CN115710012B - Method for synthesizing zinc oxide nanowire array - Google Patents
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- CN115710012B CN115710012B CN202211353249.1A CN202211353249A CN115710012B CN 115710012 B CN115710012 B CN 115710012B CN 202211353249 A CN202211353249 A CN 202211353249A CN 115710012 B CN115710012 B CN 115710012B
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- 238000000034 method Methods 0.000 title claims abstract description 37
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 12
- 239000000758 substrate Substances 0.000 claims abstract description 63
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 60
- 239000011701 zinc Substances 0.000 claims abstract description 59
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 59
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- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
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- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
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- 238000001878 scanning electron micrograph Methods 0.000 description 2
- RYCLIXPGLDDLTM-UHFFFAOYSA-J tetrapotassium;phosphonato phosphate Chemical compound [K+].[K+].[K+].[K+].[O-]P([O-])(=O)OP([O-])([O-])=O RYCLIXPGLDDLTM-UHFFFAOYSA-J 0.000 description 2
- BAERPNBPLZWCES-UHFFFAOYSA-N (2-hydroxy-1-phosphonoethyl)phosphonic acid Chemical compound OCC(P(O)(O)=O)P(O)(O)=O BAERPNBPLZWCES-UHFFFAOYSA-N 0.000 description 1
- LDMOEFOXLIZJOW-UHFFFAOYSA-N 1-dodecanesulfonic acid Chemical compound CCCCCCCCCCCCS(O)(=O)=O LDMOEFOXLIZJOW-UHFFFAOYSA-N 0.000 description 1
- RILZRCJGXSFXNE-UHFFFAOYSA-N 2-[4-(trifluoromethoxy)phenyl]ethanol Chemical compound OCCC1=CC=C(OC(F)(F)F)C=C1 RILZRCJGXSFXNE-UHFFFAOYSA-N 0.000 description 1
- OBDVFOBWBHMJDG-UHFFFAOYSA-N 3-mercapto-1-propanesulfonic acid Chemical compound OS(=O)(=O)CCCS OBDVFOBWBHMJDG-UHFFFAOYSA-N 0.000 description 1
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- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 244000137852 Petrea volubilis Species 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
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- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 description 1
- 229910001863 barium hydroxide Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 1
- 239000012964 benzotriazole Substances 0.000 description 1
- 238000005422 blasting Methods 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
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- 239000001569 carbon dioxide Substances 0.000 description 1
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- XPPKVPWEQAFLFU-UHFFFAOYSA-N diphosphoric acid Chemical compound OP(O)(=O)OP(O)(O)=O XPPKVPWEQAFLFU-UHFFFAOYSA-N 0.000 description 1
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- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 description 1
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- KCXFHTAICRTXLI-UHFFFAOYSA-N propane-1-sulfonic acid Chemical compound CCCS(O)(=O)=O KCXFHTAICRTXLI-UHFFFAOYSA-N 0.000 description 1
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- 229940005657 pyrophosphoric acid Drugs 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
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Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/542—Dye sensitized solar cells
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a method for synthesizing a zinc oxide nanowire array, which comprises the following steps: preparing a substrate, wherein a nanocrystalline zinc seed layer with the thickness larger than or equal to 10 mu m is deposited on the substrate, the nanocrystalline zinc seed layer consists of pure zinc, and the pure zinc is granular or sheet-shaped, and the granular and sheet-shaped reach nanoscale in any one or more dimensions; promoting the in-situ growth of the nanocrystalline zinc seed layer into a zinc oxide nanowire array by microwave treatment: immersing the substrate deposited with the nanocrystalline zinc seed layer into a microwave heat transfer medium, carrying out microwave for 1-30 min, taking out, naturally cooling at the room temperature of 20-25 ℃, washing with water, and drying to obtain the zinc oxide nanowire array. The prepared zinc oxide nanowire array is firmly combined with a substrate, and has strong corrosion resistance, photoelectric activity, light absorption capacity and photocatalysis performance.
Description
Technical Field
The invention belongs to the technical field of nano structure preparation, and particularly relates to a method for synthesizing a zinc oxide nanowire array.
Background
The zinc oxide nanowire array (ZnO nanowire array is ZnO NWA for short, the general wire diameter is less than 100nm, the length-diameter ratio is more than 10), and has wide application prospect in the fields of light emitting diodes, ultraviolet light detectors, dye sensitized solar cells and the like due to high photoelectric activity, large specific surface area and excellent stability. Currently, the synthetic methods of ZnO NWA can be divided into two phases, gas and liquid: the gas phase method mainly comprises physical gas phase deposition, chemical gas phase deposition, laser deposition, magnetron sputtering, thermal evaporation and thermal oxidation; liquid phase processes typically employ template-assisted electrodeposition, oxygen-assisted electrodeposition, electrochemical anodization, chemical deposition, and hydrothermal techniques. Although the quality of ZnO NWA produced by the gas phase method is higher, the method has severe conditions (high temperature or vacuum conditions are involved) and expensive equipment and higher cost. In contrast, the liquid phase method has lower treatment temperature and simple equipment, has more cost advantage in the preparation of ZnO NWA, but also has certain limitation. For example, electrodeposition is limited by the size of the template and requires continuous oxygen introduction into the electrolyte, which is inconvenient for large-scale preparation of ZnO NWA; anodic oxidation technology is limited by the substrate type (zinc foil, sheet or plate) and the subsequent heat treatment process, and is not convenient for large-scale popularization; for chemical deposition and hydrothermal methods, a gold catalytic layer or a zinc oxide nanoparticle seed layer needs to be prefabricated on the surface of the substrate, and the preparation of the prefabricated layer also involves high-cost, severe and complex preparation processes (such as magnetron sputtering, laser deposition or sol-gel technology). Although ZnO NWA can be prepared in a hydrothermal solution containing zinc ions, it is adsorbed to the surface of the substrate by physical action, and thus the binding force is poor. In addition, hydrothermal methods generally take longer, less than a few hours, more than ten hours, and have lower production efficiency, which requires development of more advanced liquid phase techniques.
Disclosure of Invention
The invention aims to overcome the defects of high cost, complex process, harsh conditions, insufficient bonding strength with a substrate, difficult mass production, long preparation period and the like in the prior art, and provides a method for synthesizing a zinc oxide nanowire array.
It is another object of the present invention to provide a zinc oxide nanowire array obtained by the above method.
The aim of the invention is achieved by the following technical scheme.
A method of synthesizing a zinc oxide nanowire array, comprising the steps of:
1) Preparing a substrate, wherein a nanocrystalline zinc seed layer with the thickness of more than or equal to 10 mu m is deposited on the substrate, the nanocrystalline zinc seed layer consists of pure zinc, the pure zinc is granular or sheet-shaped, and the granular and sheet-shaped nano-scale is achieved in any one or more dimensions;
in the step 1), the nano-scale is 10 0 ～10 2 nm。
In the step 1), one surface of the substrate for depositing the nanocrystalline zinc seed layer is a conductor.
In the above technical scheme, the material of the conductor is aluminum alloy, magnesium alloy, titanium alloy, foam copper, foam nickel, stainless steel, conductive glass, carbon paper or carbon cloth.
2) Promoting the in-situ growth of the nanocrystalline zinc seed layer into a zinc oxide nanowire array by microwave treatment: immersing the substrate deposited with the nanocrystalline zinc seed layer into a microwave heat transfer medium for 1-30 min, taking out, naturally cooling at room temperature of 20-25 ℃, washing with water, and drying to obtain a zinc oxide nanowire array, wherein the microwave heat transfer medium is water or an aqueous solution, the aqueous solution is a mixture of water and a solute, the solute is one or more of sodium hydroxide, potassium hydroxide, barium hydroxide, calcium hydroxide, sodium carbonate, sodium bicarbonate, potassium carbonate, potassium bicarbonate, hydrogen peroxide, ammonia water and zinc ion complexing agents, and the zinc ion complexing agents are at least one of citric acid, pyrophosphoric acid, ethylenediamine tetraacetic acid, dodecylsulfonic acid, hydroxyethylidene diphosphonic acid, amide, ethylenediamine, glycerol, tartaric acid, fluoroboric acid, acetic acid, polyvinylpyrrolidone, 3-mercapto-1-propanesulfonic acid, 3-S-thiopurine propanesulfonic acid, 3- (benzothiazolyl-2-mercapto) -propylsulfonate, benzotriazole, gelatin, ethylene glycol, poly propionic acid, polyacrylamide, 5-dimethylhydantoin and salts thereof.
In the step 2), the power of the microwaves is 100-800W.
In the step 2), the power of the microwave is 420 to 560W, and the microwave time is 1 to 20min, preferably 1 to 10min, more preferably 1 to 5min, still more preferably 1 to 3min.
In the above technical scheme, the concentration of the solute in the aqueous solution is less than or equal to 200g L -1 。
In the technical scheme, the method for obtaining the nanocrystalline zinc seed layer comprises the following steps:
a) Ultrasonic treating the substrate in acetone for 5-10 min, taking out, washing with deionized water, soaking the substrate in dilute sulfuric acid for 0.5-5 min, taking out the substrate, and washing with deionized water again;
in the a), the concentration of the dilute sulfuric acid is 5 to 20 and 20g L -1 。
b) Regulating the pH value of the electrolyte to be less than or equal to 2, placing the substrate obtained in the step a) into the electrolyte, performing electrodeposition for more than 8min, taking out, washing with deionized water, and obtaining a nanocrystalline zinc seed layer on the substrate, wherein the electrolyte comprises zinc sulfate, boric acid and water, and the concentration of the zinc sulfate in the electrolyte is 50-200 g L -1 The concentration of boric acid in the electrolyte is 5-100 g L -1 ；
In the step b), the electrolyte solution further includes: polyacrylamide with the concentration of 0.5-5 g L in the electrolyte -1 。
In said step b), the average current density of said electrodeposition is 1 to 20A dm -2 。
In said step b), the pH of the electrolyte is adjusted with sulfuric acid.
In said step b), the time of the electrodeposition treatment is 8 to 200min, preferably 8 to 60min.
The zinc oxide nanowire array obtained by the method.
In the above technical solution, the aspect ratio of the zinc oxide nanowires in the zinc oxide nanowire array is >10.
In the technical scheme, the diameter of the zinc oxide nanowire in the zinc oxide nanowire array is less than 100nm, and the length is more than or equal to 1 mu m.
Compared with the prior art, the invention has the following beneficial effects:
1. compared with the existing zinc oxide nanowire liquid phase preparation technology, the gold catalytic layer or the zinc oxide nanoparticle seed layer prepared by using granular or flaky pure zinc as the nanocrystalline zinc seed layer has lower preparation cost and is easier to popularize on a large scale;
2. step 2) of the invention (microwave induction technique) time-consuming preparation of the zinc oxide nanowire array from 10 of the traditional hydrothermal technique 0 ～10 1 The hour is shortened to 10 0 ～10 1 Minute (example 1), the production efficiency is greatly improved;
3. the length-diameter ratio of the zinc oxide nanowires in the zinc oxide nanowire array can be adjusted by adjusting the grain size of the nanocrystalline zinc seed layer, the composition of a microwave heat transfer medium, the microwave power and the microwave time;
4. the microwave heat transfer medium has simple composition, is convenient to maintain, does not contain toxic substances, and is environment-friendly;
5. the microwave induction technology has the advantages of simple operation, low cost, less energy consumption, short time consumption and easy large-area preparation, and has good effect through amplification experiments, and a compact and uniform zinc oxide nanowire array can be prepared on the surface of a substrate with the area of more than 10cm multiplied by 20 cm;
6. the prepared zinc oxide nanowire array is firmly combined with a substrate, has strong corrosion resistance, photoelectric activity, light absorption capacity and photocatalysis performance, and has wide application prospect in the fields of nano sensors, nano lasers, nano generators, light emitting diodes, solar cells, photocatalysis and the like.
Drawings
FIG. 1 is an SEM of (a) a nanocrystalline zinc seed layer and (b) a zinc oxide nanowire array of example 1;
FIG. 2 is an SEM of (a) a nanocrystalline zinc seed layer and (b) a zinc oxide nanowire array of example 2;
FIG. 3 is an SEM of the zinc oxide nanowire arrays obtained in examples 1 and 3-5, where a is example 3, b is example 4, c is example 5,d, and example 1;
FIG. 4 is an SEM of the zinc oxide nanowire arrays obtained in examples 1 and 6-8, where a is example 6, b is example 1, c is example 7,d, and example 8;
FIG. 5 is an SEM of a zinc oxide nanowire array obtained in example 9;
FIG. 6 is an SEM of a zinc oxide nanowire array obtained according to example 10;
FIG. 7 shows the Mott-Schottky test results of the zinc oxide nanowire arrays obtained in example 1;
FIG. 8 is a schematic illustration of photocatalytic CO using a zinc oxide nanowire array 2 Reduction test;
FIG. 9 is a nanocrystalline zinc seed layer (top) and zinc oxide nanowire array (bottom) of example 1;
FIG. 10 is an ultraviolet-visible absorption spectrum of the zinc oxide nanowire array obtained in example 1;
FIG. 11 is a photoluminescence spectrum of the zinc oxide nanowire array obtained in example 1;
fig. 12 is a flow chart of the method of the present invention.
Detailed Description
In the technical scheme of the invention, the preparation method of the nanocrystalline zinc seed layer can be as follows: electrochemical deposition, chemical deposition, vacuum evaporation, magnetron sputtering, chemical vapor deposition, physical vapor deposition, 3D printing or metal spraying plating, and zinc materials with nano surfaces can be obtained after electrochemical etching, shot blasting, hammering, laser impact or sand paper polishing. In the specific embodiment of the invention, the nano-crystalline zinc seed layer obtained by electrochemical deposition is used for illustration, and the technical scheme of the invention is further illustrated below by combining specific examples.
In the following examples, the substrate is cleaned prior to depositing the nanocrystalline zinc seed layer: it is ultrasonically degreased with alcohol and then rinsed with water.
Example 1
As shown in fig. 12, a method for synthesizing a zinc oxide nanowire array includes the steps of:
1) Preparing 180 mesh stainless steel as a substrate (substrate size 10cm×20 cm), and depositing a nanocrystalline zinc seed layer with thickness of 15 μm on the substrate, wherein the nanocrystalline zinc seed layer is composed of pure zinc, and the pure zinc is in the form of particles with grain size of about 50nm, as shown in a in fig. 1;
wherein, the method for obtaining the nanocrystalline zinc seed layer is a) and b):
a) Ultrasonic treating the substrate in acetone for 5min, taking out, washing with deionized water, and soaking the substrate to a concentration of 10g L -1 Removing rust in dilute sulfuric acid for 1min, taking out the substrate, and washing with deionized water again;
b) Adjusting the pH of the electrolyte to 1 with 98% sulfuric acid, placing the substrate obtained in step a) in the electrolyte at 25 ℃ and at an average current density of 3A dm -2 Is a strip of (2)Performing electrodeposition treatment under the substrate for 8min, taking out, washing with deionized water, and obtaining nanocrystalline zinc seed layer on the substrate, wherein the electrolyte is a mixture of zinc sulfate, polyacrylamide, boric acid and water, and the concentration of zinc sulfate in the electrolyte is 100g L -1 The concentration of boric acid in the electrolyte is 20g L -1 The concentration of polyacrylamide in the electrolyte is 1g L -1 ；
2) Promoting the in-situ growth of the nanocrystalline zinc seed layer into a zinc oxide nanowire array by microwave treatment: immersing the substrate deposited with the nanocrystalline zinc seed layer into a microwave heat transfer medium, taking out the substrate with 560W power for 2min, naturally cooling the substrate at the room temperature of 20-25 ℃, cleaning the substrate with water, and blow-drying the substrate with a blower to obtain a zinc oxide nanowire array, wherein the microwave heat transfer medium is an aqueous solution, the aqueous solution is a mixture of water and a solute, the solute is sodium hydroxide, and the concentration of the solute in the aqueous solution is 10g L -1 。
As shown in FIG. 1 b, the aspect ratio of the zinc oxide nanowires in the zinc oxide nanowire array is more than 10, the length of the zinc oxide nanowires is about 1 μm, and the diameter of the zinc oxide nanowires is about 50nm.
The microwave induction technology of the invention has simple operation, low cost, low energy consumption, short time consumption and easy large-area preparation, and has good effect through amplification experiments, and as shown in figure 9, the compact and uniform zinc oxide nanowire array can be prepared on the surface of a substrate with the area of more than 10cm multiplied by 20 cm.
Example 2
A method of synthesizing a zinc oxide nanowire array, comprising the steps of:
1) Preparing a mesh-shaped stainless steel as a substrate, and depositing a nanocrystalline zinc seed layer with the thickness of 20 mu m on the substrate, wherein the nanocrystalline zinc seed layer consists of pure zinc, and the pure zinc is sheet-shaped with the thickness of about 60nm, as shown in a in fig. 2;
wherein, the method for obtaining the nanocrystalline zinc seed layer is a) and b):
a) Ultrasonic treating the substrate in acetone for 5min, taking out, washing with deionized water, and soaking the substrate to a concentration of 10g L -1 Removing rust in dilute sulfuric acid for 1min, taking out the substrate, and washing with deionized water again;
b) Adjusting the pH of the electrolyte to 1 with 98% sulfuric acid, placing the substrate obtained in step a) in the electrolyte at 25 ℃ and at an average current density of 3A dm -2 Is subjected to electrodeposition treatment for 60min, taken out, rinsed with deionized water, and a nanocrystalline zinc seed layer is obtained on the substrate, wherein the electrolyte is a mixture of zinc sulfate, boric acid and water, and the concentration of the zinc sulfate in the electrolyte is 100g L -1 The concentration of boric acid in the electrolyte is 100g L -1 ；
2) Promoting the in-situ growth of the nanocrystalline zinc seed layer into a zinc oxide nanowire array by microwave treatment: immersing the substrate deposited with the nanocrystalline zinc seed layer into a microwave heat transfer medium, taking out the substrate with 560W power for 2min, naturally cooling the substrate at the room temperature of 20-25 ℃, cleaning the substrate with water, and blow-drying the substrate with a blower to obtain a zinc oxide nanowire array, wherein the microwave heat transfer medium is an aqueous solution, the aqueous solution is a mixture of water and a solute, the solute is sodium hydroxide, and the concentration of the solute in the aqueous solution is 10g L -1 。
As shown in FIG. 2 b, the aspect ratio of the zinc oxide nanowires in the zinc oxide nanowire array is more than 10, the length of the zinc oxide nanowires is about 1 μm, and the diameter of the zinc oxide nanowires is about 50nm.
Examples 3 to 8
A method of synthesizing a zinc oxide nanowire array, comprising the steps of:
1) Preparing a mesh-shaped stainless steel as a substrate on which a nanocrystalline zinc seed layer having a thickness of 20 μm is deposited, and obtaining the nanocrystalline zinc seed layer in the same manner as in example 1;
2) Promoting the in-situ growth of the nanocrystalline zinc seed layer into a zinc oxide nanowire array by microwave treatment: immersing the substrate deposited with the nanocrystalline zinc seed layer into a microwave heat transfer medium, taking out the substrate with P W power microwave T min, naturally cooling the substrate at the room temperature of 20-25 ℃, cleaning the substrate with water, and blow-drying the substrate with a blower to obtain a zinc oxide nanowire array, wherein the microwave heat transfer medium is an aqueous solution, the aqueous solution is a mixture of water and a solute, the solute is sodium hydroxide, and the concentration of the solute in the aqueous solution is 10g L -1 。
| Examples | P (Unit: W) | T (Unit: min) |
| Example 3 (comparative) | 140 | 2 |
| Example 4 (comparative) | 280 | 2 |
| Example 5 | 420 | 2 |
| Example 6 | 560 | 1 |
| Example 7 | 560 | 3 |
| Example 8 (comparative) | 560 | 5 |
The micro-morphology of the zinc oxide nanowire arrays prepared in examples 1, 3 to 5 is shown in fig. 3, and the micro-morphology of the zinc oxide nanowire arrays prepared in examples 1, 6 to 8 is shown in fig. 4.
As shown in fig. 3, the use of low power (140 w in example 3 and 280w in example 4) does not induce the growth of the nanocrystalline zinc seed layer into zinc oxide nanowires at the same microwave induction time of 2 min; when the microwave power is increased to 420w in the embodiment 5, the wire diameter of the grown zinc oxide nanowire is thick and uneven; in contrast, the 560w high power zinc oxide nanowires of example 1 were relatively uniform and moderate in both wire diameter and wire length.
As shown in fig. 4, at 560w power, the short time (1 min in example 6) was also insufficient to promote the growth of the nanocrystalline zinc seed layer into a zinc oxide nanowire array; as the microwave induction treatment time was prolonged (2 in example 1 and 3min in example 7), the wire diameter of the zinc oxide nanowire was gradually thickened; when the treatment time reached 5min (example 8), the wire diameter of the grown zinc oxide nanowires had exceeded 100nm. The above results demonstrate that adjusting the microwave treatment conditions can control the growth of the zinc oxide nanowire array.
As can be seen from fig. 3 and fig. 4, the zinc oxide nanowire array generated by higher power or longer time has thick wire diameter, and even is loose and easy to fall off.
Example 9
A method of synthesizing a zinc oxide nanowire array is substantially the same as example 1, except that "solute is sodium hydroxide" in example 1 is replaced with "solute is potassium hydroxide".
An SEM image of the zinc oxide nanowire array obtained in example 9 is shown in fig. 5, which illustrates that the zinc oxide nanowire array can be successfully prepared by changing the microwave heat transfer medium.
Example 10
A method for synthesizing a zinc oxide nanowire array is basically the same as that of example 1, except that "solute in example 1 is sodium hydroxide, and concentration of solute in aqueous solution is 10g L -1 The solute replaced by potassium pyrophosphate and sodium hydroxide, and the concentration of potassium pyrophosphate in the water solution is 20g L -1 The concentration of sodium hydroxide in the aqueous solution was 10gL -1 ”。
An SEM image of the zinc oxide nanowire array prepared in example 10 is shown in fig. 6, which illustrates that zinc oxide nanowire array can still be successfully grown by adding a zinc ion complexing agent to a heat transfer medium.
The zinc oxide nanowire array obtained in example 1 was subjected to a Mott-Schottky test, the test instrument was a Shanghai Hua CHI760E series double potentiostat, and the result is shown in fig. 7, and the slope of a linear fitting curve is negative, so that it can be inferred that the zinc oxide nanowire array prepared by the method is a p-type semiconductor.
Photocatalytic carbon dioxide reduction performance of the zinc oxide nanowire arrays prepared in example 1 were tested: photocatalytic CO was performed on the zinc oxide nanowire array prepared in example 1 2 The reduction test, the analysis of the gas product by a gas chromatograph, and the results are shown in FIG. 8, which shows that the zinc oxide nanowire array prepared by the invention can convert CO under the irradiation of simulated sunlight (visible light with the wavelength of 400-800 nm) 2 Catalytic reduction to CO and CH 4 And as the catalytic reaction time (abscissa in fig. 8) is prolonged, the yield of the generated mixture is gradually increased, thus proving the photocatalytic activity.
The specific experimental method comprises the following steps: photocatalytic CO 2 The reduction performance is rich in CO 2 And 100ml of ultrapure water. Specifically, first, 2X 2cm obtained in example 1 was used 2 Immersing the substrate and the zinc oxide nanowire array thereon in water; then, continuously introducing high-purity CO into the system 2 For 20min to expel air in the system to reach CO 2 Saturation; CO with simulated sunlight irradiation 2 Is successfully reduced to CO and CH on the surface of the zinc oxide nanowire array 4 The amount of reaction product can be measured in real time by gas chromatography (Agilent, model GC-6820), as shown in FIG. 8; the system temperature was maintained at 10 ℃ throughout the test.
TABLE 1 comparison of the comprehensive Properties of the present invention and the conventional liquid phase technique
Comparing the comprehensive performance of the invention with that of the traditional liquid phase technology, the comparison result is shown in table 1, and as can be seen from table 1, the invention has the advantages of shortest time consumption, no need of any template, high-cost seed layer/catalytic layer (zinc oxide nano particles or gold) and post-treatment, low cost and easy large-scale preparation.
As shown in FIG. 10, the zinc oxide nanowire array prepared in example 1 has a steep absorption edge under the illumination of 390nm, which indicates that the zinc oxide nanowire array has a strong light absorption activity in the near ultraviolet region, and the bandwidth of the zinc oxide nanowire array is about 3.15eV according to Tauc formula.
(αhv) 2 ＝D(hv-E g )
Wherein alpha is the light absorption coefficient, hv is the photon energy (eV), D is a constant, E g Bandwidth (eV).
As shown in fig. 11, the zinc oxide nanowire array prepared in example 1 shows a strong near-band edge emission peak under the illumination of 390nm wavelength, which indicates that the zinc oxide nanowire array has strong photoluminescence performance in the near ultraviolet region.
The above properties are similar to those reported in the literature for conventional hydrothermal techniques (table 2) using ZnO nanoparticles as a seed layer, as well as other liquid phase or meteorological methods (table 3) prepared zinc oxide nanowire arrays.
Compared with the existing hydrothermal technology, the method provided by the invention adopts the nanocrystalline zinc seed layer which is cheaper than the zinc oxide seed layer and simpler in preparation method, the zinc oxide nanowire array can be prepared faster through microwave treatment (taking example 1 as an example, the fastest preparation period is only 10min, and the electrodeposition zinc is 8min and the microwave treatment is 2 min), and the performance is no different from that of the zinc oxide nanowire array reported in the literature.
Table 2. The invention compares the preparation cycle and performance of zinc oxide nanowire arrays grown hydrothermally based on seed layers of zinc oxide nanoparticles made by different methods as reported in the literature.
Table 3. The invention compares the preparation cycle and performance of zinc oxide nanowire arrays prepared by weather or liquid phase methods reported in the literature.
Annotating symbolsRepresenting the preparation time during which the preparation cycle does not comprise a seed layer.
The foregoing has described exemplary embodiments of the invention, it being understood that any simple variations, modifications, or other equivalent arrangements which would not unduly obscure the invention may be made by those skilled in the art without departing from the spirit of the invention.
Claims (6)
1. The application of microwave treatment in-situ growth of a nanocrystalline zinc seed layer into a zinc oxide nanowire array is characterized in that the diameter of a zinc oxide nanowire in the zinc oxide nanowire array is less than 100nm, and the length is more than or equal to 1 mu m, and the method for synthesizing the zinc oxide nanowire array comprises the following steps:
1) Preparing a substrate, wherein a nanocrystalline zinc seed layer with the thickness of more than or equal to 10 mu m is deposited on the substrate, the nanocrystalline zinc seed layer consists of pure zinc, the pure zinc is sheet-shaped, and the sheet-shaped reaches nanoscale in any one or more dimensions;
2) Promoting the in-situ growth of the nanocrystalline zinc seed layer into a zinc oxide nanowire array by microwave treatment: immersing the substrate deposited with the nanocrystalline zinc seed layer into a microwave heat transfer medium, carrying out microwave for 2min, taking out, naturally cooling at the room temperature of 20-25 ℃, washing with water, and drying to obtain a zinc oxide nanowire array, wherein the microwave power is 560W, the microwave heat transfer medium is water or an aqueous solution, the aqueous solution is a mixture of water and a solute, the solute is sodium hydroxide, and the solute in the aqueous solutionIs 10g L in concentration -1 ；
The method for obtaining the nanocrystalline zinc seed layer comprises the following steps:
a) Ultrasonic treating the substrate in acetone for 5-10 min, taking out, washing with water, soaking the substrate in dilute sulfuric acid for 0.5-5 min, taking out the substrate, and washing with water again;
b) Adjusting the pH of the electrolyte to 1, placing the substrate obtained in the step a) in the electrolyte at 25 ℃ and obtaining the electrolyte with the average current density of 3A dm -2 The nano-crystalline zinc seed layer is obtained on the substrate after the electro-deposition treatment for 60min, the taking out and the washing, wherein the electrolyte is a mixture of zinc sulfate, boric acid and water, and the concentration of the zinc sulfate in the electrolyte is 100gL -1 The concentration of boric acid in the electrolyte is 100g L -1 。
2. The use according to claim 1, wherein in said a), the concentration of dilute sulfuric acid is 5 to 20gL -1 。
3. The use according to claim 1, characterized in that in step b) the pH of the electrolyte is adjusted with sulfuric acid.
4. The use according to claim 1, wherein in said step 1), said nanoscale is 10 0 ～10 2 nm。
5. The use according to claim 1, wherein the substrate is conductive on one side for depositing a nanocrystalline zinc seed layer.
6. The use according to claim 5, wherein the conductor is made of aluminum alloy, magnesium alloy, titanium alloy, copper foam, nickel foam, stainless steel, conductive glass, carbon paper or carbon cloth.
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| CN109467857A (en) * | 2018-10-19 | 2019-03-15 | 南京邮电大学 | A kind of zinc oxide/polytetrafluorethylenano nano composite material and preparation method |
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