CN101514486B - Cu dendritic single crystalline nano material and preparation method thereof - Google Patents
Cu dendritic single crystalline nano material and preparation method thereof Download PDFInfo
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- CN101514486B CN101514486B CN2009100467501A CN200910046750A CN101514486B CN 101514486 B CN101514486 B CN 101514486B CN 2009100467501 A CN2009100467501 A CN 2009100467501A CN 200910046750 A CN200910046750 A CN 200910046750A CN 101514486 B CN101514486 B CN 101514486B
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Abstract
The invention discloses a Cu dendritic single crystalline nano material and a preparation method thereof. The concrete technique comprises: 1) a copper sheet is polished, dipped into 30% hydrochloric acid for 8-10min and then put into acetone for ultrasonic processing, so that purified copper sheet is obtained and taken as an anode; 2) ITO conductive glass is washed by 0.1mol/L of NaOH for 8-10min, then put into acetone for ultrasonic processing and finally washed by deionized water to be taken as a cathode; 3) electrolyte is 0.5mol/L of Cu(NO3)2 and 1.0 mol/L of citric acid which is used for adjusting the PH to be 1.5-2; galvanization is carried out when the voltage is 0.8-1 V; 4) the ITO conductive glass is taken out after 1.5-2.5h, and a layer of light red attachment which is the Cu tree-like single crystalline nano material is attached on the ITO conductive glass. The invention has the characteristics of novel method and appearance, simple equipment and operation and low cost without needing catalyst.
Description
Technical field
The present invention relates to a kind of Cu dendritic single crystalline nano material and preparation method thereof, be specifically related to a kind of Cu dendritic structure that forms by nanometer structure and use electric plating method, on the copper sheet substrate, obtain the preparation method of this structure of big area.Belong to semiconductor material, photoelectron material and device technology field.
Background technology
Because nano material has the physics and the chemical property of uniquenesses such as surface effects, small-size effect, quantum size effect, macro quanta tunnel effect. make the preparation of nano material become a focus of present material research.And copper nanoparticle makes it to use very extensive because size is little, specific surface area is big, many, the characteristics such as resistance is little, quantum size effect, macro quanta tunnel effect of surfactivity center number.It is that a kind of good catalyzer draws, lubricant, and is widely used in developing in electromagnetic shielding material and the electrically conducting coating as conductive filler material.Therefore, development nanometer copper has important significance for theories and practical value.So recently, people utilize the whole bag of tricks (solid phase method, hydro-thermal synthetic etc.) to prepare various one dimension CuO rice structure, nano wire for example, the nanometer flower, nanometer rod etc., and the field emission characteristic of these nanostructures studied, yet up to the present, all one dimension Nano structures substantially all are the thermal evaporation or the preparation of hydro-thermal synthetic method of usefulness, and seldom use electric plating method to prepare the nanostructure of Cu.The nano material uniformity of electro-plating method growth, and area is big, provides a kind of new method for realizing self-assembly function nano material structure.
Summary of the invention
The objective of the invention is for a kind of Cu dendritic single crystalline nano material and preparation method thereof is provided.To solve the problems referred to above of prior art.
Cu dendritic single crystalline nano material provided by the present invention, be reported first in the world, this dendroid Cu is formed along the different directions regrowth by the Cu nanometer rod, has very intensive concentration, its length is being generally 10-20 μ m, and tip diameter is generally about 30-50nm.
The preparation method of this Cu dendritic single crystalline nano material, its concrete technology is as follows:
1) with copper sheet (the about 1.5cm of surface-area
2) polishing, with 30% salt acid soak 8-10 minute, to put in people's acetone ultrasonicly again, the pure copper sheet that obtains is as anode;
2) with ITO conductive glass (the about 1.6cm of surface-area
2) cleaned 8-10 minute with the NaOH of 0.1mol/L, it is ultrasonic to put into acetone again, uses deionized water rinsing as negative electrode at last;
3) electrolytic solution is the Cu (NO of 0.5mol/L
3)
2With the citric acid of 1.0mol/L, it is 1.5-2 that citric acid is used for regulating PH; At voltage is that 0.8-1V electroplates;
4) behind the 1.5-2.5h, take out the ITO conductive glass, adhered to the pink dirt settling of one deck above can seeing, be the Cu dendritic single crystalline nano material.
Described copper sheet purity is 99%, and thickness is 0.1-0.3mm; ITO conductive glass thickness is 0.4-0.5mm.
Described Cu (NO
3)
2With citric acid purity is 99% to originate from Shanghai Ling Feng chemical reagent company limited.
Described electroplating device, it is the bantam that build in own laboratory.Voltage range: 1-20V; Electrolyzer is a glass beaker, in order to control its current density, and our connected resistance of a 1K, whole device is sealed in the lens.
With respect to former synthetic nanostructure, outstanding feature of the present invention is: (1) method novelty, most Cu nanostructure all are by thermal evaporation or hydro-thermal synthetic, and the present invention is the electric plating method of usefulness; (2) pattern novelty, the nano wire of metal Cu, structures such as nanometer rod are synthesized in a large number, and preparation dendroid Cu nanostructure also rarely found (3) equipment is simple, common laboratory equipment can both reach requirement; (4) do not need very the operation of difficulty, very simple of method; (5) do not need catalyzer, save resource; (6) cost is low, good reproducibility, and be large-area growth.
Description of drawings
Fig. 1 is the SEM figure of a large amount of dendroid Cu nanostructures;
Fig. 2 is the TEM figure of dendroid Cu nanostructure;
Fig. 3 is the X-ray diffractogram of dendroid Cu nanostructure.
Embodiment
Further set forth characteristics of the present invention below in conjunction with accompanying drawing and specific embodiment.
Embodiment 1
This Cu dendritic single crystalline nano material and preparation method thereof, its concrete technology is as follows:
1) with copper sheet (the about 1.5cm of surface-area
2) polishing, with 30% salt acid soak 8 minutes, to put in people's acetone ultrasonicly again, the pure copper sheet that obtains is as anode;
2) with ITO conductive glass (the about 1.6cm of surface-area
2) cleaned 8 minutes with the NaOH of 0.1mol/L, it is ultrasonic to put into acetone again, uses deionized water rinsing as negative electrode at last;
3) electrolytic solution is the Cu (NO of 0.5mol/L
3)
2With the citric acid of 1.0mol/L, it is 1.5 that citric acid is used for regulating PH; At voltage is that 0.8V electroplates;
4) behind the 1.5h, take out the ITO conductive glass, adhered to the pink dirt settling of one deck above can seeing, be the Cu dendritic single crystalline nano material.
This Cu dendritic single crystalline nano material and preparation method thereof, its concrete technology is as follows:
1) with copper sheet (the about 1.5cm of surface-area
2) polishing, with 30% salt acid soak 10 minutes, to put in people's acetone ultrasonicly again, the pure copper sheet that obtains is as anode;
2) with ITO conductive glass (the about 1.6cm of surface-area
2) cleaned 10 minutes with the NaOH of 0.1mol/L, it is ultrasonic to put into acetone again, uses deionized water rinsing as negative electrode at last;
3) electrolytic solution is the Cu (NO of 0.5mol/L
3)
2With the citric acid of 1.0mol/L, it is 2 that citric acid is used for regulating PH; At voltage is that 1V electroplates;
4) behind the 2.5h, take out the ITO conductive glass, adhered to the pink dirt settling of one deck above can seeing, be the Cu dendritic single crystalline nano material.
Embodiment 3
This Cu dendritic single crystalline nano material and preparation method thereof, its concrete technology is as follows:
1) with copper sheet (the about 1.5cm of surface-area
2) polishing, with 30% salt acid soak 9 minutes, to put in people's acetone ultrasonicly again, the pure copper sheet that obtains is as anode;
2) with ITO conductive glass (the about 1.6cm of surface-area
2) cleaned 9 minutes with the NaOH of 0.1mol/L, it is ultrasonic to put into acetone again, uses deionized water rinsing as negative electrode at last;
3) electrolytic solution is the Cu (NO of 0.5mol/L
3)
2With the citric acid of 1.0mol/L, it is 1.5 that citric acid is used for regulating PH; At voltage is that 1V electroplates;
4) behind the 2h, take out the ITO conductive glass, adhered to the pink dirt settling of one deck above can seeing, be the Cu dendritic single crystalline nano material.
Embodiment 4
This Cu dendritic single crystalline nano material and preparation method thereof, its concrete technology is as follows:
1) with copper sheet (the about 1.5cm of surface-area
2) polishing, with 30% salt acid soak 10 minutes, to put in people's acetone ultrasonicly again, the pure copper sheet that obtains is as anode;
2) with ITO conductive glass (the about 1.6cm of surface-area
2) cleaned 10 minutes with the NaOH of 0.1mol/L, it is ultrasonic to put into acetone again, uses deionized water rinsing as negative electrode at last;
3) electrolytic solution is the Cu (NO of 0.5mol/L
3)
2With the citric acid of 1.0mol/L, it is 2 that citric acid is used for regulating PH; At voltage is that 1V electroplates;
4) behind the 2h, take out the ITO conductive glass, adhered to the pink dirt settling of one deck above can seeing, be the Cu dendritic single crystalline nano material.
Embodiment 5
This Cu dendritic single crystalline nano material and preparation method thereof, its concrete technology is as follows:
1) with copper sheet (the about 1.5cm of surface-area
2) polishing, with 30% salt acid soak 10 minutes, to put in people's acetone ultrasonicly again, the pure copper sheet that obtains is as anode;
2) with ITO conductive glass (the about 1.6cm of surface-area
2) cleaned 10 minutes with the NaOH of 0.1mol/L, it is ultrasonic to put into acetone again, uses deionized water rinsing as negative electrode at last;
3) electrolytic solution is the Cu (NO of 0.5mol/L
3)
2With the citric acid of 1.0mol/L, it is 2 that citric acid is used for regulating PH; At voltage is that 0.8V electroplates;
4) behind the 2h, take out the ITO conductive glass, adhered to the pink dirt settling of one deck above can seeing, be the Cu dendritic single crystalline nano material.
Resulting product behind galvanic deposit 2h under the voltage E=0.8V dendroid Cu nanostructure SEM figure as shown in Figure 1: (a) low power SEM figure, (b) high power SEM schemes as seen from the figure dendroid Cu mainly by a trunk and some symmetries neat dried compositions.
The XRD figure spectrum of the typical dendroid Cu nanostructure that ITO conductive glass galvanic deposit is as shown in Figure 2 purchased, respectively corresponding (111) and (200) peak, two main peak 2 θ=43.3 and 50.4.
The TEM of dendroid Cu nanostructure as shown in Figure 3 figure, the lower-left is SEAD figure (selected area electron diffraction figure), among the figure as can be seen dendroid Cu form by trunk and many trunks, its length is being generally 10-20 μ m, tip diameter is generally about 30-50nm.
Claims (4)
1. Cu dendritic single crystalline nano material is characterized in that: formed along the different directions regrowth by the Cu nanometer rod, dendroid Cu is by a trunk and some symmetries neat dried compositions, and its length is being 10-20 μ m, and tip diameter is 30-50nm.
2. method for preparing the described Cu dendritic single crystalline nano material of claim 1, its concrete technology is as follows:
1) with copper sheet polishing, with 30% salt acid soak 8-10 minute, to put in people's acetone ultrasonicly again, the pure copper sheet that obtains is as anode;
2) NaOH of ITO conductive glass with 0.1mol/L cleaned 8-10 minute, it is ultrasonic to put into acetone again, uses deionized water rinsing as negative electrode at last;
3) electrolytic solution is the Cu (NO of 0.5mol/L
3)
2With the citric acid of 1.0mol/L, it is 1.5-2 that citric acid is used for regulating PH; At voltage is that 0.8-1V electroplates;
4) behind the 1.5-2.5h, take out the ITO conductive glass, adhered to the pink dirt settling of one deck above can seeing, be the Cu dendritic single crystalline nano material.
3. a kind of method for preparing the Cu dendritic single crystalline nano material according to claim 2, described copper sheet purity is 99%, thickness is 0.1-0.3mm; ITO conductive glass thickness is 0.4-0.5mm.
4. a kind of method for preparing the Cu dendritic single crystalline nano material according to claim 2, described Cu (NO
3)
2With citric acid purity be 99%.
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| CN102051675B (en) * | 2010-10-28 | 2013-04-24 | 中山大学 | Method for manufacturing CuO nanowire |
| CN102251278B (en) * | 2011-05-31 | 2014-04-30 | 常州大学 | Controllable preparation method of monocrystal copper nanowires |
| JP5631910B2 (en) * | 2011-10-21 | 2014-11-26 | 三井金属鉱業株式会社 | Silver coated copper powder |
| CN102978667B (en) * | 2012-10-25 | 2016-06-22 | 烟台大学 | A kind of method of preparing nano-bronze powder using electric deposition |
| CN103088371B (en) * | 2013-01-25 | 2015-03-11 | 重庆大学 | Method for preparing nano-copper cubic particles |
| CN106435665B (en) * | 2016-09-18 | 2019-04-05 | 中山大学 | One kind having dendritic micropin wing copper surface texture of natural multi-resolution tree and preparation method thereof |
| CN107008468A (en) * | 2017-03-30 | 2017-08-04 | 华南理工大学 | Nanometer Copper Fluorin doped tin dioxide photocatalyst and preparation method and application |
| CN108796601A (en) * | 2017-05-02 | 2018-11-13 | 上海奇谋能源技术开发有限公司 | A method of producing single-crystal metal |
| CN107685155B (en) * | 2017-09-08 | 2019-03-19 | 河北工业大学 | A kind of preparation method of cupric and non-noble metal branch shape nano material |
| CN107829110A (en) * | 2017-10-13 | 2018-03-23 | 广东明方科技有限公司 | A kind of electrolyte from waste electronic wiring board recovery copper |
| CN107937943B (en) * | 2017-11-16 | 2019-04-26 | 中达电子(江苏)有限公司 | Porous wick structure and preparation method thereof |
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| US6261954B1 (en) * | 2000-02-10 | 2001-07-17 | Chartered Semiconductor Manufacturing, Ltd. | Method to deposit a copper layer |
| CN1367273A (en) * | 2001-11-28 | 2002-09-04 | 中国科学院长春应用化学研究所 | Chemical preparation method of controllable metal nano conductor |
| US6528424B1 (en) * | 2002-02-22 | 2003-03-04 | Advanced Micro Devices, Inc. | Method of electroplating a copper-zinc alloy thin film on a copper surface using a chemical solution |
| CN1438678A (en) * | 2003-03-20 | 2003-08-27 | 北京工业大学 | High-pressure electrochemical method for depositing nano Cu granule film on semiconductor Si substrate |
| CN1483540A (en) * | 2003-08-12 | 2004-03-24 | 北京科技大学 | Method for mfg nano copper powder |
| CN101264526A (en) * | 2008-05-13 | 2008-09-17 | 上海师范大学 | Preparation of nano copper particle |
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Patent Citations (6)
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|---|---|---|---|---|
| US6261954B1 (en) * | 2000-02-10 | 2001-07-17 | Chartered Semiconductor Manufacturing, Ltd. | Method to deposit a copper layer |
| CN1367273A (en) * | 2001-11-28 | 2002-09-04 | 中国科学院长春应用化学研究所 | Chemical preparation method of controllable metal nano conductor |
| US6528424B1 (en) * | 2002-02-22 | 2003-03-04 | Advanced Micro Devices, Inc. | Method of electroplating a copper-zinc alloy thin film on a copper surface using a chemical solution |
| CN1438678A (en) * | 2003-03-20 | 2003-08-27 | 北京工业大学 | High-pressure electrochemical method for depositing nano Cu granule film on semiconductor Si substrate |
| CN1483540A (en) * | 2003-08-12 | 2004-03-24 | 北京科技大学 | Method for mfg nano copper powder |
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Non-Patent Citations (1)
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