CN102181831A - Preparation method for copper oxide nano line array film - Google Patents
Preparation method for copper oxide nano line array film Download PDFInfo
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- CN102181831A CN102181831A CN 201110094054 CN201110094054A CN102181831A CN 102181831 A CN102181831 A CN 102181831A CN 201110094054 CN201110094054 CN 201110094054 CN 201110094054 A CN201110094054 A CN 201110094054A CN 102181831 A CN102181831 A CN 102181831A
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Abstract
The invention belongs to low-dimensional nano material preparation and application field of nano technology, and particularly relates to a preparation method for a copper oxide nano line array film. The preparation method comprises the following steps: sputtering a metal copper film on an FTO substrate by adopting a magnetron sputter plating method, and then annealing the prepared film under air atmosphere, thus obtaining the copper oxide nano line array film. In the preparation method, the controllability is good, the preparation is flexible, the preparation method is not limited to prepare substrate materials, the scale production in the industry can be conducted conveniently, and the application field and scope of nano line array film can be expanded to a greater degree.
Description
Technical field
The invention belongs to low-dimension nano material preparation and nanotechnology Application Areas, particularly a kind of preparation method of nanowire array of copper oxide film.
Background technology
In the middle of metal oxide, majority is the n N-type semiconductorN, and CuO is one of P-type semiconductor material few in number, because CuO can be in ferromagnetic material, high-temperature superconductor, battery electrode, air-sensitive--and wait multiple field to use, therefore be subjected to extensive concern.Than traditional block materials, the 1-dimention nano wire material is owing to have small-size effect and a big specific surface area, so it has more superior performance in the nanosecond science and technology technical field, more and more is subjected to people's attention and research.Wherein, the present especially research focus and emphasis of the preparation method of low-dimensional nano-material and utilisation technology.
At present, thermal oxidation method is adopted in the preparation of cupric oxide nano line more, promptly directly passes through the suitable temperature and time of control in the metallic copper substrate, anneals under air atmosphere, can prepare the nanowire array of copper oxide of vertical substrate, and this method is convenient, simple.But the cupric oxide nano line of this method preparation has difficulties in actual applications.Such as aspect the air-sensitive, its good application that the upper current conducting cap of nanowire array of copper oxide structure has been difficult to design limit; In addition, in the photoelectricity research field,, be difficult to intactly transfer to this nano-wire array film on the transparent substrates because the nanowire array of copper oxide film of this method preparation is subject to substrate, cause the difficulty of device preparation, make its application also be very restricted at photoelectric field.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of nanowire array of copper oxide film, to overcome the defective that present preparation method's controllability is relatively poor, be subject to substrate material.
The technical solution used in the present invention is as follows:
A kind of preparation method of nanowire array of copper oxide film adopts magnetron sputtering method splash-proofing sputtering metal copper film in substrate, the film that makes is annealed under air atmosphere promptly get described nanowire array of copper oxide film then.
When sputter prepared the metallic copper film in substrate, the sputter working current was 0.2-0.3A, and operating voltage is 250-350V, and the substrate rotating speed is 0-20r/min.The substrate rotating speed is preferably 13 r/min.
The thickness of copper film is not more than 1.5 μ m, otherwise comes off easily.
It is 99.99% copper target that the present invention adopts purity, and target is of a size of Φ=50 * 4 mm; The base vacuum degree is 3.0 * 10
-3-4.0 * 10
-3Pa, operating air pressure are 0.25-0.8 Pa, and used working gas is an argon gas, and gas flow is 15-30sccm.
The purity of argon gas preferably is not less than 99.999%.
Adopt tube furnace to anneal, temperature rise rate is 20 ℃/min.
Substrate can be selected FTO or common slide glass etc., but preferred FTO conductive glass, thus can directly be that electrode uses with FTO, as two FTO can being buckled together face-to-face, at CO, H
2The air-sensitive aspect utilization of gases such as S.
Wherein, after the copper film preparation is good, should avoid its slow oxidation in atmosphere, therefore should place tube furnace to anneal as early as possible.
Annealing temperature is 350-550 ℃, and the time is 2-10h.
In the annealing process, used tube furnace is near the sealing of sample end, and the other end and atmosphere communicate.Purpose is to guarantee that an amount of oxygen participates in thermal oxidation process.
The present invention has following advantage with respect to prior art:
The present invention is owing to the employing magnetron sputtering method, so preparation method's controllability is good, the preparation flexible, be not limited to substrate material, is convenient to form in industry large-scale production, has also expanded the Application Areas and the scope of nano-wire array film largely.
Description of drawings
Fig. 1 overlooks scanning electronic microscope (SEM) figure of face for embodiment 1 step 1) product;
Fig. 2 is the scanning electron microscope diagram of embodiment 1 step 1) product cross section;
Fig. 3 is embodiment 1 step 2) product overlooks the scanning electron microscope diagram of face;
Fig. 4 is embodiment 1 step 2) scanning electron microscope diagram of product cross section;
Fig. 5 is embodiment 1 step 2) ultraviolet-visible absorption spectroscopy (Uv-Vis) of product;
Fig. 6 is embodiment 1 step 2) X-ray diffraction (XRD) collection of illustrative plates of product.
Embodiment
Below with specific embodiment technical scheme of the present invention is described, but protection scope of the present invention is not limited thereto:
(1) be purity after 99.99% copper target and cleaned FTO put into sputtering chamber, at first to use mechanical pump and molecular pump that the vacuum tightness of sputtering chamber is extracted into 3.0 * 10
-3Pa, charge into the argon gas of purity 〉=99.999% then, flow is 23 sccm, regulate main valve and make vacuum tightness remain on 0.35Pa, regulating and making electric current is 0.25A, and voltage is 300V, the substrate rotating speed is 13 r/min, sputtering time 10min obtains the metallic copper film of about 500 nanometer thickness, characterizes and sees Fig. 1 and Fig. 2.
(2) the resulting metallic copper film of step (1) is put into tube furnace rapidly, tube furnace is near the mouth of pipe sealing of sample end, and the other end and atmosphere communicate; Heat-up rate is 20 ℃/min, anneals 8 hours for 500 ℃ under air atmosphere, promptly obtains orthotropic nanowire array of copper oxide film, characterizes and sees accompanying drawing 3-6.
Embodiment 2
1) be purity after 99.99% copper target and cleaned FTO put into sputtering chamber, at first to use mechanical pump and molecular pump that the vacuum tightness of sputtering chamber is extracted into 4 * 10
-3Pa charges into the argon gas of purity 〉=99.999% then, and flow is 20 sccm, regulates main valve and makes vacuum tightness remain on 3.0 * 10
-1Pa, regulating and making electric current is 0.2A, and voltage is 350V, and sputtering time 30min obtains the thick metallic copper film of about 1.2 μ m;
(2) the resulting metallic copper film of step (1) is put into tube furnace rapidly, tube furnace is near the mouth of pipe sealing of sample end, and the other end and atmosphere communicate; Heat-up rate is 20 ℃/min, anneals 10 hours for 450 ℃ under air atmosphere, promptly obtains orthotropic nanowire array of copper oxide film.
Claims (9)
1. the preparation method of a nanowire array of copper oxide film is characterized in that, adopts magnetron sputtering method splash-proofing sputtering metal copper film in substrate, the film that makes is annealed under air atmosphere promptly get described nanowire array of copper oxide film then.
2. the preparation method of nanowire array of copper oxide film as claimed in claim 1 is characterized in that, when sputter prepared the metallic copper film in substrate, the sputter working current was 0.2-0.3A, and operating voltage is 250-350 V, and the substrate rotating speed is 0-20r/min.
3. the preparation method of nanowire array of copper oxide film as claimed in claim 2 is characterized in that, the thickness of metallic copper film is not more than 1.5 μ m.
4. the preparation method of nanowire array of copper oxide film as claimed in claim 3 is characterized in that, the base vacuum degree is 3.0 * 10
-3-4.0 * 10
-3Pa, operating air pressure are 0.25-0.8Pa, and used working gas is an argon gas, and gas flow is 15-30sccm.
5. the preparation method of nanowire array of copper oxide film as claimed in claim 4 is characterized in that, target is the copper target of purity 99.99%, is of a size of Φ=50 * 4 mm.
6. as the preparation method of the described nanowire array of copper oxide film of one of claim 1-5, it is characterized in that annealing temperature is 350-550 ℃, the time is 2-10h.
7. the preparation method of nanowire array of copper oxide film as claimed in claim 6 is characterized in that, adopts tube furnace to anneal, and temperature rise rate is 20 ℃/min.
8. the preparation method of nanowire array of copper oxide film as claimed in claim 6 is characterized in that, substrate is FTO or common slide glass.
9. the preparation method of nanowire array of copper oxide film as claimed in claim 6 is characterized in that, in the annealing process, used tube furnace is near the sealing of sample end, and the other end and atmosphere communicate.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102345096A (en) * | 2011-06-29 | 2012-02-08 | 常州大学 | Copper nanowire / copper film composite structure and preparation method thereof |
| CN103510048A (en) * | 2013-08-19 | 2014-01-15 | 南京清航新材料科技有限公司 | Preparation method of copper nanowire arrays with porous structure and film conductivity measuring method thereof |
| CN104805409A (en) * | 2015-04-07 | 2015-07-29 | 天津科技大学 | Method for preparing Ag nanowire array electrode according to magnetron sputtering-masking assisted deposition |
| CN106086768A (en) * | 2016-06-12 | 2016-11-09 | 上海大学 | The preparation method of cuprio bed load nanostructured copper cobalt manganese composite oxide material |
| CN110592548A (en) * | 2019-10-23 | 2019-12-20 | 常州大学 | Suede CuO composite structure film and preparation method thereof |
| CN110668392A (en) * | 2019-10-10 | 2020-01-10 | 北京航空航天大学杭州创新研究院 | Enhanced heat dissipation Cu-Cu2O-core-shell nanowire array self-protection electrode and preparation method thereof |
| CN111289580A (en) * | 2018-06-27 | 2020-06-16 | 成都新柯力化工科技有限公司 | Film sensing material for detecting atmosphere hydrogen sulfide gas and preparation method thereof |
| CN112030109A (en) * | 2020-09-07 | 2020-12-04 | 江西省科学院应用物理研究所 | Copper oxide film/silicon wafer composite structure and preparation method thereof |
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| JP2006210872A (en) * | 2004-12-28 | 2006-08-10 | Kyushu Institute Of Technology | Process for forming copper pattern interconnect line, semiconductor device fabricated using that method, and nano copper metal particle |
| CN1843932A (en) * | 2006-03-03 | 2006-10-11 | 中山大学 | Localized growth method of nanowire array of copper oxide |
| CN101570853A (en) * | 2009-05-08 | 2009-11-04 | 中国科学技术大学 | Method for preparing zinc and zinc oxide nano material with controllable appearance by utilizing magnetron sputtering |
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| JP2006210872A (en) * | 2004-12-28 | 2006-08-10 | Kyushu Institute Of Technology | Process for forming copper pattern interconnect line, semiconductor device fabricated using that method, and nano copper metal particle |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102345096B (en) * | 2011-06-29 | 2014-02-05 | 常州大学 | Copper nanowire/copper film composite structure and preparation method thereof |
| CN102345096A (en) * | 2011-06-29 | 2012-02-08 | 常州大学 | Copper nanowire / copper film composite structure and preparation method thereof |
| CN103510048A (en) * | 2013-08-19 | 2014-01-15 | 南京清航新材料科技有限公司 | Preparation method of copper nanowire arrays with porous structure and film conductivity measuring method thereof |
| CN104805409B (en) * | 2015-04-07 | 2017-05-17 | 天津科技大学 | Method for preparing Ag nanowire array electrode according to magnetron sputtering-masking assisted deposition |
| CN104805409A (en) * | 2015-04-07 | 2015-07-29 | 天津科技大学 | Method for preparing Ag nanowire array electrode according to magnetron sputtering-masking assisted deposition |
| CN106086768B (en) * | 2016-06-12 | 2018-10-23 | 上海大学 | The preparation method of copper-based bed load nanostructure copper cobalt manganese composite oxide material |
| CN106086768A (en) * | 2016-06-12 | 2016-11-09 | 上海大学 | The preparation method of cuprio bed load nanostructured copper cobalt manganese composite oxide material |
| CN111289580A (en) * | 2018-06-27 | 2020-06-16 | 成都新柯力化工科技有限公司 | Film sensing material for detecting atmosphere hydrogen sulfide gas and preparation method thereof |
| CN110668392A (en) * | 2019-10-10 | 2020-01-10 | 北京航空航天大学杭州创新研究院 | Enhanced heat dissipation Cu-Cu2O-core-shell nanowire array self-protection electrode and preparation method thereof |
| CN110668392B (en) * | 2019-10-10 | 2023-03-14 | 北京航空航天大学杭州创新研究院 | Enhanced heat dissipation Cu-Cu 2 O-core-shell nanowire array self-protection electrode and preparation method thereof |
| CN110592548A (en) * | 2019-10-23 | 2019-12-20 | 常州大学 | Suede CuO composite structure film and preparation method thereof |
| CN110592548B (en) * | 2019-10-23 | 2021-09-17 | 常州大学 | Suede CuO composite structure film and preparation method thereof |
| CN112030109A (en) * | 2020-09-07 | 2020-12-04 | 江西省科学院应用物理研究所 | Copper oxide film/silicon wafer composite structure and preparation method thereof |
| CN112030109B (en) * | 2020-09-07 | 2022-07-29 | 江西省科学院应用物理研究所 | Copper oxide film/silicon wafer composite structure and preparation method thereof |
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Application publication date: 20110914 |