CN102127779A - Method for preparing copper oxide nano tube - Google Patents
Method for preparing copper oxide nano tube Download PDFInfo
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- CN102127779A CN102127779A CN 201010621185 CN201010621185A CN102127779A CN 102127779 A CN102127779 A CN 102127779A CN 201010621185 CN201010621185 CN 201010621185 CN 201010621185 A CN201010621185 A CN 201010621185A CN 102127779 A CN102127779 A CN 102127779A
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Abstract
The invention relates to a method for preparing a copper oxide nano tube, belongs to the field of electrochemical synthesis and discloses a technical scheme for preparing a copper oxide nano tube by an electrochemical method with mild conditions, no secondary pollution, simpleness in technological operation, low energy consumption, short reaction time and manageable reaction process. The method is characterized in that the copper oxide nano tube is synthesized in an ionic liquid by the electrochemical method based on an aluminium oxide template. The diameter of the copper oxide nano tube prepared by the invention is about 30-100nm, the length is 3-5 mu m, and the current efficiency is more than or equal to 65%. In the invention, the electrochemical method is used for synthesizing a metallic oxide nano tube, thus a brand new way is provided for the filed of synthesizing the metallic oxide nano tube, and the way can greatly promote the synthesis research and industrialization process of the metallic oxide nano tube.
Description
Technical field
A kind of method for preparing oxide copper nanometer tube of the present invention belongs to metallic substance and technical field of electrochemistry, is specifically related to a kind of technical scheme of using the method for electrochemical production oxide copper nanometer tube in ionic liquid.
Background technology
Nanotube is a kind of special hi-tech type material, wherein oxide copper nanometer tube (CuO) has characteristics such as photoelectricity and magnetics again, it has extremely profound application prospect, at present, the preparation method of oxide copper nanometer tube is also few, it is that precursor is prepared oxide copper nanometer tube with the copper hydroxide that the people such as Zhang Weixin (CN1817785A) of HeFei University of Technology in 2006 utilize chemical deposition, and still, this method transformation efficiency is not high and nanotube is misaligned; The Chemical Material of the U.S. in 2004 (2004, the 16th (26) volume, 5559-5561 page or leaf) has reported the method for utilizing template to prepare oxide copper nanometer tube, with the organometallics Cu (tmhd) of complexity
2Be the copper source, utilize chemical Vapor deposition process (MOCVD) to prepare oxide copper nanometer tube under High Temperature High Pressure, the condition harshness is wayward.
Summary of the invention
A kind of method purpose for preparing oxide copper nanometer tube of the present invention is: in order to solve the insoluble problem that exists in the above prior art, thereby disclose the technical scheme that ionic liquid combined with electrochemical method that a kind of utilization has environmental protection prepares oxide copper nanometer tube.
A kind of method for preparing oxide copper nanometer tube of the present invention is characterized in that it being a kind of based on alumina formwork method with the electrochemical production oxide copper nanometer tube in the ionic liquid of environmental protection, and concrete processing step is:
The preparation of I, alumina formwork
At first be that 99% aluminium foil places the acetone ultrasonic cleaning after 5-15 minute with purity, with massfraction is the oxide film that the 3-10% soaking with sodium hydroxide was removed aluminium foil in 1-3 minute, behind deionized water rinsing, in volume ratio is under the voltage of 10-20V in perchloric acid-ethanol solution of 1: 4, with the aluminium foil is anode, graphite is negative electrode, carries out electropolishing 2-5 minute; Then in inorganic acid solution, be anode with the polished aluminium foil under the voltage of 15-70V, graphite is negative electrode, the controlled alumina formwork of pore size is prepared in anodic oxidation 1-2 time 2-8 hour altogether; Speed with 1-5V/s is depressurized to the blocking layer that 0V comes the attenuate alumina formwork at last, to help conduction, is used for the deposition template of oxide copper nanometer tube through the alumina formwork of thinning barrier layer;
II, ion liquid configuration
Taking by weighing the mixture of 15～60g analytical pure level urea solid and two kinds of halide salts of 10～40g analytical pure level and an amount of analytical pure level mantoquita mixes and looses in the exsiccant beaker, airtight, became liquid in 3-10 hour 60-100 ℃ of heating, take out and add analytical pure level boric acid and analytical pure level tensio-active agent again, back isopyknic organic solvent liquid acid amides of adding or alcohols mixing stir, and filter, finally obtain blue ionic liquid;
III, galvanic deposit
Select the exsiccant beaker as undivided cell, with the ionic liquid of above-mentioned II configuration as electrolytic solution, in undivided cell, be negative electrode with the prepared alumina formwork of I, with the platinum filament is that anode carries out galvanic deposit, controlled temperature is at 10-60 ℃, and voltage is 1-3V, galvanic deposit 1-3 hour, promptly, take out the alumina formwork that deposits the copper nanotube then and wash 1-2min respectively with alcohol and distilled water at alumina formwork surface deposition copper nanotube;
IV, thermal treatment
The alumina formwork that deposits the copper nanotube that III is made moves into retort furnace, calcines 2-5 hour down at 400-700 ℃, cools to room temperature then with the furnace, uses the pattern that conventional SEM means characterize this nanotube.
Above-mentioned a kind of method for preparing oxide copper nanometer tube is characterized in that: mineral acid is oxalic acid, phosphoric acid or sulfuric acid among the described step I.
Above-mentioned a kind of method for preparing oxide copper nanometer tube is characterized in that: analytical pure level mantoquita solid is a kind of in cupric chloride, copper sulfate and the cupric nitrate in the described Step II.
Above-mentioned a kind of method for preparing oxide copper nanometer tube is characterized in that: analytical pure level halide salt solid is in sodium-chlor, Repone K, magnesium chloride, Sodium Bromide, Potassium Bromide and the magnesium bromide any two kinds in the described Step II.
Above-mentioned a kind of method for preparing oxide copper nanometer tube is characterized in that: the tensio-active agent in the affiliated Step II is a kind of in sodium lauryl sulphate, Sodium dodecylbenzene sulfonate and the stearin.
Above-mentioned a kind of method for preparing oxide copper nanometer tube is characterized in that: analytical pure level organic solvent is a kind of in methane amide, ethylene glycol and the glycerol in the described Step II.
A kind of method for preparing oxide copper nanometer tube of the present invention compared with prior art has following advantage:
Advantage such as that ionic liquid has is non-volatile, electroconductibility is strong, vapour pressure is little, stable in properties and electrochemical window are wide, therefore, ionic liquid is described as " green solvent " in the chemical reaction.The method that utilization of the present invention has an ionic liquid combined with electrochemical of environmental protection prepares that the oxide copper nanometer tube experiment effect is good, operation is easy to control, promptly controls voltage and can control the beginning of reaction at any time, interrupts and stop; Advantages such as the nanotube marshalling that obtains.The oxide copper nanometer tube diameter of the present invention's preparation is about 30-100nm, long 3-5 μ m, current efficiency 〉=65%.Therefore, the present invention proposes electrochemical method coupled ion liquid is used for the synthesis of nano pipe, and this approach will promote nanotube study on the synthesis and industrialization process greatly.
Description of drawings
Fig. 1 is the macro morphology figure (stereoscan photograph) of embodiment 1 products therefrom
Fig. 2 is the macro morphology figure (stereoscan photograph) of embodiment 2 products therefroms
Embodiment
Embodiment 1
At 50ml, the alumina formwork that obtains through oxidation under the 40V condition in the oxalic acid of 0.3mol/L utilizes the blocking layer of ladder voltage drop method attenuate template, dries standby after taking out then and cleaning up; Taking by weighing 30g analytical pure level urea, 10g analytical pure grade sodium chloride and 2g analytical pure level Potassium Bromide and 1g analytical pure level cupric chloride mixes and to loose in the exsiccant beaker, airtight, became liquid in 6 hours 80 ℃ of heating, take out and add 1.5g analytical pure level boric acid and 0.02g analytical pure level Sodium dodecylbenzene sulfonate again, the isopyknic methane amide mixing of back adding stirs, and filter, finally obtain blue ionic liquid; With the alumina formwork of above-mentioned preparation in alcohol ultrasonic 10 minutes, drying the back is reaming 45 minutes in 5% the phosphoric acid at 30 ℃ of massfractions, be that negative electrode, platinum filament are that the ionic liquid of anode, above-mentioned preparation is that electrolytic solution is at 50 ℃ with the template after the reaming then, voltage is the condition deposit 2 hours of 1V, take out template and use earlier alcohol wash, clean up the back with deionized water again and calcined 3 hours down at 400 ℃, be cooled to room temperature after, take out, obtain oxide copper nanometer tube.
Embodiment 2
At 50ml, the alumina formwork that obtains through oxidation under the 30V condition in the oxalic acid of 0.3mol/L utilizes the blocking layer of ladder voltage drop method attenuate template, dries standby after taking out then and cleaning up; Taking by weighing 30g analytical pure level urea, 10g analytical pure grade magnesium chloride and 2g analytical pure level Sodium Bromide and 1g analytical pure level cupric nitrate mixes and to loose in the exsiccant beaker, airtight, became liquid in 6 hours 80 ℃ of heating, take out and add 1.5g analytical pure level boric acid and 0.02g analytical pure level Sodium dodecylbenzene sulfonate again, the isopyknic methane amide mixing of back adding stirs, and filter, finally obtain blue ionic liquid; With the alumina formwork of above-mentioned preparation in alcohol ultrasonic 10 minutes, drying the back is reaming 45 minutes in 5% the phosphoric acid at 30 ℃ of massfractions, be that negative electrode, platinum filament are that the ionic liquid of anode, above-mentioned preparation is that electrolytic solution is at 60 ℃ with the template after the reaming then, voltage is the condition deposit 2 hours of 2V, take out template and use earlier alcohol wash, clean up the back with deionized water again and calcined 3 hours down at 500 ℃, be cooled to room temperature after, take out, obtain oxide copper nanometer tube.
Embodiment 3
At 50ml, the alumina formwork that obtains through oxidation under the 50V condition in the oxalic acid of 0.3mol/L utilizes the blocking layer of ladder voltage drop method attenuate template, dries standby after taking out then and cleaning up; Taking by weighing 30g analytical pure level urea, 10g analytical pure grade sodium chloride and 2g analytical pure level Potassium Bromide and 1g analytical pure level cupric chloride mixes and to loose in the exsiccant beaker, airtight, became liquid in 6 hours 80 ℃ of heating, take out and add 1.5g analytical pure level boric acid and 0.02g analytical pure level sodium lauryl sulphate again, the isopyknic ethylene glycol mixing of back adding stirs, and filter, finally obtain blue ionic liquid; With the alumina formwork of above-mentioned preparation in alcohol ultrasonic 10 minutes, drying the back is reaming 45 minutes in 5% the phosphoric acid at 30 ℃ of massfractions, be that negative electrode, platinum filament are that the ionic liquid of anode, above-mentioned preparation is that electrolytic solution is at 40 ℃ with the template after the reaming then, voltage is the condition deposit 2 hours of 3V, take out template and use earlier alcohol wash, clean up the back with deionized water again and calcined 4 hours down at 500 ℃, be cooled to room temperature after, take out, obtain oxide copper nanometer tube.
Embodiment 4
At 50ml, massfraction is the blocking layer that the alumina formwork that obtains through oxidation under the 60V condition in 5% phosphoric acid utilizes ladder voltage drop method attenuate template, dries standby after taking out then and cleaning up; Taking by weighing 30g analytical pure level urea, 10g analytical pure grade sodium chloride and 2g analytical pure level Potassium Bromide and 1g analytical pure grade bluestone mixes and to loose in the exsiccant beaker, airtight, became liquid in 6 hours 80 ℃ of heating, take out and add 1.5g analytical pure level boric acid and 0.02g analytical pure level Sodium dodecylbenzene sulfonate again, the isopyknic methane amide mixing of back adding stirs, and filter, finally obtain blue ionic liquid; With the alumina formwork of above-mentioned preparation in alcohol ultrasonic 10 minutes, dry the back 30 ℃ of massfractions be 5% phosphoric acid in reaming 45 minutes, be that negative electrode, platinum filament are that the ionic liquid of anode, above-mentioned preparation is that electrolytic solution is at 50 ℃ with the template after the reaming then, voltage is the condition deposit 1 hour of 2V, take out template and use earlier alcohol wash, clean up the back with deionized water again and calcined 3 hours down at 500 ℃, be cooled to room temperature after, take out, obtain oxide copper nanometer tube.
Embodiment 5
At 50ml, massfraction is the blocking layer that the alumina formwork that obtains through oxidation under the 70V condition in 5% phosphoric acid utilizes ladder voltage drop method attenuate template, dries standby after taking out then and cleaning up; Taking by weighing 30g analytical pure level urea, 10g analytical pure grade potassium chloride and 2g analytical pure level Sodium Bromide and 1g analytical pure level cupric chloride mixes and to loose in the exsiccant beaker, airtight, became liquid in 6 hours 80 ℃ of heating, take out and add 1.5g analytical pure level boric acid and 0.02g analytical pure level Sodium dodecylbenzene sulfonate again, the isopyknic glycerol mixing of back adding stirs, and filter, finally obtain blue ionic liquid; With the alumina formwork of above-mentioned preparation in alcohol ultrasonic 10 minutes, dry the back 30 ℃ of massfractions be 5% phosphoric acid in reaming 45 minutes, be that negative electrode, platinum filament are that the ionic liquid of anode, above-mentioned preparation is that electrolytic solution is at 50 ℃ with the template after the reaming then, voltage is the condition deposit 1 hour of 3V, take out template and use earlier alcohol wash, clean up the back with deionized water again and calcined 3 hours down at 600 ℃, be cooled to room temperature after, take out, obtain oxide copper nanometer tube.
Embodiment 6
At 50ml, massfraction is the blocking layer that the alumina formwork that obtains through oxidation under the 15V condition in 15% sulfuric acid utilizes ladder voltage drop method attenuate template, dries standby after taking out then and cleaning up; Taking by weighing 30g analytical pure level urea, 10g analytical pure grade sodium chloride and 2g analytical pure level magnesium bromide and 1g analytical pure level cupric chloride mixes and to loose in the exsiccant beaker, airtight, became liquid in 6 hours 80 ℃ of heating, take out and add 1.5g analytical pure level boric acid and 0.02g analytical pure level stearin again, the isopyknic methane amide mixing of back adding stirs, and filter, finally obtain blue ionic liquid; With the alumina formwork of above-mentioned preparation in alcohol ultrasonic 10 minutes, drying the back is reaming 45 minutes in 5% the phosphoric acid at 30 ℃ of massfractions, be that negative electrode, platinum filament are that the ionic liquid of anode, above-mentioned preparation is that electrolytic solution is at 50 ℃ with the template after the reaming then, voltage is the condition deposit 3 hours of 1V, take out template and use earlier alcohol wash, clean up the back with deionized water again and calcined 3 hours down at 700 ℃, be cooled to room temperature after, take out, obtain oxide copper nanometer tube.
Claims (6)
1. a method for preparing oxide copper nanometer tube is characterized in that it being a kind of based on alumina formwork method with the electrochemical production oxide copper nanometer tube in the ionic liquid of environmental protection, and concrete processing step is:
The preparation of I, alumina formwork
At first be that 99% aluminium foil places the acetone ultrasonic cleaning after 5-15 minute with purity, with massfraction is the oxide film that the 3-10% soaking with sodium hydroxide was removed aluminium foil in 1-3 minute, behind deionized water rinsing, in volume ratio is under the voltage of 10-20V in perchloric acid-ethanol solution of 1: 4, with the aluminium foil is anode, graphite is negative electrode, carries out electropolishing 2-5 minute; Then in inorganic acid solution, be anode with the polished aluminium foil under the voltage of 15-70V, graphite is negative electrode, the controlled alumina formwork of pore size is prepared in anodic oxidation 1-2 time 2-8 hour altogether; Speed with 1-5V/s is depressurized to the blocking layer that 0V comes the attenuate alumina formwork at last, to help conduction, is used for the deposition template of oxide copper nanometer tube through the alumina formwork of thinning barrier layer;
II, ion liquid configuration
Taking by weighing the mixture of 15～60g analytical pure level urea solid and two kinds of halide salts of 10～40g analytical pure level and an amount of analytical pure level mantoquita mixes and looses in the exsiccant beaker, airtight, became liquid in 3-10 hour 60-100 ℃ of heating, take out and add analytical pure level boric acid and analytical pure level tensio-active agent again, back isopyknic organic solvent liquid acid amides of adding or alcohols mixing stir, and filter, finally obtain blue ionic liquid;
III, galvanic deposit
Select the exsiccant beaker as undivided cell, with the ionic liquid of above-mentioned II configuration as electrolytic solution, in undivided cell, be negative electrode with the prepared alumina formwork of I, with the platinum filament is that anode carries out galvanic deposit, controlled temperature is at 10-60 ℃, and voltage is 1-3V, galvanic deposit 1-3 hour, promptly, take out the alumina formwork that deposits the copper nanotube then and wash 1-2min respectively with alcohol and distilled water at alumina formwork surface deposition copper nanotube;
IV, thermal treatment
The alumina formwork that deposits the copper nanotube that III is made moves into retort furnace, calcines 2-5 hour down at 400-700 ℃, cools to room temperature then with the furnace, uses the pattern that conventional SEM means characterize this nanotube.
2. according to the described a kind of method for preparing oxide copper nanometer tube of claim 1, it is characterized in that: mineral acid is oxalic acid, phosphoric acid or sulfuric acid among the described step I.
3. according to the described a kind of method for preparing oxide copper nanometer tube of claim 1, it is characterized in that: analytical pure level mantoquita solid is a kind of in cupric chloride, copper sulfate and the cupric nitrate in the described Step II.
4. according to the described a kind of method for preparing oxide copper nanometer tube of claim 1, it is characterized in that: analytical pure level halide salt solid is in sodium-chlor, Repone K, magnesium chloride, Sodium Bromide, Potassium Bromide and the magnesium bromide any two kinds in the described Step II.
5. according to the described a kind of method for preparing oxide copper nanometer tube of claim 1, it is characterized in that: the tensio-active agent in the affiliated Step II is a kind of in sodium lauryl sulphate, Sodium dodecylbenzene sulfonate and the stearin.
6. according to the described a kind of method for preparing oxide copper nanometer tube of claim 1, it is characterized in that: analytical pure level organic solvent is a kind of in methane amide, ethylene glycol and the glycerol in the described Step II.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102828210A (en) * | 2012-09-10 | 2012-12-19 | 太原理工大学 | Method for electroplating zinc-nickel alloy through neodymium iron boron magnet ionic liquid |
| CN102839403A (en) * | 2012-09-10 | 2012-12-26 | 太原理工大学 | Method for electroplating aluminum in ionic liquid |
| CN103160853A (en) * | 2011-12-12 | 2013-06-19 | 中国科学院过程工程研究所 | Method for electrolyzing aluminum by using amino-functionalized ionic liquid electrolyte |
| CN105618778A (en) * | 2015-12-29 | 2016-06-01 | 中国石油化工股份有限公司 | Preparation method for copper nanotube with copper oxide nano-particles embedded therein |
| 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 |
| CN107217287A (en) * | 2017-02-10 | 2017-09-29 | 江苏城乡建设职业学院 | A kind of method in regulation and control titania nanotube footpath |
| CN107331830A (en) * | 2017-07-01 | 2017-11-07 | 合肥国轩高科动力能源有限公司 | A kind of anode composite of lithium-sulfur cell and preparation method thereof |
| CN108753056A (en) * | 2018-05-18 | 2018-11-06 | 蚌埠心里程电子科技有限公司 | A kind of infrared radiation coating containing cordierite |
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| CN101030606A (en) * | 2007-01-12 | 2007-09-05 | 武汉理工大学 | Use of CuO nano-needle/Cu base-plate material in solar dye battery |
| CN101486485A (en) * | 2009-02-27 | 2009-07-22 | 华东师范大学 | Honeycomb CuO nano material and preparation thereof |
| US20100047523A1 (en) * | 2008-08-25 | 2010-02-25 | Yong Hyup Kim | Hydrophobic composites and methods of making the same |
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| CN1462720A (en) * | 2003-06-10 | 2003-12-24 | 东北师范大学 | Method for preparing nano tube of some metalloid oxides and metals with size and shape being controllable |
| CN101030606A (en) * | 2007-01-12 | 2007-09-05 | 武汉理工大学 | Use of CuO nano-needle/Cu base-plate material in solar dye battery |
| US20100047523A1 (en) * | 2008-08-25 | 2010-02-25 | Yong Hyup Kim | Hydrophobic composites and methods of making the same |
| CN101486485A (en) * | 2009-02-27 | 2009-07-22 | 华东师范大学 | Honeycomb CuO nano material and preparation thereof |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103160853A (en) * | 2011-12-12 | 2013-06-19 | 中国科学院过程工程研究所 | Method for electrolyzing aluminum by using amino-functionalized ionic liquid electrolyte |
| CN102839403A (en) * | 2012-09-10 | 2012-12-26 | 太原理工大学 | Method for electroplating aluminum in ionic liquid |
| CN102828210B (en) * | 2012-09-10 | 2014-03-26 | 太原理工大学 | Method for electroplating zinc-nickel alloy through neodymium iron boron magnet ionic liquid |
| CN102839403B (en) * | 2012-09-10 | 2015-02-25 | 太原理工大学 | Method for electroplating aluminum in ionic liquid |
| CN102828210A (en) * | 2012-09-10 | 2012-12-19 | 太原理工大学 | Method for electroplating zinc-nickel alloy through neodymium iron boron magnet ionic liquid |
| CN105618778A (en) * | 2015-12-29 | 2016-06-01 | 中国石油化工股份有限公司 | Preparation method for copper nanotube with copper oxide nano-particles embedded therein |
| CN107217287B (en) * | 2017-02-10 | 2021-02-19 | 江苏城乡建设职业学院 | Method for regulating and controlling diameter of titanium dioxide nanometer pipe |
| CN107217287A (en) * | 2017-02-10 | 2017-09-29 | 江苏城乡建设职业学院 | A kind of method in regulation and control titania nanotube footpath |
| 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 |
| CN106947995B (en) * | 2017-04-28 | 2018-12-21 | 合肥工业大学 | A kind of single-phase CuO nanometer sheet array film and preparation method thereof |
| CN107331830B (en) * | 2017-07-01 | 2019-12-13 | 合肥国轩高科动力能源有限公司 | Composite positive electrode of lithium-sulfur battery and preparation method thereof |
| CN107331830A (en) * | 2017-07-01 | 2017-11-07 | 合肥国轩高科动力能源有限公司 | A kind of anode composite of lithium-sulfur cell and preparation method thereof |
| CN108753056A (en) * | 2018-05-18 | 2018-11-06 | 蚌埠心里程电子科技有限公司 | A kind of infrared radiation coating containing cordierite |
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