CN101538725A - Method for preparing Tb-Co alloy layer by utilizing ionic liquid electrodeposition technology - Google Patents
Method for preparing Tb-Co alloy layer by utilizing ionic liquid electrodeposition technology Download PDFInfo
- Publication number
- CN101538725A CN101538725A CN200910071687A CN200910071687A CN101538725A CN 101538725 A CN101538725 A CN 101538725A CN 200910071687 A CN200910071687 A CN 200910071687A CN 200910071687 A CN200910071687 A CN 200910071687A CN 101538725 A CN101538725 A CN 101538725A
- Authority
- CN
- China
- Prior art keywords
- alloy layer
- ionic liquid
- prepare
- electrodeposition technology
- liquid electrodeposition
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Abstract
The invention relates to a method for preparing a Tb-Co alloy layer by utilizing ionic liquid electrodeposition technology, in particular to a method for preparing the Tb-Co alloy layer, aiming at solving the problems of complicated manufacturing technique and equipment, high cost and uneven surface of a settled layer when the Tb-Co alloy layer is prepared by the prior art. The preparation method comprises: 1. 1- methyl-3- butyllnildaanlium tetrafluoroborate, anhydrous cobalt fluoroborate and anhydrous terbium fluoroborate are mixed together for preparing ionic liquid electrolyte; 2. electrodeposition; 3. after being washed by ethanol and distilled water and dried, the sample is dried to obtain the Tb-Co alloy layer. The method utilizes the ionic liquid electrodeposition technology to synthesize the smooth, flat and uniform Tb-Co alloy layer. The invention has simple technique and equipment as well as low cost.
Description
Technical field
The present invention relates to a kind of method of the Tb-Co of preparation alloy layer.
Background technology
From nineteen eighty-two, Wilkes reported with chlorination 1-methyl-3-ethyl imidazol(e) (1-ethyl-3-methylimidazoliumchloride, EMIC) and AlCl
3After mixing the good ionic liquid at room temperature of available energy, ionic liquid has obtained paying close attention to widely in every field.Ionic liquid is compared with ordinary organic solvents, not only most of inorganicss and organism is had good solubility, and simultaneously it also has very wide electrochemical window, good electroconductibility, does not almost have vapour pressure, higher advantages such as thermostability.Therefore, ionic liquid has obtained using widely aspect electrodeposit metals.The Tb-Co alloy layer is subjected to people's attention owing to have special magnetic property always, the Tb-Co alloy layer is mainly prepared by physical methods such as injection, vacuum sputterings at present, but these methods exist technology, equipment complexity, the higher and uneven first-class defective in settled layer surface of cost.
Summary of the invention
The objective of the invention is when preparing the Tb-Co alloy layer, to have preparation technology and the surperficial inhomogenous problem of equipment complexity, cost height and settled layer, and a kind of method of utilizing ionic liquid electrodeposition technology to prepare the Tb-Co alloy layer is provided in order to solve prior art.
The method of utilizing ionic liquid electrodeposition technology to prepare the Tb-Co alloy layer realizes according to the following steps: one, in ar gas environment, by 1～7: 1～3: 1～6 mol ratio mixes 1-methyl-3-butyl imidazole a tetrafluoro borate, anhydrous fluoroboric acid cobalt and anhydrous fluoroboric acid terbium, gets il electrolyte; Two, adopting the method for galvanic deposit to put into il electrolyte through pretreated matrix, is that 20～100 ℃, current density are 20～120A/m in temperature
2, the distance between anode and the matrix is under the condition of 1～10cm, electroplating processes 5～10min, test specimen; Three, adopt ethanol and distilled water flushing successively behind the taking-up test specimen, drying promptly gets the Tb-Co alloy layer; As anode, matrix is as negative electrode with platinized platinum or graphite in galvanic deposit in the step 2.
Carry out electron-microscope scanning according to the Tb-Co alloy layer that the present invention is obtained and observe, utilize the method for ionic liquid electrodeposition to synthesize the Tb-Co alloy layer of smooth smooth, homogeneous.Technology of the present invention is simple and equipment is simple, (starting material are market and buy) with low cost.
Description of drawings
Fig. 1 is the stereoscan photograph of resultant product Tb-Co alloy layer in the embodiment 14, Fig. 2 is the stereoscan photograph of embodiment 15 resultant product Tb-Co alloy layers, and Fig. 3 is the stereoscan photograph of embodiment 16 resultant product Tb-Co alloy layers.
Embodiment
Embodiment one: the method that present embodiment utilizes ionic liquid electrodeposition technology to prepare the Tb-Co alloy layer realizes according to the following steps: one, in ar gas environment, by 1～7: 1～3: 1～6 mol ratio mixes 1-methyl-3-butyl imidazole a tetrafluoro borate, anhydrous fluoroboric acid cobalt and anhydrous fluoroboric acid terbium, gets il electrolyte; Two, adopting the method for galvanic deposit to put into il electrolyte through pretreated matrix, is that 20～100 ℃, current density are 20～120A/m in temperature
2, the distance between anode and the matrix is under the condition of 1～10cm, electroplating processes 5～10min, test specimen; Three, adopt ethanol and distilled water flushing successively behind the taking-up test specimen, drying promptly gets the Tb-Co alloy layer; As anode, matrix is as negative electrode with platinized platinum or graphite in galvanic deposit in the step 2.
Employed starting material are all bought in market in the present embodiment.
Embodiment two: present embodiment and embodiment one are different is that the mol ratio of 1-methyl in the step 1-3-butyl imidazole a tetrafluoro borate, anhydrous fluoroboric acid cobalt and anhydrous fluoroboric acid terbium is 2～6: 1.5～2.5: 2～5.Other step and parameter are identical with embodiment one.
Embodiment three: present embodiment and embodiment one are different is that the mol ratio of 1-methyl in the step 1-3-butyl imidazole a tetrafluoro borate, anhydrous fluoroboric acid cobalt and anhydrous fluoroboric acid terbium is 4: 2: 3.Other step and parameter are identical with embodiment one.
Embodiment four: present embodiment and embodiment one to three are different is that the preprocessing process of matrix is that sodium hydroxide solution, the mass concentration of using 3mol/L successively is 20% hydrochloric acid soln washing in the step 2, and water cleans and finishes then.Other step and parameter are identical with embodiment one to three.
It is that the purpose of 20% hydrochloric acid soln is greasy dirt and the oxide compound in order to erode matrix surface that present embodiment adds the NaOH solution of 3mol/L and mass concentration.
Embodiment five: what present embodiment and embodiment one to four were different is that temperature is 40 ℃ in the step 2.Other step and parameter are identical with embodiment one to four.
Embodiment six: what present embodiment and embodiment four were different is that current density is 40～100A/m in the step 2
2Other step and parameter are identical with embodiment four.
Embodiment seven: what present embodiment and embodiment four were different is that current density is 60A/m in the step 2
2Other step and parameter are identical with embodiment four.
Embodiment eight: present embodiment and embodiment one, two, three, six or seven are different is that the distance between anode and the matrix is 2～8cm in the step 2.Other step and parameter are identical with embodiment one, two, three, six or seven.
Embodiment nine: present embodiment and embodiment one, two, three, six or seven are different is that the distance between anode and the matrix is 5cm in the step 2.Other step and parameter are identical with embodiment one, two, three, six or seven.
Embodiment ten: present embodiment is different with embodiment eight or nine be in the step 2 electroplating processes time be 6～9min.Other step and parameter are identical with embodiment eight or nine.
Embodiment 11: present embodiment is different with embodiment eight or nine be in the step 2 electroplating processes time be 8min.Other step and parameter are identical with embodiment eight or nine.
Embodiment 12: what present embodiment and embodiment one, two, three, six, seven, ten or 11 were different is that matrix is copper sheet, gold plaque, platinized platinum, silver strip or iron plate in the step 2.Other step and parameter are identical with embodiment one, two, three, six, seven, ten or 11.
Embodiment 13: what present embodiment and embodiment 12 were different is that alcoholic acid purity is 99.9% in the step 3.Other step and parameter are identical with embodiment 12.
Embodiment 14: the method that present embodiment utilizes ionic liquid electrodeposition technology to prepare the Tb-Co alloy layer realizes according to the following steps: one, in ar gas environment, by 3: 1: 2 mol ratios 1-methyl-3-butyl imidazole a tetrafluoro borate, anhydrous fluoroboric acid cobalt and anhydrous fluoroboric acid terbium are mixed, get il electrolyte; Two, adopting the method for galvanic deposit to put into il electrolyte through pretreated copper sheet, is that 60 ℃, current density are 100A/m in temperature
2, the distance between platinized platinum and the copper sheet is under the condition of 2.5cm, electroplating processes 5min, test specimen; Three, adopt ethanol and distilled water flushing successively behind the taking-up test specimen, drying promptly gets the Tb-Co alloy layer.
The method of the galvanic deposit in the present embodiment step 2 is employing HY1791-5S D.C. regulated power supply power supply stream and realization.
The terbium content of the Tb-Co alloy layer that present embodiment obtains is 15%, and cobalt contents is 85%.
The Tb-Co alloy layer that present embodiment obtains has metalluster.
Adopt the Tb-Co alloy layer of present embodiment preparation, the scanning electron microscope analysis figure of Tb-Co alloy layer as shown in Figure 1.Tb-Co alloy layer surface presents state smooth, uniform surface.
Embodiment 15: the method that present embodiment utilizes ionic liquid electrodeposition technology to prepare the Tb-Co alloy layer realizes according to the following steps: one, in ar gas environment, by 2: 1: 6 mol ratios 1-methyl-3-butyl imidazole a tetrafluoro borate, anhydrous fluoroboric acid cobalt and anhydrous fluoroboric acid terbium are mixed, get il electrolyte; Two, adopting the method for galvanic deposit to put into il electrolyte through pretreated gold plaque, is that 30 ℃, current density are 80A/m in temperature
2, the distance between platinized platinum and the gold plaque is under the condition of 1cm, electroplating processes 5min, test specimen; Three, adopt ethanol and distilled water flushing successively behind the taking-up test specimen, drying promptly gets the Tb-Co alloy layer.
The method of the galvanic deposit in the present embodiment step 2 adopts the HY1791-5S D.C. regulated power supply that electric current is provided and realizes.
The terbium content of the Tb-Co alloy layer that present embodiment obtains is 22%, and cobalt contents is 78%.
The Tb-Co alloy layer that present embodiment obtains has metalluster.
Adopt the Tb-Co alloy layer of present embodiment preparation, the scanning electron microscope analysis figure of Tb-Co alloy layer as shown in Figure 2.Tb-Co alloy layer surface presents state smooth, uniform surface.
Embodiment 16: the method that present embodiment utilizes ionic liquid electrodeposition technology to prepare the Tb-Co alloy layer realizes according to the following steps: one, in ar gas environment, by 3: 2: 5 mol ratios 1-methyl-3-butyl imidazole a tetrafluoro borate, anhydrous fluoroboric acid cobalt and anhydrous fluoroboric acid terbium are mixed, get il electrolyte; Two, adopting the method for galvanic deposit to put into il electrolyte through pretreated matrix, is that 100 ℃, current density are 80A/m in temperature
2, the distance between platinized platinum and the gold plaque is under the condition of 5cm, electroplating processes 10min, test specimen; Three, adopt ethanol and distilled water flushing successively behind the taking-up test specimen, drying promptly gets the Tb-Co alloy layer.
The method of the electrophoretic deposition in the present embodiment step 2 adopts the HY1791-5S D.C. regulated power supply that electric current is provided and realizes.
The terbium content of the Tb-Co alloy layer that present embodiment obtains is 18%, and cobalt contents is 82%.
The Tb-Co alloy layer that present embodiment obtains has metalluster.
Adopt the Tb-Co alloy layer of present embodiment preparation, the scanning electron microscope analysis figure of Tb-Co alloy layer as shown in Figure 3.Tb-Co alloy layer surface presents state smooth, uniform surface.
Claims (8)
1, a kind of method of utilizing ionic liquid electrodeposition technology to prepare the Tb-Co alloy layer, it is characterized in that the method for utilizing ionic liquid electrodeposition technology to prepare the Tb-Co alloy layer realizes according to the following steps: one, in ar gas environment, by 1～7: 1～3: 1～6 mol ratio mixes 1-methyl-3-butyl imidazole a tetrafluoro borate, anhydrous fluoroboric acid cobalt and anhydrous fluoroboric acid terbium, gets il electrolyte; Two, adopting the method for galvanic deposit to put into il electrolyte through pretreated matrix, is that 20～100 ℃, current density are 20～120A/m in temperature
2, the distance between anode and the matrix is under the condition of 1～10cm, electroplating processes 5～10min, test specimen; Three, adopt ethanol and distilled water flushing successively behind the taking-up test specimen, drying promptly gets the Tb-Co alloy layer; As anode, matrix is as negative electrode with platinized platinum or graphite in galvanic deposit in the step 2.
2, a kind of method of utilizing ionic liquid electrodeposition technology to prepare the Tb-Co alloy layer according to claim 1 is characterized in that the mol ratio of 1-methyl in the step 1-3-butyl imidazole a tetrafluoro borate, anhydrous fluoroboric acid cobalt and anhydrous fluoroboric acid terbium is 2～6: 1.5～2.5: 2～5.
3, a kind of method of utilizing ionic liquid electrodeposition technology to prepare the Tb-Co alloy layer according to claim 1 and 2, it is characterized in that the preprocessing process of matrix in the step 2 is that working concentration is that the sodium hydroxide solution of 3mol/L and mass concentration are 20% hydrochloric acid soln washing successively, water cleans and finishes then.
4, a kind of method of utilizing ionic liquid electrodeposition technology to prepare the Tb-Co alloy layer according to claim 3 is characterized in that current density is 40～100A/m in the step 2
2
5,, it is characterized in that the distance between the anode and matrix is 2～8cm in the step 2 according to claim 1,2 or 4 described a kind of methods of utilizing ionic liquid electrodeposition technology to prepare the Tb-Co alloy layer.
6, a kind of method of utilizing ionic liquid electrodeposition technology to prepare the Tb-Co alloy layer according to claim 5 is characterized in that the electroplating processes time is 6～9min in the step 2.
7, according to claim 1,2,4 or 6 described a kind of methods of utilizing ionic liquid electrodeposition technology to prepare the Tb-Co alloy layer, it is characterized in that matrix is copper sheet, gold plaque, platinized platinum, silver strip or iron plate in the step 2.
8, a kind of method of utilizing ionic liquid electrodeposition technology to prepare the Tb-Co alloy layer according to claim 7 is characterized in that alcoholic acid purity is 99.9% in the step 3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100716877A CN101538725B (en) | 2009-03-31 | 2009-03-31 | Method for preparing Tb-Co alloy layer by utilizing ionic liquid electrodeposition technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100716877A CN101538725B (en) | 2009-03-31 | 2009-03-31 | Method for preparing Tb-Co alloy layer by utilizing ionic liquid electrodeposition technology |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101538725A true CN101538725A (en) | 2009-09-23 |
| CN101538725B CN101538725B (en) | 2010-09-22 |
Family
ID=41122104
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009100716877A Expired - Fee Related CN101538725B (en) | 2009-03-31 | 2009-03-31 | Method for preparing Tb-Co alloy layer by utilizing ionic liquid electrodeposition technology |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101538725B (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101949044A (en) * | 2010-09-20 | 2011-01-19 | 大连海事大学 | Niobium electro-osmosis method for steel surface in ionic liquid |
| CN102936738A (en) * | 2012-10-24 | 2013-02-20 | 彩虹集团公司 | Low-temperature cobalt electrodeposition method utilizing ionic liquid |
| WO2016023785A1 (en) * | 2014-08-11 | 2016-02-18 | Siemens Aktiengesellschaft | Electrochemical deposition of a heavy rare earth material for increasing the coercive field strength of rare earth permanent magnets |
| CN105648487A (en) * | 2014-12-03 | 2016-06-08 | 北京中科三环高技术股份有限公司 | Electro-deposition method, electro-deposition liquid and method for preparing rare earth permanent magnetic material in electro-deposition manner |
| CN105839152A (en) * | 2015-10-21 | 2016-08-10 | 北京中科三环高技术股份有限公司 | Electrodeposition method, electrodeposition solution and method for preparation of rare earth permanent magnetic material by electrodeposition |
| CN108642536A (en) * | 2018-04-11 | 2018-10-12 | 上海大学 | The method of electrodeposit metals zinc in using 1,2- dichloroethanes as the ionic liquid of additive |
| CN110415969A (en) * | 2019-09-02 | 2019-11-05 | 江西理工大学 | A kind of method that Low-temperature electro-deposition prepares Dy-Ni alloy film |
-
2009
- 2009-03-31 CN CN2009100716877A patent/CN101538725B/en not_active Expired - Fee Related
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101949044A (en) * | 2010-09-20 | 2011-01-19 | 大连海事大学 | Niobium electro-osmosis method for steel surface in ionic liquid |
| CN101949044B (en) * | 2010-09-20 | 2011-12-28 | 大连海事大学 | Niobium electro-osmosis method for steel surface in ionic liquid |
| CN102936738A (en) * | 2012-10-24 | 2013-02-20 | 彩虹集团公司 | Low-temperature cobalt electrodeposition method utilizing ionic liquid |
| WO2016023785A1 (en) * | 2014-08-11 | 2016-02-18 | Siemens Aktiengesellschaft | Electrochemical deposition of a heavy rare earth material for increasing the coercive field strength of rare earth permanent magnets |
| CN105648487A (en) * | 2014-12-03 | 2016-06-08 | 北京中科三环高技术股份有限公司 | Electro-deposition method, electro-deposition liquid and method for preparing rare earth permanent magnetic material in electro-deposition manner |
| CN105839152A (en) * | 2015-10-21 | 2016-08-10 | 北京中科三环高技术股份有限公司 | Electrodeposition method, electrodeposition solution and method for preparation of rare earth permanent magnetic material by electrodeposition |
| WO2017067251A1 (en) * | 2015-10-21 | 2017-04-27 | 北京中科三环高技术股份有限公司 | Electrodeposition method, bath and rare earth permanent magnet materials preparation method using same |
| JP2018502212A (en) * | 2015-10-21 | 2018-01-25 | 北京中科三環高技術股▲ふん▼有限公司 | Electrodeposition method, electrodeposition liquid and method for producing rare earth permanent magnet material by electrodeposition |
| DE112016000145B4 (en) | 2015-10-21 | 2023-06-22 | Beijing Zhong Ke San Huan High-Tech Co., Ltd. | Electrodeposition method, electrodeposition bath and method for producing a rare earth permanent magnet material by electrodeposition |
| CN108642536A (en) * | 2018-04-11 | 2018-10-12 | 上海大学 | The method of electrodeposit metals zinc in using 1,2- dichloroethanes as the ionic liquid of additive |
| CN110415969A (en) * | 2019-09-02 | 2019-11-05 | 江西理工大学 | A kind of method that Low-temperature electro-deposition prepares Dy-Ni alloy film |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101538725B (en) | 2010-09-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101538725B (en) | Method for preparing Tb-Co alloy layer by utilizing ionic liquid electrodeposition technology | |
| Eftekharinia et al. | Optimization of charge transport in a Co–Pi modified hematite thin film produced by scalable electron beam evaporation for photoelectrochemical water oxidation | |
| Wang et al. | A novel silver oxides oxygen evolving catalyst for water splitting | |
| US7651639B2 (en) | Conductive polymer and solid electrolytic capacitor using the same | |
| CN103014755B (en) | Fabrication method of long-life titanium base electrode | |
| Sun et al. | Conformal coating of superhydrophilic metal-organic complex toward substantially improved photoelectrochemical water oxidation | |
| Chen et al. | High-performance and low-cost dye-sensitized solar cells based on kesterite Cu2ZnSnS4 nanoplate arrays on a flexible carbon cloth cathode | |
| Duan et al. | Counter electrode electrocatalysts from one-dimensional coaxial alloy nanowires for efficient dye-sensitized solar cells | |
| CN106591890A (en) | Method for preparing micro-nano-porous silver based on eutectic flux in-situ alloy deposition/alloy removing method | |
| CN106149026A (en) | The preparation of a kind of Graphene/golden nanometer particle composite and characterizing method | |
| Yang et al. | Nickel interlayer enables indirect corrosion protection of magnesium alloy by photoelectrochemical cathodic protection | |
| CN108314085B (en) | The preparation method of tungstic trioxide nano-slice complex light anode | |
| CN113106512A (en) | Surface modification method of titanium substrate for fuel cell | |
| CN113403663A (en) | Preparation method of polyaniline-based composite coating applied to stainless steel bipolar plate | |
| CN113235124A (en) | S-FeOOH/bismuth vanadate composite photo-anode and preparation method thereof | |
| CN102628214A (en) | Carbon fiber composite material with ZnO layer electrolytically deposited on surface as well as preparation method and application thereof | |
| Xiong et al. | Revealing the enhanced photoelectrochemical water oxidation activity of Fe-based metal-organic polymer-modified BiVO4 photoanode | |
| CN104966835A (en) | Method for manufacturing AgVO<3> thin films on Ag substrates by means of electrolysis | |
| Shi et al. | BiOI/WO 3 photoanode with enhanced photoelectrochemical water splitting activity | |
| Chigane et al. | Titanium dioxide thin films prepared by electrolysis from aqueous solution of titanium–lactic acid complex for dye-sensitized solar cells | |
| Zhang et al. | Fabrication of hierarchically structured S-doped NiFe hydroxide/oxide electrodes for solar-assisted oxygen evolution reaction in seawater splitting | |
| JP2009102676A (en) | Corrosion-resistant conductive-coated material and its use | |
| CN101509142B (en) | Method for producing TbFeCo alloy film by using ionic liquid impulse electrodeposition technology | |
| CN109972149A (en) | A kind of Bi2Te3/Bi2O3/TiO2The preparation method of ternary heterojunction film | |
| Knapik et al. | Cathodic deposition of SnO2 layers on transparent conductive substrates and their photoelectrochemical activity |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20100922 Termination date: 20110331 |