CN103240422B - Prepare the method for zinc oxide nano rod-Yin micron dish composite heterogenous junction structure - Google Patents
Prepare the method for zinc oxide nano rod-Yin micron dish composite heterogenous junction structure Download PDFInfo
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Abstract
The present invention relates to the method preparing zinc oxide nano rod-Yin micron dish composite heterogenous junction structure, in the water-formamide solution reaction system of silver nitrate and ascorbic acid, is that adjusting control agent prepares silver-colored micron dish with holes with dextran sulfate sodium; Then on silver-colored micron dish, carry out the deposition of zinc oxide crystal seed, then again the silver plate depositing crystal seed is spun on electro-conductive glass sheet, after cleaning is dried, be positioned in the ethanolic solution of hexamethylenetetramine and zinc nitrate the growth carrying out silver-colored micron dish nanometic zinc oxide rod array, after water fully washs, naturally dry, namely obtain product.It is the senior Heterogeneous Composite structure that nanometic zinc oxide rod array is grown on silver-colored micron dish with holes that the present invention prepares product, wherein the diameter of silver-colored micron dish is ~ 4 microns, nanometic zinc oxide rod array has regulatable size and structure, this preparation method's structure-controllable, reproducible, product characteristics is stablized, and has superior photocatalysis performance.
Description
Technical field
The present invention relates to a kind of preparation method of SEMICONDUCTOR-METAL advanced composite material (ACM) of structure-controllable, especially relate to a kind of method preparing the senior composite heterogenous junction structure of zinc oxide nano rod-Yin micron dish.
Background technology
The nano composite material with heterojunction structure can obtain the novel physics chemical property and multi-functional characteristic that homogenous material do not have, thus to be with a wide range of applications " SynthesisofBranched ' nanotrees ' byControlledSeedingofMultipleBranchingEvents " [Dick, K.A. at numerous areas; Deppert, K.; Larsson, M.W.; Martensson, T.; Seifert, W.; Wallenberg, L.R.; Samuelson, L.Nat.Mater.3,380-384. (2004)].Wherein, metal-semiconductor heterojunction composite especially has unique optics, electricity, magnetic property.For noble metal (as Ag) and broad stopband oxide semiconductor (ZnO), due to the surface plasma resonance effect (SurfacePlasmonResonance of noble metal uniqueness, SPR), metal-semiconductor composite after composite noble metal, can realize response " the UltrafastPlasmon-InducedElectronTransferfromGoldNanodots intoTiO to visible ray
2nanoparticle " [Furube, A., Du, L., Hara, K., Katoh, R.andTachiya, M.J.Am.Chem.Soc.129,14852-14853. (2007)]; And, noble metal and the interface charge segregation phenomenon " CatalysiswithTiO of semiconductor because of the different formation of fermi level
2/ GoldNanocomposites.EffectofMetalParticleSizeontheFermiLe velEquilibration " [Subramanian; V.; Wolf; E.E.andKamat; PV.J.Am.Chem.Soc.; 126,4943-4950. (2004)], composite can be made to have higher photoelectric activity.
Mostly noble metal-zinc oxide composite prepared is at present that (a) noble metal in-situ deposition is scattered among semi-conducting material in semiconductor material surface or (b), and these simple composite structures have some unfavorable factors.First be that composite is narrow to light abstraction width: the noble metal-semiconductor composite before reported to the response range of light mainly at ultraviolet (< 400nm) and some visible light district (500-700nm), utilize very limited (700-2500nm) to the response in infrared band light district, this directly can have influence on the Utilization ability of material to long-wave band light; Secondly, in metal-semiconductor composite construction, charge transport ability is low, charge recombination rate is high: as the situation above as described in (a), (b), because isolate each other between metal or semiconductor grain, light induced electron and hole do not have effective approach to carry out high efficiency of transmission and release, and the compact texture of composite is unfavorable for again infiltration and the absorption of electronics, hole acceptor, the charge recombination chance in material is caused to increase and catalytic activity reduction.For the problems referred to above and analysis, we design new nanometer synthetic route, adopt seed deposition and oriented growth technology, prepare a kind of semiconductor-noble metal based on a peacekeeping two-dimensional nanostructure primitive (zinc oxide nano rod-Yin micron dish) senior Heterogeneous Composite structure, the wide spectral being expected to simultaneously realize material absorbs and efficent electronic transmission.
Summary of the invention
Object of the present invention can be achieved through the following technical solutions: object of the present invention is exactly to cause the deficiency of material property because of fault of construction for overcoming current semiconductor-metallic composite, is had the senior heterogeneous material compound of the zinc oxide nano rod-Yin micron dish of special construction and performance by a kind of new synthetic method preparation.
Prepare the method for zinc oxide nano rod-Yin micron dish composite heterogenous junction structure, comprise the following steps:
(1) taking dextran sulfate sodium is dissolved in the mixed solution of water and formamide, then under agitation successively by etc. the ascorbic acid of molar concentration and silver nitrate add in mixed solution, then 24 hours are left standstill in room temperature, obtained silver-colored micron dish product with holes, by product centrifugation and washing to be soaked in the aqueous solution of the polyvinylpyrrolidone of 0.1 grams per liter 4 hours after drying, polyvinylpyrrolidone is adsorbed on silver plate;
(2) anhydrous zinc acetate is dissolved in absolute ethyl alcohol, be mixed with the solution of 10 mM/ls, be that the ethanolic solution of the potassium hydroxide of 30 mM/ls dropwise joins in above-mentioned solution by concentration, at 60 DEG C, Keep agitation 2 hours, prepares zinc oxide crystal seed solution;
(3) the silver-colored micron dish of polyvinylpyrrolidone absorption in step (1) is distributed in the zinc oxide crystal seed solution in step (2), soak 4 hours, then the silver plate being adsorbed with zinc oxide crystal seed is spun on electro-conductive glass sheet, within 1 hour, removes ethanol at oven drying;
(4) zinc nitrate hexahydrate of molar concentration and the mixed aqueous solution of hexamethylene tetramine such as the electro-conductive glass sheet being adsorbed with zinc oxide crystal seed to be placed in, controlling reaction temperature is 85 DEG C of growths carrying out zinc oxide nano rod, take out substrate, cleaning, drying, namely obtains the senior Heterogeneous Composite structure of zinc oxide nano rod-Yin micron dish.
In mixed solution described in step (1), the volume ratio of water and formamide is 5: (4-5), and the concentration of dextran sulfate sodium in mixed solution is 0.01 grams per milliliter.
The molar concentration of the ascorbic acid described in step (1) and silver nitrate is 0.2 mol/L, and the ascorbic acid added and silver nitrate mol ratio are 1: 1; Ascorbic acid and the silver nitrate concentration in mixed solution is 2 mM/ls.
The molecular weight of the dextran sulfate sodium described in step (1) is 40000, and the molecular weight of described polyvinylpyrrolidone is 12000.
In step (2), the volume ratio of the ethanolic solution of anhydrous zinc acetate and the ethanolic solution of potassium hydroxide is (1.8-2): 1.
The mol ratio of the zinc nitrate hexahydrate described in step (4) and hexamethylene tetramine is 1: 1; Zinc nitrate hexahydrate and the hexamethylene tetramine concentration in mixed aqueous solution is 2 ~ 10 mM/ls.
In step (4), the reaction time of zinc oxide nano rod growth is 2 ~ 24 hours.
In the zinc oxide nano rod-Yin micron dish senior Heterogeneous Composite structure prepared, the diameter of silver-colored micron dish is 1 ~ 4 micron, and the excellent diameter of zinc oxide nano rod is 20 ~ 200 nanometers, and length is 100-1800 nanometer, and shape is tubulose, cone-shaped or bar-shaped.
Compared with prior art, the senior Heterogeneous Composite structure of zinc oxide nano rod-Yin micron dish of the method synthesis that the present invention adopts, crystallization is good; Nanometic zinc oxide rod array gives the high specific area of material and open structure, is conducive to and the absorption of surrounding material and exchange; The plasma resonance effect of silver micron dish, makes composite also can absorb visible ray, has widened the absorption spectrum of material; Simultaneous oxidation zinc nanometer rods and Silver nanodisks, respectively as the transferring charge approach of a peacekeeping two dimension, make composite have unique electronic three-dimensional transmission characteristic; Due to the advantage of said structure and composition aspect, zinc oxide nano rod-silver plate shows superior photoelectric activity in the test of photocatalytic pollutant degradation.And preparation method is controlled, reproducible, product characteristics is stablized, and can be widely used as the high-efficient electrode material etc. of the electrode material of photochemical catalyst, solar cell and lithium battery, microelectronic component and sensor.
Accompanying drawing explanation
Fig. 1 is the stereoscan photograph (A-B) of the presedimentary silver-colored micron dish with holes of zinc oxide crystal seed, transmission electron microscope (C-D), X ray diffracting spectrum (E) and the post-depositional stereoscan photograph of zinc oxide crystal seed (F-G).
Fig. 2 is that zinc oxide array is grown on the stereoscan photograph (A, C-D) of the senior Heterogeneous Composite structure on silver-colored micron dish and the low power (E) of X ray diffracting spectrum (B) and single zinc oxide nano rod and high-resolution (F) transmission electron microscope photo.
Fig. 3 is the stereoscan photograph that zinc oxide array is grown on the senior Heterogeneous Composite structure on silver-colored micron dish.Wherein (A-B): growth time is 2 hours; (C-E): growth time is 24 hours.
Detailed description of the invention
Prepare the method for zinc oxide nano rod-Yin micron dish composite heterogenous junction structure, comprise the following steps:
(1) take molecular weight be 40000 dextran sulfate sodium be dissolved into water and formamide is 5 by volume: in the mixed solution that (4-5) obtains, the concentration of dextran sulfate sodium in mixed solution is 0.01 grams per milliliter, then under agitation successively general etc. molar concentration, isopyknic ascorbic acid and silver nitrate add in mixed solution, the molar concentration of ascorbic acid and silver nitrate is 0.2 mol/L, ascorbic acid and the silver nitrate concentration in mixed solution is 2 mM/ls, then 24 hours are left standstill in room temperature, obtained silver-colored micron dish product with holes, by product centrifugation and washing to be soaked in the aqueous solution of the polyvinylpyrrolidone (molecular weight is 12000) of 0.1 grams per liter 4 hours after drying, polyvinylpyrrolidone is adsorbed on silver plate,
(2) anhydrous zinc acetate is dissolved in absolute ethyl alcohol, be mixed with the solution of 10 mM/ls, be that the ethanolic solution of the potassium hydroxide of 30 mM/ls dropwise joins in above-mentioned solution by concentration, the volume ratio of the ethanolic solution of anhydrous zinc acetate and the ethanolic solution of potassium hydroxide is (1.8-2): 1, Keep agitation 2 hours at 60 DEG C, prepares zinc oxide crystal seed solution again;
(3) the silver-colored micron dish of polyvinylpyrrolidone absorption in step (1) is distributed in the zinc oxide crystal seed solution in step (2), soak 4 hours, then the silver plate being adsorbed with zinc oxide crystal seed is spun on electro-conductive glass sheet, within 1 hour, removes ethanol at oven drying;
(4) zinc nitrate hexahydrate of molar concentration and the mixed aqueous solution of hexamethylene tetramine such as the electro-conductive glass sheet being adsorbed with zinc oxide crystal seed to be placed in, the mol ratio of zinc nitrate hexahydrate and hexamethylene tetramine is 1: 1, zinc nitrate hexahydrate and the hexamethylene tetramine concentration in mixed aqueous solution is 2 ~ 10 mM/ls, control reaction temperature is 85 DEG C and carries out zinc oxide nano rod growth 2 ~ 24 hours, take out substrate, cleaning, dry, namely the senior Heterogeneous Composite structure of zinc oxide nano rod-Yin micron dish is obtained, wherein the diameter of silver-colored micron dish is 1 ~ 4 micron, the excellent diameter of zinc oxide nano rod is 20 ~ 200 nanometers, length is 100-1800 nanometer, shape is tubulose, cone-shaped or bar-shaped.
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Embodiment 1
Taking 0.1 gram of dextran sulfate sodium (molecular weight 40000) is dissolved in the mixed solution of water and formamide, then under agitation successively by etc. the ascorbic acid of 0.1 milliliter of molar concentration (0.2 mol/L) and the silver nitrate of 0.1 milliliter add in mixed solution, room temperature leaves standstill 24 hours, obtained silver-colored micron dish product with holes.Product centrifugation, wash, dry after to be soaked in the aqueous solution of the polyvinylpyrrolidone (PVP, molecular weight 12000) of 0.1 grams per liter 4 hours, thus PVP is adsorbed onto on silver plate.Meanwhile, separately get the ethanolic solution of the zinc acetate of 125 milliliters 10 mM/ls, dropwise join in above-mentioned solution by the ethanolic solution of the potassium hydroxide of 65 milliliters 30 mM/ls, at 60 DEG C, Keep agitation 2 hours, prepares zinc oxide crystal seed solution.Then the silver-colored micron dish of PVP process is distributed in above-mentioned zinc oxide crystal seed solution, soaks 4 hours with abundant adsorption and oxidation zinc crystal seed (its microstructure as shown in Figure 1).Then the silver plate being adsorbed with zinc oxide crystal seed is spun on electro-conductive glass sheet, be placed in oven drying 1 hour, be placed in 20 milliliters of zinc nitrate hexahydrates of 10 mM/ls and the aqueous solution of hexamethylene tetramine subsequently again, carry out the growth of zinc oxide nano rod, after reaction carries out 8 hours at 85 DEG C, take out substrate, cleaning, drying, namely obtains the senior Heterogeneous Composite structure of zinc oxide nano rod-Yin micron dish.In this product, the diameter of zinc oxide nano rod is ~ 80 nanometers, and length is 1-1.2 micron (Fig. 2).
Embodiment 2
Taking 0.1 gram of dextran sulfate sodium (molecular weight 40000) is dissolved in the mixed solution of water and formamide, then under agitation successively by etc. the ascorbic acid of 0.1 milliliter of molar concentration (0.2 mol/L) and the silver nitrate of 0.1 milliliter add in mixed solution, room temperature leaves standstill 24 hours, obtained silver-colored micron dish product with holes.Product centrifugation, wash, dry after to be soaked in the aqueous solution of the polyvinylpyrrolidone (PVP, molecular weight 12000) of 0.1 grams per liter 4 hours, thus PVP is adsorbed onto on silver plate.Meanwhile, separately get the ethanolic solution of the zinc acetate of 125 milliliters 10 mM/ls, dropwise join in above-mentioned solution by the ethanolic solution of the potassium hydroxide of 65 milliliters 30 mM/ls, at 60 DEG C, Keep agitation 2 hours, prepares zinc oxide crystal seed solution.Then the silver-colored micron dish of PVP process is distributed in above-mentioned zinc oxide crystal seed solution, soaks 4 hours with abundant adsorption and oxidation zinc crystal seed.Then the silver plate being adsorbed with zinc oxide crystal seed is spun on electro-conductive glass sheet, be placed in oven drying 1 hour, be placed in 20 milliliters of zinc nitrate hexahydrates of 10 mM/ls and the aqueous solution of hexamethylene tetramine subsequently again, carry out the growth of zinc oxide nano rod, react carry out 2 hours at 85 DEG C after, take out substrate, cleaning, dry, namely obtain the senior Heterogeneous Composite structure of zinc oxide nano rod-Yin micron dish.In this product, the diameter of zinc oxide nano rod is ~ 30 nanometers, and length is 600-800 nanometer (in Fig. 3 A-B).
Embodiment 3
Taking 0.1 gram of dextran sulfate sodium (molecular weight 40000) is dissolved in the mixed solution of water and formamide, then under agitation successively by etc. the ascorbic acid of 0.1 milliliter of molar concentration (0.2 mol/L) and the silver nitrate of 0.1 milliliter add in mixed solution, room temperature leaves standstill 24 hours, obtained silver-colored micron dish product with holes.Product centrifugation, wash, dry after to be soaked in the aqueous solution of the polyvinylpyrrolidone (PVP, molecular weight 12000) of 0.1 grams per liter 4 hours, thus PVP is adsorbed onto on silver plate.Meanwhile, separately get the ethanolic solution of the zinc acetate of 125 milliliters 10 mM/ls, dropwise join in above-mentioned solution by the ethanolic solution of the potassium hydroxide of 65 milliliters 30 mM/ls, at 60 DEG C, Keep agitation 2 hours, prepares zinc oxide crystal seed solution.Then the silver-colored micron dish of PVP process is distributed in above-mentioned zinc oxide crystal seed solution, soaks 4 hours with abundant adsorption and oxidation zinc crystal seed.Then the silver plate being adsorbed with zinc oxide crystal seed is spun on electro-conductive glass sheet, be placed in oven drying 1 hour, be placed in 20 milliliters of zinc nitrate hexahydrates of 10 mM/ls and the aqueous solution of hexamethylene tetramine subsequently again, carry out the growth of zinc oxide nano rod, react carry out 24 hours at 85 DEG C after, take out substrate, cleaning, dry, namely obtain the senior Heterogeneous Composite structure of zinc oxide nano rod-Yin micron dish.In this product, the diameter of zinc oxide nano rod is ~ 150 nanometers, and length is 1.8 microns, and nanometer rods has taper tip (in Fig. 3 C-E), and this feature is expected in Flied emission, find important application.
Embodiment 4
A method for the senior Heterogeneous Composite structure of zinc oxide nano rod-silver-colored micron dish with holes, the method comprises the following steps:
1) taking 0.1 gram of dextran sulfate sodium (molecular weight 40000) is dissolved in the mixed solution of water and formamide, then under agitation successively by etc. the ascorbic acid of 0.1 milliliter of molar concentration (0.2 mol/L) and the silver nitrate of 0.1 milliliter add in mixed solution, then 24 hours are left standstill in room temperature, obtained silver-colored micron dish product with holes.Product centrifugation, washing three times, to be soaked in the aqueous solution of the polyvinylpyrrolidone (PVP, molecular weight 12000) of 0.1 grams per liter 4 hours after drying, thus PVP is adsorbed on silver plate.
(2) certain mass anhydrous zinc acetate is dissolved in 125 milliliters of absolute ethyl alcohols, is mixed with the solution of 10 mM/ls.Then, dropwise join in above-mentioned solution by the ethanolic solution of the potassium hydroxide of 65 milliliters 30 mM/ls, at 60 DEG C, Keep agitation 2 hours, prepares zinc oxide crystal seed solution;
(3) the silver-colored micron dish of PVP process in step (1) is distributed in the zinc oxide crystal seed solution in step (2), soaks 4 hours with abundant adsorption and oxidation zinc crystal seed.Then the silver plate being adsorbed with zinc oxide crystal seed is spun on electro-conductive glass sheet, stand-by after oven drying removes ethanol in 1 hour;
(4) the electro-conductive glass sheet being adsorbed with zinc oxide crystal seed is placed in 20 milliliters of zinc nitrate hexahydrates of 2 mM/ls and the aqueous solution of hexamethylene tetramine, carry out the growth of zinc oxide nano rod, after reaction carries out 5 hours at 85 DEG C, take out substrate, cleaning, drying, namely obtains the senior Heterogeneous Composite structure of zinc oxide nano rod-Yin micron dish.In this product, the diameter of zinc oxide nano rod is 50-100 nanometer, and length is 100-200 nanometer, the bowl-mouth shape structure of tip in depression of nanometer rods.
Embodiment 5
A method for the senior Heterogeneous Composite structure of zinc oxide nano rod-silver-colored micron dish with holes, the method comprises the following steps:
1) taking 0.1 gram of dextran sulfate sodium (molecular weight 40000) is dissolved in the mixed solution of water and formamide, then under agitation successively by etc. the ascorbic acid of 0.1 milliliter of molar concentration (0.2 mol/L) and the silver nitrate of 0.1 milliliter add in mixed solution, then 24 hours are left standstill in room temperature, obtained silver-colored micron dish product with holes.Product centrifugation, washing three times, to be soaked in the aqueous solution of the polyvinylpyrrolidone (PVP, molecular weight 12000) of 0.1 grams per liter 4 hours after drying, thus PVP is adsorbed on silver plate.
(2) certain mass anhydrous zinc acetate is dissolved in 125 milliliters of absolute ethyl alcohols, is mixed with the solution of 10 mM/ls.Then, dropwise join in above-mentioned solution by the ethanolic solution of the potassium hydroxide of 65 milliliters 30 mM/ls, at 60 DEG C, Keep agitation 2 hours, prepares zinc oxide crystal seed solution;
(3) the silver-colored micron dish of PVP process in step (1) is distributed in the zinc oxide crystal seed solution in step (2), soaks 4 hours with abundant adsorption and oxidation zinc crystal seed.Then the silver plate being adsorbed with zinc oxide crystal seed is spun on electro-conductive glass sheet, stand-by after oven drying removes ethanol in 1 hour;
(4) the electro-conductive glass sheet being adsorbed with zinc oxide crystal seed is placed in 20 milliliters of zinc nitrate hexahydrates of 5 mM/ls and the aqueous solution of hexamethylene tetramine, carry out the growth of zinc oxide nano rod, after reaction carries out 5 hours at 85 DEG C, take out substrate, cleaning, drying, namely obtains the senior Heterogeneous Composite structure of zinc oxide nano rod-Yin micron dish.In this product, the diameter of zinc oxide nano rod is 20-150 nanometer, and length is 150-300 nanometer, and the tip of nanometer rods in tubular construction.
Compared with prior art, the senior Heterogeneous Composite structure (Fig. 2-3) be grown on for nanometic zinc oxide rod array on silver-colored micron dish with holes of the method synthesis that the present invention adopts, wherein the diameter of silver-colored micron dish is ~ 4 microns, in nanometic zinc oxide rod array, nanorod diameter is 20 ~ 200 nanometers, length is 100-1800 nanometer, and shape is tubulose, pointed cone and bar-shaped.This preparation method's structure-controllable, reproducible, product characteristics is stablized, and has superior photocatalysis performance.Therefore can be used for the numerous areas such as photocatalysis, solar cell, lithium battery, microelectronic component, gas sensing.
Claims (7)
1. prepare the method for zinc oxide nano rod-Yin micron dish composite heterogenous junction structure, it is characterized in that, the method comprises the following steps:
(1) taking dextran sulfate sodium is dissolved in the mixed solution of water and formamide, then under agitation successively by etc. the ascorbic acid of molar concentration and silver nitrate add in mixed solution, then 24 hours are left standstill in room temperature, obtained silver-colored micron dish product with holes, by product centrifugation and washing to be soaked in the aqueous solution of the polyvinylpyrrolidone of 0.1 grams per liter 4 hours after drying, polyvinylpyrrolidone is adsorbed on silver plate, the molecular weight of described dextran sulfate sodium is 40000, and the molecular weight of described polyvinylpyrrolidone is 12000;
(2) anhydrous zinc acetate is dissolved in absolute ethyl alcohol, be mixed with the solution of 10 mM/ls, be that the ethanolic solution of the potassium hydroxide of 30 mM/ls dropwise joins in above-mentioned solution by concentration, at 60 DEG C, Keep agitation 2 hours, prepares zinc oxide crystal seed solution;
(3) the silver-colored micron dish of polyvinylpyrrolidone absorption in step (1) is distributed in the zinc oxide crystal seed solution in step (2), soak 4 hours, then the silver plate being adsorbed with zinc oxide crystal seed is spun on electro-conductive glass sheet, within 1 hour, removes ethanol at oven drying;
(4) zinc nitrate hexahydrate of molar concentration and the mixed aqueous solution of hexamethylene tetramine such as the electro-conductive glass sheet being adsorbed with zinc oxide crystal seed to be placed in, controlling reaction temperature is 85 DEG C of growths carrying out zinc oxide nano rod, take out substrate, cleaning, drying, namely obtains the senior Heterogeneous Composite structure of zinc oxide nano rod-Yin micron dish.
2. the method preparing zinc oxide nano rod-Yin micron dish composite heterogenous junction structure according to claim 1, it is characterized in that, in mixed solution described in step (1), the volume ratio of water and formamide is 5:(4-5), the concentration of dextran sulfate sodium in mixed solution is 0.01 grams per milliliter.
3. the method preparing zinc oxide nano rod-Yin micron dish composite heterogenous junction structure according to claim 1, it is characterized in that, the molar concentration of the ascorbic acid described in step (1) and silver nitrate is 0.2 mol/L, and ascorbic acid and the silver nitrate concentration in mixed solution is 2 mM/ls.
4. the method preparing zinc oxide nano rod-Yin micron dish composite heterogenous junction structure according to claim 1, it is characterized in that, in step (2), the volume ratio of the ethanolic solution of anhydrous zinc acetate and the ethanolic solution of potassium hydroxide is (1.8-2): 1.
5. the method preparing zinc oxide nano rod-Yin micron dish composite heterogenous junction structure according to claim 1, it is characterized in that, the mol ratio of the zinc nitrate hexahydrate described in step (4) and hexamethylene tetramine is 1:1; Zinc nitrate hexahydrate and the hexamethylene tetramine concentration in mixed aqueous solution is 2 ~ 10 mM/ls.
6. the method preparing zinc oxide nano rod-Yin micron dish composite heterogenous junction structure according to claim 1, is characterized in that, in step (4), the reaction time of zinc oxide nano rod growth is 2 ~ 24 hours.
7. the method preparing zinc oxide nano rod-Yin micron dish composite heterogenous junction structure according to claim 1, it is characterized in that, in the zinc oxide nano rod-Yin micron dish Heterogeneous Composite structure prepared, the diameter of silver-colored micron dish is 1 ~ 4 micron, the excellent diameter of zinc oxide nano rod is 20 ~ 200 nanometers, length is 100-1800 nanometer, and shape is tubulose, cone-shaped or bar-shaped.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107159218A (en) * | 2017-05-10 | 2017-09-15 | 同济大学 | The preparation method of nanometer copper sheet/Zinc oxide nano sheet composite and application |
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| CN103480373B (en) * | 2013-09-05 | 2016-03-02 | 同济大学 | The preparation method of dandelion shape nucleocapsid structure AuZnO heterojunction photocatalyst |
| CN104162681B (en) * | 2014-07-30 | 2016-01-27 | 青岛科技大学 | A kind of preparation method of silver-ZnO nano composite structure |
| CN106563811B (en) * | 2015-10-13 | 2018-07-03 | 中国科学院大连化学物理研究所 | A kind of method that sea urchin shape Ag-ZnO nano-particles are continuously prepared using micro passage reaction |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102581273A (en) * | 2012-03-05 | 2012-07-18 | 安徽师范大学 | Porous core-shell nano auriferous alloy and preparation method for same |
| CN102747424A (en) * | 2012-08-06 | 2012-10-24 | 苏州汶颢芯片科技有限公司 | Method for preparing zinc oxide nano wire/pipe arrays with controllable diameters and heights on indium tin oxide (ITO) glass |
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|---|---|---|---|---|
| US20120114941A1 (en) * | 2010-11-08 | 2012-05-10 | Korea Institute Of Energy Research | Synthesis method of graphitic shell-alloy core heterostructure nanowires and longitudinal metal oxide heterostructure nanowires, and reversible synthesis method between nanowires thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102581273A (en) * | 2012-03-05 | 2012-07-18 | 安徽师范大学 | Porous core-shell nano auriferous alloy and preparation method for same |
| CN102747424A (en) * | 2012-08-06 | 2012-10-24 | 苏州汶颢芯片科技有限公司 | Method for preparing zinc oxide nano wire/pipe arrays with controllable diameters and heights on indium tin oxide (ITO) glass |
Non-Patent Citations (1)
| Title |
|---|
| 《Double-sided ZnO nanorod arrays on single-crystal Ag holed microdisks with enhanced photocataltytic efficiency》;Yanhui Zuo等;《Nanoscale》;20130312(第5期);4388-4394 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107159218A (en) * | 2017-05-10 | 2017-09-15 | 同济大学 | The preparation method of nanometer copper sheet/Zinc oxide nano sheet composite and application |
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