CN114933729A - Preparation method of p-type ZnO nanowire array - Google Patents
Preparation method of p-type ZnO nanowire array Download PDFInfo
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- CN114933729A CN114933729A CN202210702408.8A CN202210702408A CN114933729A CN 114933729 A CN114933729 A CN 114933729A CN 202210702408 A CN202210702408 A CN 202210702408A CN 114933729 A CN114933729 A CN 114933729A
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Abstract
The invention discloses a preparation method of a p-type ZnO nanowire array, which relates to the technical field of ZnO nanowire arrays, and the technical scheme comprises the following key points: the method comprises the following steps: spin coating treatment: spin-coating a layer of photoresist on the upper surface of a substrate made of a semiconductor material; step two: transfer processing: imprinting a template of a nano array on the imprinting glue of the substrate, and transferring the nano array onto the imprinting glue; step three: array processing: and inverting the substrate transferred with the nano array, combining the substrate with the silicon substrate to form a nano-scale micro-channel array, and dripping the ZnO salt solution to one end of the micro-channel array so that the ZnO salt solution is under the action of capillary force of the micro-channel array. Through to the impression glue follow when the silicon substrate is uncovered, through carrying out the persistence heating to the separation region, make impression glue and silicon substrate separate, ensure that ZnO nanowire array can keep the integrality, avoid appearing the fracture of ZnO nanowire array in the separation.
Description
Technical Field
The invention relates to the technical field of ZnO nanowire arrays, in particular to a preparation method of a p-type ZnO nanowire array.
Background
A nanowire can be defined as a one-dimensional structure with lateral confinement below 100 nm (without longitudinal confinement), with suspended nanowires meaning that the end of the nanowire is fixed under vacuum conditions. Typical nanowires have aspect ratios above 1000, so they are often referred to as one-dimensional materials. The nanowires may be classified into various types, including metal nanowires, semiconductor nanowires, and insulator nanowires, according to the composition material. The nanowires can be made by a suspension method, a deposition method, or an elemental synthesis method. The suspended nanowires can be produced by chemical etching of the thick wires, or by bombarding the thick wires with energetic particles (atoms or molecules). Nanowires grown in the laboratory are divided into two types, namely nanowires perpendicular to the plane of the substrate and nanowires parallel to the plane of the substrate.
During the preparation of the ZnO nanowire array, certain defects exist, for example, during the separation of the imprinting glue from the silicon substrates, the imprinting glue may remain on the surfaces of the silicon substrates, so that the nanowire array is damaged, and the overall array effect is affected.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method of a p-type ZnO nanowire array.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a p-type ZnO nanowire array comprises the following steps:
the method comprises the following steps: spin coating treatment: spin-coating a layer of photoresist on the upper surface of a substrate made of a semiconductor material;
step two: transfer processing: imprinting a template of a nano array on the imprinting glue of the substrate, and transferring the nano array onto the imprinting glue;
step three: array processing: inverting the substrate transferred with the nano array, combining the substrate with the silicon substrate to form a nano-scale micro-channel array, and dripping a ZnO salt solution to one end of the micro-channel array so that the ZnO salt solution flows into the micro-channel array under the action of capillary force of the micro-channel array and self-assembles in the micro-channel array to form a nano-wire array;
step four: heating treatment: heating the micro-channel array to shape the nanowire array;
step five: separation treatment: and removing the imprinting glue from the silicon substrate, heating the separation region in the removing process, and obtaining the p-type ZnO nanowire array on the substrate.
As a further scheme of the invention, in the fourth step, the time for heating the micro-channel array is 5-10 min, and the heating temperature is 100-130 ℃.
In a further embodiment of the present invention, the substrate is selected from Polydimethylsiloxane (PDMS) and polyethylene terephthalate (PET).
As a further aspect of the present invention, the imprint glue includes: ultraviolet curing impression compound, thermoplasticity impression compound or thermosetting impression compound, the ZnO nanowire array includes at least but not limited to one of the following: linear array, curved array, cross array, and cylindrical array structures.
As a further scheme of the invention, the preparation of the ZnO salt solution comprises the following steps:
s1, weighing ZnO powder for quantification, mixing with alkaline liquid, and placing in a high-pressure kettle;
s2, setting the temperature of the autoclave in the S1 at 200-250 ℃, and reacting for 1-2 h;
s3, finally obtaining the ZnO salt solution.
In a further embodiment of the present invention, the ratio of the ZnO powder to the alkali solution in step S1 is 0.5 to 1 g: 1-50 mL.
As a further scheme of the invention, the microchannel array is self-assembled to form a nanowire array, wherein the ZnO salt solution is prepared from 200mg/ml of copper nitrate aqueous solution, and the self-assembly environment has the humidity of 50%, the temperature of 35 ℃ and the atmospheric pressure.
As a further scheme of the invention, in the fifth step, the substrate is moved to a tube furnace, inert gas is introduced into the tube furnace, and the tube furnace is heated at 800 ℃ for 2 hours to decompose the p-type ZnO nanowire array to form metal oxide, so that the metal oxide nanowire array is obtained on the substrate.
Compared with the prior art, the invention has the following beneficial effects:
through to the impression glue follow when the silicon substrate is uncovered, through carrying out the persistence heating to the separation region, make impression glue and silicon substrate separate, ensure that ZnO nanowire array can keep the integrality, avoid appearing the fracture of ZnO nanowire array in the separation.
Drawings
FIG. 1 is a flow chart of a method for preparing a p-type ZnO nanowire array according to the present invention.
Detailed Description
Referring to fig. 1, an embodiment of a method for fabricating a p-type ZnO nanowire array of the present invention is further illustrated.
A preparation method of a p-type ZnO nanowire array comprises the following steps:
the method comprises the following steps: spin coating treatment: a layer of photoresist is spin coated on the upper surface of a substrate made of semiconductor material. When spin coating is performed, resist can be maximally etched by rotating the substrate.
Step two: transfer processing: and imprinting the template of the nano array on the imprinting glue of the substrate, so that the nano array is transferred to the imprinting glue. In transfer, it is necessary to keep the temperature at 50 ℃ to maintain a constant softness, thereby improving the efficiency of transfer.
Step three: array processing: and inverting the substrate transferred with the nano array, combining the substrate with the silicon substrate to form a nano-scale micro-channel array, dripping a ZnO salt solution to one end of the micro-channel array so that the ZnO salt solution flows into the micro-channel array under the action of capillary force of the micro-channel array, and performing self-assembly in the micro-channel array to form the nano-wire array.
Step four: heating treatment: and heating the micro-channel array to shape the nanowire array.
Step five: separation treatment: and removing the imprinting glue from the silicon substrate, heating the separation region in the removing process, and obtaining the p-type ZnO nanowire array on the substrate.
In the fourth step, the time for heating the micro-channel array is 5-10 min, and the heating temperature is 100-130 ℃.
The material of the substrate is selected from Polydimethylsiloxane (PDMS) and polyethylene terephthalate (PET).
The imprint glue includes: ultraviolet curing impression compound, thermoplasticity impression compound or thermosetting impression compound, the ZnO nanowire array includes at least but not limited to one of the following: linear array, curved array, cross array, and cylindrical array structures.
The preparation of the ZnO salt solution comprises the following steps:
s1, weighing ZnO powder for quantification, mixing with alkaline liquid, and placing in a high-pressure kettle;
s2, setting the temperature of the autoclave in the S1 at 200 ℃ and 250 ℃, and reacting for 1-2 h;
s3, finally obtaining the ZnO salt solution.
The using amount ratio of the ZnO powder to the alkali solution in the step S1 is 0.5-1 g: 1-50 mL.
And self-assembling in the micro-channel array to form the nanowire array, wherein the ZnO salt solution is prepared from 200mg/ml of copper nitrate aqueous solution, and the self-assembling environment has the humidity of 50%, the temperature of 35 ℃ and the atmospheric pressure.
And in the fifth step, the substrate is moved to a tube furnace, inert gas is introduced into the tube furnace, the p-type ZnO nanowire array is heated for 2 hours at 800 ℃, so that the p-type ZnO nanowire array is decomposed to form metal oxide, and the metal oxide nanowire array is obtained on the substrate.
The working principle is as follows:
the method comprises the following steps: spin coating treatment: spin-coating a layer of photoresist on the upper surface of a substrate made of a semiconductor material;
step two: transfer processing: imprinting a template of a nano array on the imprinting glue of the substrate, and transferring the nano array onto the imprinting glue;
step three: array processing: inverting the substrate transferred with the nano array, combining the substrate with a silicon substrate to form a nano-scale micro-channel array, dripping a ZnO salt solution to one end of the micro-channel array so that the ZnO salt solution flows into the micro-channel array under the action of capillary force of the micro-channel array and is self-assembled in the micro-channel array to form a nano-wire array;
step four: heating treatment: heating the micro-channel array to shape the nanowire array;
step five: separation treatment: and removing the imprinting glue from the silicon substrate, heating the separation region in the removing process, and obtaining the p-type ZnO nanowire array on the substrate.
In the description of the present invention, it is to be understood that the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise. In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meanings of the above terms in the present invention can be understood according to specific situations by those of ordinary skill in the art.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above 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 adaptations to those skilled in the art without departing from the principles of the present invention should also be considered as within the scope of the present invention.
Claims (8)
1. A preparation method of a p-type ZnO nanowire array is characterized by comprising the following steps:
the method comprises the following steps: spin coating treatment: spin-coating a layer of photoresist on the upper surface of a substrate made of a semiconductor material;
step two: transfer processing: imprinting a template of a nano array on the imprinting glue of the substrate, and transferring the nano array onto the imprinting glue;
step three: array processing: inverting the substrate transferred with the nano array, combining the substrate with the silicon substrate to form a nano-scale micro-channel array, and dripping a ZnO salt solution to one end of the micro-channel array so that the ZnO salt solution flows into the micro-channel array under the action of capillary force of the micro-channel array and self-assembles in the micro-channel array to form a nano-wire array;
step four: heating treatment: heating the micro-channel array to shape the nanowire array;
step five: separation treatment: and removing the imprinting glue from the silicon substrate, heating the separation region in the removing process, and obtaining the p-type ZnO nanowire array on the substrate.
2. The method as claimed in claim 1, wherein in the fourth step, the micro-channel array is heated for 5-10 min at a temperature of 100-130 ℃.
3. The method of claim 1, wherein the substrate is selected from Polydimethylsiloxane (PDMS) and polyethylene terephthalate (PET).
4. The method of claim 1, wherein the imprint glue comprises: ultraviolet curing imprinting glue, thermoplastic imprinting glue or thermosetting imprinting glue, wherein the ZnO nanowire array at least comprises one of the following materials: linear array, curved array, cross array, and cylindrical array structures.
5. The method for preparing the p-type ZnO nanowire array according to claim 1, wherein the preparation of the ZnO salt solution comprises the following steps:
s1, weighing ZnO powder, quantifying, mixing with alkaline liquid, and placing in a high-pressure kettle;
s2, setting the temperature of the autoclave in the S1 at 200-250 ℃, and reacting for 1-2 h;
s3, finally obtaining the ZnO salt solution.
6. The method for preparing the p-type ZnO nanowire array according to claim 5, wherein the using amount ratio of the ZnO powder to the alkali solution in the step S1 is 0.5-1 g: 1-50 mL.
7. The method of claim 1, wherein the microchannel array is self-assembled to form the nanowire array, and wherein the ZnO salt solution is prepared from 200mg/ml of copper nitrate solution, and the self-assembly is performed at an ambient humidity of 50%, a temperature of 35 ℃ and an atmospheric pressure.
8. The method for preparing p-type ZnO nanowire array according to claim 1, wherein in the fifth step, the substrate is moved to a tube furnace, inert gas is introduced into the tube furnace, and the p-type ZnO nanowire array is heated at 800 ℃ for 2 hours to decompose the p-type ZnO nanowire array to form metal oxide, so that the metal oxide nanowire array is obtained on the substrate.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583227A (en) * | 2012-03-13 | 2012-07-18 | 浙江大学 | Three-dimensional ZnO homogeneous pn junction nano array and preparation method thereof |
| CN103760336A (en) * | 2014-01-02 | 2014-04-30 | 中国科学院苏州生物医学工程技术研究所 | Linear array ZnO (zinc oxide) nanowire heterojunction LED (light emitting diode) biosensor and preparation method thereof |
| US20190191560A1 (en) * | 2016-08-17 | 2019-06-20 | The University Of North Carolina At Chapel Hill | Flexible conductive transparent films, articles and methods of making same |
| CN111924799A (en) * | 2020-07-02 | 2020-11-13 | 天津大学 | Preparation method of metal oxide nanowire array and nanowire array prepared by same |
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- 2022-06-20 CN CN202210702408.8A patent/CN114933729A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583227A (en) * | 2012-03-13 | 2012-07-18 | 浙江大学 | Three-dimensional ZnO homogeneous pn junction nano array and preparation method thereof |
| CN103760336A (en) * | 2014-01-02 | 2014-04-30 | 中国科学院苏州生物医学工程技术研究所 | Linear array ZnO (zinc oxide) nanowire heterojunction LED (light emitting diode) biosensor and preparation method thereof |
| US20190191560A1 (en) * | 2016-08-17 | 2019-06-20 | The University Of North Carolina At Chapel Hill | Flexible conductive transparent films, articles and methods of making same |
| CN111924799A (en) * | 2020-07-02 | 2020-11-13 | 天津大学 | Preparation method of metal oxide nanowire array and nanowire array prepared by same |
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