CN101555608A - Method for preparing nano materials by direct electrodeposit in ionic liquid microemulsion - Google Patents
Method for preparing nano materials by direct electrodeposit in ionic liquid microemulsion Download PDFInfo
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- CN101555608A CN101555608A CNA2009100433401A CN200910043340A CN101555608A CN 101555608 A CN101555608 A CN 101555608A CN A2009100433401 A CNA2009100433401 A CN A2009100433401A CN 200910043340 A CN200910043340 A CN 200910043340A CN 101555608 A CN101555608 A CN 101555608A
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Abstract
The invention relates to a method for preparing nano materials by direct electrodeposit in ionic liquid microemulsion, a new technology for preparing nano materials, which combines an electrochemical method and a microemulsion method. Under the effect of surface active agent polyoxyethylene octyl phenyl ether, 1-butyl-3-methylimidazole hexaflourophosphate salt ionic liquid and aqueous solution form water drum ionic liquid microemulsion with relatively high electroconductibility; an electroconductive electrode and the water drum ionic liquid microemulsion form an electrode system. A nano metal plating featuring controllable size and even distribution is prepared in a 'nano pool' in ionic liquid microemulsion by a current control method or an electric potential control method; wherein, size of the nano particles can be controlled by the mol ratio between water and the surface active agent; the technology for preparing novel nano materials has the advantages of low equipment cost, easy operation and easy control.
Description
Technical field:
The present invention relates to a kind of in ion liquid microemulsion the direct novel method of prepared by electrodeposition nano material.
Background technology:
Nano material is the type material paid close attention to of people extremely in recent years.Nanoparticle is little because of its particle diameter, specific surface area is big, and has unique physics and chemical property, is widely used in fields such as catalysis, electricity, optics, biosensor.The method for preparing at present nano material has a lot, and wherein microemulsion method is to use one of wider method.
Microemulsion is meant two kinds of immiscible liquid under the effect of surfactant molecule interfacial film, the Thermodynamically stable of formation, isotropy, transparent or semitransparent dispersion system.The droplet dia of microemulsion disperse phase is generally 0～100nm, is a kind of solution system with special construction and performance.Because this ordered molecular molectron (nanometer pond) with nano-scale has been proved to be nano material synthetic effecting reaction device, by regulation and control to factors such as the size of this nano-reactor, materials, can synthesize nano material easily with ad hoc structure and character, over nearly 20 years, follow the progress of nanoscale science and technology, the basis of microemulsion and applied research have obtained development rapidly.Because the electroconductibility extreme difference of general reverse microemulsion system is difficult to use in electrochemical research, utilize microemulsion to prepare nanoparticle at present and mainly adopt chemical method, electrochemical method adopts seldom.
Ionic liquid is made of the relative less inorganic or organic anion with volume of the bigger organic cation of volume, is a kind of low temperature or room temperature fused salt of being made up of ion fully.Compare with the traditional organic solvent or the aqueous solution, ionic liquid has the outstanding advantage of series: (1) does not almost have vapour pressure, non-volatile, colourless nothing to smell; (2) thermostability height has very wide liquid temperature scope; (3) chemical stability is good, has the electrochemical window of broad etc.Therefore ionic liquid is subjected to paying close attention to widely in material preparation, chemosynthesis, biotechnology field as a kind of emerging green solvent.Because ionic liquid has the potential window of good electrical conductivity and broad, is used to electrochemical research very early, be used for some aqueous solution by high praise especially and be difficult to the electrochemical process that carries out.
Ionic liquid and water can constitute microemulsion under the effect of tensio-active agent, the novel ion liquid microemulsion of this kind has similar microtexture to traditional reverse micro emulsion, but it has higher electroconductibility, so can be used for the electrochemical applications process.Electrochemical method is simple to operate, with low cost because of it, be easy to control is extensively paid close attention to.Therefore, the electrochemical production nano material technology that adopts in ion liquid microemulsion of the present invention's proposition has a good application prospect.
Summary of the invention:
Purpose of the present invention aims to provide the method for a kind of novelty, convenience, controllable preparation nano material, adopts this method to need not specific installation and special process flow process, the nano-deposit that can prepare controllable size, is evenly distributed.
It is characterized in that conductor electrode is placed the water bag ion liquid microemulsion that contains metal-salt, adopt certain current density or control certain electropotential, can obtain uniformity in short period of time, the metal plating of particle diameter between 0～100nm, and size can be controlled by parameter regulation.
The objective of the invention is to realize by following manner:
The present invention as electrolyte system, and makes up electrode system with itself and electrode with novel water bag ion liquid microemulsion, utilizes " nanometer pond " in the microemulsion as reactor, realizes the preparation of controllable nano coating by electrochemical method.
Corresponding metal salt brine solution, surfactant polyethylene octyl phenyl ether and 1-butyl-3-Methylimidazole hexafluorophosphate ionic liquid is mixed according to a certain percentage, under the ultrasonic wave effect, be uniformly dispersed, form transparent homogeneous phase ionic liquid bag water microemulsion.Metal-salt wherein can be copper sulfate, Silver Nitrate, hydrochloro-auric acid etc. according to the deposition needs, and its concentration of aqueous solution can change in the relative broad range of 0.01～0.1mol/L.
Described galvanic deposit basal electrode material can be copper, nickel, stainless steel, glass carbon, need counter electrode to carry out certain pre-treatment before the deposition, promptly adopt the superfine alumina powder counter electrode to polish earlier, place dilute nitric acid solution, ethanol, the ultrasonic 3～5min of redistilled water then respectively.
Described galvanic deposit be with copper, nickel, stainless steel, glass carbon etc. as working electrode, the big area platinized platinum is put into the ion liquid microemulsion ionogen as to the utmost point, adopts certain electrochemical method to realize galvanic deposit.Can adopt control current method or CONTROLLED POTENTIAL method: when adopting the control current method, its current density is controlled at 3～20mA/cm
2When adopting the CONTROLLED POTENTIAL method, its current potential can be controlled in-0.4～0.2V (Ag/AgCl electropotential relatively).
Described galvanic deposit is that the electrode through pre-treatment is directly placed water bag ion liquid microemulsion, constant current or constant potential 5～30min.
Described galvanic deposit is that the electrode through pre-treatment is directly placed the water bag ion liquid microemulsion of temperature in 10～40 ℃ of scopes.
Described controllable size, the nano metal coating that is evenly distributed are meant that the nano metal coating particle diameter of acquisition can be by the mole control recently of water and surfactant polyethylene octyl phenyl ether.When the control certain molar ratio, can form one deck granular size unanimity, the metal nanoparticle of particle diameter between 0～100nm at electrode surface through after the galvanic deposit of certain hour.
The object of the present invention is to provide a kind of new method for preparing nano-deposit.Adopt the inventive method microemulsion method and two kinds of advantages that prepare nano material of electrochemical method can be united two into one.Adopt the ion liquid microemulsion of high conductivity to replace traditional reverse micro emulsion, thereby make galvanic deposit become possibility; Adopt electrochemical method equipment cheap, simple to operate, be easy to control, can regulate the microscopic appearance of coating easily by controlled variable.Finally can difference according to demand obtain various functional nano materials.
Description of drawings
Accompanying drawing 1 is the stereoscan photograph that embodiment 1 adopts the silver-colored nano-deposit of the inventive method gained.
Accompanying drawing 2 is the stereoscan photograph that embodiment 2 adopts the gold nano coating of the inventive method gained.
Accompanying drawing 3 is about the stereoscan photograph of the gold nano coating of 40nm for embodiment 3 adopts the particle diameter of the inventive method gained.
Accompanying drawing 4 is about the stereoscan photograph of the gold nano coating of 25nm for embodiment 3 adopts the particle diameter of the inventive method gained.
Accompanying drawing 5 is about the stereoscan photograph of the gold nano coating of 10nm for embodiment 3 adopts the particle diameter of the inventive method gained.
Specific embodiments
Following examples are intended to illustrate the present invention rather than limitation of the invention further.
[embodiment 1]
0.05mol/L silver nitrate aqueous solution, surfactant polyethylene octyl phenyl ether and 1-butyl-3-Methylimidazole hexafluorophosphate ionic liquid is mixed by 10%, 45%, 45% volume ratio respectively, and ultrasonic then 10min mixes it.The glass-carbon electrode that with diameter is 3mm polishes smooth on the ultra-fine alumina powder, places each ultrasonic 5min of diluted nitric acid aqueous solution, dehydrated alcohol and redistilled water after the washing respectively, dried for standby.Then glass carbon is connect power cathode as working electrode, the big area platinized platinum is put into the ion liquid microemulsion that contains Silver Nitrate for preparing in advance for the utmost point is connect positive source, and control current density is 5mA/cm
2, can on electrode, obtain required coating behind the deposition 5min.(SEM, JSM-6700F, JEOLCompany Japan) finds its coating even particle distribution through scanning electron microscope, and particle diameter is about 15nm.
[embodiment 2]
Aqueous solution of chloraurate, surfactant polyethylene octyl phenyl ether and 1-butyl-3-Methylimidazole hexafluorophosphate ionic liquid of 0.01mol/L is mixed by 10%, 55%, 35% volume ratio respectively, and ultrasonic then 10min mixes it.Be 0.5cm with surface-area simultaneously
2Stainless steel electrode on the ultra-fine alumina powder, polish smooth to minute surface, place each ultrasonic 5min of diluted nitric acid aqueous solution, dehydrated alcohol and redistilled water after the washing respectively, dried for standby.Then with stainless steel as working electrode, the big area platinized platinum is to the utmost point, and anhydrous Ag/AgCl is a reference electrode, puts into the ion liquid microemulsion that contains hydrochloro-auric acid for preparing in advance, the control electrode current potential is 0.2V, can obtain required coating behind the deposition 30min on stainless steel electrode.(SEM, JSM-6700F, JEOL Company Japan) finds its coating even particle distribution through scanning electron microscope, particle diameter is about 50nm, characterize its gold grain of discovery through X-ray diffraction (XRD, Bruker D8Advance Diffractometer, Cu K α 1) and be face-centred cubic structure.
[embodiment 3]
Aqueous solution of chloraurate, surfactant polyethylene octyl phenyl ether and 1-butyl-3-Methylimidazole hexafluorophosphate ionic liquid of 0.1mol/L is mixed by certain volume ratio respectively, prepare the microemulsion of three parts of water and tensio-active agent different mol ratio, its mol ratio is respectively 5.25,7.7,9.0, and ultrasonic then 10min mixes it.Be 0.5cm with surface-area simultaneously
2Nickel electrode on abrasive paper for metallograph, polish the light, place each ultrasonic 5min of dehydrated alcohol and redistilled water after the washing respectively, dried for standby.Then nickel electrode is connected power cathode as working electrode, the big area platinized platinum is that the utmost point is connected positive source, put into three kinds of water and tensio-active agent different mol ratio that prepare in advance, the ion liquid microemulsion that contains hydrochloro-auric acid, control current density is 10mA/cm
2, promptly find on nickel electrode, to have obtained metal plating behind the deposition 8min.(SEM, JSM-6700F, JEOL Company Japan) finds its coating even particle distribution through scanning electron microscope, and particle diameter is respectively 40nm, 25nm, 10nm, and the more little coating grain diameter of the mol ratio of water and tensio-active agent is just more little.
Claims (10)
1. direct method of prepared by electrodeposition nano material in ion liquid microemulsion, it is characterized in that: with metal electrode or glass-carbon electrode etc. as negative electrode, platinized platinum places the ion liquid microemulsion that is dissolved with metal-salt to constitute the cathodic polarization system as anode, adopt certain current density or control certain electropotential, the nano metal coating that can obtain one deck controllable size at electrode surface, be evenly distributed is handled in cathodic polarization through certain hour.
2. according to claim 1: as to it is characterized in that the aqueous solution and 1-butyl-3-Methylimidazole hexafluorophosphate ionic liquid, surfactant polyethylene octyl phenyl ether and the water that will be dissolved with metal-salt constitute water bag ion liquid microemulsion according to a certain percentage.
3. according to claim 2: it is characterized in that metal-salt can be copper sulfate, Silver Nitrate, hydrochloro-auric acid etc., its concentration of aqueous solution is 0.01～0.1mol/L.
4. according to claim 1: as to it is characterized in that the electrode materials that is adopted can be copper, nickel, stainless steel, glass carbon.
5. according to claim 1: it is characterized in that described galvanic deposit is that the electrode through pre-treatment is directly placed water bag ion liquid microemulsion, its current density can be controlled in 3～20mA/cm
2
6. according to claim 1: it is characterized in that described galvanic deposit is that the electrode through pre-treatment is directly placed water bag ion liquid microemulsion, its current potential (Ag/AgCl electropotential relatively) can be controlled in-0.4～0.2V.
7. according to claim 1: as to it is characterized in that described galvanic deposit is that the electrode through pre-treatment is directly placed water bag ion liquid microemulsion, constant current or constant potential 5～30min.
8. according to claim 1: as to it is characterized in that electrodeposition temperature can be controlled in 10～40 ℃.
9. according to claim 1: as to it is characterized in that its particle diameter of nano metal coating that obtains is 0～100nm.
10. according to claim 1: as to it is characterized in that nano particle diameter can be by the mole control recently of water and surfactant polyethylene octyl phenyl ether.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105518185A (en) * | 2013-03-14 | 2016-04-20 | 思力柯集团 | Electrodeposition in ionic liquid electrolytes |
| CN105714350A (en) * | 2016-04-26 | 2016-06-29 | 陕西师范大学 | Method for preparing Ni-Fe hydroxide nanometer films through electrodeposition |
| CN105862091A (en) * | 2016-04-26 | 2016-08-17 | 陕西师范大学 | Method for preparing nanometer Ni-Fe alloy through tetrabasic ionic liquid micro-emulsion |
| CN105965032A (en) * | 2016-07-26 | 2016-09-28 | 陕西师范大学 | Electrochemical method for preparing Ag-Pd nano-alloy in quaternary ionic liquid microemulsion |
| CN106661753A (en) * | 2014-04-15 | 2017-05-10 | 尼奥工业有限责任公司 | Ionic liquid electrolyte and method to electrodeposit metals |
| CN109530717A (en) * | 2018-12-03 | 2019-03-29 | 安徽工业大学 | The method of microemulsion method controlledly synthesis Ag metal nano material in original position from Ag-containing solution |
| CN114101656A (en) * | 2021-12-07 | 2022-03-01 | 浙江大学 | Preparation method and application of silver nanoparticles with universal dispersion characteristics |
| CN114759169A (en) * | 2022-04-21 | 2022-07-15 | 山东合泰新能源有限公司 | Zinc electrode containing zinc corrosion inhibitor triton X-100 and preparation method thereof |
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2009
- 2009-05-11 CN CNA2009100433401A patent/CN101555608A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105518185A (en) * | 2013-03-14 | 2016-04-20 | 思力柯集团 | Electrodeposition in ionic liquid electrolytes |
| CN105518185B (en) * | 2013-03-14 | 2019-11-15 | 思力柯集团 | Electro-deposition in ionic liquid electrolyte |
| US10190227B2 (en) | 2013-03-14 | 2019-01-29 | Xtalic Corporation | Articles comprising an electrodeposited aluminum alloys |
| US11105013B2 (en) | 2014-04-15 | 2021-08-31 | Neo Industries Llc | Ionic liquid electrolyte and method to electrodeposit metals |
| CN106661753A (en) * | 2014-04-15 | 2017-05-10 | 尼奥工业有限责任公司 | Ionic liquid electrolyte and method to electrodeposit metals |
| CN105862091B (en) * | 2016-04-26 | 2018-07-10 | 陕西师范大学 | The method that chemical machining nano Ni-Fe alloy is prepared using quaternary ion liquid microemulsion |
| CN105714350B (en) * | 2016-04-26 | 2018-07-10 | 陕西师范大学 | A kind of method that electro-deposition prepares Ni-Fe hydroxide nano films |
| CN105862091A (en) * | 2016-04-26 | 2016-08-17 | 陕西师范大学 | Method for preparing nanometer Ni-Fe alloy through tetrabasic ionic liquid micro-emulsion |
| CN105714350A (en) * | 2016-04-26 | 2016-06-29 | 陕西师范大学 | Method for preparing Ni-Fe hydroxide nanometer films through electrodeposition |
| CN105965032A (en) * | 2016-07-26 | 2016-09-28 | 陕西师范大学 | Electrochemical method for preparing Ag-Pd nano-alloy in quaternary ionic liquid microemulsion |
| CN109530717A (en) * | 2018-12-03 | 2019-03-29 | 安徽工业大学 | The method of microemulsion method controlledly synthesis Ag metal nano material in original position from Ag-containing solution |
| CN114101656A (en) * | 2021-12-07 | 2022-03-01 | 浙江大学 | Preparation method and application of silver nanoparticles with universal dispersion characteristics |
| CN114759169A (en) * | 2022-04-21 | 2022-07-15 | 山东合泰新能源有限公司 | Zinc electrode containing zinc corrosion inhibitor triton X-100 and preparation method thereof |
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Application publication date: 20091014 |