 12
In embodiment 10, be 30% H with massfraction
2O
216g joins in the 60g distilled water, stirring at room 5 minutes, add PVP K-30 0.096g, stirring at room 10 minutes, add zinc acetate dihydrate 1.756g, stirring at room 20 minutes, adding 0.8mL amount of substance concentration is the NaOH aqueous solution of 5mol/L, PVP K-30 and zinc acetate dihydrate, massfraction are 30% H
2O
2, distilled water, NaOH mass ratio be 1: 18.29: 166.7: 625: 1.667, other steps were identical with corresponding embodiment, are prepared into micrometer structure zinc oxide.Products therefrom characterizes with Quanta 200 type environmental scanning electronic microscopes, the results are shown in Figure 12.
As seen from Figure 12, products therefrom is a micron sugarcoated haws on a stick shape zinc oxide, inserts a taper zinc oxide in the middle of the flower shape zinc oxide ball, and the diameter of ball is 10～20 μ m, and the length of cone is that 30～50 μ m, diameter are 5～10 μ m.
Embodiment 13
In embodiment 1～12, white opacity solution is poured in the hydrothermal reaction kettle that liner is tetrafluoroethylene, the sealing hydrothermal reaction kettle, it is 80 ℃ baking oven reaction 20 hours that hydrothermal reaction kettle is put into temperature, other steps are identical with corresponding embodiment, are prepared into micrometer structure zinc oxide.
Embodiment 14
In embodiment 1～12, white opacity solution is poured in the hydrothermal reaction kettle that liner is tetrafluoroethylene, the sealing hydrothermal reaction kettle, it is 200 ℃ baking oven reaction 0.5 hour that hydrothermal reaction kettle is put into temperature, other steps are identical with corresponding embodiment, are prepared into micrometer structure zinc oxide.
Claims (7)
1. the method for a method for preparing micro structural zinc oxide by hydrothermal is characterized in that: be 30% H with massfraction
2O
2Add in the distilled water, stirring at room 5 minutes, add PVP K-30, stirring at room 10 minutes, add zinc acetate dihydrate, stirring at room 20 minutes, adding amount of substance concentration is the NaOH aqueous solution of 5mol/L, PVP K-30 and zinc acetate dihydrate, massfraction are 30% H
2O
2, distilled water, NaOH mass ratio be 1: 0.3658～36.58: 8.333～166.7: 466.7～625: 0.1667～25, stirring at room, after producing white opacity, continues solution to stir 5 minutes, white opacity solution is poured in the hydrothermal reaction kettle that liner is tetrafluoroethylene, the sealing hydrothermal reaction kettle, it is that 80～200 ℃ baking oven reacted 0.5～24 hour that hydrothermal reaction kettle is put into temperature, centrifugation, precipitation is alternately washed 3 times with distilled water, dehydrated alcohol successively, 60 ℃ of vacuum-drying 24 hours is prepared into micrometer structure zinc oxide.
2. the method for method for preparing micro structural zinc oxide by hydrothermal according to claim 1, it is characterized in that: described PVP K-30 and zinc acetate dihydrate, massfraction are 30% H
2O
2, distilled water, NaOH mass ratio be 1: 0.3658～10.98: 8.333～166.7: 466.7～625: 3.333～25, a preparation micron sea urchin shape zinc oxide.
3. the method for method for preparing micro structural zinc oxide by hydrothermal according to claim 2, it is characterized in that: described PVP K-30 and zinc acetate dihydrate, massfraction are 30% H
2O
2, distilled water, NaOH mass ratio be 1: 3.658: 41.67: 591.7: 6.667, be prepared into a micron sea urchin shape zinc oxide.
4. the method for method for preparing micro structural zinc oxide by hydrothermal according to claim 1, it is characterized in that: described PVP K-30 and zinc acetate dihydrate, massfraction are 30% H
2O
2, distilled water, NaOH mass ratio be 1: 18.29: 8.333～166.7: 466.7～625: 3.333～25, be prepared into a micron taper zinc oxide.
5. the method for method for preparing micro structural zinc oxide by hydrothermal according to claim 4, it is characterized in that: described PVP K-30 and zinc acetate dihydrate, massfraction are 30% H
2O
2, distilled water, NaOH mass ratio be 1: 18.29: 41.67: 591.7: 6.667, be prepared into a micron taper zinc oxide.
6. the method for method for preparing micro structural zinc oxide by hydrothermal according to claim 1, it is characterized in that: described PVP K-30 and zinc acetate dihydrate, massfraction are 30% H
2O
2, distilled water, NaOH mass ratio be 1: 29.27～36.58: 8.333～166.7: 466.7～625: 3.333～25, be prepared into the solid spherical zinc oxide of micron six prismatic self-assemblies.
7. the method for method for preparing micro structural zinc oxide by hydrothermal according to claim 6, it is characterized in that: described PVP K-30 and zinc acetate dihydrate, massfraction are 30% H
2O
2, distilled water, NaOH mass ratio be 1: 29.27: 41.67: 591.7: 6.667, be prepared into the solid spherical zinc oxide of micron six prismatic self-assemblies.
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| KR101358098B1 (en) | 2012-07-13 | 2014-02-05 | 재단법인 멀티스케일 에너지시스템 연구단 | 3-dimensional nanoparticle structure and gas sensor using same |
| CN104326504A (en) * | 2014-10-13 | 2015-02-04 | 李大枝 | Preparation method for urchin-like nanometer zinc oxide |
| CN104607194B (en) * | 2015-01-29 | 2017-04-05 | 陕西科技大学 | A kind of Hemicentrotus seu Strongylocentrotuss shape modified nano-ZnO photocatalyst and its preparation method and application |
| CN107359244B (en) * | 2016-12-20 | 2020-03-17 | 凯里学院 | Perovskite solar cell electronic transmission layer based on three-dimensional sea urchin-shaped ZnO superstructure array and preparation method and application thereof |
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| CN1245777A (en) * | 1999-09-08 | 2000-03-01 | 中国科学院广州化学研究所 | Preparation method of zinc oxide microparticles with specific form |
| CN1539741A (en) * | 2003-04-21 | 2004-10-27 | 中国科学院理化技术研究所 | Rod-shaped zinc oxide particles and its preparation method and use |
| US7491423B1 (en) * | 2005-05-02 | 2009-02-17 | Sandia Corporation | Directed spatial organization of zinc oxide nanostructures |
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| CN1245777A (en) * | 1999-09-08 | 2000-03-01 | 中国科学院广州化学研究所 | Preparation method of zinc oxide microparticles with specific form |
| CN1539741A (en) * | 2003-04-21 | 2004-10-27 | 中国科学院理化技术研究所 | Rod-shaped zinc oxide particles and its preparation method and use |
| US7491423B1 (en) * | 2005-05-02 | 2009-02-17 | Sandia Corporation | Directed spatial organization of zinc oxide nanostructures |
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