CN102381726A - Bell-shaped ZnO nanometer device material and preparation method thereof - Google Patents
Bell-shaped ZnO nanometer device material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a bell-shaped ZnO nanometer device material and a preparation method thereof. A new product is added for ZnO nanometer structural materials, and gaps of the prior art at home and abroad are filled. Soluble zinc salt, deionized water and hexamethylene tetramine are adopted as raw materials of the bell-shaped ZnO nanometer device material and mixed and dissolved to generate the bell-shaped ZnO nanometer device material by a one-step ultrasonic irradiation process, the bell-shaped ZnO nanometer device material is bell-shaped, a nanometer tube and a nanometer bar are automatically assembled to form the bell-shaped ZnO nanometer device material, the basic structure of the nanometer tube (a bell cover) is a six-prism-shaped tube, a tube opening of the nanometer tube is hexagonal, deformation shapes include a triangle and a diamond, and the nanometer bar (a bell tongue) is cylindrical. The bell-shaped nanometer structure is better in scattering property, two bells are connected locally to form a coaxial cable structure, and a plurality of bells are gathered together to form a trumpet-flower structure. The bell-shaped ZnO nanometer device material is novel in structure and can be applied to fields of medical antibiosis, photoelectric devices, gas sensors, solar batteries and the like.
Description
Technical field
The present invention relates to belong to the preparation field of semi-conductor photoelectronic nano material, specifically, relate to a kind of small bell shape ZnO nano material and preparation method thereof.
Background technology
Zinc oxide (ZnO) is as a kind of semiconductor material with wide forbidden band of direct band gap, its at room temperature energy gap be 3.37eV, and exciton bind energy is up to 60meV.The ZnO of nanoscale has light, electricity, magnetic, mechanics and the chemical property of a series of excellences, all is widely used in fields such as solar cell, photodiode, biosensor, photochemical catalysis, varistors.At present; At home and abroad under scholar's the unremitting effort; Various ZnO nano structural materials have been prepared; Orderly superstructure of two and three dimensions that assembles like nanometer rod, nano wire, nanotube, nano belt, nano-rings, nanometer ball, nano-comb with by a peacekeeping two-dimensional nanostructure unit etc., related preparation method mainly contains sputtering method, chemical Vapor deposition process, high temperature pyrolytic cracking (HTP), and the hot method of hydrothermal/solvent etc.But with regard to literature survey, Shang Weijian has the report of small bell shape nano structure of zinc oxide.
Summary of the invention
The object of the present invention is to provide a kind of small bell shape ZnO nano-device material and its preparation method, to fill up the blank of prior art, for the ZnO nano structural material adds new variety.
Small bell shape ZnO nano-device material provided by the invention is characterized in that said ZnO nano material is the small bell shape; Be the nano-device that is formed by nanotube and nanometer rod self-assembly, the substruction of nanotube (small bell cover) is the hexagon pipe, and the mouth of pipe is hexagon; Deformed shape has trilateral and rhombus; The about 8nm of tube thickness, nanometer rod (small bell tongue) is cylindrical, diameter is between 30～60nm.Small bell shape nanostructure is better dispersed, but there is clustering phenomena the part, has two small bells to link together and is coaxial cable structure, also has a plurality of small bells to flock together and is the trumpet flower structure.
Technical scheme of the present invention is to adopt a step ultrasound wave irradiation method to prepare small bell shape ZnO nano-device material; Promptly; With soluble zinc salt, deionized water and hexamethylenetetramine is raw material, after stirring and dissolving, gets precursor solution, and precursor solution is generated behind ultrasound wave irradiation.Its concrete process step is following:
(1) takes by weighing soluble zinc salts such as 1mmol zinc acetate and be mixed with solution A with deionized water;
(2) take by weighing a certain amount of hexamethylenetetramine and be mixed with solution B with deionized water, the mol ratio of zinc salt and hexamethylenetetramine is 1: 4～1: 6;
(3) under stirring state, solution A is joined in the solution B, form precursor solution C, overall solution volume is 60mL, continues to stir 10 minutes;
(4) precursor solution C is transferred in the screw thread bottle of sealing of 100mL, place the ultrasonic cleaner that fills 80 ± 10 ℃ of tap water, ultrasound wave irradiation 7～15 minutes, ultrasonic power are 50W;
(5) taking-up naturally cools to room temperature, filtering precipitate, and water and absolute ethanol washing are 2～3 times respectively;
(6) place baking oven to heat 6～12 hours throw out, temperature is 40～60 ℃, collects white products and promptly obtains small bell shape ZnO nano-device material of the present invention.
Soluble zinc salt in the said step (1) is zinc acetate, zinc nitrate etc.
The zinc salt in the said step (2) and the mol ratio of hexamethylenetetramine are 1: 5.
The ultrasound wave irradiation time in the said step (4) is 10 minutes.
The small bell shape ZnO nano-device material that the present invention obtains is a kind of ZnO nano material with novel structure, superior performance, is expected to obtain important application at numerous areas such as medicinal antibiosis, opto-electronic device, gas sensor and solar cells.Said preparation technology's equipment is simple, and envrionment temperature is low, and is easy and simple to handle, good reproducibility; Do not adopt organic solvent and tensio-active agent to do template, the environmental friendliness cleaning; With short production cycle, productive rate is high, raw material sources are extensive, and are with low cost, suitability for industrialized production.
Beneficial effect of the present invention is embodied in:
(1) the present invention has adopted under the normal temperature and pressure method without templet to prepare small bell shape ZnO nano-device material.
(2) the inventive method adopts the ultrasound wave irradiation technology, can improve the crystallization velocity of product on the one hand, and operation steps is simple on the other hand, is swift in response control easily, high-efficiency environment friendly.
Description of drawings
Fig. 1 is X-ray diffraction analysis (XRD) figure of the embodiment of the invention 1 small bell shape ZnO nano-device material;
Fig. 2 is low power field scan electron microscope (SEM) photo of the embodiment of the invention 1 small bell shape ZnO nano-device material;
Fig. 3 is high power field scan electron microscope (SEM) photo of the embodiment of the invention 1 small bell shape ZnO nano-device material.
Embodiment
Below technical scheme of the present invention is done the description of further detailed complete through concrete embodiment.Following embodiment further specifies of the present invention, and does not limit the scope of the invention.
Embodiment 1
The present invention adopts a step ultrasound wave irradiation method to prepare small bell shape ZnO nano-device material, that is, be raw material with soluble zinc salt, deionized water and hexamethylenetetramine, after stirring and dissolving, gets precursor solution, and precursor solution is generated behind ultrasound wave irradiation.Its concrete process step is following:
(1) takes by weighing the 0.2193g zinc acetate and be mixed with solution A with the 10mL deionized water;
(2) take by weighing the 0.6999g hexamethylenetetramine and be mixed with solution B with the 50mL deionized water, the mol ratio of zinc salt and hexamethylenetetramine is 1: 5;
(3) under stirring state, solution A is joined in the solution B, form precursor solution C, overall solution volume is 60mL, continues to stir 10 minutes;
(4) precursor solution C is transferred in the screw thread bottle of sealing of 100mL, place the ultrasonic cleaner that fills 80 ℃ of tap water, ultrasound wave irradiation 10 minutes, ultrasonic power are 50W;
(5) taking-up naturally cools to room temperature, filtering precipitate, and water and absolute ethanol washing are 2～3 times respectively;
(6) throw out is placed baking oven heating 8 hours, temperature is 60 ℃, collects white products and promptly obtains small bell shape ZnO nano-device material of the present invention.
Referring to accompanying drawing 1; X-ray diffraction (XRD) figure of the small bell shape ZnO nano-device material that makes by embodiment 1 described method; The spectral line peak position is corresponding one by one with (100), (002), (101), (102), (110), (103), (200), (112), (201) diffraction crystal face of JCPDF card (05-664) among the figure; Be the ZnO of hexagonal wurtzite structure, spacer P63mc.Diffraction peak is strong and sharp-pointed, does not have the dephasign peak, shows good crystallinity, the purity height of powder.
Referring to accompanying drawing 2 and Fig. 3, field scan Electronic Speculum (SEM) photo of the colour of skin ZnO porous nano club-shaped material that makes by embodiment 1 described method, visible ZnO nano material is the small bell shape; Be the nano-device that is formed by nanotube and nanometer rod self-assembly, the substruction of nanotube (small bell cover) is the hexagon pipe, and the mouth of pipe is hexagon; Deformed shape has trilateral and rhombus; The about 8nm of tube thickness, nanometer rod (small bell tongue) is cylindrical, diameter is between 30～60nm.Small bell shape nanostructure is better dispersed, but there is clustering phenomena the part, has two small bells to link together and is coaxial cable structure, also has a plurality of small bells to flock together and is the trumpet flower structure.
Embodiment 2
The present invention adopts a step ultrasound wave irradiation method to prepare small bell shape ZnO nano-device material, that is, be raw material with soluble zinc salt, deionized water and hexamethylenetetramine, after stirring and dissolving, gets precursor solution, and precursor solution is generated behind ultrasound wave irradiation.Its concrete process step is following:
(1) takes by weighing the 0.2195g zinc acetate and be mixed with solution A with the 10mL deionized water;
(2) take by weighing 0.700 2g hexamethylenetetramine and be mixed with solution B with the 50mL deionized water, the mol ratio of zinc salt and hexamethylenetetramine is 1: 5;
(3) under stirring state, solution A is joined in the solution B, form precursor solution C, overall solution volume is 60mL, continues to stir 10 minutes;
(4) precursor solution C is transferred in the screw thread bottle of sealing of 100mL, place the ultrasonic cleaner that fills 90 ℃ of tap water, ultrasound wave irradiation 7.5 minutes, ultrasonic power are 50W;
(5) taking-up naturally cools to room temperature, filtering precipitate, and water and absolute ethanol washing are 2～3 times respectively;
(6) throw out is placed baking oven heating 6 hours, temperature is 60 ℃, collects white products and promptly obtains small bell shape ZnO nano-device material of the present invention.
The small bell shape ZnO nano-device material that makes by embodiment 2 described methods is viewed as the nano-device that nanotube and nanometer rod self-assembly form with SEM, is small bell shape structure.
Embodiment 3
The present invention adopts a step ultrasound wave irradiation method to prepare small bell shape ZnO nano-device material, that is, be raw material with soluble zinc salt, deionized water and hexamethylenetetramine, after stirring and dissolving, gets precursor solution, and precursor solution is generated behind ultrasound wave irradiation.Its concrete process step is following:
(1) takes by weighing the 0.2192g zinc acetate and be mixed with solution A with the 10mL deionized water;
(2) take by weighing the 0.7001g hexamethylenetetramine and be mixed with solution B with the 50mL deionized water, the mol ratio of zinc salt and hexamethylenetetramine is 1: 5;
(3) under stirring state, solution A is joined in the solution B, form precursor solution C, overall solution volume is 60mL, continues to stir 10 minutes;
(4) precursor solution C is transferred in the screw thread bottle of sealing of 100mL, place the ultrasonic cleaner that fills 70 ℃ of tap water, ultrasound wave irradiation 12.5 minutes, ultrasonic power are 50W;
(5) taking-up naturally cools to room temperature, filtering precipitate, and water and absolute ethanol washing are 2～3 times respectively;
(6) throw out is placed baking oven heating 12 hours, temperature is 60 ℃, collects white products and promptly obtains small bell shape ZnO nano-device material of the present invention.
The small bell shape ZnO nano-device material that makes by embodiment 3 described methods is viewed as the nano-device that nanotube and nanometer rod self-assembly form with SEM, is small bell shape structure.
Embodiment 4
The present invention adopts a step ultrasound wave irradiation method to prepare small bell shape ZnO nano-device material, that is, be raw material with soluble zinc salt, deionized water and hexamethylenetetramine, after stirring and dissolving, gets precursor solution, and precursor solution is generated behind ultrasound wave irradiation.Its concrete process step is following:
(1) takes by weighing the 0.2906g zinc nitrate and be mixed with solution A with the 10mL deionized water;
(2) take by weighing the 0.6998g hexamethylenetetramine and be mixed with solution B with the 50mL deionized water, the mol ratio of zinc salt and hexamethylenetetramine is 1: 5;
(3) under stirring state, solution A is joined in the solution B, form precursor solution C, overall solution volume is 60mL, continues to stir 10 minutes;
(4) precursor solution C is transferred in the screw thread bottle of sealing of 100mL, place the ultrasonic cleaner that fills 80 ℃ of tap water, ultrasound wave irradiation 10 minutes, ultrasonic power are 50W;
(5) taking-up naturally cools to room temperature, filtering precipitate, and water and absolute ethanol washing are 2～3 times respectively;
(6) throw out is placed baking oven heating 8 hours, temperature is 60 ℃, collects white products and promptly obtains small bell shape ZnO nano-device material of the present invention.
The small bell shape ZnO nano-device material that makes by embodiment 4 described methods is viewed as the small bell shape structure nano device that nanotube and nanometer rod self-assembly form with SEM.
Claims (5)
1. a small bell shape ZnO nano-device material is characterized in that said ZnO nano material is the small bell shape; Be the nano-device that is formed by nanotube and nanometer rod self-assembly, the substruction of nanotube (small bell cover) is the hexagon pipe, and the mouth of pipe is hexagon; Deformed shape has trilateral and rhombus; The about 8nm of tube thickness, nanometer rod (small bell tongue) is cylindrical, diameter is between 30～60nm.Small bell shape nanostructure is better dispersed, but there is clustering phenomena the part, has two small bells to link together and is coaxial cable structure, also has a plurality of small bells to flock together and is the trumpet flower structure.
2. the described small bell shape of claim 1 ZnO nano-device preparation methods is characterized in that said method comprises following concrete steps:
(1) takes by weighing soluble zinc salts such as 1mmol zinc acetate and be mixed with solution A with deionized water;
(2) take by weighing a certain amount of hexamethylenetetramine and be mixed with solution B with deionized water, the mol ratio of zinc salt and hexamethylenetetramine is 1: 4～1: 6;
(3) under stirring state, solution A is joined in the solution B, form precursor solution C, overall solution volume is 60mL, continues to stir 10 minutes;
(4) precursor solution C is transferred in the screw thread bottle of sealing of 100mL, place the ultrasonic cleaner that fills 80 ± 10 ℃ of tap water, ultrasound wave irradiation 7～15 minutes, ultrasonic power are 50W;
(5) taking-up naturally cools to room temperature, filtering precipitate, and water and absolute ethanol washing are 2～3 times respectively;
(6) place baking oven to heat 6～12 hours throw out, temperature is 40～60 ℃, collects white products and promptly obtains small bell shape ZnO nano-device material of the present invention.
3. small bell shape ZnO nano-device preparation methods according to claim 2 is characterized in that: soluble zinc salt is zinc acetate, zinc nitrate etc. in the step (1).
4. small bell shape ZnO nano-device preparation methods according to claim 2, it is characterized in that: in the step (2), the mol ratio of zinc salt and hexamethylenetetramine is 1: 5.
5. small bell shape ZnO nano-device preparation methods according to claim 2, it is characterized in that: in the step (4), the ultrasound wave irradiation time is 10 minutes, and the ultrasound bath temperature is 80 ℃.
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Cited By (6)
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|---|---|---|---|---|
| CN102872851A (en) * | 2012-10-10 | 2013-01-16 | 常州大学 | Preparation method of zinc oxide/attapulgite composite photocatalytic material |
| GB2495074A (en) * | 2011-09-12 | 2013-04-03 | Univ Swansea | ZnO nanomaterials and gas sensors made using the nanomaterials |
| 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 |
| CN103930364A (en) * | 2012-07-13 | 2014-07-16 | 首尔大学校产学协力团 | Optical element using three-dimensional structure assembled with nanoparticles |
| CN105498745A (en) * | 2015-12-15 | 2016-04-20 | 金陵科技学院 | Nano acanthosphere-shaped zinc oxide photocatalyst and preparation method thereof |
| CN106006706A (en) * | 2016-05-19 | 2016-10-12 | 青岛大学 | Preparation method of dumbbell-shaped ZnO micro-ring gas-sensitive material |
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| JP2008162885A (en) * | 2007-01-03 | 2008-07-17 | Samsung Electronics Co Ltd | Method for manufacturing zinc oxide nanowire by using ultrasonic energy |
| CN101407334A (en) * | 2007-10-12 | 2009-04-15 | 新疆大学 | Method for synthesizing rod-like nano-zinc oxide |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2495074A (en) * | 2011-09-12 | 2013-04-03 | Univ Swansea | ZnO nanomaterials and gas sensors made using the nanomaterials |
| 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 |
| CN103930364A (en) * | 2012-07-13 | 2014-07-16 | 首尔大学校产学协力团 | Optical element using three-dimensional structure assembled with nanoparticles |
| CN103781723B (en) * | 2012-07-13 | 2015-12-02 | 首尔大学校产学协力团 | 3D nanoparticle collecting structure body and use its gas sensor |
| CN103930364B (en) * | 2012-07-13 | 2015-12-09 | 首尔大学校产学协力团 | Adopt the Optical devices of 3D nanoparticle structure |
| US9222190B2 (en) | 2012-07-13 | 2015-12-29 | Snu R&Db Foundation | 3-dimensional nanoparticle assembly structure and gas sensor using same |
| CN102872851A (en) * | 2012-10-10 | 2013-01-16 | 常州大学 | Preparation method of zinc oxide/attapulgite composite photocatalytic material |
| CN105498745A (en) * | 2015-12-15 | 2016-04-20 | 金陵科技学院 | Nano acanthosphere-shaped zinc oxide photocatalyst and preparation method thereof |
| CN106006706A (en) * | 2016-05-19 | 2016-10-12 | 青岛大学 | Preparation method of dumbbell-shaped ZnO micro-ring gas-sensitive material |
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Application publication date: 20120321 |