CN101624208A - Method for preparing zinc oxide nanowire array based on coordination chemical reaction theory - Google Patents
Method for preparing zinc oxide nanowire array based on coordination chemical reaction theory Download PDFInfo
- Publication number
- CN101624208A CN101624208A CN200910069961A CN200910069961A CN101624208A CN 101624208 A CN101624208 A CN 101624208A CN 200910069961 A CN200910069961 A CN 200910069961A CN 200910069961 A CN200910069961 A CN 200910069961A CN 101624208 A CN101624208 A CN 101624208A
- Authority
- CN
- China
- Prior art keywords
- zinc
- zno
- template
- presoma
- reaction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
A chemical preparation method (coordination reaction method) for preparing ZnO nanowire array which is based on coordination chemical reaction theory and used in porous anode aluminum oxide template is disclosed. The reactant of the method is dissoluble zinc salt added with aqueous ammonia, but different from the direct deposition method, the product of the preceding reaction Zn(OH)2 is not directly deposited on the pore channel of the aluminum oxide template but is subject to coordination reaction to be precursor---zinc ammonium coordinate, and crystallizing ions in the form of precursor is conveyed into the pore channel of the aluminum oxide template; the precursor is subject to hydrolysis reaction and is converted into Zn(OH)2 in the pore channel of the aluminum oxide template to be deposited; then, Zn(OH)2 is baked to be the target product ZnO in the end. The ZnO nanowire prepared by the method of the invention has high pore channel filling rate and continuous, compact and filled line, and when using high quality aluminum oxide template, the ZnO nanowire array is regular and uniform.
Description
[technical field]:
The invention belongs to the micro Nano material manufacture technology field, particularly be applied to the preparation of the micro Nano material of opto-electronic device.
[background technology]:
ZnO is because of having higher chemical stability, bigger energy gap (E
g=3.4eV) and higher exciton bind energy (60meV), and electricity, luminous and spectrochemical property with uniqueness, in fields such as solar cell, catalysis, air-sensitive, nanometer laser, micro-nano power supply and semiconductor materials of future generation, all have broad application prospects, thereby received great concern.In recent years, the research of assembling ZnO nano-wire array is increasing, and has produced novel micro nanometer opto-electronic devices such as nano generator, nano laser thus
[1]In current research field about preparation ZnO nano-wire array, there is an important research direction to be exactly, (Porous AnodicAlumina is abbreviated as PAA, in the document that has by ZnO being injected into porous anodic aluminium oxide, write as Anodic Aluminum Oxide again, abbreviate AAO as, as shown in Figure 1 and Figure 2) in the nano level duct of template, to form the ZnO nano-wire array, and expect that it realizes the electroluminescent of no p-n junction, thereby obtain a kind of novel electroluminescent device
[2]
At present, the method for utilizing porous anodic alumina template (PAA) to prepare the ZnO nano wire has multiple, and Xiang Guan domestic and international major technique and relative merits thereof are respectively therewith:
(1) sol-gel method: the Brinda B.Lakshm of the upright university in Colorado in 1997
[3]In the alumina formwork (PAA) in 200nm aperture, successfully assembled the ZnO nanometer line ordered array Deng employing sol-gel (Sol-Gel) method.The outstanding advantage of sol-gel method is and can carries out the synthetic of nano unit array according to stoichiometric ratio, its shortcoming is, exist the alumina formwork duct by the colloidal particle phenomenon of blocking on the one hand, make in some duct, can't obtain continuous, complete nano wire that especially hour this shortcoming is more apparent outstanding when the aperture; The precursor sol that enters the template duct on the other hand need just can become ZnO through necessary roasting since the solid phase ratio of ZnO lower (～5vol.%), cause the filling ratio in duct low.
(2) electrophoretic method: 2004, the Y.C.Wang of Taiwan National Chenggong University
[4]ZnO nano wire and nano-tube array in PAA, have been synthesized Deng the utilization electrophoretic deposition.This method is to develop on the basis of sol-gel method, utilize the electrophoretic characteristic of colloidal sol to increase the motivating force that colloidal sol imports, can solve the inadequate problem of filling that is run in some sol-gel method processes like this, but, cause the filling ratio in duct still not high because solid load is less after all in the colloidal sol.
(3) electrodip process: 2000, the Zhang Lide of Inst., of Solid Physics, Chinese Academy of Sciences
[5]The method that leader's scientific research group adopts first electrodeposit metals simple substance zinc to reoxidize, having synthesized diameter in PAA is the ZnO nano-wire array of 40nm, and has tested its photoluminescence performance.The outstanding advantage of electro-deposition method is to fill fullly, and can regulate nano wire aspect ratio in the template duct by the control electrodeposition time.Its shortcoming is that liberation of hydrogen and the oxygen uptake reaction in the electrodeposition process easily produces bubble, causes some nano wire fracture.
(4) direct precipitation method: direct precipitation method is a kind ofly to make two kinds of solution directly carry out chemical reaction and generate the sedimentary chemical precipitation method of target, its concrete manifestation form may be varied according to the difference of reactant, but its common feature is significant, and promptly two kinds of solution directly carry out chemical reaction and generate the target throw out.For example, 2005, the Zhang Lide group of Inst., of Solid Physics, Chinese Academy of Sciences used zinc nitrate and ammoniacal liquor reaction, has directly assembled the ZnO nano-wire array in PAA
[6]For direct precipitation method, because the initial concentration of configurational ion is certain, can't in deposition process, be controlled, the sedimentary speed of resultant is very fast, this has just caused on the one hand, the configurational ion that is introduced into the template duct reacts to each other and generates post precipitation and easily the duct is stopped up, and makes the configurational ion diffusion limited in the duct and can not get replenishing; On the other hand, the configurational ion at template surface place can form precipitation equally and the port in template duct is blocked, thereby hinders the diffusion of configurational ion in the duct outside the duct.Like this, finally in the template duct, be difficult to obtain the nano wire of high aspect ratio (promptly carefully growing).
[summary of the invention]:
The present invention seeks to overcome the prior art above shortcomings, a kind of chemical preparation process based on coordination chemical reaction theory (can be referred to as the coordination reaction method, or indirectly the precipitator method) is provided, is used at the orderly ZnO nano-wire array of porous anodic aluminium oxide (PAA) template preparation.
The reactant of the inventive method is that soluble zinc salt adds ammoniacal liquor, but different with direct precipitation method is the resultant Zn (OH) of this preceding order reaction
2Be not the duct that directly deposits to alumina formwork, but become precursor liquid through coordination reaction---zinc amine complex (Zn (NH
3)
4 2+) solution, configurational ion is carried in the duct of alumina formwork with the form of precursor liquid; Precursor liquid changes into Zn (OH) again through hydrolysis reaction in the duct of alumina formwork
2Precipitation; Then, Zn (OH)
2Through roasting, become final objective product ZnO.
Coordination reaction method (or indirectly precipitator method) has fundamentally changed the mode of transportation of substances in the duct of porous anodic alumina template, has overcome the shortcoming that speed of reaction in the direct sedimentation is too fast, can't be controlled in deposition process.Adopt the ZnO nano wire of coordination reaction method preparation, duct filling ratio height, continuous, the full densification of lines, when using high-quality alumina formwork, ZnO nano-wire array rule, neat.
Employing coordination reaction method provided by the invention prepares the method for zinc oxide nano-wire array in porous alumina formwork, comprise the steps:
The first, precursor liquid---the preparation of zinc amine complex solution:
At ambient temperature, to concentration is that the mass concentration that dropwise adds new preparation in the soluble Zn salts solution of 0.01～1mol/L is 1～10% ammoniacal liquor, drip on one side, vibration on one side, to promote the carrying out of solution mixing and coordination reaction, just be colourless, clarification, transparence until solution, stop dropping ammonia immediately; Leaving standstill 60 minutes, then precursor liquid---zinc amine complex solution is made;
The second, presoma---zinc hydroxide is sedimentary synthetic:
The precursor liquid of new preparation of step is gone up in the immersion of porous anodic aluminium oxide (PAA) template---in the zinc amine complex solution, use ultrasonic oscillation 10 minutes; Left standstill then 1 hour, and made precursor liquid be full of whole alumina formwork duct; Again whole reaction system (containing template, precursor liquid and container) is put into 30～50 ℃ thermostat water bath, insulation is more than 5 hours; Above-mentioned alumina formwork is taken out and puts into distilled water from container, more than 3 times, put into loft drier at last, can obtain being assembled with presoma in 60 ℃ of oven dry with ultrasonic cleaning---the alumina formwork of zinc hydroxide; The main component of presoma is the zinc hydroxide that contains crystal water and planar water; This moment, the template outward appearance was white, opaque shape;
" water-bath " in this step of the present invention is an important techniques link, and its optimal processing parameter is: bath temperature is 30～50 ℃, and the water-bath time is more than 5 hours.
Three, the roasting of presoma:
The above-mentioned alumina formwork that is assembled with presoma is put into sintering oven, roasting in air atmosphere.During roasting, earlier 130 ℃ of insulations 1 hour, after be warming up to 500 ℃ of insulations 5 hours, be cooled to room temperature at last.Through roasting, presoma---zinc hydroxide decomposes and crystallization generates zinc oxide, thereby finally obtains being assembled in the zinc oxide nano-wire array in porous anodic aluminium oxide (PAA) template.
Advantage of the present invention and positively effect:
The present invention adopts the coordination reaction method, has fundamentally changed the mode of transportation of substances in the duct of porous anodic alumina template, has overcome the shortcoming that speed of reaction in the direct sedimentation is too fast, can't be controlled in deposition process.In the coordination reaction method, on the one hand, at precursor liquid (zinc amine complex, Zn (NH
3)
4 2+) be transformed into presoma (Zn (OH)
2) hydrolysis reaction in, the brilliant positively charged ion (Zn of structure
2+) slowly release by title complex, thereby sedimentation rate is slow, and the speed of this reaction can also be controlled by the temperature and time that changes water-bath; On the other hand, precursor liquid can be imported the duct glibly, and the title complex that consumes is replenished, therefore says on the whole, the coordination reaction method be slowly, smoothness with controllable.
Adopt the coordination reaction method in porous alumina formwork, to prepare zinc oxide nano-wire array, overcome in the past shortcomings such as the duct filling ratio is not high among the preparation method, nano wire is interrupted, nano-wire array is irregular.Compare with original preparation method, the coordination reaction method has following advantage:
(1) material of carrying to the nano level duct of porous alumina formwork is a precursor liquid---zinc amine complex solution, the viscosity of this precursor liquid is suitable with the viscosity of water, therefore be easy to enter the duct of template, only template need be put into complex solution leaves standstill for some time, just can make precursor liquid be full of whole duct.
(2) presoma---Zn (OH)
2Form by the precursor liquid hydrolysis, in hydrolysis reaction, title complex removes and slowly discharges the brilliant positively charged ion (Zn of structure
2+) in addition, also in the duct, discharge ammonia (NH simultaneously
3), the latter (is combined into NH with water
4OH) can not only provide structure brilliant negatively charged ion (OH
-), can also dissolve the throw out of part block channel, the mobile passage of opening up for title complex inside and outside the duct is not easy to block the duct like this.
(3) the ZnO nano wire that adopts the coordination reaction method to prepare, duct filling ratio height, continuous, the full densification of lines, when using high-quality alumina formwork, ZnO nano-wire array rule, neat.
(4) theoretically, this technology not only can prepare zinc oxide nanowire, can also expand to the preparation of other metal oxide nano-wires (as the silver suboxide nano wire).
(5) this technical matters is simple, and needed production cost is lower, is easy to large-scale production, and environmentally safe matches with the greenization laboratory of current promotion.
[description of drawings]:
Fig. 1 is the outside drawing of porous anodic aluminium oxide (PAA) template;
Fig. 2 is the SEM figure of porous anodic aluminium oxide (PAA) template;
Fig. 3 is Zn (OH)
2The outside drawing of/PAA assembly;
Fig. 4 is the sem photograph of ZnO/PAA assembly, and wherein: (a) and (b) are surface and sectional drawings of ZnO/PAA assembly; (c) be the ZnO nano wire of bottom; (d) sectional drawing of ZnO/PAA assembly;
Fig. 5 is after the PAA template of ZnO/PAA assembly is dissolved, the TEM figure of the ZnO nano wire that obtains;
Fig. 6 is the EDAX results of ZnO/PAA section;
Fig. 7 is the XRD analysis result;
Fig. 8 is the PL spectrogram of ZnO/PAA;
Table 1 is the composition analysis result of ZnO/PAA assembly.
[embodiment]:
Embodiment 1: use twice anonizing to prepare porous anodic aluminium oxide (PAA) template
Selecting thickness for use is that 0.3mm, purity are 99.999% aluminium foil, is cut into the substrate that specification is 20mm * 30mm, passes through following processing step successively, makes porous anodic aluminium oxide (PAA) template.
(1) annealing: with identical aluminium foil environmental sealing, is 10 in vacuum tightness with the aluminium foil that cuts
-3Pa, temperature are annealing 5 hours under 500 ℃ the condition, then cool to room temperature with the furnace.
(2) degreasing: the aluminium foil after will annealing is put into acetone and was cleaned 20 minutes, takes out the back and, dries up more than 3 times with distilled water flushing, puts into ethanol then and cleans more than 3 times, dries up.
(3) electropolishing: the dose volume ratio is 4: 1 ethanol and a perchloric acid electrolytic solution, to put into electrolyzer as anode through the aluminium foil of above two step process, select another aluminium flake as negative electrode, with WYJ type D.C. regulated power supply is power supply, select 20V voltage to carry out electropolishing, the temperature of electrolytic solution remains on 60 ℃ in the polishing, and current density is controlled at 250mA/cm
2, polishing time is 4～5 minutes.Polishing is taken out the anode aluminium flake rapidly after finishing from electrolytic solution, soaked 15 minutes in ethanol, cleans with distilled water then.
(4) anodic oxidation for the first time: at the 0.3mol/L oxalic acid solution is under the condition of electrolytic solution, about 15 ℃ of room temperatures, voltage 40V, and the aluminium foil of handling through (3) step is carried out the anodic oxidation first time, and the time is 10 hours.
(5) anodic oxidation for the second time: will be through the aluminium foil that contains oxide film of the anodic oxidation treatment first time, placing by mass concentration is that 3% phosphoric acid and mass concentration are the mixed acid solution that 1.8% chromic acid mixes, in 60 ℃ of thermostat water baths, handled 10 hours, to remove this layer oxide film.After the taking-up, clean, and carry out the anodic oxidation second time by the processing parameter identical with the anodic oxidation first time in (4) step with distilled water.
(6) remove aluminium substrate: will be through the template after above twice anodic oxidation treatment, after wiping out the aluminium foil of unexecuted oxide treatment wherein, put into saturated CuCl
2In the solution, to remove the aluminium substrate of template.Take out after 7～8 minutes, obtain faint yellow transparent product, this is " a first type alumina formwork ".
(7) remove blocking layer and reaming: the preparation mass concentration is 5% phosphoric acid, put into 30 ℃ water-bath then, " first type alumina formwork " stopped aspect (being the primary aluminum basal surface) down, lie in a horizontal plane in the surface of acid solution, sample will float on the liquid level, when sample surfaces has liquid to ooze out, show that the duct is penetrating up and down, the blocking layer is removed.The time of through hole is approximately 30 minutes.Sample behind the through hole is immersed 5% phosphoric acid solution, and put into ultrasonic wave concussion 10 minutes, to carry out reaming.
Through above step, resulting porous anodic aluminium oxide (PAA) template outward appearance as shown in Figure 1.Fig. 2 is the SEM figure of porous anodic aluminium oxide (PAA) template.
Embodiment 2: the preparation of zinc oxide nano-wire array
(1) precursor liquid---the preparation of zinc amine complex solution.At ambient temperature, to the concentration that fills 10mL the Zn (NO of 0.1mol/L with dropper
3)
26H
2In the beaker of O solution, the mass concentration that dropwise adds new preparation is 2% ammoniacal liquor, drip on one side, the beaker that vibrates on one side, to promote solution to mix and the carrying out of coordination reaction, that the solution in beaker is is colourless, clarification, transparence, stops dropping ammonia immediately; Leaving standstill 60 minutes, then precursor liquid---zinc amine complex solution is made.This precursor liquid will promptly be joined promptly and used.
(2) presoma---zinc hydroxide is sedimentary synthetic.The porous anodic aluminium oxide that size is suitable (PAA) template (seeing embodiment 1) immerses in the zinc amine complex solution (being precursor liquid) of new preparation, uses ultrasonic oscillation 10 minutes; Left standstill then 1 hour.Because wicking action, zinc amine complex solution will be full of whole alumina formwork duct.Again whole reaction system (comprising beaker, precursor liquid and alumina formwork) is put into 40 ℃ thermostat water bath, be incubated after 7 hours and take out; Above-mentioned alumina formwork is put into the beaker that fills distilled water, uses ultrasonic cleaning 4 times, put into loft drier at last, can obtain being assembled with presoma in 60 ℃ of oven dry---the alumina formwork of zinc hydroxide.The main component of presoma is the zinc hydroxide that contains crystal water and planar water.This moment, the template outward appearance was white, opaque shape, as shown in Figure 3.
(3) roasting of presoma.The above-mentioned alumina formwork that is assembled with presoma is put into the electron tubes type high temperature sintering furnace, roasting in air atmosphere.During roasting, prior to 130 ℃ the insulation 1 hour, after be warming up to 500 ℃ the insulation 5 hours, be cooled to room temperature at last.Through roasting, presoma---zinc hydroxide decomposes and crystallization generates zinc oxide, thereby finally obtains being assembled in the zinc oxide nano-wire array in porous anodic aluminium oxide (PAA) template.
The sign of embodiment 3:ZnO/PAA assembly
(1) FE-SEM analyzes
To the porous anodic alumina template (see embodiment 2, be designated hereinafter simply as the ZnO/PAA assembly) that is assembled with zinc oxide nanowire, get its section and carry out the FE-SEM observation.The Nanosem 430 type thermal field emission scan electron microscopes that adopt U.S. FEI Co. to make.The pattern of gained as shown in Figure 4, from figure we as can be seen, all oxidized zinc nano wire in most ducts of alumina formwork is filled.By Fig. 4 (a) as can be seen zinc oxide nanowire all keep the shape growth in original alumina formwork duct, the even thickness of nano wire.Fig. 4 (b) is the section and the exterior view of zinc oxide nanowire, and nano wire is in good order epontic as seen from the figure.Fig. 4 (c) is the amplification of Fig. 4 (b).The part nano wire has phenomenon of rupture among the figure, is because due to zinc oxide nanowire is damaged when the preparation electron microscopic sample.By Fig. 4 (d) as can be seen, the zinc oxide nanowire queueing discipline, whole nano wire is continuous in the alumina formwork duct, and has very high filling ratio.
(2) tem analysis
One small pieces ZnO/PAA assembly is put into small beaker, add the NaOH solution of an amount of 1mol/L then, treat after the PAA dissolving, clean the ZnO nano wire from template, separate more than 3 times with distilled water, using dehydrated alcohol then instead washs more than 3 times again, handle the back through ultrasonic dispersing and take a sample, drop on the copper mesh of carbon support membrane and dry, to carry out tem observation with dropper.
The JEOL 100CX-II type field transmission electron microscope that adopts NEC company to make, to separating from the ZnO/PAA assembly and carrying out TEM morphology observation and analysis through the ZnO of dispersion treatment nano wire, its result as shown in Figure 5.Can see that by Fig. 5 (a) pattern of zinc oxide nanowire is different in size, thickness is roughly even.Partial oxidation zinc nano wire sticks together, may be since alumina formwork do not dissolve clean due to, also may be due to the power that attracts each other that produces owing to big specific surface area.Fig. 5 (b) has provided the pattern of single nano-wire, and as seen from the figure, the ZnO nanowire diameter is greatly about about 60～80nm, and the lines densification of nano wire.
(3) EDS analyzes
Prepared ZnO/PAA assembly system is cooled off in liquid nitrogen, and the purpose of this operation is to guarantee that the section sample of preparation is more smooth, the unlikely fracture that nano wire occurs.Then sample is put into the X-gamma spectrometer and carried out energy spectrum analysis, the instrument that is adopted is the X-gamma spectrometer of the Genesis XM2APEX60SEM type of U.S. EDAX company production.Fig. 6 is that the section to sample carries out the EDS figure that energy spectrum analysis obtains, and table 1 is the result to the composition analysis of assembly section.
Table 1ZnO/PAA assembly section composition analysis result
Element wt per-cent atomic percent
OK 31.82 45.99
AlK 59.39 50.90
ZnK 8.79 3.11
(4) XRD analysis
It is powder that the ZnO/PAA assembly is ground, adopt Japan's (Rigaku) D/Max-2500 type of science x-ray diffractometer, carried out structural analysis, gained XRD composes as shown in Figure 7, with the PDF card contrast of ZnO, the result confirms to have assembled zinc oxide (ZnO) material in the duct of PAA template.
The photoluminescence of embodiment 4:ZnO/PAA
The FL3-2-IHR212-NIR-TCSPC type spectrograph that adopts HRIBA Jobin Yvon company to produce has carried out the test of photoluminescence (PL) spectrum to the ZnO/PAA assembly.Under the exciting of 325nm light, the PL of resulting ZnO/PAA assembly composes as shown in Figure 8, the glow peak in a broadband occurred at the 496nm place, corresponding to the photoluminescence of the number of drawbacks of ZnO.
Reference
[1]Wang?Z?L，Song?J?H.Piezoelectric?nanogenerators?based?on?zinc?oxide?nanowirearrays[J]Science，2006，312：242
[2] Ruan Yongfeng, Yang Hongbo etc., " the zinc oxide electroluminescent device that utilizes porous alumina formwork to make ", Chinese patent (utility model), patent No. ZL200620027253.9
[3]Lakshmi?B?B，Dorhout?P?K，Martin?C?R，Sol-gel?template?synthesis?of?semiconductornanostructures，Chem.Mater.，1997，9(3)：857～862.
[4]Wang?Y?C，Leu?I?C，Hon?M?H，Dielectric?property?and?structure?of?anodic?alumina?templateand?their?effects?on?the?electrophoretic?deposition?characteristics?of?ZnO?nanowire?arrays，J.Appl.Phys.，2004，95(3)：1444～1449.
[5]Li?Y，Meng?G?W，Zhang?L?D，Ordered?semiconductor?ZnO?nanowire?arrays?and?theirphotoluminescence?properties，Appl.Phys.Lett.，2000，76(15)：2011～2013.
[6]Yanhe?Xiao，Liang?Li，Yan?Li，Synthesis?of?mesoporous?ZnO?nanowires?through?a?simple?insitu?precipitation?method，NANOTECHNOLOGY，2005，671～674
Claims (1)
1, a kind of based on chemical preparation process coordination chemical reaction theory, that be used for preparing the ZnO nano-wire array at porous anodic alumina template, it is characterized in that this method comprises the steps:
The first, precursor liquid---the preparation of zinc amine complex solution:
At ambient temperature, to concentration is that the mass concentration that dropwise adds new preparation in the soluble Zn salts solution of 0.01～1mol/L is 1～10% ammoniacal liquor, drip on one side, vibration on one side, to promote the carrying out of solution mixing and coordination reaction, just be colourless, clarification, transparence until solution, stop dropping ammonia immediately; Leaving standstill 60 minutes, then precursor liquid---zinc amine complex solution is made;
The second, presoma---zinc hydroxide is sedimentary synthetic:
The precursor liquid of new preparation of step is gone up in the porous anodic alumina template immersion---in the zinc amine complex solution, use ultrasonic oscillation 10 minutes; Left standstill then 1 hour, and made precursor liquid be full of whole alumina formwork duct; Whole reaction system is put into 30～50 ℃ thermostat water bath, insulation is more than 5 hours again; Above-mentioned alumina formwork is taken out and puts into distilled water from container, more than 3 times, put into loft drier at last, can obtain being assembled with presoma in 60 ℃ of oven dry with ultrasonic cleaning---the alumina formwork of zinc hydroxide;
Three, the roasting of presoma:
The above-mentioned alumina formwork that is assembled with presoma is put into sintering oven, roasting in air atmosphere, during roasting, prior to 130 ℃ the insulation 1 hour, after be warming up to 500 ℃ the insulation 5 hours, be cooled to room temperature at last; Through roasting, presoma---zinc hydroxide decomposes and crystallization generates zinc oxide, thereby finally obtains being assembled in the zinc oxide nano-wire array in the porous anodic alumina template.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910069961A CN101624208A (en) | 2009-07-31 | 2009-07-31 | Method for preparing zinc oxide nanowire array based on coordination chemical reaction theory |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910069961A CN101624208A (en) | 2009-07-31 | 2009-07-31 | Method for preparing zinc oxide nanowire array based on coordination chemical reaction theory |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101624208A true CN101624208A (en) | 2010-01-13 |
Family
ID=41520224
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910069961A Pending CN101624208A (en) | 2009-07-31 | 2009-07-31 | Method for preparing zinc oxide nanowire array based on coordination chemical reaction theory |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101624208A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011135514A3 (en) * | 2010-04-28 | 2012-01-19 | Basf Se | Process for preparing a zinc complex in solution |
| CN102691204A (en) * | 2012-05-30 | 2012-09-26 | 南通大学 | Preparation method of nano-zinc-oxide-loaded antibacterial ultraviolet-resistant fibers or textiles |
| CN102856446A (en) * | 2011-06-28 | 2013-01-02 | 兆鑫光电科技股份有限公司 | Epitaxial substrate with nano structure and manufacturing method of light-emitting diode |
| CN104743507A (en) * | 2015-03-30 | 2015-07-01 | 上海应用技术学院 | Method of regional growth of zinc oxide nanowire array on micro device surface |
| CN110002479A (en) * | 2019-05-22 | 2019-07-12 | 浙江工业大学 | A method of preparing nano bar-shape magnesium fluoride |
| CN113533297A (en) * | 2021-07-07 | 2021-10-22 | 陕西师范大学 | Super-hydrophobic CuO @ Ag nanowire array and application thereof in circulating SERS detection of malachite green |
-
2009
- 2009-07-31 CN CN200910069961A patent/CN101624208A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011135514A3 (en) * | 2010-04-28 | 2012-01-19 | Basf Se | Process for preparing a zinc complex in solution |
| CN102858690A (en) * | 2010-04-28 | 2013-01-02 | 巴斯夫欧洲公司 | Process for preparing a zinc complex in solution |
| US8691168B2 (en) | 2010-04-28 | 2014-04-08 | Basf Se | Process for preparing a zinc complex in solution |
| CN102858690B (en) * | 2010-04-28 | 2014-11-05 | 巴斯夫欧洲公司 | Process for preparing a zinc complex in solution |
| CN102856446A (en) * | 2011-06-28 | 2013-01-02 | 兆鑫光电科技股份有限公司 | Epitaxial substrate with nano structure and manufacturing method of light-emitting diode |
| CN102856446B (en) * | 2011-06-28 | 2015-01-21 | 兆鑫光电科技股份有限公司 | Epitaxial substrate with nano structure and manufacturing method of light-emitting diode |
| CN102691204A (en) * | 2012-05-30 | 2012-09-26 | 南通大学 | Preparation method of nano-zinc-oxide-loaded antibacterial ultraviolet-resistant fibers or textiles |
| CN104743507A (en) * | 2015-03-30 | 2015-07-01 | 上海应用技术学院 | Method of regional growth of zinc oxide nanowire array on micro device surface |
| CN104743507B (en) * | 2015-03-30 | 2016-06-22 | 上海应用技术学院 | A kind of method in micro element surface regionality growth of zinc oxide nano linear array |
| CN110002479A (en) * | 2019-05-22 | 2019-07-12 | 浙江工业大学 | A method of preparing nano bar-shape magnesium fluoride |
| CN113533297A (en) * | 2021-07-07 | 2021-10-22 | 陕西师范大学 | Super-hydrophobic CuO @ Ag nanowire array and application thereof in circulating SERS detection of malachite green |
| CN113533297B (en) * | 2021-07-07 | 2023-02-24 | 陕西师范大学 | Super-hydrophobic CuO @ Ag nanowire array and application of array in circulating SERS (surface enhanced Raman scattering) detection of malachite green |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Luo et al. | Preparation of porous micro–nano-structure NiO/ZnO heterojunction and its photocatalytic property | |
| La et al. | Template synthesis of CeO2 ordered nanowire arrays | |
| CN101624208A (en) | Method for preparing zinc oxide nanowire array based on coordination chemical reaction theory | |
| CN103628106B (en) | A kind of method preparing indium/tellurium porous nano linear array | |
| Guo et al. | Effects of preparing conditions on the electrodeposition of well-aligned ZnO nanorod arrays | |
| CN101429680A (en) | Production method for direct growth of one-dimensional nano cuprous oxide array on metallic copper substrate | |
| Downing et al. | Hydrothermal growth of ZnO nanorods: The role of KCl in controlling rod morphology | |
| CN102503169A (en) | Preparation method of zinc oxide/cuprous oxide heterojunction | |
| Xu et al. | Seed layer-free electrodeposition and characterization of vertically aligned ZnO nanorod array film | |
| Han et al. | The electrochemical self-assembly of hierarchical dendritic Bi 2 Se 3 nanostructures | |
| Choi et al. | Electrochemical synthesis of inorganic polycrystalline electrodes with controlled architectures | |
| Bicer et al. | Electrochemical synthesis of CdS nanowires by underpotential deposition in anodic alumina membrane templates | |
| Yeh et al. | Fabrication and characterization of ZnO nanorods on polished titanium substrate using electrochemical–hydrothermal methods | |
| CN104846411B (en) | The method and its product of flower-like nanometer metal cobalt are prepared using anodic oxidation aluminium formwork | |
| CN102795665B (en) | Preparation method of titanium dioxide nanotube (rod) array | |
| CN103880062A (en) | Zinc oxide nano-column thin film and preparation method thereof | |
| CN102181890A (en) | Method for preparing Zn/ZnO nano tube by direct current deposition | |
| Ling-min et al. | Shape-controlled cluster growth of ZnO nanoflowers using sol–gel method | |
| CN102061498A (en) | Preparation method of injector-shaped ZnO nanostructural array for field emission | |
| Pawar et al. | Surfactant mediated growth of ZnO nanostructures and their dye sensitized solar cell properties | |
| Inguanta et al. | Formation of lead by reduction of electrodeposited PbO 2: comparison between bulk films and nanowires fabrication | |
| CN104828774B (en) | A kind of method modified based on p-type silicon microchannel surface even | |
| Eyraud et al. | Electrochemical fabrication of oriented ZnO nanorods on TiO2 nanotubes | |
| Min et al. | Microwave-assisted aqueous synthesis of ultralong ZnO nanowires: photoluminescence and photovoltaic performance for dye-sensitized solar cell | |
| CN101984148B (en) | Controllable preparation method of Sb monocrystal nanowires in different growth directions |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20100113 |