CN102776469A - Method for preparing copper nanowires and copper nano pointed cones - Google Patents
Method for preparing copper nanowires and copper nano pointed cones Download PDFInfo
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- CN102776469A CN102776469A CN2012102646955A CN201210264695A CN102776469A CN 102776469 A CN102776469 A CN 102776469A CN 2012102646955 A CN2012102646955 A CN 2012102646955A CN 201210264695 A CN201210264695 A CN 201210264695A CN 102776469 A CN102776469 A CN 102776469A
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- 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
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- 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
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a method for preparing copper nanowires and copper nano pointed cones. The method comprises the steps of heating a copper substrate in oxygenated atmosphere to form a copper oxide thin film or a copper oxide nanowire thin film, placing the films into a vacuum chamber, performing bombarding by using a argon ion source, and controlling the energy and the time of the ion bombarding to obtain nanowires or copper nano pointed cone arrays. According to the method, no catalyst is used, copper nanowires and copper nano pointed cones, which have different density and sizes are prepared on the substrate conveniently, and the prepared copper nanowires and copper nano pointed arrays can be applied to photoelectric devices such as a display device, a lithium battery, a super capacitor and the like.
Description
Technical field
The present invention relates to the preparation method of a kind of copper nano-wire and Nano pointed cone, belong to the nano material manufacture technology field.
Background technology
Metal nanometer line and Nano pointed cone material have important use aspect field emission cold-cathode.The single tungsten pointed cone of the early stage general employing of people is made cold cathode [E.W.M ü ller, Ergeb.Exakt.Naturwiss 27,290 (1953) .].To nineteen sixty-eight, people such as Spindt adopt micro-machined method to produce the cold cathode of molybdenum pointed cone array [C.Spindt, J.Appl.Phys.39,3504 (1968)].And in recent years, also have the investigator to report that the method that adopts self-organizing growth prepares nanometer line cold-cathode [Chao Wang, the Yuehui He of tungsten or metal molybdenum; Shiliang Wang; Quan Zhang, Xinli Liu, J.Cryst.Growth 338:214 – 217 (2012); J.Zhou, S.Z.Deng, LGong, Y.Ding, J.Chen, J.X.Huang, Jun Chen, N.S.Xu, Z.L.Wang, J.Phys.Chem.B110 (21): 10296-10302 (2006)].The reason of selecting tungsten or molybdenum for use is because they have high melt point, thereby can bear higher transmitter current.In fact, on material is selected, except the fusing point height; Admissible in addition candidate material comprise specific conductivity high with the high material of thermal conductivity, this type material is because resistance is little, electric current through the time be not easy to generate heat; And heat conduction is very fast; Thereby its temperature is lower when emission, can tolerate higher temperature, thereby realize high current emission.Copper is a kind of material that possesses high conductivity and high thermal conductivity simultaneously, if thereby can form nano wire or Nano pointed cone, just can be used as a kind of cold cathode of high emission electric current.
The present invention proposes a kind of CuO film or cupric oxide nano line film of utilizing and make mask, through the method for ion bombardment making copper nano-wire and Nano pointed cone,
Summary of the invention
The present invention proposes a kind of CuO film or cupric oxide nano line film of utilizing and make mask; Obtain the method for copper nano-wire or Nano pointed cone and the copper nano-wire of made and the application of Nano pointed cone on the cold cathode of high emission electric current through the method for ion bombardment.
In order to solve prior art problems, preparation method of the present invention carries out according to following steps: copper substrate is cleaned in (1), removes the impurity on the substrate; (2) be heated to 350～600 ℃ under the gas atmosphere of oxygen having, and be incubated 10 minutes～6 hours, cooling naturally then is so that the copper substrate surface forms one deck copper oxide or cupric oxide nano line; (3) above-mentioned sample is put into vacuum chamber, use argon ion bombardment, on substrate, to form copper nano-wire or copper Nano pointed cone array.
Substrate of the present invention can adopt single crystal Cu, and polycrystalline copper also can adopt the silicon chip, glass or the tinsel that are coated with the copper film.
Energy during argon ion bombardment of the present invention is 100eV to～1000eV, and bombardment time is 1min to 120min.
Ion source during ion bombardment of the present invention is Kaufman ion source, microwave ECR ion source or RF ion source.
The copper nano-wire or the Nano pointed cone array of the present invention's preparation can be applied to field emission cold-cathode, and other needs in the photoelectric device of this kind copper nanostructure also can be applied to lithium cell, super capacitor etc.
The method for preparing copper nano-wire and Nano pointed cone of the present invention need not through complicated micro fabrication, and making method is easy, and can effectively regulate and control the pattern of sample through parameters such as control bombardment time, ion energies, and controllability is good.
Description of drawings
Fig. 1 adopts ion bombardment to make the process step synoptic diagram of copper nano-wire and Nano pointed cone.
The surface topography SEM figure of the copper sheet after Fig. 2 oxidation.
Fig. 3 adopts the SEM figure of the copper nano-wire array of ion bombardment making.
Fig. 4 adopts the SEM figure of the copper Nano pointed cone array of ion bombardment making.
Field emission-the voltage response of Fig. 5 copper Nano pointed cone array.
Nomenclature among the figure: 1. copper substrate; 2. copper oxide and cupric oxide nano line film; 3. argon ion; 4. argon ion source; 5. copper nano-wire; 6. copper Nano pointed cone.
Embodiment
In order more clearly to provide the method that the above-mentioned method of passing through ion bombardment is made copper nano-wire and Nano pointed cone, it is the step of substrate preparation copper nano-wire and Nano pointed cone that Fig. 1 has provided with the copper sheet.
At first clean copper sheet substrate (Fig. 1 (a)), adopt acetone, alcohol and deionized water to distinguish ultrasonic cleaning 15 minutes, use nitrogen to dry up.Copper substrate is put into tube furnace or cabinet-type electric furnace, and aerating oxygen or air are heated to 350～600 ℃, and be incubated 10 minutes～6 hours, last cooling naturally.Through behind the above-mentioned thermal oxidation process, the copper substrate surface can form one deck copper oxide or cupric oxide nano line, shown in Fig. 1 (b).Have the sample of CuO film or cupric oxide nano line film to put into vacuum chamber growth, use ion source to produce argon ion, the bombardment sample is shown in Fig. 1 (c).The energy of argon ion is 100eV ~ 1000eV, and bombardment time is 1min to 120min.When the time of bombardment hangs down than short or energy, form copper nano-wire, shown in Fig. 1 (d).When long or energy is higher when the time of bombardment, can form the copper Nano pointed cone, shown in Fig. 1 (e).
Present embodiment is given in the process of preparation copper nano-wire array on the copper sheet.At first distinguish ultrasonic cleaning copper sheet 15 minutes, use nitrogen to dry up with acetone, alcohol and deionized water.The copper sheet that cleans up is put into tube furnace, and elevated temperature to 400 ℃ is incubated 3 hours, then naturally cooling.The surface topography of the copper sheet after the oxidation is as shown in Figure 2, can see growing cupric oxide nano line film on the copper sheet.
Have the sample of oxidation copper nano-wire film to put into Vakuumkammer growth, produce the argon ion bombardment sample with the Kaufman ion source, the argon ion energy is 700eV, and bombardment time is 10min.The SEM figure that accompanying drawing 3 provides the copper nano-wire array of bombardment back generation can see on the copper sheet substrate having formed nano-wire array that the center line average of nano wire is about 1.5 μ m, and diameter is about 82nm.
Present embodiment is given in the process of preparation copper Nano pointed cone array on the copper sheet.At first distinguish ultrasonic cleaning copper sheet 15 minutes, use nitrogen to dry up with acetone, alcohol and deionized water.The copper sheet that cleans up is put into tube furnace, and elevated temperature to 400 ℃ is incubated 3 hours, then naturally cooling.
Have the sample of oxidation copper nano-wire film to put into Vakuumkammer growth, produce the argon ion bombardment sample with the Kaufman ion source, the argon ion energy is 700eV, and bombardment time is 60min.Characterize the sample for preparing with SEM, can look unfamiliar into the copper Nano pointed cone by table of discovery.Accompanying drawing 4 is given the SEM figure of copper Nano pointed cone array.The height of formed copper pointed cone is about 4.4 μ m, and vertical diameter is about 500nm, and density is about 7 * 10
10/ m
2
Adopt two-level structure to measure the field emission characteristic of the formed copper pointed cone array of bombardment, the current density-voltage response of gained is shown in accompanying drawing 5.Definition obtains 10mA/cm
2The corresponding electric field of current density be to launch a threshold field, the threshold field that can obtain copper pointed cone array is 15.6MV/m, the maximum current density 51mA/cm that it can reach
2
Claims (5)
1. method for preparing copper nano-wire and copper Nano pointed cone is characterized in that: carry out according to following steps:
(1) cleans copper substrate, remove the impurity on the substrate;
(2) be heated to 350～600 ℃ under the gas atmosphere of oxygen having, and be incubated 10 minutes～6 hours, cooling naturally then is so that the copper substrate surface forms one deck copper oxide or cupric oxide nano line;
(3) above-mentioned sample is put into vacuum chamber, use argon ion bombardment, on substrate, to form copper nano-wire or copper Nano pointed cone array.
2. the method for preparing copper nano-wire and copper Nano pointed cone according to claim 1, it is characterized in that: said substrate is a single crystal Cu, polycrystalline copper, or be coated with silicon chip, glass or the tinsel of copper film.
3. the method for preparing copper nano-wire and copper Nano pointed cone according to claim 1 is characterized in that: the energy of said argon ion bombardment is 100eV to～1000eV, and bombardment time is 1min to 120min.
4. the method for preparing copper nano-wire and copper Nano pointed cone according to claim 1 is characterized in that: the ion source of said ion bombardment is Kaufman ion source, microwave ECR ion source or RF ion source.
5. by claim 1, the copper nano-wire of 2,3 or 4 described methods preparations or copper Nano pointed cone array are at field emission cold-cathode or have the application on the photoelectric device of lithium cell, ultracapacitor.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103065916A (en) * | 2012-12-27 | 2013-04-24 | 青岛艾德森能源科技有限公司 | Copper oxide nanowire field emission cathode |
| CN103219503A (en) * | 2013-03-12 | 2013-07-24 | 北京理工大学 | Combined electrode material and preparation method thereof |
| CN103833065A (en) * | 2012-11-23 | 2014-06-04 | 北京师范大学 | Method for preparing cuprous oxide nanowire by thermal evaporation technique |
| CN103921497A (en) * | 2013-01-10 | 2014-07-16 | 海洋王照明科技股份有限公司 | Conductive thin film, preparation method and application thereof |
| CN111392762A (en) * | 2020-04-09 | 2020-07-10 | 沈阳师范大学 | Preparation method of copper oxide nanowire array field emission cathode material based on metal ion implantation |
| CN115287765A (en) * | 2022-07-11 | 2022-11-04 | 大连理工大学 | Single crystal copper oxide nanowire and simple preparation method of copper nanowire |
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| CN100435261C (en) * | 2002-12-26 | 2008-11-19 | 财团法人汉城大学校产学协力财团 | Low temperature formation method for electron emission chip comprising copper oxide or copper nanowire |
| CN102051675A (en) * | 2010-10-28 | 2011-05-11 | 中山大学 | Method for manufacturing CuO nanowire |
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Patent Citations (2)
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| CN100435261C (en) * | 2002-12-26 | 2008-11-19 | 财团法人汉城大学校产学协力财团 | Low temperature formation method for electron emission chip comprising copper oxide or copper nanowire |
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| XIAOMENG SONG等: "Field emission from copper microcones formed by ion bombardment of copper substrate using an oxide masking", 《VACUUM NANOELECTRONICS CONFERENCE》, 13 July 2012 (2012-07-13), pages 1 - 2, XP032245397, DOI: doi:10.1109/IVNC.2012.6316977 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103833065A (en) * | 2012-11-23 | 2014-06-04 | 北京师范大学 | Method for preparing cuprous oxide nanowire by thermal evaporation technique |
| CN103833065B (en) * | 2012-11-23 | 2015-11-25 | 北京师范大学 | A kind of method preparing nano cuprous oxide wire with thermal evaporation techniques |
| CN103065916A (en) * | 2012-12-27 | 2013-04-24 | 青岛艾德森能源科技有限公司 | Copper oxide nanowire field emission cathode |
| CN103921497A (en) * | 2013-01-10 | 2014-07-16 | 海洋王照明科技股份有限公司 | Conductive thin film, preparation method and application thereof |
| CN103219503A (en) * | 2013-03-12 | 2013-07-24 | 北京理工大学 | Combined electrode material and preparation method thereof |
| CN103219503B (en) * | 2013-03-12 | 2016-02-24 | 北京理工大学 | A kind of combination electrode material and preparation method thereof |
| CN111392762A (en) * | 2020-04-09 | 2020-07-10 | 沈阳师范大学 | Preparation method of copper oxide nanowire array field emission cathode material based on metal ion implantation |
| CN115287765A (en) * | 2022-07-11 | 2022-11-04 | 大连理工大学 | Single crystal copper oxide nanowire and simple preparation method of copper nanowire |
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