CN114015990A - Preparation method and application of nickel oxide-gold-zinc oxide coaxial nano array - Google Patents
Preparation method and application of nickel oxide-gold-zinc oxide coaxial nano array Download PDFInfo
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- CN114015990A CN114015990A CN202111190422.6A CN202111190422A CN114015990A CN 114015990 A CN114015990 A CN 114015990A CN 202111190422 A CN202111190422 A CN 202111190422A CN 114015990 A CN114015990 A CN 114015990A
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- -1 nickel oxide-gold-zinc oxide Chemical compound 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 106
- 239000002070 nanowire Substances 0.000 claims abstract description 46
- 239000011787 zinc oxide Substances 0.000 claims abstract description 43
- 238000004544 sputter deposition Methods 0.000 claims abstract description 38
- 239000000758 substrate Substances 0.000 claims abstract description 35
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 32
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 31
- 239000010931 gold Substances 0.000 claims abstract description 26
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 25
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052737 gold Inorganic materials 0.000 claims abstract description 21
- 239000004246 zinc acetate Substances 0.000 claims abstract description 21
- DXWQDVZGROCFPG-UHFFFAOYSA-N [O--].[Zn++].[Au+3] Chemical compound [O--].[Zn++].[Au+3] DXWQDVZGROCFPG-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910000480 nickel oxide Inorganic materials 0.000 claims abstract description 18
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052786 argon Inorganic materials 0.000 claims abstract description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 16
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims abstract description 16
- 239000004312 hexamethylene tetramine Substances 0.000 claims abstract description 16
- 239000001301 oxygen Substances 0.000 claims abstract description 16
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 13
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- 239000007789 gas Substances 0.000 claims abstract description 9
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000007864 aqueous solution Substances 0.000 claims abstract description 7
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 42
- 239000012498 ultrapure water Substances 0.000 claims description 42
- 239000000463 material Substances 0.000 claims description 21
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 18
- 239000013077 target material Substances 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 239000002131 composite material Substances 0.000 claims description 15
- 239000011521 glass Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 14
- 238000002294 plasma sputter deposition Methods 0.000 claims description 13
- 238000011065 in-situ storage Methods 0.000 claims description 10
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- 238000013329 compounding Methods 0.000 claims description 9
- 238000009210 therapy by ultrasound Methods 0.000 claims description 9
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 4
- 229910052697 platinum Inorganic materials 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 239000004332 silver Substances 0.000 claims description 4
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 3
- 239000008204 material by function Substances 0.000 abstract description 2
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- 235000019441 ethanol Nutrition 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
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Abstract
The invention discloses a preparation method and application of a nickel oxide-gold-zinc oxide coaxial nano array. Belongs to the field of nano photoelectric functional materials, and comprises the following specific steps: 1. placing the pretreated conductive substrate in a magnetron sputtering instrument, and sputtering a zinc oxide target in a mixed gas of high-purity oxygen and high-purity argon to obtain a zinc oxide seed layer; 2. then adding the zinc oxide nanowire array into an aqueous solution of zinc acetate and hexamethylenetetramine, and carrying out hydrothermal synthesis to obtain a zinc oxide nanowire array; 3. then washing and drying the obtained product, and then carrying out plasma nano-gold sputtering; obtaining a gold-zinc oxide nanowire array; 4. and finally, placing the gold-coated zinc oxide nanowire array (gold-zinc oxide nanowire array) in a magnetron sputtering instrument for modifying nickel oxide, and finally obtaining the nickel oxide-gold-zinc oxide coaxial nanowire array. The nickel oxide-gold-zinc oxide coaxial nanowire array has the characteristics of controllable appearance, photoelectric cooperation, good repeatability and the like.
Description
Technical Field
The invention belongs to the field of nano photoelectric functional materials, and relates to a preparation method of a nickel oxide-gold-zinc oxide coaxial nanowire array for photoelectric sensing and application thereof in photoelectric sensing.
Background
The nano photoelectric material, especially the semiconductor material, has wide application prospect in the fields of photoelectric detection, luminescent devices, catalytic degradation, gas sensing and the like. The composition, morphology and size of the nano photoelectric material can affect the application performance of the nano photoelectric material. Therefore, the acquisition of nano-heterojunctions with different compositions, morphologies and sizes attracts the research interest. As transition metal oxides, zinc oxide and nickel oxide exhibit excellent properties in the fields of photodetection, light-emitting devices, catalytic degradation, gas sensing, and the like. Compared with a single component, the p-n heterojunction compositely constructed by the zinc oxide and the nickel oxide can greatly improve the photoelectric property of the material. Meanwhile, the surface plasmon resonance effect of the nano metal particles (such as nano gold) can further improve the photoelectric conversion of the semiconductor. Therefore, the composite material based on zinc oxide, nickel oxide and nanogold is expected to achieve the synergistic enhancement of photoelectric signals.
The current preparation method for synthesizing nickel oxide-gold-zinc oxide composite material generally comprises the following steps: surface reaction, self-assembly, solution, hydrothermal, electrodeposition, and the like. For the nickel oxide-gold-zinc oxide composite material, a solution method is generally adopted to ensure that a shell material achieves a uniform and compact wrapping effect, but the solution preparation environment is complex, the process stability is poor, large-area growth is difficult to carry out, and the zinc oxide substrate is soaked in an aqueous solution for many times or for a long time, so that the surface defect state of the zinc oxide can be changed in the process.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a coaxial heterojunction composite material based on a nickel oxide-gold-zinc oxide nanowire, the other aim of the invention is to controllably construct a ternary system coaxial heterojunction through a physical deposition method, and the other aim of the invention is to realize photoelectric detection of the composite material in a liquid environment.
The technical scheme is as follows: the invention relates to a preparation method of a nickel oxide-gold-zinc oxide coaxial nanowire array; the preparation method comprises the following specific steps:
(1) putting the pretreated conductive substrate into a magnetron sputtering instrument, and vacuumizing by a mechanical pump and a molecular pump to ensure that the vacuum degree in the cavity is less than or equal to 7.0 multiplied by 10-4Pa, adjusting a radio frequency system to glow a zinc oxide target material, firstly carrying out pre-sputtering to clean the surface of the target material, and then introducing high-purity oxygen and high-purity argon to obtain a substrate sputtered with a zinc oxide seed layer;
(2) preparing zinc acetate and hexamethylenetetramine aqueous solution with equal mol, adding the substrate obtained in the step (1), the zinc acetate and the hexamethylenetetramine aqueous solution into a hydrothermal reaction kettle, putting the hydrothermal reaction kettle into a drying oven with the temperature of 90-120 ℃ for reaction for 4-10h, washing the hydrothermal reaction kettle with ultrapure water, and airing or drying the hydrothermal reaction kettle to obtain a zinc oxide nanowire array;
(3) placing the obtained zinc oxide nanowire array in a plasma sputtering instrument and sputtering under a gold target to obtain a gold-zinc oxide nanowire array;
(4) and finally, placing the obtained gold-zinc oxide nanowire array in a magnetron sputtering instrument for in-situ compounding of a nickel oxide layer, thereby finally obtaining the nickel oxide-gold-zinc oxide coaxial nanowire array.
Further, in the step (1), the conductive substrate is FTO conductive glass;
the pretreated conductive substrate refers to: and (3) carrying out ultrasonic treatment on the untreated conductive substrate in ultrapure water, acetone, absolute ethyl alcohol and ultrapure water in sequence, then cleaning with ultrapure water, and airing to obtain the pretreated conductive substrate.
Further, in the step (1), the radio frequency power of the magnetron sputtering instrument is 50-200W;
further, in the step (1), the gas flow rate of the high-purity oxygen is 5-15sccm, the gas flow rate of the high-purity argon is 40-100sccm, and the working pressure of the high-purity oxygen and the high-purity argon is 1-3 Pa.
Further, in the step (1), the thickness of the substrate of the obtained sputtered zinc oxide seed layer is 10-30 nm.
Further, in the step (2), the concentration of the zinc acetate and the hexamethylene tetramine is 0.005-0.05 mol/L.
Further, in the step (3), the sputtering time of the plasma sputtering instrument is 45-120 s.
Further, in the step (4), the magnetron sputtering time of the magnetron sputtering apparatus is 1-20 min.
Further, the nano photoelectric functional material with the coaxial structure is prepared by the method.
Furthermore, the nano photoelectric functional material has synergistically enhanced photoelectric sensing performance.
Further, the application of the nano photoelectric functional material with the coaxial structure in photoelectric sensing; the application is specifically as follows: the photoelectric sensing under the liquid environment is completed by taking the conductive substrate of the modified composite material as a working electrode and taking a platinum net and a silver/silver chloride electrode as a counter electrode and a reference electrode respectively; the photoelectric superiority of the prepared nickel oxide-gold-zinc oxide nanowire array is verified by comparing the current responses of different modified materials; the nano photoelectric functional material has excellent photoelectric sensing performance.
Has the advantages that: compared with the prior art, when the zinc oxide nanowire array is prepared, the zinc oxide seed layer is prepared by adopting magnetron sputtering, and the obtained zinc oxide nanowire preferentially grows along one crystal face; the coaxial heterojunction of the nickel oxide-gold-zinc oxide nanowire array is obtained by a physical deposition method (such as plasma sputtering and magnetron sputtering); the zinc oxide is an n-type semiconductor, has wide direct band gap (3.37eV) and high exciton confinement energy (60meV), and is more beneficial to light absorption and carrier separation and transportation by a zinc oxide array; the nano-gold has good surface plasma resonance effect; and the nickel oxide serving as the p-type semiconductor can form a p-n heterojunction with zinc oxide to promote the transport of carriers, so that the nano composite material prepared by combining the nickel oxide, the nano gold and the zinc oxide has excellent photoelectric properties.
Drawings
FIG. 1 is an X-ray diffraction pattern of example four of the present invention;
FIG. 2 is a scanning electron microscope image and a transmission electron microscope image of a fourth embodiment of the present invention;
FIG. 3 is a UV-VIS diffuse reflectance spectrum of example V of the present invention;
FIG. 4 is a fluorescence spectrum of example six of the present invention;
FIG. 5 is a photo current result graph of the composite material modified electrode obtained in the fourth embodiment of the present invention in a liquid environment;
FIG. 6 is a flow chart of the operation of the present invention.
Detailed Description
The invention is further described below with reference to the following figures and specific examples.
As shown in fig. 6, a method for preparing a nickel oxide-gold-zinc oxide coaxial nanowire array according to the present invention; the preparation method comprises the following specific steps:
(1) putting the pretreated conductive substrate into a magnetron sputtering instrument, and vacuumizing by a mechanical pump and a molecular pump to ensure that the vacuum degree in the cavity is less than or equal to 7.0 multiplied by 10-4Pa, adjusting a radio frequency system to glow a zinc oxide target material, pre-sputtering for a period of time to clean the surface of the target material, stabilizing the system, and introducing high-purity oxygen and high-purity argon to obtain a substrate sputtered with a zinc oxide seed layer;
(2) preparing equimolar zinc acetate [ Zn (CH)3COO)2·2H2O]And hexamethylenetetramine [ (CH)2)6N4]Adding the substrate obtained in the step (1), zinc acetate and a hexamethylenetetramine aqueous solution into a hydrothermal reaction kettle, putting the hydrothermal reaction kettle into a drying oven at the temperature of 90-120 ℃ for reaction for 4-10 hours, washing the hydrothermal reaction kettle with ultrapure water, and airing or drying the hydrothermal reaction kettle to obtain a zinc oxide nanowire array;
(3) placing the zinc oxide nanowire array obtained in the step (2) in a plasma sputtering instrument and sputtering under a gold target to obtain a gold-zinc oxide nanowire array;
(4) and finally, placing the gold-zinc oxide nanowire array obtained in the step (3) in a magnetron sputtering instrument for in-situ compounding of a nickel oxide layer, thereby finally obtaining the nickel oxide-gold-zinc oxide coaxial nanowire array.
Further, in the step (1), the conductive substrate is FTO conductive glass;
the pretreated conductive substrate refers to: and (3) carrying out ultrasonic treatment on the untreated conductive substrate in ultrapure water, acetone, absolute ethyl alcohol and ultrapure water in sequence, then cleaning with ultrapure water, and airing to obtain the pretreated conductive substrate.
Further, in the step (1), the radio frequency power of the magnetron sputtering instrument is 50-200W;
further, in the step (1), the gas flow rate of the high-purity oxygen is 5-15sccm, the gas flow rate of the high-purity argon is 40-100sccm, and the working pressure of the high-purity oxygen and the high-purity argon is 1-3 Pa.
Further, in the step (1), the thickness of the substrate of the obtained sputtered zinc oxide seed layer is 10-30 nm.
Further, in the step (2), the concentration of the zinc acetate and the hexamethylene tetramine is 0.005-0.05 mol/L.
Further, in the step (3), the sputtering time of the plasma sputtering instrument is 45-120 s.
Further, in the step (4), the magnetron sputtering time of the magnetron sputtering apparatus is 1-20 min.
Further, the nano photoelectric functional material with the coaxial structure is prepared by the method.
Furthermore, the nano photoelectric functional material has synergistically enhanced photoelectric sensing performance.
Further, the application of the nano photoelectric functional material with the coaxial structure in photoelectric chemical sensing; the application is specifically as follows: the photoelectric sensing under the liquid environment is completed by taking the conductive substrate of the modified composite material as a working electrode and taking a platinum net and a silver/silver chloride electrode as a counter electrode and a reference electrode respectively; the photoelectric superiority of the prepared nickel oxide-gold-zinc oxide nanowire array is verified by comparing the current responses of different modified materials; the nano photoelectric functional material has excellent photoelectric sensing performance.
The working principle is as follows: the physical deposition method is an in-situ synthesis method, and can be used for controllably synthesizing the multielement nano composite material by adjusting the appearance of the material. The composition, morphology, energy level structure, etc. of the photoelectric material can affect the photoelectric characteristics.
The first embodiment,
(1) Cutting the FTO conductive glass into 0.5 multiplied by 1.0cm2Slicing, sequentially subjecting to ultrasonic treatment in ultrapure water, acetone, anhydrous ethanol, and ultrapure water for 10min, cleaning with ultrapure water, air drying, and soaking in anhydrous ethanol;
(2) firstly, fixing a clean FTO conductive glass by using a high-temperature resistant adhesive tape at a height of 0.5 multiplied by 0.5cm2The electrode area is arranged in a magnetic control cavity, and then the vacuum degree in the cavity is pumped by a mechanical pump and a molecular pump to reach 5.0 multiplied by 10-4Pa, adjusting a radio frequency system to start the zinc oxide target, pre-sputtering for a period of time to clean the surface of the target, and stabilizing the system; when the temperature in the cavity is stable, simultaneously introducing 5sccm high-purity oxygen and 50sccm high-purity argon, wherein the working pressure is 2Pa, the radio frequency power is 50W, and the sputtering time is 40min to obtain a sputtered zinc oxide seed layer with the thickness of 12 nm;
(3) dissolving 0.219g of zinc acetate in 100mL of ultrapure water, magnetically stirring for 10min to completely dissolve the zinc acetate, then adding 0.140g of hexamethylenetetramine, continuously stirring for 10min, and uniformly mixing to obtain a precursor solution; adding the solution into a hydrothermal reaction kettle, soaking the FTO conductive substrate modified in the step (2) in the precursor solution at a certain angle with the conductive surface facing downwards relative to the wall of the hydrothermal reaction kettle, putting the hydrothermal reaction kettle into an oven, carrying out hydrothermal treatment for 4 hours at 90 ℃, washing with ultrapure water, and drying at 40 ℃ to obtain a zinc oxide nanowire array;
(4) placing the zinc oxide nanorod array obtained in the step (3) in a plasma sputtering instrument to sputter 50s of nano-gold to obtain a gold-zinc oxide nanowire array;
(5) and (5) placing the gold-zinc oxide nanowire array obtained in the step (4) in a magnetron sputtering instrument for sputtering for 3min to obtain the nickel oxide-gold-zinc oxide nanowire array by in-situ compounding of nickel oxide.
Example two
(1) Cutting the FTO conductive glass into 0.5 multiplied by 1.0cm2Slicing, sequentially subjecting to ultrasonic treatment in ultrapure water, acetone, anhydrous ethanol, and ultrapure water for 10min, cleaning with ultrapure water, air drying, and soaking in anhydrous ethanol;
(2) firstly, fixing a clean FTO conductive glass by using a high-temperature resistant adhesive tape at a height of 0.5 multiplied by 0.5cm2The electrode area is arranged in a magnetic control cavity, and then the vacuum degree in the cavity is pumped by a mechanical pump and a molecular pump to reach 6.0 multiplied by 10-4Pa, adjusting a radio frequency system to glow the zinc oxide target material, pre-sputtering for a period of time to clean the surface of the target material, and stabilizing the system; when the temperature in the cavity is stable, simultaneously introducing 10sccm high-purity oxygen and 100sccm high-purity argon, wherein the working pressure is 3Pa, the radio frequency power is 200W, and the sputtering time is 40min to obtain a sputtered zinc oxide seed layer with the thickness of 36 nm;
(3) 2.190g of zinc acetate is dissolved in 100mL of ultrapure water, the mixture is magnetically stirred for 10min to be completely dissolved, then 1.400g of hexamethylenetetramine is added, the mixture is continuously stirred for 10min and is uniformly mixed, and a precursor solution is obtained; adding the solution into a hydrothermal reaction kettle, soaking the FTO conductive substrate modified in the step (2) in the precursor solution at a certain angle with the conductive surface facing downwards relative to the wall of the hydrothermal reaction kettle, putting the hydrothermal reaction kettle into an oven, carrying out hydrothermal treatment for 10 hours at 120 ℃, washing with ultrapure water, and drying in the sun to obtain a zinc oxide nanowire array;
(4) placing the zinc oxide nanowire array obtained in the step (3) in a plasma sputtering instrument to sputter 110s of nano-gold to obtain a gold-zinc oxide nanowire array;
(5) and (5) placing the gold-zinc oxide nanowire array obtained in the step (4) in a magnetron sputtering instrument for sputtering for 8min to obtain the nickel oxide-gold-zinc oxide nanowire array by in-situ compounding of nickel oxide.
EXAMPLE III
(1) Cutting the FTO conductive glass into 0.5 multiplied by 1.0cm2Slicing, sequentially subjecting to ultrasonic treatment in ultrapure water, acetone, anhydrous ethanol, and ultrapure water for 10min, cleaning with ultrapure water, air drying, and soaking in anhydrous ethanol;
(2) firstly, fixing a clean FTO conductive glass by using a high-temperature resistant adhesive tape at a height of 0.5 multiplied by 0.5cm2The electrode area is arranged in a magnetic control cavity, and then the vacuum degree in the cavity is pumped by a mechanical pump and a molecular pump to reach 4.0 multiplied by 10-4Pa, adjusting a radio frequency system to glow the zinc oxide target material, pre-sputtering for a period of time to clean the surface of the target material, and stabilizing the system; when the temperature in the cavity is stable, simultaneously introducing 8sccm high-purity oxygen and 80sccm high-purity argon, wherein the working pressure is 2Pa, the radio frequency power is 125W, and the sputtering time is 40min to obtain a sputtered zinc oxide seed layer with the thickness of 24 nm;
(3) dissolving 1.095g of zinc acetate in 100mL of ultrapure water, magnetically stirring for 10min to completely dissolve the zinc acetate, then adding 0.700g of hexamethylenetetramine, continuously stirring for 10min, and uniformly mixing to obtain a precursor solution; adding the solution into a hydrothermal reaction kettle, soaking the FTO conductive substrate modified in the step (2) in the precursor solution at a certain angle relative to the wall of the hydrothermal reaction kettle with the conductive surface facing downwards, putting the hydrothermal reaction kettle into an oven, carrying out hydrothermal treatment for 7 hours at 105 ℃, washing with ultrapure water, and drying at 50 ℃ to obtain a zinc oxide nanowire array;
(4) placing the zinc oxide nanowire array obtained in the step (3) in a plasma sputtering instrument to sputter 90s of nano-gold to obtain a gold-zinc oxide nanowire array;
(5) and (5) placing the gold-zinc oxide nanowire array obtained in the step (4) in a magnetron sputtering instrument for sputtering for 12min to obtain the nickel oxide-gold-zinc oxide nanowire array by in-situ compounding of nickel oxide.
Example four
(1) Cutting the FTO conductive glass into 0.5 multiplied by 1.0cm2Slicing, sequentially subjecting to ultrasonic treatment in ultrapure water, acetone, anhydrous ethanol, and ultrapure water for 10min, cleaning with ultrapure water, air drying, and soaking in anhydrous ethanol;
(2) firstly, fixing a clean FTO conductive glass by using a high-temperature resistant adhesive tape at a height of 0.5 multiplied by 0.5cm2The electrode area is arranged in a magnetic control cavity, and then the vacuum degree in the cavity is pumped by a mechanical pump and a molecular pump to reach 7.0 multiplied by 10-4Pa, adjusting a radio frequency system to glow the zinc oxide target material, pre-sputtering for a period of time to clean the surface of the target material, and stabilizing the system; when the temperature in the cavity is stable, simultaneously introducing 5sccm high-purity oxygen and 55sccm high-purity argon, wherein the working pressure is 2Pa, the radio frequency power is 100W, and the sputtering time is 40min to obtain a sputtered zinc oxide seed layer with the thickness of 15 nm;
(3) dissolving 0.549g of zinc acetate in 100mL of ultrapure water, magnetically stirring for 10min to completely dissolve the zinc acetate, then adding 0.351g of hexamethylenetetramine, continuously stirring for 10min, and uniformly mixing to obtain a precursor solution; adding the solution into a hydrothermal reaction kettle, soaking the FTO conductive substrate modified in the step (2) in the precursor solution at a certain angle with the conductive surface facing downwards relative to the wall of the hydrothermal reaction kettle, putting the hydrothermal reaction kettle into an oven, carrying out hydrothermal treatment for 4 hours at 90 ℃, washing with ultrapure water, and drying at 60 ℃ to obtain a zinc oxide nanowire array;
(4) placing the zinc oxide nanowire array obtained in the step (3) in a plasma sputtering instrument to sputter nano-gold for 70s to obtain a gold-zinc oxide nanowire array;
(5) and (5) placing the gold-zinc oxide nanowire array obtained in the step (4) in a magnetron sputtering instrument for sputtering for 10min to obtain the nickel oxide-gold-zinc oxide nanowire array by in-situ compounding of nickel oxide.
EXAMPLE five
(1) Cutting the FTO conductive glass into 0.5 multiplied by 1.0cm2Slicing the obtained product in ultrapure water, acetone, and anhydrous ethyl acetatePerforming ultrasonic treatment in alcohol and ultrapure water for 10min respectively, cleaning with ultrapure water, air drying, and soaking in anhydrous ethanol;
(2) firstly, fixing a clean FTO conductive glass by using a high-temperature resistant adhesive tape at a height of 0.5 multiplied by 0.5cm2The electrode area is arranged in a magnetic control cavity, and then the vacuum degree in the cavity is pumped by a mechanical pump and a molecular pump to reach 7.0 multiplied by 10-4Pa, adjusting a radio frequency system to glow the zinc oxide target material, pre-sputtering for a period of time to clean the surface of the target material, and stabilizing the system; when the temperature in the cavity is stable, simultaneously introducing 5sccm high-purity oxygen and 55sccm high-purity argon, wherein the working pressure is 2Pa, the radio frequency power is 100W, and the sputtering time is 30min to obtain a sputtered zinc oxide seed layer with the thickness of 24 nm;
(3) dissolving 0.549g of zinc acetate in 100mL of ultrapure water, magnetically stirring for 10min to completely dissolve the zinc acetate, then adding 0.351g of hexamethylenetetramine, continuously stirring for 10min, and uniformly mixing to obtain a precursor solution; adding the solution into a hydrothermal reaction kettle, soaking the FTO conductive substrate modified in the step (2) in the precursor solution at a certain angle with the conductive surface facing downwards relative to the wall of the hydrothermal reaction kettle, putting the hydrothermal reaction kettle into an oven, carrying out hydrothermal treatment for 4 hours at 90 ℃, washing with ultrapure water at 60 ℃ and drying to obtain a zinc oxide nanowire array;
(4) placing the zinc oxide nanowire array obtained in the step (3) in a plasma sputtering instrument for respectively sputtering nano-gold for 10s, 30s, 50s, 70s, 90s and 110s to obtain a gold-zinc oxide nanowire array;
(5) and (5) placing the gold-zinc oxide nanowire array obtained in the step (4) in a magnetron sputtering instrument for sputtering nickel oxide for 15min to carry out in-situ compounding, so as to obtain the nickel oxide-gold-zinc oxide nanowire array.
EXAMPLE six
(1) Cutting the FTO conductive glass into 0.5 multiplied by 1.0cm2Slicing, sequentially subjecting to ultrasonic treatment in ultrapure water, acetone, anhydrous ethanol, and ultrapure water for 10min, cleaning with ultrapure water, air drying, and soaking in anhydrous ethanol;
(2) firstly, fixing a clean FTO conductive glass by using a high-temperature resistant adhesive tape at a height of 0.5 multiplied by 0.5cm2The area of the electrode(s) of (a),placing in a magnetic control cavity, and vacuumizing by a mechanical pump and a molecular pump to make the vacuum degree in the cavity reach 7.0 × 10-4Pa, adjusting a radio frequency system to glow the zinc oxide target material, pre-sputtering for a period of time to clean the surface of the target material, and stabilizing the system; when the temperature in the cavity is stable, simultaneously introducing 5sccm high-purity oxygen and 55sccm high-purity argon, wherein the working pressure is 2Pa, the radio frequency power is 100W, and the sputtering time is 30min to obtain a sputtered zinc oxide seed layer with the thickness of 24 nm;
(3) dissolving 0.549g of zinc acetate in 100mL of ultrapure water, magnetically stirring for 10min to completely dissolve the zinc acetate, then adding 0.351g of hexamethylenetetramine, continuously stirring for 10min, and uniformly mixing to obtain a precursor solution; adding the solution into a hydrothermal reaction kettle, soaking the FTO conductive substrate modified in the step (2) in the precursor solution at a certain angle with the conductive surface facing downwards relative to the wall of the hydrothermal reaction kettle, putting the hydrothermal reaction kettle into an oven, carrying out hydrothermal treatment for 4 hours at 90 ℃, washing with ultrapure water at 60 ℃ and drying to obtain a zinc oxide nanowire array;
(4) and (4) placing the zinc oxide nanowire array obtained in the step (3) in a plasma sputtering instrument to sputter nano-gold for 70s respectively to obtain a gold-zinc oxide nanowire array.
(5) And (3) placing the gold-zinc oxide nanowire array obtained in the step (4) in a magnetron sputtering instrument for sputtering nickel oxide for 5, 8, 10 and 15min in-situ compounding to obtain the nickel oxide-gold-zinc oxide nanowire array.
Wherein, the X-ray diffraction pattern, the scanning electron microscope pattern and the transmission electron microscope pattern of the nickel oxide-gold-zinc oxide modified electrode (NiO-Au NPs-ZnO NWs/FTO) obtained in the fourth embodiment are respectively shown in figures 1 and 2; as can be seen from FIG. 1, the diffraction peaks of NiO-Au NPs-ZnO NRs/FTO match those of the standard card (NiO: 47-1049, Au: 04-0784, ZnO: 36-1451, FTO: 41-1445); as shown in fig. 2 (a), the ternary composite material obtained based on nickel oxide-gold-zinc oxide is in the form of a nano-array; further, as shown in fig. 2 (b), it can be seen that nickel oxide and gold nanoparticles are uniformly distributed on the surface of the zinc oxide nanowire, and a ternary coaxial heterojunction is formed.
The absorption spectra of the nanogold-zinc oxide composite material obtained by sputtering nanogold in the fifth example at different times are shown in fig. 3, and the sputtering times corresponding to the nanogold are 10, 30, 50, 70, 90 and 110 s; as can be seen from fig. 3 (a), the nano-gold particles are distributed on the surface of the zinc oxide nanowire, so that the ultraviolet absorption of the zinc oxide is reduced; as shown in fig. 3 (b), as the sputtering time of the nano-gold increases, the visible region absorption spectrum of the composite structure is significantly red-shifted and the intensity becomes larger; the red shift of the absorption spectrum is related to the size of the surface nano gold particles, and when the spectral intensity is increased, the energy transfer between the zinc oxide and the nano gold is realized; the ultraviolet absorption strength and the visible absorption strength of the composite structure are comprehensively considered, and the nano-gold sputtered on the surface of the zinc oxide nano-wire for 70s is taken as the basis of the subsequent experiment.
In the sixth embodiment, a layer of NiO is continuously modified on the surface of Au NPs/ZnO NWs to construct a P-N heterojunction, so that the photoelectric conversion efficiency is further improved; the sputtering time of the nickel oxide is respectively 5min, 8min, 10min and 15min, and as can be seen from a fluorescence spectrogram (figure 4), the luminescence of the composite structure is gradually weakened along with the prolonging of the sputtering time, and the luminescence is weakest when the sputtering time is 10 min; then sputtering for 15min to increase the luminous intensity; therefore, sputtering of 10min NiO was selected.
The photoelectric composite material obtained by the invention is applied to a liquid environment, and shows excellent photoelectric sensing performance:
in addition, the NiO-Au NPs-ZnO NWs/FTO in the fourth example is placed in an electrolyte with the concentration of 0.01mol/L phosphate buffer solution (PBS, pH 7.0), and a platinum mesh and a silver/silver chloride electrode are respectively used as a counter electrode and a reference electrode; measuring the photocurrent of the composite material under simulated sunlight for 10s of illumination and 10s of darkness; as can be seen from fig. 5, after the surfaces of nickel oxide and nano-gold re-zinc oxide are modified, the photocurrent response is enhanced, and when the ternary composite material is formed, the photocurrent response is strongest.
The above is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above-mentioned embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and embellishments within the scope of the invention may be made by those skilled in the art without departing from the principle of the invention.
Claims (10)
1. A preparation method of a nickel oxide-gold-zinc oxide coaxial nanowire array is characterized by comprising the following steps of; the preparation method comprises the following specific steps:
(1) putting the pretreated conductive substrate into a magnetron sputtering instrument, and vacuumizing by a mechanical pump and a molecular pump to ensure that the vacuum degree in the cavity is less than or equal to 7.0 multiplied by 10-4Pa, adjusting a radio frequency system to glow a zinc oxide target material, firstly carrying out pre-sputtering to clean the surface of the target material, and then introducing high-purity oxygen and high-purity argon to obtain a substrate sputtered with a zinc oxide seed layer;
(2) preparing zinc acetate and hexamethylenetetramine aqueous solution with equal mol, adding the substrate obtained in the step (1), the zinc acetate and the hexamethylenetetramine aqueous solution into a hydrothermal reaction kettle, putting the hydrothermal reaction kettle into a drying oven with the temperature of 90-120 ℃ for reaction for 4-10h, washing the hydrothermal reaction kettle with ultrapure water, and airing or drying the hydrothermal reaction kettle to obtain a zinc oxide nanowire array;
(3) placing the obtained zinc oxide nanowire array in a plasma sputtering instrument and sputtering under a gold target to obtain a gold-zinc oxide nanowire array;
(4) and finally, placing the obtained gold-zinc oxide nanowire array in a magnetron sputtering instrument for in-situ compounding of a nickel oxide layer, thereby finally obtaining the nickel oxide-gold-zinc oxide coaxial nanowire array.
2. The method for preparing the nickel oxide-gold-zinc oxide coaxial nanowire array according to claim 1, wherein in the step (1), the conductive substrate is FTO conductive glass;
the pretreated conductive substrate refers to: and (3) carrying out ultrasonic treatment on the untreated conductive substrate in ultrapure water, acetone, absolute ethyl alcohol and ultrapure water in sequence, then cleaning with ultrapure water, and airing to obtain the pretreated conductive substrate.
3. The method for preparing the nickel oxide-gold-zinc oxide coaxial nanowire array as claimed in claim 1, wherein in the step (1), the rf power of the magnetron sputtering apparatus is 50-200W.
4. The method for preparing a nickel oxide-gold-zinc oxide coaxial nanowire array as claimed in claim 1, wherein in the step (1), the gas flow rate of the high purity oxygen is 5-15sccm, the gas flow rate of the high purity argon is 40-100sccm, and the working pressure of the high purity oxygen and the high purity argon is 1-3 Pa.
5. The method for preparing the nickel oxide-gold-zinc oxide coaxial nanowire array as claimed in claim 1, wherein in the step (1), the thickness of the substrate of the obtained sputtered zinc oxide seed layer is 10-30 nm.
6. The method for preparing the nickel oxide-gold-zinc oxide coaxial nanowire array according to claim 1, wherein in the step (2), the concentration of the zinc acetate and the hexamethylenetetramine is 0.005-0.05 mol/L.
7. The method for preparing the nickel oxide-gold-zinc oxide coaxial nanowire array as recited in claim 1, wherein in the step (3), the sputtering time of the plasma sputtering apparatus is 45-120 s.
8. The method for preparing the nickel oxide-gold-zinc oxide coaxial nanowire array according to claim 1, wherein in the step (4), the magnetron sputtering time of the magnetron sputtering apparatus is 1-20 min.
9. A nanometer photoelectric functional material with a coaxial structure is characterized in that: prepared by the process of claims 1-8.
10. The application of the nano-photoelectric functional material of the coaxial structure in photoelectric sensing according to claim 9, wherein: the application is specifically as follows: and the photoelectric sensing under the liquid environment is completed by taking the conductive substrate of the modified composite material as a working electrode and taking a platinum net and a silver/silver chloride electrode as a counter electrode and a reference electrode respectively.
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