CN107460514A - A kind of simple method for preparing zinc oxide nano popped rice - Google Patents
A kind of simple method for preparing zinc oxide nano popped rice Download PDFInfo
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- CN107460514A CN107460514A CN201710499190.XA CN201710499190A CN107460514A CN 107460514 A CN107460514 A CN 107460514A CN 201710499190 A CN201710499190 A CN 201710499190A CN 107460514 A CN107460514 A CN 107460514A
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- China
- Prior art keywords
- zinc oxide
- oxide nano
- popped rice
- zinc
- nano popped
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
- C25D9/08—Electrolytic coating other than with metals with inorganic materials by cathodic processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The present invention discloses a kind of simple method for preparing zinc oxide nano popped rice, belongs to field of nano material preparation, comprises the following steps：(1) substrate cleaning treatment；(2) preparation of liquid is deposited；(3) electrochemical deposition zinc oxide；(4) cleaning, drying product.The present invention is prepared using electrochemical deposition method, using zinc chloride, citric acid and potassium chloride as deposition liquid, then prepares zinc-oxide nano flower-like structure under the sedimentary condition of heating and constant potential.Compared to other preparation methods, present invention process is simple, cost is low, easy to operate, and quick 5min, controllability is good and pollution-free, and the supplementary instrument complicated without template etc., is suitable for being prepared on a large scale zinc-oxide nano floral structure.
Description
Technical field
The invention belongs to the technical field of novel nano-material preparation method, more particularly to one kind simply to prepare zinc oxide nano
The method of popped rice.
Background technology
A kind of II-VI group semiconductor (Eg=3.37eV) of the nano-ZnO as broad stopband, with its distinctive bulk effect,
Skin effect, quantum size effect and tunnel-effect, and its distinctive novel performance (such as piezo-electric effect and photocatalysis property),
It is set to have very big application prospect in fields such as optics, electricity, materialogy and biomedicines.Due to structure and morphology and material
Performance and application are closely related, and therefore, the control of ZnO nano material pattern is always the focus in the investigation of materials field.
Wherein, turn into one of study hotspot in the field in recent years for the ZnO preparation methods of different-shape structure, compare
Common preparation method has vapor growth method, hydro-thermal method, thermal evaporation, template, metal oxide vapor phase deposition method, electrochemistry
Sedimentation etc..The pattern that distinct methods prepare ZnO nano material is each variant, explores the preparation method of new nanostructured, still
It is so one of target of Material Field research.
Although above-mentioned preparation method has its advantage, these methods usually require instrument and technology, the preparation of auxiliary
Step is complicated, it is difficult to is widely used in the application for requiring inexpensive, efficient nano photoelectric device；In addition, these
Preparation method complex process, energy consumption are big, synthesis condition is harsh and are difficult to large-scale production, seriously limit ZnO nano
The application of brilliant material in the opto-electronic device.But the existing most severe reaction conditions of preparation method, production cost is high, does not apply to
In large-scale industrial production.
Therefore, the preparation method for exploring the ZnO nano-structure for developing new relative ease is still necessary.The present invention adopts
With relatively simple electrochemical deposition technique, it may not be necessary to complicated step and supplementary instrument in other preparation methods, so as to
Further simplify operating procedure, the present invention has the characteristics of simple and practical, for it is extensive it is quick, prepare efficiently at low cost
ZnO nano-structure provides new scheme.
The content of the invention
The purpose of the present invention is to provide a kind of simple preparation quick, program is easy, preparation cost is low regarding to the issue above
The method of zinc oxide nano popped rice.
The technical scheme is that：A kind of simple method for preparing zinc oxide nano popped rice, is realized by following steps：
(1) substrate cleaning treatment；(2) preparation of liquid is deposited；(3) electrochemical deposition zinc oxide；(4) cleaning, drying product.
(1) substrate cleaning treatment：Before deposition, substrate pure copper foil is passed through in certain density hydrochloric acid, deionized water, third respectively
It is cleaned by ultrasonic in ketone, deionized water.
(2) preparation of liquid is deposited：Zinc salt is dissolved in 100ml deionized water, adds sylvite and citric acid by certain
Mixed in molar ratio, by mixed liquor stir 10min after, it is stand-by.
(3) electrochemical deposition：Using graphite and pure copper foil as working electrode, with the mixed of zinc chloride, citric acid and potassium chloride
The deposition liquid that liquid is spent as growth of zinc oxide nano is closed, certain time is deposited under conditions of certain temperature and constant potential.
(4) cleaning, drying product：The substrate pure copper foil deionized water rinsing of developing zinc oxide is taken out, is placed in one in baking oven
Determine to dry certain time at temperature, finally obtain dry nanometer flower structure zinc oxide.
It is clear to carry out ultrasound in 0.1M hydrochloric acid, deionized water, acetone, deionized water respectively for substrate pure copper foil in step (1)
Wash 10min.
The mol ratio of zinc salt and sylvite is 2.5-1 in step (2), and the mol ratio of the citric acid and sylvite is 0.1-1, shape
The deposition liquid spent into the growth of zinc oxide nano of certain mol proportion；
In step (3) sedimentary condition be heating-up temperature be 90 DEG C, constant potential is 1.5V and sedimentation time is 5min.
The substrate pure copper foil deionized water rinsing of developing zinc oxide 3 times in step (4), it is placed in 100 DEG C of drying in baking oven
15min。
The structure of described zinc oxide nano popped rice is obtained after drying.As can be seen that the present invention is implemented from Fig. 1 and Fig. 2
The electrochemical deposition method that example provides can obtain zinc-oxide nano floral structure.
Compared with prior art, the present invention using electrochemical deposition method prepare, using zinc chloride, citric acid and potassium chloride as
Liquid is deposited, then prepares zinc-oxide nano flower-like structure under the sedimentary condition of heating and constant potential.Compared to other preparation methods, sheet
Invention novelty is simple, each step process is simple, cost is low, easy to operate, and quick (5min), controllability is good and pollution-free, and
And the supplementary instrument complicated without template etc., it is suitable for being prepared on a large scale zinc-oxide nano floral structure, there is good application and hair
Exhibition prospect.Prepared zinc-oxide nano floral structure is expected to be applied in fields such as novel nano photoelectric devices.
Brief description of the drawings
Fig. 1 is the low power scanning electron for the nanometer flower structure zinc oxide that the method for implementing to provide according to the present invention is prepared
Microphotograph (scale is 10 μm).
Fig. 2 is the high power scanning electron for the nanometer flower structure zinc oxide that the method for implementing to provide according to the present invention is prepared
Microphotograph (scale is 1 μm).
Embodiment
The implementation to the present invention elaborates below in conjunction with the accompanying drawings：This implementation is with the technical scheme is that premise
Under implemented, for illustrating the present invention, give detailed embodiment and specific operating process, but the protection of the present invention
Scope is not limited to following implementation.
M in the embodiment is mol/L.
The simple method for preparing zinc oxide nano popped rice of the present invention, specific preparation process are as follows；
Step (1) substrate cleaning treatment：Before deposition, substrate pure copper foil is individually placed to 0.1M hydrochloric acid, deionized water, third
Ultrasonic cleaning 10min is carried out in ketone, deionized water, is dried up with nitrogen, it is stand-by.
Step (2) deposits the preparation of liquid：By zinc salt, sylvite and citric acid according to 2.5:1:0.1 mol ratio is dissolved in
Mixed in 100ml deionized water, and by mixed liquor stir 10min after, it is stand-by.
Step (3) electrochemical deposition：Using graphite and pure copper foil as working electrode, with above-mentioned zinc chloride, citric acid and chlorine
Change the deposition liquid that the mixed liquor of potassium is spent as growth of zinc oxide nano, it is heated under conditions of 90 DEG C, electrochemistry is set
Constant potential is 1.5V, after sedimentation time is 5min, can in pure copper foil deposition growing zinc oxide nano popped rice.
Step (4) cleaning, drying product：After the substrate pure copper foil for taking out developing zinc oxide, 3 are rinsed with deionized water
After secondary, it be placed in baking oven and 15min is dried at 100 DEG C, finally obtains the zinc oxide of dry nanometer flower structure.
As can be seen that electrochemical deposition method provided in an embodiment of the present invention can obtain zinc-oxide nano from Fig. 1 and Fig. 2
Floral structure.The inventive method is novel simple than existing other methods for preparing nano structure of zinc oxide, each step process letter
It is single, without the instrument and template of complexity, thus there are good application and development prospect.Prepared zinc-oxide nano floral structure has
Prestige is applied in fields such as novel nano photoelectric devices.
In summary, above with generality illustrates, the present invention is described in detail for embodiment, but
On the basis of the present invention, the modifications or improvements on the basis of without departing from the present invention, belong to patent of the present invention and cover model
Enclose.
Claims (8)
- A kind of 1. simple method for preparing zinc oxide nano popped rice, it is characterised in that it is realized by following step：Zinc salt is dissolved In deionized water, add sylvite and citric acid presses certain mixed in molar ratio, after mixed liquor is stirred into certain time, using electricity Chemical deposition, using graphite and pure copper foil as working electrode, aoxidized using the mixed liquor of zinc salt, sylvite and citric acid as growth The deposition liquid of zinc nano flower, deposits certain time under conditions of certain temperature and constant potential, then takes out developing zinc oxide Substrate pure copper foil deionization cleans, and is placed in drying certain time under certain temperature in baking oven, finally obtains dry nano flower Structure zinc oxide.
- 2. the method as claimed in claim 1 for simply preparing zinc oxide nano popped rice, it is characterised in that the also cleaning including substrate Step；The substrate cleaning treatment is passed through in 0.1M hydrochloric acid, distilled water, acetone, steaming respectively for the substrate pure copper foil before deposition It is cleaned by ultrasonic in distilled water.
- 3. the method as claimed in claim 1 for simply preparing zinc oxide nano popped rice, it is characterised in that be dissolved in the zinc salt In 100ml deionized water, add sylvite and citric acid presses certain mixed in molar ratio, mixed liquor is stirred into 10min.
- 4. the simple method for preparing zinc oxide nano popped rice as described in claim 1 or 3, it is characterised in that the zinc salt and potassium The mol ratio of salt is 2.5-1, and the mol ratio of the citric acid and sylvite is 0.1-1.
- 5. the as claimed in claim 1 method for simply preparing zinc oxide nano popped rice, it is characterised in that the condition of the deposition is Heating-up temperature is 90 DEG C, constant potential is 1.5V and sedimentation time is 5min.
- 6. the simple method for preparing zinc oxide nano popped rice as described in claim 1 or 3, it is characterised in that the zinc salt is chlorination Zinc.
- 7. the simple method for preparing zinc oxide nano popped rice as described in claim 1 or 3, it is characterised in that the sylvite is chlorine Change potassium.
- 8. the method as claimed in claim 1 for simply preparing zinc oxide nano popped rice, it is characterised in that the developing zinc oxide Substrate copper foil deionized water rinsing 3 times, it is placed in 100 DEG C of drying 15min in baking oven.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101348931A (en) * | 2008-09-11 | 2009-01-21 | 北京科技大学 | Method for preparing uniform transparent zinc oxide nanorod array film by pulse electrodeposition |
| CN103101964A (en) * | 2013-01-16 | 2013-05-15 | 浙江大学 | Preparation method of zinc oxide nanoflower of spiauterite structure |
| CN103318943A (en) * | 2013-06-05 | 2013-09-25 | 上海交通大学 | Flower-like ZnO nano-rod cluster preparation method |
| CN103320827A (en) * | 2013-06-13 | 2013-09-25 | 江苏大学 | Preparation method of inorganic-salt-doped nano zinc oxide film |
| WO2014175653A1 (en) * | 2013-04-23 | 2014-10-30 | 인제대학교 산학협력단 | Method for preparing nanostructure by electrochemical deposition, and nanostructure prepared thereby |
| CN106381513A (en) * | 2016-08-31 | 2017-02-08 | 昆明理工大学 | Preparation method and application of multi-stage nanosheet zinc oxide |
-
2017
- 2017-06-27 CN CN201710499190.XA patent/CN107460514A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101348931A (en) * | 2008-09-11 | 2009-01-21 | 北京科技大学 | Method for preparing uniform transparent zinc oxide nanorod array film by pulse electrodeposition |
| CN103101964A (en) * | 2013-01-16 | 2013-05-15 | 浙江大学 | Preparation method of zinc oxide nanoflower of spiauterite structure |
| WO2014175653A1 (en) * | 2013-04-23 | 2014-10-30 | 인제대학교 산학협력단 | Method for preparing nanostructure by electrochemical deposition, and nanostructure prepared thereby |
| CN103318943A (en) * | 2013-06-05 | 2013-09-25 | 上海交通大学 | Flower-like ZnO nano-rod cluster preparation method |
| CN103320827A (en) * | 2013-06-13 | 2013-09-25 | 江苏大学 | Preparation method of inorganic-salt-doped nano zinc oxide film |
| CN106381513A (en) * | 2016-08-31 | 2017-02-08 | 昆明理工大学 | Preparation method and application of multi-stage nanosheet zinc oxide |
Non-Patent Citations (1)
| Title |
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| 王艳坤等: "Co掺杂ZnO纳米棒的电沉积法制备及其光学性能", 《半导体光电》 * |
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Application publication date: 20171212 |