CN103240422A - Method for preparing composite heterostructure of zinc oxide nano rods and silver micron plate - Google Patents
Method for preparing composite heterostructure of zinc oxide nano rods and silver micron plate Download PDFInfo
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Abstract
The invention relates to a method for preparing a composite heterostructure of zinc oxide nano rods and a silver micron plate. The method includes: utilizing dextran sulphate sodium as regulating agent to prepare a perforated silver micron plate in a reaction system of silver nitrate and an ascorbic acid solution of water and methanamide; depositing zinc oxide seed crystals on the silver micron plate, coating the silver micron plate with the deposition of the zinc oxide seed crystals on an electric-conducting glass sheet in a rotating manner, cleaning, drying, placing the electric-conducting glass sheet in an ethanol solution of hexamethylene tetramine and zinc nitrate to grow a zinc oxide nano rod array on the silver micron plate, fully cleaning with water, and naturally drying to obtain the finished product. The product prepared by the method is a high-level composite heterostructure with the zinc oxide nano rod array growing on the perforated silver micron plate, wherein the diameter of the silver micron plate is about 4 microns, and the size and the structure of the zinc oxide nano rod array are adjustable and controller. The method for preparing the composite heterostructure of the zinc oxide nano rods and the silver micron plate is structurally controllable, good in repeatability and stable in product property, and has excellent photocatalytic performance.
Description
Technical field
The present invention relates to the preparation method of the controlled semiconductor of a kind of structure-metal advanced composite material (ACM), especially relate to a kind of method for preparing the senior composite heterogenous junction structure of zinc oxide nano rod-Yin micron dish.
Background technology
Nano composite material with heterojunction structure can obtain novel physicochemical properties and the multi-functional characteristic that homogenous material does not have, thereby be with a wide range of applications " Synthesis of Branched ' nanotrees ' by Controlled Seeding of Multiple Branching Events " [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, the metal-semiconductor heterojunction composite especially has unique optics, electricity, magnetic property.Be example with noble metal (as Ag) and broad stopband oxide semiconductor (ZnO), because surface plasma resonance effect (the Surface Plasmon Resonance of noble metal uniqueness, SPR), metal-semiconductor composite behind the compound noble metal can be realized response " the Ultrafast Plasmon-Induced Electron Transfer from Gold Nanodots into TiO to visible light
2Nanoparticle " [Furube, A., Du, L., Hara, K., Katoh, R.and Tachiya, M.J. Am.Chem.Soc.129,14852-14853. (2007)]; And, noble metal and interface charge segregation phenomenon " the Catalysis with TiO of semiconductor because of the different formation of fermi level
2/ Gold Nanocomposites.Effect of Metal Particle Size on the Fermi Level Equilibration " [Subramanian; V.; Wolf; E.E.and Kamat; PV.J.Am.Chem.Soc.; 126,4943-4950. (2004)], can make composite have higher photoelectric activity.
Mostly prepared noble metal-zinc oxide composite is that (a) noble metal in-situ deposition is scattered among the semi-conducting material in semiconductor material surface or (b) at present, and these simple composite structures have some unfavorable factors.At first be that composite is narrow to light abstraction width: before Bao Dao noble metal-semiconductor composite to the response range of light mainly ultraviolet (＜400nm) and part visible region (500-700nm), to the response utilization in infrared band light district very limited (700-2500nm), this can directly have influence on material to the ability of utilizing of long-wave band light; Secondly, low, the charge recombination rate height of charge transport ability in the metal-semiconductor composite construction: as the described situation of top (a) and (b), because it is isolated each other between metal or the semiconductor grain, light induced electron and hole do not have valid approach to carry out high efficiency of transmission and release, and the compact texture of composite is unfavorable for infiltration and the absorption of electronics, hole acceptor again, causes the charge recombination chance in the material to increase and the catalytic activity reduction.At the problems referred to above and analysis, we design new nanometer synthetic route, adopt seed deposition and oriented growth technology, prepare the senior Heterogeneous Composite structure of a kind of semiconductor-noble metal based on a peacekeeping two-dimensional nanostructure primitive (zinc oxide nano rod-Yin micron dish), be expected to realize simultaneously wide spectral absorption and the efficent electronic transmission of material.
Summary of the invention
Purpose of the present invention can be achieved through the following technical solutions: purpose of the present invention is exactly to cause the deficiency of material property for overcoming current semiconductor-metallic composite because of fault of construction, has 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, may further comprise the steps:
(1) taking by weighing dextran sulfate sodium is dissolved in the mixed solution of water and formamide, then under agitation successively will wait ascorbic acid and the silver nitrate of molar concentration to add in the mixed solution, left standstill 24 hours in room temperature then, make silver micron dish product with holes, product centrifugation and washing were soaked in after drying in the aqueous solution of polyvinylpyrrolidone of 0.1 grams per liter 4 hours, polyvinylpyrrolidone is adsorbed on the silver plate;
(2) anhydrous zinc acetate is dissolved in the absolute ethyl alcohol, be mixed with 10 mMs/liter solution, with concentration be 30 mMs/liter the ethanolic solution of potassium hydroxide dropwise join in the above-mentioned solution, continue down to stir 2 hours in 60 ℃, prepare zinc oxide crystal seed solution;
(3) the silver micron with polyvinylpyrrolidone absorption in the step (1) coils in the zinc oxide crystal seed solution that is distributed in the step (2), soaked 4 hours, then the silver plate that is adsorbed with zinc oxide crystal seed is spun on the electro-conductive glass sheet, removed ethanol in 1 hour at oven drying;
(4) the electro-conductive glass sheet that will be adsorbed with zinc oxide crystal seed such as places at the zinc nitrate hexahydrate of molar concentration and the mixed aqueous solution of six methylene tetramines, the control reaction temperature is 85 ℃ of growths of carrying out zinc oxide nano rod, take out substrate, clean, drying namely obtains zinc oxide nano rod-Yin micron and coils senior Heterogeneous Composite structure.
The volume ratio of water and formamide is 5 in the mixed solution described in the step (1): (4-5), the concentration of dextran sulfate sodium in mixed solution is 0.01 grams per milliliter.
The molar concentration of the ascorbic acid described in the step (1) and silver nitrate is 0.2 mol, and the ascorbic acid of adding and silver nitrate mol ratio are 1: 1; Ascorbic acid and the silver nitrate concentration in mixed solution be 2 mMs/liter.
The molecular weight of the dextran sulfate sodium described in the step (1) is 40000, and the molecular weight of described polyvinylpyrrolidone is 12000.
The volume ratio of the ethanolic solution of the ethanolic solution of anhydrous zinc acetate and potassium hydroxide is (1.8-2) in the step (2): 1.
The mol ratio of the zinc nitrate hexahydrate described in the step (4) and six methylene tetramines is 1: 1; Zinc nitrate hexahydrate and the concentration of six methylene tetramines in mixed aqueous solution be 2～10 mMs/liter.
The reaction time of zinc oxide nano rod growth is 2～24 hours in the step (4).
The diameter that the zinc oxide nano rod for preparing-Yin micron coils silver micron dish in the senior Heterogeneous Composite structure is 1～4 micron, and the excellent diameter of zinc oxide nano rod is 20～200 nanometers, and length is the 100-1800 nanometer, is shaped as tubulose, cone-shaped or bar-shaped.
Compared with prior art, the synthetic zinc oxide nano rod-Yin micron of the method that the present invention adopts coils senior Heterogeneous Composite structure, and crystallization is good; Nanometic zinc oxide rod array is given the high specific area of material and open structure, is conducive to absorption and exchange with surrounding material; The plasma resonance effect of silver micron dish makes composite also can absorb visible light, has widened the absorption spectrum of material; Simultaneous oxidation zinc nanometer rods and silver nanoparticle dish make composite have unique electronic three-dimensional transmission characteristic respectively as the electric charge delivering path of a peacekeeping two dimension; Because the advantage of said structure and composition aspect, zinc oxide nano rod-silver plate has shown superior photoelectric activity in the test of photocatalytic degradation pollutant.And the preparation method is controlled, good reproducibility, and product characteristics is stable, can be widely used as the high-efficient electrode material etc. of electrode material, microelectronic component and the sensor of photochemical catalyst, solar cell and lithium battery.
Description of drawings
Fig. 1 is stereoscan photograph (A-B), transmission electron microscope (C-D), X ray diffracting spectrum (E) and the post-depositional stereoscan photograph of zinc oxide crystal seed (F-G) of the presedimentary silver micron dish with holes of zinc oxide crystal seed.
Fig. 2 for zinc oxide array grow in the senior Heterogeneous Composite structure on the silver micron dish stereoscan photograph (A, C-D) 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 grows in the stereoscan photograph of the senior Heterogeneous Composite structure on the silver micron dish for zinc oxide array.Wherein (A-B): growth time is 2 hours; (C-E): growth time is 24 hours.
The specific embodiment
Prepare the method for zinc oxide nano rod-Yin micron dish composite heterogenous junction structure, may further comprise the steps:
(1) taking by weighing molecular weight is that 40000 dextran sulfate sodium is 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 will wait molar concentration, isopyknic ascorbic acid and silver nitrate add in the mixed solution, the molar concentration of ascorbic acid and silver nitrate is 0.2 mol, ascorbic acid and the silver nitrate concentration in mixed solution be 2 mMs/liter, left standstill 24 hours in room temperature then, make silver micron dish product with holes, product centrifugation and washing were soaked in after drying in the aqueous solution of polyvinylpyrrolidone (molecular weight is 12000) of 0.1 grams per liter 4 hours, polyvinylpyrrolidone is adsorbed on the silver plate;
(2) anhydrous zinc acetate is dissolved in the absolute ethyl alcohol, be mixed with 10 mMs/liter solution, with concentration be 30 mMs/liter the ethanolic solution of potassium hydroxide dropwise join in the above-mentioned solution, the volume ratio of the ethanolic solution of anhydrous zinc acetate and the ethanolic solution of potassium hydroxide is (1.8-2): 1, continue down to stir 2 hours in 60 ℃ again, prepare zinc oxide crystal seed solution;
(3) the silver micron with polyvinylpyrrolidone absorption in the step (1) coils in the zinc oxide crystal seed solution that is distributed in the step (2), soaked 4 hours, then the silver plate that is adsorbed with zinc oxide crystal seed is spun on the electro-conductive glass sheet, removed ethanol in 1 hour at oven drying;
(4) the electro-conductive glass sheet that will be adsorbed with zinc oxide crystal seed such as places at the zinc nitrate hexahydrate of molar concentration and the mixed aqueous solution of six methylene tetramines, the mol ratio of zinc nitrate hexahydrate and six methylene tetramines is 1: 1, zinc nitrate hexahydrate and the concentration of six methylene tetramines in mixed aqueous solution be 2～10 mMs/liter, the control reaction temperature is 85 ℃ and carries out zinc oxide nano rod growth 2～24 hours, take out substrate, clean, dry, namely obtain zinc oxide nano rod-Yin micron and coil senior Heterogeneous Composite structure, wherein the diameter of silver micron dish is 1～4 micron, the excellent diameter of zinc oxide nano rod is 20～200 nanometers, length is the 100-1800 nanometer, is shaped as tubulose, cone-shaped or bar-shaped.
The present invention is described in detail below in conjunction with the drawings and specific embodiments.
Embodiment 1
Taking by weighing 0.1 gram dextran sulfate sodium (molecular weight 40000) is dissolved in the mixed solution of water and formamide, then under agitation successively will wait 0.1 milliliter ascorbic acid of molar concentration (0.2 mol) and 0.1 milliliter silver nitrate to add in the mixed solution, room temperature left standstill 24 hours, made silver micron dish product with holes.Be soaked in the product centrifugation, after washing, drying in the aqueous solution of polyvinylpyrrolidone (PVP, molecular weight 12000) of 0.1 grams per liter 4 hours, thereby PVP is adsorbed onto on the silver plate.Simultaneously, other get 125 milliliter of 10 mM/liter the ethanolic solution of zinc acetate, with 65 milliliter of 30 mM/liter the ethanolic solution of potassium hydroxide dropwise join in the above-mentioned solution, continue down to stir 2 hours in 60 ℃, prepare zinc oxide crystal seed solution.The silver micron dish of then PVP being handled is distributed in the 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 that is adsorbed with zinc oxide crystal seed is spun on the electro-conductive glass sheet, placed oven drying 1 hour, place again subsequently 20 milliliter of 10 mM/liter zinc nitrate hexahydrate and the aqueous solution of six methylene tetramines, carry out the growth of zinc oxide nano rod, be reflected at carry out 8 hours under 85 ℃ after, take out substrate, clean, drying namely obtains zinc oxide nano rod-Yin micron and coils senior Heterogeneous Composite structure.The diameter of zinc oxide nano rod is～80 nanometers in this product, and length is 1-1.2 micron (Fig. 2).
Taking by weighing 0.1 gram dextran sulfate sodium (molecular weight 40000) is dissolved in the mixed solution of water and formamide, then under agitation successively will wait 0.1 milliliter ascorbic acid of molar concentration (0.2 mol) and 0.1 milliliter silver nitrate to add in the mixed solution, room temperature left standstill 24 hours, made silver micron dish product with holes.Be soaked in the product centrifugation, after washing, drying in the aqueous solution of polyvinylpyrrolidone (PVP, molecular weight 12000) of 0.1 grams per liter 4 hours, thereby PVP is adsorbed onto on the silver plate.Simultaneously, other get 125 milliliter of 10 mM/liter the ethanolic solution of zinc acetate, with 65 milliliter of 30 mM/liter the ethanolic solution of potassium hydroxide dropwise join in the above-mentioned solution, continue down to stir 2 hours in 60 ℃, prepare zinc oxide crystal seed solution.The silver micron dish of then PVP being handled is distributed in the above-mentioned zinc oxide crystal seed solution, soaks 4 hours with abundant adsorption and oxidation zinc crystal seed.Then the silver plate that is adsorbed with zinc oxide crystal seed is spun on the electro-conductive glass sheet, placed oven drying 1 hour, place again subsequently 20 milliliter of 10 mM/liter zinc nitrate hexahydrate and the aqueous solution of six methylene tetramines, carry out the growth of zinc oxide nano rod, be reflected at carry out 2 hours under 85 ℃ after, take out substrate, clean, drying namely obtains zinc oxide nano rod-Yin micron and coils senior Heterogeneous Composite structure.The diameter of zinc oxide nano rod is～30 nanometers in this product, and length is 600-800 nanometer (A-B among Fig. 3).
Taking by weighing 0.1 gram dextran sulfate sodium (molecular weight 40000) is dissolved in the mixed solution of water and formamide, then under agitation successively will wait 0.1 milliliter ascorbic acid of molar concentration (0.2 mol) and 0.1 milliliter silver nitrate to add in the mixed solution, room temperature left standstill 24 hours, made silver micron dish product with holes.Be soaked in the product centrifugation, after washing, drying in the aqueous solution of polyvinylpyrrolidone (PVP, molecular weight 12000) of 0.1 grams per liter 4 hours, thereby PVP is adsorbed onto on the silver plate.Simultaneously, other get 125 milliliter of 10 mM/liter the ethanolic solution of zinc acetate, with 65 milliliter of 30 mM/liter the ethanolic solution of potassium hydroxide dropwise join in the above-mentioned solution, continue down to stir 2 hours in 60 ℃, prepare zinc oxide crystal seed solution.The silver micron dish of then PVP being handled is distributed in the above-mentioned zinc oxide crystal seed solution, soaks 4 hours with abundant adsorption and oxidation zinc crystal seed.Then the silver plate that is adsorbed with zinc oxide crystal seed is spun on the electro-conductive glass sheet, placed oven drying 1 hour, place again subsequently 20 milliliter of 10 mM/liter zinc nitrate hexahydrate and the aqueous solution of six methylene tetramines, carry out the growth of zinc oxide nano rod, be reflected at carry out 24 hours under 85 ℃ after, take out substrate, clean, drying namely obtains zinc oxide nano rod-Yin micron and coils senior Heterogeneous Composite structure.The diameter of zinc oxide nano rod is～150 nanometers in this product, and length is 1.8 microns, and nanometer rods has taper tip (C-E among Fig. 3), and this feature is expected to find important use in the emission on the scene.
Embodiment 4
The method of the senior Heterogeneous Composite structure of a kind of zinc oxide nano rod-silver micron dish with holes, this method may further comprise the steps:
1) taking by weighing 0.1 gram dextran sulfate sodium (molecular weight 40000) is dissolved in the mixed solution of water and formamide, then under agitation successively will wait 0.1 milliliter ascorbic acid of molar concentration (0.2 mol) and 0.1 milliliter silver nitrate to add in the mixed solution, left standstill 24 hours in room temperature then, make silver micron dish product with holes.Product centrifugation, washing three times, be soaked in after drying in the aqueous solution of polyvinylpyrrolidone (PVP, molecular weight 12000) of 0.1 grams per liter 4 hours, thereby PVP is adsorbed on the silver plate.
(2) the certain mass anhydrous zinc acetate is dissolved in 125 milliliters of absolute ethyl alcohols, be mixed with 10 mMs/liter solution.Then, with 65 milliliter of 30 mM/liter the ethanolic solution of potassium hydroxide dropwise join in the above-mentioned solution, continue down to stir 2 hours in 60 ℃, prepare zinc oxide crystal seed solution;
(3) the silver micron of PVP in the step (1) being handled coils in the zinc oxide crystal seed solution that is distributed in the step (2), soaks 4 hours with abundant adsorption and oxidation zinc crystal seed.Then the silver plate that is adsorbed with zinc oxide crystal seed is spun on the electro-conductive glass sheet, stand-by after oven drying was removed ethanol in 1 hour;
(4) the electro-conductive glass sheet that will be adsorbed with zinc oxide crystal seed place 20 milliliter of 2 mM/liter zinc nitrate hexahydrate and the aqueous solution of six methylene tetramines, carry out the growth of zinc oxide nano rod, be reflected at carry out 5 hours under 85 ℃ after, take out substrate, clean, drying namely obtains zinc oxide nano rod-Yin micron and coils senior Heterogeneous Composite structure.The diameter of zinc oxide nano rod is the 50-100 nanometer in this product, and length is the 100-200 nanometer, and the tip of nanometer rods is the bowl-mouth shape structure of depression.
Embodiment 5
The method of the senior Heterogeneous Composite structure of a kind of zinc oxide nano rod-silver micron dish with holes, this method may further comprise the steps:
1) taking by weighing 0.1 gram dextran sulfate sodium (molecular weight 40000) is dissolved in the mixed solution of water and formamide, then under agitation successively will wait 0.1 milliliter ascorbic acid of molar concentration (0.2 mol) and 0.1 milliliter silver nitrate to add in the mixed solution, left standstill 24 hours in room temperature then, make silver micron dish product with holes.Product centrifugation, washing three times, be soaked in after drying in the aqueous solution of polyvinylpyrrolidone (PVP, molecular weight 12000) of 0.1 grams per liter 4 hours, thereby PVP is adsorbed on the silver plate.
(2) the certain mass anhydrous zinc acetate is dissolved in 125 milliliters of absolute ethyl alcohols, be mixed with 10 mMs/liter solution.Then, with 65 milliliter of 30 mM/liter the ethanolic solution of potassium hydroxide dropwise join in the above-mentioned solution, continue down to stir 2 hours in 60 ℃, prepare zinc oxide crystal seed solution;
(3) the silver micron of PVP in the step (1) being handled coils in the zinc oxide crystal seed solution that is distributed in the step (2), soaks 4 hours with abundant adsorption and oxidation zinc crystal seed.Then the silver plate that is adsorbed with zinc oxide crystal seed is spun on the electro-conductive glass sheet, stand-by after oven drying was removed ethanol in 1 hour;
(4) the electro-conductive glass sheet that will be adsorbed with zinc oxide crystal seed place 20 milliliter of 5 mM/liter zinc nitrate hexahydrate and the aqueous solution of six methylene tetramines, carry out the growth of zinc oxide nano rod, be reflected at carry out 5 hours under 85 ℃ after, take out substrate, clean, drying namely obtains zinc oxide nano rod-Yin micron and coils senior Heterogeneous Composite structure.The diameter of zinc oxide nano rod is the 20-150 nanometer in this product, and length is the 150-300 nanometer, and the tip of nanometer rods in tubular construction.
Compared with prior art, what the method that the present invention adopts was synthetic grows in the senior Heterogeneous Composite structure (Fig. 2-3) that silver micron with holes coils for nanometic zinc oxide rod array, wherein the diameter of silver micron dish is～4 microns, the nanometer rods diameter is 20～200 nanometers in the nanometic zinc oxide rod array, length is the 100-1800 nanometer, is shaped as tubulose, pointed cone and bar-shaped.This preparation method's structure is controlled, good reproducibility, and product characteristics is stable, and has superior photocatalysis performance.Therefore can be used for numerous areas such as photocatalysis, solar cell, lithium battery, microelectronic component, gas sensing.
Claims (8)
1. prepare the method for zinc oxide nano rod-Yin micron dish composite heterogenous junction structure, it is characterized in that this method may further comprise the steps:
(1) taking by weighing dextran sulfate sodium is dissolved in the mixed solution of water and formamide, then under agitation successively will wait ascorbic acid and the silver nitrate of molar concentration to add in the mixed solution, left standstill 24 hours in room temperature then, make silver micron dish product with holes, product centrifugation and washing were soaked in after drying in the aqueous solution of polyvinylpyrrolidone of 0.1 grams per liter 4 hours, polyvinylpyrrolidone is adsorbed on the silver plate;
(2) anhydrous zinc acetate is dissolved in the absolute ethyl alcohol, be mixed with 10 mMs/liter solution, with concentration be 30 mMs/liter the ethanolic solution of potassium hydroxide dropwise join in the above-mentioned solution, continue down to stir 2 hours in 60 ℃, prepare zinc oxide crystal seed solution;
(3) the silver micron with polyvinylpyrrolidone absorption in the step (1) coils in the zinc oxide crystal seed solution that is distributed in the step (2), soaked 4 hours, then the silver plate that is adsorbed with zinc oxide crystal seed is spun on the electro-conductive glass sheet, removed ethanol in 1 hour at oven drying;
(4) the electro-conductive glass sheet that will be adsorbed with zinc oxide crystal seed such as places at the zinc nitrate hexahydrate of molar concentration and the mixed aqueous solution of six methylene tetramines, the control reaction temperature is 85 ℃ of growths of carrying out zinc oxide nano rod, take out substrate, clean, drying namely obtains zinc oxide nano rod-Yin micron and coils senior Heterogeneous Composite structure.
2. the method for preparing zinc oxide nano rod-Yin micron dish composite heterogenous junction structure according to claim 1, it is characterized in that, the volume ratio of water and formamide is 5 in the mixed solution described in the step (1): (4-5), the concentration of dextran sulfate sodium in mixed solution is 0.01 grams per milliliter.
3. the method for 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 the step (1) and silver nitrate is 0.2 mol, and the ascorbic acid of adding and silver nitrate mol ratio are 1: 1; Ascorbic acid and the silver nitrate concentration in mixed solution be 2 mMs/liter.
4. the method for preparing zinc oxide nano rod-Yin micron dish composite heterogenous junction structure according to claim 1 is characterized in that the molecular weight of the dextran sulfate sodium described in the step (1) is 40000, and the molecular weight of described polyvinylpyrrolidone is 12000.
5. the method for preparing zinc oxide nano rod-Yin micron dish composite heterogenous junction structure according to claim 1 is characterized in that, the volume ratio of the ethanolic solution of the ethanolic solution of anhydrous zinc acetate and potassium hydroxide is (1.8-2) in the step (2): 1.
6. the method for preparing zinc oxide nano rod-Yin micron dish composite heterogenous junction structure according to claim 1 is characterized in that the mol ratio of the zinc nitrate hexahydrate described in the step (4) and six methylene tetramines is 1: 1; Zinc nitrate hexahydrate and the concentration of six methylene tetramines in mixed aqueous solution be 2～10 mMs/liter.
7. the method for preparing zinc oxide nano rod-Yin micron dish composite heterogenous junction structure according to claim 1 is characterized in that, the reaction time of zinc oxide nano rod growth is 2～24 hours in the step (4).
8. the method for preparing zinc oxide nano rod-Yin micron dish composite heterogenous junction structure according to claim 1, it is characterized in that, the diameter that the zinc oxide nano rod for preparing-Yin micron coils silver micron dish in the senior Heterogeneous Composite structure is 1～4 micron, the excellent diameter of zinc oxide nano rod is 20～200 nanometers, length is the 100-1800 nanometer, is shaped as tubulose, cone-shaped or bar-shaped.
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| 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 |
| CN106563811A (en) * | 2015-10-13 | 2017-04-19 | 中国科学院大连化学物理研究所 | Method for continuously preparing urchin-like Ag-ZnO nano particles by using microchannel reactor |
| CN105944720B (en) * | 2016-05-05 | 2018-06-26 | 同济大学 | Ag nanometer sheets/SnO2The preparation method of nanometer rods nano material photochemical catalyst |
| CN105944720A (en) * | 2016-05-05 | 2016-09-21 | 同济大学 | Preparation method of Ag nanosheet/SnO2 nanorod nanomaterial photocatalyst |
| CN109261156A (en) * | 2018-10-26 | 2019-01-25 | 同济大学 | Nickel film and zinc oxide nano rod composite material and preparation method and application |
| CN109261156B (en) * | 2018-10-26 | 2021-08-10 | 同济大学 | Nickel film and zinc oxide nanorod composite material as well as preparation method and application thereof |
| CN109494371A (en) * | 2018-11-15 | 2019-03-19 | 合肥国轩高科动力能源有限公司 | Nano-tube-shaped LiFePO of lithium ion battery4Preparation method of film material |
| CN109494371B (en) * | 2018-11-15 | 2021-04-09 | 合肥国轩高科动力能源有限公司 | Nano-tube-shaped LiFePO of lithium ion battery4Preparation method of film material |
| CN109603824A (en) * | 2018-12-29 | 2019-04-12 | 合肥学院 | A kind of preparation method and application of silver/zinc oxide composite material |
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