CN101486485A - Honeycomb CuO nano material and preparation thereof - Google Patents
Honeycomb CuO nano material and preparation thereof Download PDFInfo
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- CN101486485A CN101486485A CNA2009100467520A CN200910046752A CN101486485A CN 101486485 A CN101486485 A CN 101486485A CN A2009100467520 A CNA2009100467520 A CN A2009100467520A CN 200910046752 A CN200910046752 A CN 200910046752A CN 101486485 A CN101486485 A CN 101486485A
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- copper sheet
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Abstract
The invention discloses a preparation method of honeycombed CuO nano structure, which includes concrete steps as follows: copper sheet is burnished and soaked in 30% hydrochloric acid for 8 minutes to 10 minutes, and then put into acetone for ultrasonic processing to obtain pure copper sheet which is taken as a positive electrode; graphite is selected as a negative electrode; 3mol/L KOH is adopted as an electrolytic solution; voltage ranges from 3V to 5V; after electrolytic deposition is carried out for 3h to 5h, the copper sheet is taken out and a layer of blue Cu(OH)2 precursor is generated on the surface of the copper sheet; and under the protection of N2, the obtained Cu(OH)2 precursor is heated at 150 DEG C to 160 DEG C for 2.5h to 3.5h and then taken out, and a layer of black honeycombed nano CuO is generated on the surface of the copper sheet. Compared with the nano structure synthesized in the past, the preparation method is prominently characterized by: (1) novel method; (2) novel appearance; (3) simple equipment; (4) simple operation; (5) no requirement of catalysts, resource conservation; and (6) low cost.
Description
Technical field
The present invention relates to a kind of nano material, be specially a kind of honeycomb CuO nano material, and this preparation of nanomaterials; Belong to semiconductor material, photoelectron material and device technology field.
Background technology
CuO is a kind of wide bandgap semiconductor, and has bigger exciton bind energy, very big application prospect is arranged in opto-electronic device, photochemical catalysis and solar cell, again because its thermostability, special property such as high mechanical strength and chemical stability has caused the interest of people to the field emission characteristic research of its nanostructure.Particularly in recent years, the continuous progress of video technique causes people's improving constantly visual experience.Original C RT (cathode tube) and LCD liquid-crystal display thereof show out their some drawbacks especially, the problem that isoionic cost is too high, people are more and more interested in Field Emission Display, also more and more higher to its expected value, what probably the display equipment of being made by field emmision material in the near future will be large quantities of is universal.So recently, people utilize the whole bag of tricks (solid phase method, hydro-thermal synthetic etc.) to prepare various CuO nano-needle 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 CuO.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 honeycomb CuO nanostructure and preparation method thereof is provided.To solve the problems referred to above of prior art.
Honeycomb CuO nanostructure provided by the present invention and preparation method thereof, be reported first in the world, this honeycomb CuO nanostructure is to be formed by the nano wire oriented growth, has very intensive concentration, its length is being generally 10-20 μ m, and diameter is generally at 100-300nm.
The preparation method of this honeycomb CuO nanostructure, its concrete steps are 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; Select graphite (the about 1.6cm of surface-area for use
2) as negative electrode;
2) with the KOH of 3mol/L as electrolytic solution; Voltage is 3-5V;
3) behind the galvanic deposit 3-5h; Take out copper sheet, can see that the copper sheet surface generates the Cu (OH) of one deck blueness
2Precursor;
4) at N
2Under the protection, with the Cu (OH) that step 3) obtained
2Precursor at 150 ℃-160 ℃ heating 2.5-3.5h, takes out then, and the copper sheet surface generates the cellular nano CuO of one deck black.
Described copper sheet purity is 99%, and thickness is 0.1-0.3mm.
KOH purity is 82% 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.
The present invention is a kind of honeycomb CuO nanostructure.With respect to former synthetic nanostructure, outstanding feature of the present invention is: (1) method novelty, most CuO nanostructure all are by thermal evaporation or hydro-thermal synthetic, and the present invention is the electric plating method of usefulness; (2) pattern novelty, former synthetic CuO nanostructure mostly is nano wire, nanometer rod and so on, (3) equipment is simple still first and prepare cellular CuO, and 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 X-ray diffractogram of honeycomb CuO nanostructure;
Fig. 2 is the SEM figure and the TEM figure of a large amount of honeycomb CuO nanostructures;
Fig. 3 is different time sections Cu (OH)
2The SEM figure of precursor.
Embodiment
Further set forth technical characterstic of the present invention below in conjunction with accompanying drawing and specific embodiment.
Embodiment 1
With surface-area is 1.5cm
2Copper sheet polishing with 30% salt acid soak 8 minutes, is put in people's acetone ultrasonicly again, and the pure copper sheet that obtains is as anode; Select for use surface-area to be about 1.6cm
2Graphite is (as negative electrode; With the KOH of 3mol/L as electrolytic solution; Voltage is 3V; Behind the galvanic deposit 3h; Take out copper sheet, can see that the copper sheet surface generates the Cu (OH) of one deck blueness
2Precursor; At N
2Under the protection, with the Cu (OH) that is obtained
2Precursor at 150 ℃ of heating 2.5h, takes out then, and the copper sheet surface generates the cellular nano CuO of one deck black.
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; Select graphite (the about 1.6cm of surface-area for use
2) as negative electrode; With the KOH of 3mol/L as electrolytic solution; Voltage is 5V; Behind the galvanic deposit 5h; Take out copper sheet, can see that the copper sheet surface generates the Cu (OH) of one deck blueness
2Precursor; At N
2Under the protection, with the Cu (OH) that is obtained
2Precursor at 160 ℃ of heating 3.5h, takes out then, and the copper sheet surface generates the cellular nano CuO of one deck black.
Embodiment 3
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; Select graphite (the about 1.6cm of surface-area for use
2) as negative electrode; With the KOH of 3mol/L as electrolytic solution; Voltage is 4V; Behind the galvanic deposit 4h; Take out copper sheet, can see that the copper sheet surface generates the Cu (OH) of one deck blueness
2Precursor; At N
2Under the protection, with the Cu (OH) that is obtained
2Precursor at 155 ℃ of heating 3h, takes out then, and the copper sheet surface generates the cellular nano CuO of one deck black.
Embodiment 4
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; Select graphite (the about 1.6cm of surface-area for use
2) as negative electrode; With the KOH of 3mol/L as electrolytic solution; Voltage is 4V; Behind the galvanic deposit 4h; Take out copper sheet, can see that the copper sheet surface generates the Cu (OH) of one deck blueness
2Precursor; At N
2Under the protection, with the Cu (OH) that is obtained
2Precursor at 160 ℃ of heating 3h, takes out then, and the copper sheet surface generates the cellular nano CuO of one deck black.
Embodiment 5
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; Select graphite (the about 1.6cm of surface-area for use
2) as negative electrode; With the KOH of 3mol/L as electrolytic solution; Voltage is 3V; Behind the galvanic deposit 3h; Take out copper sheet, can see that the copper sheet surface generates the Cu (OH) of one deck blueness
2Precursor; At N
2Under the protection, with the Cu (OH) that is obtained
2Precursor at 160 ℃ of heating 3h, takes out then, and the copper sheet surface generates the cellular nano CuO of one deck black.
The X-ray diffractogram of the product that obtains for the foregoing description 1-5 method as shown in Figure 1, typical honeycomb CuO nanostructure and Cu (OH)
2The XRD figure spectrum of precursor: (a) Cu (OH)
2Precursor, (b) honeycomb CuO.Among the figure: Cu (OH)
2Consistent with the peak value of CuO with the standard peak value.Because substrate, we see 2 sharp-pointed copper peaks in addition from figure.
Under one group of different voltage as shown in Figure 2, the SEM figure of the honeycomb CuO nanostructure that the utilization electrochemical deposition obtains: (a, b) E=3V; (c, d) E=5V; High power SEM figure can find out that the honeycomb CuO nanostructure is to combine the TEM figure that (e) figure is the CuO nano wire by the nano wire orientation, and illustration is corresponding SAED figure (selected area electron diffraction figure).
Under the E=3V voltage as shown in Figure 3, the Cu of different depositing times (OH)
2The SEM figure of precursor: (a) 30min, (b) 1h, (c) 2h, (d) we draw 3h from figure: Cu (OH)
2Generate nano wire earlier, under electric field action, self-assembly forms cellular nano structure C u (OH) then
2It has very intensive concentration, and its length is being generally 10-20 μ m, and diameter is generally at 100-300nm.
Claims (4)
1, a kind of honeycomb CuO nanostructure is characterized in that: be to be formed by the nano wire oriented growth, have very intensive concentration, its length is being 10-20 μ m, and diameter is 100-300nm, has cellular structure.
2, a kind of preparation method who prepares the described honeycomb CuO nanostructure of claim 1, its concrete steps are 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; Select for use graphite as negative electrode;
2) with the KOH of 3mol/L as electrolytic solution; Voltage is 3-5V;
3) behind the galvanic deposit 3-5h; Take out copper sheet, can see that the copper sheet surface generates the Cu (OH) of one deck blueness
2Precursor;
4) at N
2Under the protection, with the Cu (OH) that step 3) obtained
2Precursor at 150 ℃-160 ℃ heating 2.5-3.5h, takes out then, and the copper sheet surface generates the cellular nano CuO of one deck black.
3, the preparation method of a kind of honeycomb CuO nanostructure according to claim 2 is characterized in that: described copper sheet purity is 99%, and thickness is 0.1-0.3mm.
4, the preparation method of a kind of honeycomb CuO nanostructure according to claim 2 is characterized in that: described KOH purity is 82%.
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| CNA2009100467520A CN101486485A (en) | 2009-02-27 | 2009-02-27 | Honeycomb CuO nano material and preparation thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102127779A (en) * | 2010-12-25 | 2011-07-20 | 太原理工大学 | Method for preparing copper oxide nano tube |
| CN102527614A (en) * | 2012-03-02 | 2012-07-04 | 华南理工大学 | Copper surface gradient wetting self-assembly film and preparation method thereof |
| CN103834963A (en) * | 2014-01-09 | 2014-06-04 | 山西大同大学 | A preparation method of silver phosphate and M-O (M=Cu+, fe3+, zn2+) narrow bandgap semiconductor nanoparticles |
| CN105839128A (en) * | 2016-03-09 | 2016-08-10 | 中南大学 | Preparation method for CuO nanoflake powdery material |
| CN106947995A (en) * | 2017-04-28 | 2017-07-14 | 合肥工业大学 | A kind of single-phase CuO nanometer sheet array film and preparation method thereof |
| CN106947994A (en) * | 2017-04-01 | 2017-07-14 | 上海琛岫自控科技有限公司 | A kind of coat of metal based on cupric oxide nano line |
| CN110342563A (en) * | 2019-07-17 | 2019-10-18 | 湖北大学 | A kind of cupric oxide nano line and its preparation method and application |
| CN110756411A (en) * | 2019-11-04 | 2020-02-07 | 哈尔滨工业大学 | Method for enhancing mechanical strength of inorganic material micron/nanometer microstructure |
-
2009
- 2009-02-27 CN CNA2009100467520A patent/CN101486485A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102127779A (en) * | 2010-12-25 | 2011-07-20 | 太原理工大学 | Method for preparing copper oxide nano tube |
| CN102127779B (en) * | 2010-12-25 | 2012-08-22 | 太原理工大学 | Method for preparing copper oxide nano tube |
| CN102527614A (en) * | 2012-03-02 | 2012-07-04 | 华南理工大学 | Copper surface gradient wetting self-assembly film and preparation method thereof |
| CN103834963A (en) * | 2014-01-09 | 2014-06-04 | 山西大同大学 | A preparation method of silver phosphate and M-O (M=Cu+, fe3+, zn2+) narrow bandgap semiconductor nanoparticles |
| CN105839128A (en) * | 2016-03-09 | 2016-08-10 | 中南大学 | Preparation method for CuO nanoflake powdery material |
| CN106947994A (en) * | 2017-04-01 | 2017-07-14 | 上海琛岫自控科技有限公司 | A kind of coat of metal based on cupric oxide nano line |
| CN106947995A (en) * | 2017-04-28 | 2017-07-14 | 合肥工业大学 | A kind of single-phase CuO nanometer sheet array film and preparation method thereof |
| CN110342563A (en) * | 2019-07-17 | 2019-10-18 | 湖北大学 | A kind of cupric oxide nano line and its preparation method and application |
| CN110756411A (en) * | 2019-11-04 | 2020-02-07 | 哈尔滨工业大学 | Method for enhancing mechanical strength of inorganic material micron/nanometer microstructure |
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Open date: 20090722 |