CN102259906A - Method for preparing hollow zinc oxide microspheres - Google Patents
Method for preparing hollow zinc oxide microspheres Download PDFInfo
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- CN102259906A CN102259906A CN2011101480873A CN201110148087A CN102259906A CN 102259906 A CN102259906 A CN 102259906A CN 2011101480873 A CN2011101480873 A CN 2011101480873A CN 201110148087 A CN201110148087 A CN 201110148087A CN 102259906 A CN102259906 A CN 102259906A
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- zinc oxide
- hollow zinc
- ball
- hollow
- oxide microspheres
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Abstract
The invention relates to a method for preparing hollow zinc oxide microspheres, which is characterized by comprising the following steps of: adding saccharose into deionized water to obtain a transparent solution; transferring the transparent solution into a high pressure hydrothermal kettle with a polytetrafluoroethylene liner to obtain monodisperse carbon balls; adding Zn(AC)2.2H2O, performing ultrasonic treatment, and drying to obtain precursors of the hollow zinc oxide spheres; and calcining the precursors of the zinc oxide microspheres to obtain the hollow zinc oxide microspheres. In the method for preparing the hollow zinc oxide microspheres with high gas selectivity and high sensitivity, the carbon balls are taken as templates, and the hollow zinc oxide spheres with hierarchical structures are synthesized by an ultrasonic method have high H2S gas selectivity and high sensitivity and can serve as a H2S gas sensor.
Description
Technical field
The present invention relates to a kind of preparation method of hollow zinc oxide micrometer ball, is a kind of preparation method with specified shape zinc oxide, has the hollow zinc oxide sphere preparation of nanomaterials of hierarchy.This hollow zinc oxide sphere is to H
2S gas has higher selectivity and sensitivity.
Background technology
Zinc oxide is a kind of wide bandgap semiconductor oxide compound, its fusing point is 1973 ℃, with respect to other oxide compound, fusing point is higher, aerial better heat stability, have outstanding multi-functional characteristic, can be widely used in fields such as gas sensitive, anti-biotic material, catalytic material, the application aspect transmitter has better heat stability, advantage such as with low cost.Hollow ball-shape ZnO is owing to have bigger specific surface area and more gas adsorption center can be provided, and it has air-sensitive performance preferably, is suitable as gas sensitive.
A synthetic research focus that becomes in recent years of relevant hollow zinc oxide sphere adopts the high pressure solvent thermal to prepare the hollow zinc oxide micrometer ball of being assembled by the flake nano structure such as patent 200910113125.4.Although the Zinc oxide hollow spheres of this method preparation has big specific surface area and good dispersiveness, in preparation process, adopt solvent thermal, cause the preparation process complexity, cost is higher, and solvent for use pollutes environment easily simultaneously.And we adopt colloidal carbon sphere as template, and it is simple to utilize the sonochemistry intermediate processing to prepare hollow zinc oxide sphere method, the productive rate height, and cost is low, and the solvent of employing is a water, can not pollute environment.
Summary of the invention
The technical problem that solves
For fear of the deficiencies in the prior art part, the present invention proposes a kind of preparation method of hollow zinc oxide micrometer ball.
Technical scheme
A kind of preparation method of hollow zinc oxide micrometer ball is characterized in that step is as follows:
Step 1: 2～10g sucrose joined in 20～50ml deionized water form clear solution;
Step 2: clear solution is transferred in the high pressure water heating kettle that liner is a polytetrafluoroethylliner liner, prepared single dispersed carbon ball at 120～200 ℃ of reaction 3～5h;
Step 3: the Zn (AC) that in the above-mentioned aqueous solution that contains the charcoal ball, adds 1～3g
22H
2O behind supersound process 1～3h, through centrifugal, washing, obtains the precursor of Zinc oxide hollow spheres after the drying in vacuum drying oven;
Step 4: precursor 300～800 ℃ of calcinings under air conditions were obtained hollow zinc oxide micrometer ball in 1.5～4 hours.
Beneficial effect
The preparation method of a kind of hollow zinc oxide micrometer ball that the present invention proposes, preparation method with good gas selectivity, highly sensitive hollow zinc oxide micrometer ball, present method utilizes the carbon ball to be template, adopts the synthetic hollow zinc oxide sphere with hierarchy of ultrasonic method, and they are to H
2S gas has higher selectivity and sensitivity, can be H
2The S gas sensor.
Description of drawings
Fig. 1 executes the stereoscan photograph and the XRD figure spectrum of prepared hollow zinc oxide micrometer ball in the example 1 for the present invention
A: stereoscan photograph; The b:XRD collection of illustrative plates
Fig. 2 executes the stereoscan photograph and the XRD figure spectrum of prepared hollow zinc oxide micrometer ball in the example 2 for the present invention
A: stereoscan photograph; The b:XRD collection of illustrative plates
Embodiment
Now in conjunction with the embodiments, accompanying drawing is further described the present invention:
Embodiment 1:
With quality be 6g sucrose (molecular formula is C
12H
22O
11) be dissolved into the transparent solution of formation in the 44mL deionized water, then it is transferred in the polytetrafluoroethyllining lining water heating kettle that volume is 56mL, in constant temperature oven, be incubated 4h under 180 ℃ of conditions, treat that water heating kettle naturally cools to room temperature, collection deposits to the black product of container bottom, centrifuge washing obtains single dispersed carbon ball with product vacuum-drying 2h under 80 ℃ of conditions then.
With quality is 1.3483g Zn (AC)
22H
2O is dissolved in the 40mL deionized water, is continuing to add carbon ball and the continuation stirring 30min that quality is 0.15g under the stirring condition on the magnetic stirring apparatus in solution then.It is 40kHz that the beaker that this solution will be housed is then put frequency into, and output rating is ultrasonic reaction 3h in the 90-W Vltrasonic device.Collect beaker bottom gained grey black look sedimentation products, centrifugation, washing.Presoma can be obtained hollow zinc oxide micrometer ball at 600 ℃ of calcining 2h under air conditions.
Embodiment 2:
With quality be 5g sucrose (molecular formula is C
12H
22O
11) be dissolved into the transparent solution of formation in the 40mL deionized water, then it is transferred in the polytetrafluoroethyllining lining water heating kettle that volume is 56mL, in constant temperature oven, be incubated 4h under 160 ℃ of conditions, treat that water heating kettle naturally cools to room temperature, collection deposits to the black product of container bottom, centrifuge washing obtains single dispersed carbon ball with product vacuum-drying 2h under 80 ℃ of conditions then.
With quality is 1.200g Zn (AC)
22H
2O is dissolved in the 35mL deionized water, is continuing to add carbon ball and the continuation stirring 30min that quality is 0.10g under the stirring condition on the magnetic stirring apparatus in solution then.It is 40kHz that the beaker that this solution will be housed is then put frequency into, and output rating is ultrasonic reaction 1.5h in the 90-W Vltrasonic device.Collect beaker bottom gained grey black look sedimentation products, centrifugation, washing.Presoma can be obtained hollow zinc oxide micrometer ball at 500 ℃ of calcining 2h under air conditions.
Embodiment 3:
With quality be 6g sucrose (molecular formula is C
12H
22O
11) be dissolved into the transparent solution of formation in the 44mL deionized water, then it is transferred in the polytetrafluoroethyllining lining water heating kettle that volume is 56mL, in constant temperature oven, be incubated 5h under 160 ℃ of conditions, treat that water heating kettle naturally cools to room temperature, collection deposits to the black product of container bottom, centrifuge washing obtains single dispersed carbon ball with product vacuum-drying 3h under 60 ℃ of conditions then.
With quality is 1.3483g Zn (AC)
22H
2O is dissolved in the 40mL deionized water, is continuing to add carbon ball and the continuation stirring 30min that quality is 0.15g under the stirring condition on the magnetic stirring apparatus in solution then.It is 40kHz that the beaker that this solution will be housed is then put frequency into, and output rating is ultrasonic reaction 3h in the 90-W Vltrasonic device.Collect beaker bottom gained grey black look sedimentation products, centrifugation, washing.Presoma can be obtained hollow zinc oxide micrometer ball at 600 ℃ of calcining 3h under air conditions.
Claims (1)
1. the preparation method of a hollow zinc oxide micrometer ball is characterized in that step is as follows:
Step 1: 2～10g sucrose joined in 20～50ml deionized water form clear solution;
Step 2: clear solution is transferred in the high pressure water heating kettle that liner is a polytetrafluoroethylliner liner, prepared single dispersed carbon ball at 120～200 ℃ of reaction 3～5h;
Step 3: the Zn (AC) that in the above-mentioned aqueous solution that contains the charcoal ball, adds 1～3g
22H
2O behind supersound process 1～3h, through centrifugal, washing, obtains the precursor of Zinc oxide hollow spheres after the drying in vacuum drying oven;
Step 4: precursor 300～800 ℃ of calcinings under air conditions were obtained hollow zinc oxide micrometer ball in 1.5～4 hours.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102543456A (en) * | 2011-12-23 | 2012-07-04 | 中国科学院过程工程研究所 | Zinc oxide membrane electrode material for dye sensitized solar cell and preparation method thereof |
| CN106000126A (en) * | 2016-06-29 | 2016-10-12 | 浙江工业大学 | Antibacterial film based on nano zinc oxide as well as preparation method and application thereof |
| CN106732513A (en) * | 2016-11-24 | 2017-05-31 | 河南师范大学 | Zinc oxide visible light catalytic material with hollow structure and preparation method thereof |
| CN107958995A (en) * | 2017-12-22 | 2018-04-24 | 湖南工业大学 | A kind of dried persimmon shape core shell structure C/ZnO lithium-ion negative pole electrode piece preparation methods and its fastening lithium ionic cell |
| CN108054372A (en) * | 2017-12-22 | 2018-05-18 | 湖南工业大学 | A kind of dried persimmon shape nucleocapsid C/ZnO lithium ion battery negative materials and preparation method thereof |
| CN108408761A (en) * | 2018-05-21 | 2018-08-17 | 西南科技大学 | The controllable method for preparing of three-dimensional honeycomb structure ZnO nano material |
| CN108715730A (en) * | 2018-05-28 | 2018-10-30 | 界首市金龙机械设备有限公司 | A kind of novel environment friendly decontamination paint and preparation method thereof |
| CN108948719A (en) * | 2018-06-12 | 2018-12-07 | 安徽喜宝高分子材料有限公司 | A kind of heat-insulated counnter attack optical thin film of instrument desk and preparation method thereof |
| CN109675553A (en) * | 2018-12-21 | 2019-04-26 | 鲁东大学 | A kind of preparation method of silver tiny balloon photochemical catalyst |
| CN110498440A (en) * | 2019-07-11 | 2019-11-26 | 江苏大学 | A kind of zinc oxide air-sensitive membrane material, preparation method and applications |
| CN115367787A (en) * | 2022-09-19 | 2022-11-22 | 中国民航大学 | Synthesis method of zinc metastannate gas-sensitive material with hollow structure |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101066776A (en) * | 2007-06-05 | 2007-11-07 | 武汉理工大学 | Zinc oxide synthesizing process |
| CN101948130A (en) * | 2010-10-11 | 2011-01-19 | 厦门大学 | Zinc oxide hollow microspheres and preparation method thereof |
-
2011
- 2011-06-02 CN CN2011101480873A patent/CN102259906A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101066776A (en) * | 2007-06-05 | 2007-11-07 | 武汉理工大学 | Zinc oxide synthesizing process |
| CN101948130A (en) * | 2010-10-11 | 2011-01-19 | 厦门大学 | Zinc oxide hollow microspheres and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| XIAOHUA JIA, ET AL.: "Using sonochemistry for the fabrication of hollow ZnO microspheres", 《ULTRASONICS SONOCHEMISTRY》, vol. 17, 26 September 2009 (2009-09-26) * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102543456A (en) * | 2011-12-23 | 2012-07-04 | 中国科学院过程工程研究所 | Zinc oxide membrane electrode material for dye sensitized solar cell and preparation method thereof |
| CN106000126A (en) * | 2016-06-29 | 2016-10-12 | 浙江工业大学 | Antibacterial film based on nano zinc oxide as well as preparation method and application thereof |
| CN106732513A (en) * | 2016-11-24 | 2017-05-31 | 河南师范大学 | Zinc oxide visible light catalytic material with hollow structure and preparation method thereof |
| CN107958995A (en) * | 2017-12-22 | 2018-04-24 | 湖南工业大学 | A kind of dried persimmon shape core shell structure C/ZnO lithium-ion negative pole electrode piece preparation methods and its fastening lithium ionic cell |
| CN108054372A (en) * | 2017-12-22 | 2018-05-18 | 湖南工业大学 | A kind of dried persimmon shape nucleocapsid C/ZnO lithium ion battery negative materials and preparation method thereof |
| CN108408761A (en) * | 2018-05-21 | 2018-08-17 | 西南科技大学 | The controllable method for preparing of three-dimensional honeycomb structure ZnO nano material |
| CN108715730A (en) * | 2018-05-28 | 2018-10-30 | 界首市金龙机械设备有限公司 | A kind of novel environment friendly decontamination paint and preparation method thereof |
| CN108948719A (en) * | 2018-06-12 | 2018-12-07 | 安徽喜宝高分子材料有限公司 | A kind of heat-insulated counnter attack optical thin film of instrument desk and preparation method thereof |
| CN109675553A (en) * | 2018-12-21 | 2019-04-26 | 鲁东大学 | A kind of preparation method of silver tiny balloon photochemical catalyst |
| CN110498440A (en) * | 2019-07-11 | 2019-11-26 | 江苏大学 | A kind of zinc oxide air-sensitive membrane material, preparation method and applications |
| CN115367787A (en) * | 2022-09-19 | 2022-11-22 | 中国民航大学 | Synthesis method of zinc metastannate gas-sensitive material with hollow structure |
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Application publication date: 20111130 |