CN101509142A - Method for producing TbFeCo alloy film by using ionic liquid impulse electrodeposition technology - Google Patents
Method for producing TbFeCo alloy film by using ionic liquid impulse electrodeposition technology Download PDFInfo
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- CN101509142A CN101509142A CNA2009100716881A CN200910071688A CN101509142A CN 101509142 A CN101509142 A CN 101509142A CN A2009100716881 A CNA2009100716881 A CN A2009100716881A CN 200910071688 A CN200910071688 A CN 200910071688A CN 101509142 A CN101509142 A CN 101509142A
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Abstract
The invention provides a method for preparing a TbFeCo alloy film by using the technology of ionic liquid pulse electrodeposition, relating to a method for preparing the TbFeCo alloy film. The invention resolves the problems of complex preparation process and equipment, high cost and inhomogenous surface of the deposit layer in the prior art when preparing the TbFeCo alloy film. The method is as follows: 1, mixing 1-methyl-3-butyllnildaanlium tetrafluoroborate, anhydrous ferric fluoborate, anhydrous codmium fluoborate and anhydrous terbium fluoborate to prepare ionic liquid electrolyte; 2, pulse electrodopositing; and 3, washing a test piece by ethyl alcohol and distilled water, and drying the test piece to obtain the TbFeCo alloy film. The invention uses the ionic liquid pulse electrodeposition method to synthesize the TbFeCo alloy film which has smooth, plane and uniform surface. The invention has simple process and equipment as well as low cost.
Description
Technical field
The present invention relates to a kind of method of the TbFeCo of preparation alloy firm.
Background technology
At present, rare earth-transition group alloy is subjected to people's attention owing to have special magneto-optical property always, and it is mainly used in the magneto-optic disk field of storage, and the TbFeCo alloy firm is the most frequently used magnetoopticmemory material.Rare earth-the transition group alloy firm is mainly prepared by physical methods such as injection, vacuum sputterings, but these methods exist technology, equipment complexity, the higher and inhomogenous defective in settled layer surface of cost.
Summary of the invention
The objective of the invention is when preparing the TbFeCo alloy firm, 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 impulse electrodeposition technology to prepare the TbFeCo alloy firm is provided in order to solve prior art.
The method of utilizing ionic liquid impulse electrodeposition technology to prepare the TbFeCo alloy firm realizes according to the following steps: one, in ar gas environment, by 1～7: 1～5: 1～4: 1～6 mol ratio mixes 1-methyl-3-butyl imidazole a tetrafluoro borate, anhydrous ferric fluoborate, anhydrous fluoroboric acid cobalt and anhydrous fluoroboric acid terbium, gets il electrolyte; Two, adopt the method for pulse electrodeposition to put into il electrolyte through pretreated matrix, be in temperature that 20～80 ℃, pulsewidth are 10%～99%, frequency is that 0.5～4.5kHz, voltage are that distance between 2.0～10.0V, anode and the matrix is under the condition of 2～8cm, electroplating processes 10min gets test specimen; Three, adopt ethanol and distilled water flushing successively behind the taking-up test specimen, drying promptly gets the TbFeCo alloy firm; As anode, matrix is as negative electrode with platinized platinum or graphite in galvanic deposit in the step 2.
Carry out scanning electron microscopic observation according to the TbFeCo alloy firm that the present invention is obtained, utilize the method for ionic liquid impulse electrodeposition to synthesize the TbFeCo alloy firm of smooth smooth, uniform surface.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 TbFeCo alloy firm in the embodiment 16, Fig. 2 is the stereoscan photograph of embodiment 17 resultant product TbFeCo alloy firms, Fig. 3 is the stereoscan photograph of embodiment 18 resultant product TbFeCo alloy firms, and Fig. 4 is the stereoscan photograph of embodiment 19 resultant product TbFeCo alloy firms.
Embodiment
Embodiment one: the method that present embodiment utilizes ionic liquid impulse electrodeposition technology to prepare the TbFeCo alloy firm realizes according to the following steps: one, in ar gas environment, by 1～7: 1～5: 1～4: 1～6 mol ratio mixes 1-methyl-3-butyl imidazole a tetrafluoro borate, anhydrous ferric fluoborate, anhydrous fluoroboric acid cobalt and anhydrous fluoroboric acid terbium, gets il electrolyte; Two, adopt the method for pulsed deposition to put into il electrolyte through pretreated matrix, be in temperature that 20～80 ℃, pulsewidth are 10%～99%, frequency is that 0.5～4.5kHz, voltage are that distance between 2.0～10.0V, anode and the matrix is under the condition of 2～8cm, electroplating processes 10min gets test specimen; Three, adopt ethanol and distilled water flushing successively behind the taking-up test specimen, drying promptly gets the TbFeCo alloy firm; 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.
The anode of galvanic deposit is insoluble to il electrolyte in the present embodiment step 2.
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 ferric fluoborate, anhydrous fluoroboric acid cobalt and anhydrous fluoroboric acid terbium is 2～6: 2～4: 2～3: 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 ferric fluoborate, anhydrous fluoroboric acid cobalt and anhydrous fluoroboric acid terbium is 4: 3: 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 pulsewidth is 30%～70% in the step 2.Other step and parameter are identical with embodiment one to four.
Embodiment six: what present embodiment and embodiment one to four were different is that pulsewidth is 50% in the step 2.Other step and parameter are identical with embodiment one to four.
Embodiment seven: what present embodiment and embodiment one, two, three, five or six were different is that the step 2 medium frequency is 1.5～3.5kHz.Other step and parameter are identical with embodiment one, two, three, five or six.
Embodiment eight: what present embodiment and embodiment one, two, three, five or six were different is that the step 2 medium frequency is 2kHz.Other step and parameter are identical with embodiment one, two, three, five or six.
Embodiment nine: what present embodiment was different with embodiment seven or eight is that voltage is 4.0～8.0V in the step 2.Other step and parameter are identical with embodiment seven or eight.
Embodiment ten: what present embodiment was different with embodiment seven or eight is that voltage is 6.0V in the step 2.Other step and parameter are identical with embodiment seven or eight.
Embodiment 11: present embodiment and embodiment one, two, three, six, seven, nine or ten are different is that the distance between anode and the matrix is 4～6cm in the step 2.Other step and parameter are identical with embodiment one, two, three, six, seven, nine or ten.
Embodiment 12: present embodiment and embodiment one, two, three, six, seven, nine or ten 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, seven, nine or ten.
Embodiment 13: what present embodiment was different with embodiment 11 or 12 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 11 or 12.
Embodiment 14: what present embodiment and embodiment one, two, three, six, seven, nine, ten or 13 were different is that temperature is 40～60 ℃ in the step 2.Other step and parameter are identical with embodiment one, two, three, six, seven, nine, ten or 13.
Embodiment 15: what present embodiment and embodiment one, two, three, six, seven, nine, ten or 13 were different is that temperature is 50 ℃ in the step 2.Other step and parameter are identical with embodiment one, two, three, six, seven, nine, ten or 13.
Embodiment 16: what present embodiment was different with embodiment 14 or 15 is that alcoholic acid purity is 99.9% in the step 3.Other step and parameter are identical with embodiment 14 or 15.
Embodiment 17: the method that present embodiment utilizes ionic liquid impulse electrodeposition technology to prepare the TbFeCo alloy firm realizes according to the following steps: one, in ar gas environment, by 3: 2: 1: 3 mol ratio mixed 1-methyl-3-butyl imidazole a tetrafluoro borate, anhydrous ferric fluoborate, anhydrous fluoroboric acid cobalt and anhydrous fluoroboric acid terbium, got il electrolyte; Two, adopt the method for pulse electrodeposition to put into il electrolyte through pretreated copper sheet, be in temperature that 30 ℃, pulsewidth are 20%, frequency is that 1.5kHz, voltage are that distance between 3.0V, platinized platinum and the copper sheet is under the condition of 2.5cm, electroplating processes 10min gets test specimen; Three, adopt ethanol and distilled water flushing successively behind the taking-up test specimen, drying promptly gets the TbFeCo alloy firm; As anode, copper sheet is as negative electrode with platinized platinum in galvanic deposit in the step 2.
The method of the galvanic deposit in the present embodiment step 2 is to adopt DMC-30M type high frequency positive pulse electroplating power supply to realize.
The terbium content of the TbFeCo alloy firm that present embodiment obtains is 10%, and cobalt contents is 34%, and iron level is 56%.
The TbFeCo alloy firm that present embodiment obtains has metalluster.
Adopt the TbFeCo alloy firm of present embodiment preparation, the scanning electron microscope analysis figure of TbFeCo alloy firm as shown in Figure 1.TbFeCo alloy firm surface presents the state of smooth smooth, uniform surface.
Embodiment 17: the method that present embodiment utilizes ionic liquid impulse electrodeposition technology to prepare the TbFeCo alloy firm realizes according to the following steps: one, in ar gas environment, by 3: 2: 1: 6 mol ratio mixed 1-methyl-3-butyl imidazole a tetrafluoro borate, anhydrous ferric fluoborate, anhydrous fluoroboric acid cobalt and anhydrous fluoroboric acid terbium, got il electrolyte; Two, adopt the method for pulse electrodeposition to put into il electrolyte through pretreated gold plaque, be in temperature that 50 ℃, pulsewidth are 40%, frequency is that 2.0kHz, voltage are that distance between 4.5V, platinized platinum and the gold plaque is under the condition of 3cm, electroplating processes 10min gets test specimen; Three, adopt ethanol and distilled water flushing successively behind the taking-up test specimen, drying promptly gets the TbFeCo alloy firm; As anode, gold plaque is as negative electrode with platinized platinum in galvanic deposit in the step 2.
The method of the galvanic deposit in the present embodiment step 2 is to adopt DMC-30M type high frequency positive pulse electroplating power supply to realize.
The terbium content of the TbFeCo alloy firm that present embodiment obtains is 19%, and cobalt contents is 30%, and iron level is 51%.
The TbFeCo alloy firm that present embodiment obtains has metalluster.
Adopt the TbFeCo alloy firm of present embodiment preparation, the scanning electron microscope analysis figure of TbFeCo alloy firm as shown in Figure 2.TbFeCo alloy firm surface presents the state of smooth smooth, uniform surface.
Embodiment 18: the method that present embodiment utilizes ionic liquid impulse electrodeposition technology to prepare the TbFeCo alloy firm realizes according to the following steps: one, in ar gas environment, by 4: 3: 2: 5 mol ratio mixed 1-methyl-3-butyl imidazole a tetrafluoro borate, anhydrous ferric fluoborate, anhydrous fluoroboric acid cobalt and anhydrous fluoroboric acid terbium, got il electrolyte; Two, adopt the method for pulse electrodeposition to put into il electrolyte through pretreated platinized platinum, be in temperature that 40 ℃, pulsewidth are 40%, frequency is that 4.0kHz, voltage are that distance between 8.0V, graphite and the platinized platinum is under the condition of 5cm, electroplating processes 10min gets test specimen; Three, adopt ethanol and distilled water flushing successively behind the taking-up test specimen, drying promptly gets the TbFeCo alloy firm; As anode, platinized platinum is as negative electrode with graphite in galvanic deposit in the step 2.
The method of the galvanic deposit in the present embodiment step 2 is to adopt DMC-30M type high frequency positive pulse electroplating power supply to realize.
The terbium content of the TbFeCo alloy firm that present embodiment obtains is 12% for terbium content, and cobalt contents is 38%, and iron level is 50%.
The TbFeCo alloy firm that present embodiment obtains has metalluster.
Adopt the TbFeCo alloy firm of present embodiment preparation, the scanning electron microscope analysis figure of TbFeCo alloy firm as shown in Figure 3.TbFeCo alloy firm surface presents the state of smooth smooth, uniform surface.
Embodiment 19: the method that present embodiment utilizes ionic liquid impulse electrodeposition technology to prepare the TbFeCo alloy firm realizes according to the following steps: one, in ar gas environment, by 4: 3: 2: 5 mol ratio mixed 1-methyl-3-butyl imidazole a tetrafluoro borate, anhydrous ferric fluoborate, anhydrous fluoroboric acid cobalt and anhydrous fluoroboric acid terbium, got il electrolyte; Two, adopt the method for pulse electrodeposition to put into il electrolyte through pretreated iron plate, be in temperature that 80 ℃, pulsewidth are 60%, frequency is that 3.5kHz, voltage are that distance between 7.0V, graphite and the iron plate sheet is under the condition of 5cm, electroplating processes 10min gets test specimen; Three, adopt ethanol and distilled water flushing successively behind the taking-up test specimen, drying promptly gets the TbFeCo alloy firm; As anode, iron plate is as negative electrode with graphite in galvanic deposit in the step 2.
The method of the galvanic deposit in the present embodiment step 2 is to adopt DMC-30M type high frequency positive pulse electroplating power supply to realize.
The terbium content of the TbFeCo alloy firm that present embodiment obtains is 8%, and cobalt contents is 38%, and iron level is 50%, and other are impurity.
The TbFeCo alloy firm that present embodiment obtains has metalluster.
Adopt the TbFeCo alloy firm of present embodiment preparation, the scanning electron microscope analysis figure of TbFeCo alloy firm as shown in Figure 4.TbFeCo alloy firm surface presents the state of smooth smooth, uniform surface.
Claims (10)
1, a kind of method of utilizing ionic liquid impulse electrodeposition technology to prepare the TbFeCo alloy firm, it is characterized in that the method for utilizing ionic liquid impulse electrodeposition technology to prepare the TbFeCo alloy firm realizes according to the following steps: one, in ar gas environment, by 1～7: 1～5: 1～4: 1～6 mol ratio mixes 1-methyl-3-butyl imidazole a tetrafluoro borate, anhydrous ferric fluoborate, anhydrous fluoroboric acid cobalt and anhydrous fluoroboric acid terbium, gets il electrolyte; Two, adopt the method for pulse electrodeposition to put into il electrolyte through pretreated matrix, be in temperature that 20～80 ℃, pulsewidth are 10%～99%, frequency is that 0.5～4.5kHz, voltage are that distance between 2.0～10.0V, anode and the matrix is under the condition of 2～8cm, electroplating processes 10min gets test specimen; Three, adopt ethanol and distilled water flushing successively behind the taking-up test specimen, drying promptly gets the TbFeCo alloy firm; 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 impulse electrodeposition technology to prepare the TbFeCo alloy firm according to claim 1 is characterized in that the mol ratio of 1-1 methyl isophthalic acid 3-butyl imidazole a tetrafluoro borate, anhydrous ferric fluoborate, anhydrous fluoroboric acid cobalt and anhydrous fluoroboric acid terbium in the step 1 is 2～6: 2～4: 2～3: 2～5.
3, a kind of method of utilizing ionic liquid impulse electrodeposition technology to prepare the TbFeCo alloy firm 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 impulse electrodeposition technology to prepare the TbFeCo alloy firm according to claim 3 is characterized in that pulsewidth is 30%～70% in the step 2.
5, according to claim 1,2 or 4 described a kind of methods of utilizing ionic liquid impulse electrodeposition technology to prepare the TbFeCo alloy firm, it is characterized in that the step 2 medium frequency is 1.5～3.5kHz.
6, a kind of method of utilizing ionic liquid impulse electrodeposition technology to prepare the TbFeCo alloy firm according to claim 5 is characterized in that voltage is 4.0～8.0V in the step 2.
7,, it is characterized in that the distance between the anode and matrix is 4～6cm in the step 2 according to claim 1,2,4 or 6 described a kind of methods of utilizing ionic liquid impulse electrodeposition technology to prepare the TbFeCo alloy firm.
8, a kind of method of utilizing ionic liquid impulse electrodeposition technology to prepare the TbFeCo alloy firm according to claim 7 is characterized in that matrix is copper sheet, gold plaque, platinized platinum, silver strip or iron plate in the step 2.
9, according to claim 1,2,4,6 or 8 described a kind of methods of utilizing ionic liquid impulse electrodeposition technology to prepare the TbFeCo alloy firm, it is characterized in that temperature is 40～60 ℃ in the step 2.
10, a kind of method of utilizing ionic liquid impulse electrodeposition technology to prepare the TbFeCo alloy firm according to claim 9 is characterized in that alcoholic acid purity is 99.9% in the step 3.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107460505A (en) * | 2017-08-23 | 2017-12-12 | 河北工业大学 | The preparation method of Tb Fe Co ternary RE alloy magnetic nanometer films |
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2009
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107460505A (en) * | 2017-08-23 | 2017-12-12 | 河北工业大学 | The preparation method of Tb Fe Co ternary RE alloy magnetic nanometer films |
| CN107460505B (en) * | 2017-08-23 | 2019-02-12 | 河北工业大学 | The preparation method of Tb-Fe-Co ternary RE alloy magnetic nanometer film |
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