CN102134091A - Method for preparing micro structural zinc oxide by hydrothermal method - Google Patents
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- CN102134091A CN102134091A CN 201110024679 CN201110024679A CN102134091A CN 102134091 A CN102134091 A CN 102134091A CN 201110024679 CN201110024679 CN 201110024679 CN 201110024679 A CN201110024679 A CN 201110024679A CN 102134091 A CN102134091 A CN 102134091A
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Abstract
The invention discloses a method for preparing micro structural zinc oxide by a hydrothermal method. Polyvinyl pyrrolidone K-30 is used as a template, zinc acetate dihydrate is used as a zinc source, and H2O2 is used as an oxidant; and a zinc oxide material with four micro structures of sea urchin shape, taper, hexagonal prism self-assembled solid sphere and sugarcoated haw shape is prepared by controlling the reactant concentration, the hydrothermal growth time and the reaction temperature. The method is simple and has the advantages of low cost, mild condition, no environmental pollution and the like. The prepared micro zinc oxide material has high purity, regular crystal structure, good shape controllability and short production period, and has huge application prospect on the aspects of 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 four kinds of special appearance zinc oxide of emulsion assisting alcohol-hydrothermal method preparation.
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 excellent in chemical characteristic, 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, 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 vapor deposition (CVD) etc.Yet in the preparation process of micron zinc oxide material, ubiquity 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 controllable size, crystalline structure is regular, monodispersity is good micrometer structure zinc oxide.
Solving the problems of the technologies described above the technical scheme that adopts is: be 30% H with mass fraction
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, mass fraction 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, treat to continue to stir 5 minutes after solution produces white opacity, white opacity solution is poured in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), 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, absolute ethyl alcohol successively, 60 ℃ of vacuum drying 24 hours are prepared into micrometer structure zinc oxide.
In the inventive method, PVP K-30 and zinc acetate dihydrate, mass fraction 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, mass fraction 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, mass fraction 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, mass fraction 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, mass fraction 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 medicine ball 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, mass fraction 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, mass fraction 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 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, mass fraction 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 Preparation to become 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 great application prospect arranged.
Description of drawings
Fig. 1 is the sem photograph of the micron sea urchin shape zinc oxide of the embodiment of the invention 1 preparation.
Fig. 2 is the sem photograph of the micron sea urchin shape zinc oxide of the embodiment of the invention 2 preparations.
Fig. 3 is the sem photograph of the micron sea urchin shape zinc oxide of the embodiment of the invention 3 preparations.
Fig. 4 is the sem photograph of the micron taper zinc oxide of the embodiment of the invention 4 preparations.
Fig. 5 is the sem photograph of the micron taper zinc oxide of the embodiment of the invention 5 preparations.
Fig. 6 is the sem photograph of the micron taper zinc oxide of the embodiment of the invention 6 preparations.
Fig. 7 is the 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 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 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 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 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 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 mass fraction
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, mass fraction are 30% H
2O
2, distilled water, NaOH mass ratio be 1: 3.658: 41.67: 591.7: 6.667, stirring at room, treat to continue to stir 5 minutes after solution produces white opacity, white opacity solution is poured in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), 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, absolute ethyl 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 mass fraction
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, mass fraction 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 mass fraction
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, mass fraction 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 mass fraction
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, mass fraction are 30% H
2O
2, distilled water, NaOH mass ratio be 1: 18.29: 41.67: 591.7: 6.667, stirring at room, treat to continue to stir 5 minutes after solution produces white opacity, white opacity solution is poured in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), 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, absolute ethyl 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 awl is that 15～30 μ m, diameter are 0.5～1 μ m.
Embodiment 5
In embodiment 4, be 30% H with mass fraction
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, mass fraction 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 awl is that 50～80 μ m, diameter are 5～10 μ m.
Embodiment 6
In embodiment 4, be 30% H with mass fraction
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, mass fraction 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 awl 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 mass fraction
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, mass fraction are 30% H
20
2, distilled water, Na0H mass ratio be 1: 29.27: 41.67: 591.7: 6.667, stirring at room, treat to continue to stir 5 minutes after solution produces white opacity, white opacity solution is poured in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), 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, absolute ethyl 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 six prismatical length are that 40～60 μ m, diameter are 3～5 μ m.
Embodiment 8
In embodiment 7, be 30% H with mass fraction
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, mass fraction 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 six prismatical length are that 40～50 μ m, diameter are 3～4 μ m.
Embodiment 9
In embodiment 7, be 30% H with mass fraction
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, mass fraction 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 six prismatical length are that 45～55 μ m, diameter are 2～4 μ m.
Embodiment 10
Take preparation micron sugarcoated haws shape zinc oxide material as example, its concrete preparation method is as follows:
Be 30% H with mass fraction
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, mass fraction are 30% H
2O
2, distilled water, NaOH mass ratio be 1: 3.658: 41.67: 616.7: 1.667, stirring at room, treat to continue to stir 5 minutes after solution produces white opacity, white opacity solution is poured in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), 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, absolute ethyl 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 awl is that 10～20 μ m, diameter are 0.5～1.5 μ m.
Embodiment 11
In embodiment 10, be 30% H with mass fraction
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, mass fraction 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 awl is that 20～30 μ m, diameter are 2～5 μ m.
Embodiment 12
In embodiment 10, be 30% H with mass fraction
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, mass fraction 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 awl 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 a 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 a 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 (9)
1. method for preparing micro structural zinc oxide by hydrothermal is characterized in that: be 30% H with mass fraction
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, mass fraction 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, treat to continue to stir 5 minutes after solution produces white opacity, white opacity solution is poured in the hydrothermal reaction kettle that liner is polytetrafluoroethylene (PTFE), 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, absolute ethyl alcohol successively, 60 ℃ of vacuum drying 24 hours are prepared into micrometer structure zinc oxide.
2. 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, mass fraction 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. 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, mass fraction 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. 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, mass fraction 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. 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, mass fraction 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. 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, mass fraction 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. 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, mass fraction 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.
8. 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, mass fraction 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 shape zinc oxide.
9. method for preparing micro structural zinc oxide by hydrothermal according to claim 8, it is characterized in that: described PVP K-30 and zinc acetate dihydrate, mass fraction are 30% H
2O
2, distilled water, NaOH mass ratio be 1: 3.658: 41.67: 616.7: 1.667, be prepared into a micron sugarcoated haws shape zinc oxide.
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| CN102912436A (en) * | 2011-08-05 | 2013-02-06 | 国家纳米科学中心 | Preparation method of conical zinc oxide sub-micron rods and array thereof |
| CN103781723A (en) * | 2012-07-13 | 2014-05-07 | 首尔大学校产学协力团 | Three-dimensional nanoparticle assembly 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 |
| CN104607194A (en) * | 2015-01-29 | 2015-05-13 | 陕西科技大学 | Sea urchin-shaped modified nanometer ZnO photocatalyst as well as preparation method and application of photocatalyst |
| CN106252455A (en) * | 2016-09-13 | 2016-12-21 | 复旦大学 | A kind of self-driven Se/ZnO heterojunction ultraviolet photodetector and preparation method thereof |
| CN107359244A (en) * | 2016-12-20 | 2017-11-17 | 凯里学院 | Perovskite solar cell electron transfer layer based on three-dimensional sea urchin shape ZnO superstructure arrays and its preparation method and application |
| CN109364927A (en) * | 2018-11-26 | 2019-02-22 | 中国华能集团清洁能源技术研究院有限公司 | A kind of preparation method of prism-shaped copper oxide-zinc oxide catalyst |
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