CN105648477A - Preparation method of template-free electro-deposition SmCo nanowires - Google Patents
Preparation method of template-free electro-deposition SmCo nanowires Download PDFInfo
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- CN105648477A CN105648477A CN201610006127.3A CN201610006127A CN105648477A CN 105648477 A CN105648477 A CN 105648477A CN 201610006127 A CN201610006127 A CN 201610006127A CN 105648477 A CN105648477 A CN 105648477A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C5/00—Electrolytic production, recovery or refining of metal powders or porous metal masses
- C25C5/02—Electrolytic production, recovery or refining of metal powders or porous metal masses from solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0547—Nanofibres or nanotubes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C7/00—Constructional parts, or assemblies thereof, of cells; Servicing or operating of cells
- C25C7/02—Electrodes; Connections thereof
Abstract
The invention relates to the field of ionic liquid electro-deposition technologies, in particular to a method of template-free electro-deposition SmCo nanowires. The method comprises the following steps: preparing new ionic liquid SmCl3-CoCl2-EMIC at first; and carrying out potentiostatic deposition on the new ionic liquid to obtain the SmCOnanowires with the diameters being about 50 nm. Through change of electrochemical parameters, the SmCo alloy nanowires with different lengths and alloying components can be prepared in a controllable manner, and meanwhile, a hysteresis curve shows that the nanowires have obvious magnetic anisotropy. By the method, template manufacturing and dissolving processes are omitted. The method has the advantages of low cost, low consumption, simple technology and the like.
Description
Technical field
The present invention relates to ionic liquid electrodeposition technology field, specifically, be the preparation method of a kind of nano wire of SmCo without template electric-sedimentation.
Background technology
SmCo alloy, as the first generation and second filial generation permanent magnet material, because of its higher Curie temperature, coercivity and magnetic energy product, has important using value, it is adaptable to microelectromechanical systems and high density magnetic recording material. The classical shortcoming that the rare earth permanent-magnetic material preparation method such as method such as powder metallurgy, magnetron sputtering has cost height, technological requirement is high. Compared to above method, electrochemical deposition can control pattern and composition, and equipment is simple, easy to operate, and production efficiency is high. But, owing to the standard electrode potential of Sm is more negative, electro-deposition is limited in aqueous, is merely able to be realized by fused salt electro-deposition. Generally, high-temperature molten salt electro-deposition needs the temperature of more than 300 DEG C, experiment condition is required harshness, meanwhile, hardly results in nano level deposit under hot conditions. The diameter of nano material, at 1nm-100nm, has small-size effect and skin effect. Nano-scale magnetic material becomes single domain due to smaller from multidomain, thus has high-coercive force, big signal to noise ratio and ferromagnetism, thus obtains more concern, and Low-temperature electro-deposition nano material receives more and more attention. Low-temperature molten salt (ionic liquid) has broader electrochemical window, good electric conductivity, low vapour pressure and stable chemical property can be applied to electrodeposit metals and research, it is possible to achieve the electro-deposition of active metal. Use ionic liquid electrodeposition metal in recent years, the report of alloy also gets more and more.
V.Neu etc. adopt the method for pulsed laser deposition to produce SmCo thin film and NbFeB thin film, have studied the rare earth element impact on structure and magnetic, but this method also exists cost height, efficiency is low, form the shortcomings such as wayward. Electrodeposition process is less costly, fine can must control deposit composition by controlling cathode potential and electric current density. J.P.Zhang etc. have deposited nano level SmCo particle film in water solution system, and have studied its magnetic property, but aqueous solution electro-deposition has side reaction and occurs, the problems such as current efficiency is low, and product is impure. The electro-deposition in low-temperature molten salt such as Li Jiaxin gone out SmCo alloy firm, it is to avoid the generation of side reaction, and analyzes the crystalline phase before and after sample annealing and magnetic property change. Compared with general thin magnetic film, regularly arranged nano wire has bigger magnetic recording area, has the magnetic anisotropy of excellence, it is adaptable to high density magnetic recording material, this has been carried out substantial amounts of research by people.P.-X.Yang etc. utilize alumina formwork method, and from Co-EMIC-glycol system, electro-deposition has gone out Co nano wire, but, this method needs to produce on pretreatment template, dissolves template after experiment. Comparatively speaking, template-free method electro-deposition is simple, saves time. Y.-T.Hsieh etc. utilize this ionic liquid of EMIC, and direct electro-deposition has gone out the nano wire such as Al, CuSn, FeCoZn and Co. So far also do not have the report of the direct electro-deposition SmCo nano wire of template-free method, therefore, seek a kind of can the method for direct electro-deposition SmCo alloy, solve SmCo nano wire electro-deposition difficulty and problem that template wastes time and energy be imperative.
Summary of the invention
A kind of method that it is an object of the invention to provide nano wire of SmCo without template electric-sedimentation, efficiently solves the problem that template wastes time and energy, is greatly simplified experiment flow. SmCo nano wire is as magnetic material, and big draw ratio can effectively improve magnetic recording area.
The method of a kind of nano wire of SmCo without template electric-sedimentation of the present invention can be realized by following concrete mode:
One, electrode pre-treatment, utilizes three-electrode system to be deposited experiment, with electrode of working, cobalt sheet or graphite such as tungsten, molybdenum, ferrum, noble metal platinum and gold as to electrode, Co2+/ Co electrode is reference electrode, and it consists of cobalt silk and is immersed in 40:60mol%CoCl2In the porous glass tube of-EMIC ionic liquid. Before using, all electrodes need with by thin sand papering to minute surface, and graphite, cobalt sheet and the cobalt ultrasonic 20min of silk acetone wash away Organic substance, more standby with deionized water cleaning, drying. Working electrode first to use 2M nitric acid (HNO3) the ultrasonic 20min of solution washes away oxide, then wash away Organic substance with the ultrasonic 20min of acetone, finally cleans post-drying with deionized water standby. Glove box is put into after all electrode assemblings are become electrolyzer;
Two, preparation electrolyte, weighs SmCl according to certain mol proportion in glove box3��CoCl2And EMIC, after mix homogeneously, with the heating rate of 0.5 DEG C/min, at 120 DEG C, it is incubated 2h removes moisture, blue-colored ionic liquid SmCl after stirring, can be obtained3-CoCl2-EMIC;
Three, electro-chemical test, arranges parameter and different ionic liquids is circulated volt-ampere test, and to determine the sedimentation potential of Co and Sm, sweep limits is 0.6V��-1.3V, scanning speed 50mVs-1, as in figure 2 it is shown, Fig. 2 occurs in that three reduction peak B, C, D. Similar with peak A at the peak B that current potential is-0.5V, represent the reduction of Co. Peak C and peak D occurs in-0.85V, represents SmCo codeposition;
Four, SmCo alloy electrodeposition, when electro-deposition, sedimentation potential is set in-0.4V��-1.0V by us, and sedimentation time is set to 100s��5000s, and temperature range is 70��150 DEG C. After deposition terminates, by working electrode, first clean three times in acetonitrile, deionizing liquid, then wash away acetonitrile with acetone, be then placed in glove box and dry.
Five, SmCo nanowire magnetic can be tested, the B-H loop of test nano wire, has obvious magnetic anisotropy.
A first aspect of the present invention, it is provided that a kind of method of nano wire of SmCo without template electric-sedimentation, specifically comprises the following steps that
A, employing three-electrode system, with electrode of working, cobalt sheet or graphite such as tungsten, molybdenum, ferrum, noble metal platinum or gold as to electrode, Co2+/ Co electrode is reference electrode, and it consists of cobalt silk and is immersed in 40:60mol%CoCl2In the porous glass tube of-EMIC ionic liquid; Working electrode is before the use, it is necessary to sand paperings at different levels to minute surface, adopts 2M salpeter solution ultrasonic cleaning to remove oxide-film, adopts deionized water cleaning electrode post-drying afterwards;All electrodes ultrasonic cleaning organics removal in acetone;
B, ionic liquid preparation: in the glove box in argon gas atmosphere, to 1-ethyl-3-methylimidazolium chloride (EMIC) adds SmCl3And CoCl2, heated and stirred, the blue new ionic liquid SmCl being uniformly mixed3-CoCl2-EMIC, SmCl3Molar percentage be 1.00-6.00%, CoCl2The molar percentage that molar percentage is 30.00-60.00%, EMIC be 34.00-69.00%; Preferably weigh SmCl according to the mol ratio of 1.67:60:603��CoCl2And EMIC, it is mixed with ionic liquid;
C, SmCl in stepb3-CoCl2-EMIC ionic liquid carries out potentiostatic electrodeposition, sedimentation potential-0.4V��-1.0V (preferably-0.68V, to ensure suitable depletion rate), time 100s��5000s (preferred 1200s, as time went on, nanowire length increases, can according to Len req adjustment), temperature range is 70��150 DEG C (preferably 120 DEG C);
After D, electro-deposition terminate, the working electrode in step C is first cleaned three times with acetonitrile, wash ionic liquid off, then clean removal acetonitrile solution with acetone, dry and obtain solid product;
E, dry: baking step D to wash the solid product obtained, is SmCo nano wire.
F, magnetism testing, carry out B-H loop test to nano wire, has obvious magnetic anisotropy.
The described SmCo nano wire prepared is black, and diameter is at 50��100nm, and length is at 5 ��m��30 ��m. The leaf that working electrode (WE) is stable in properties, is the cobalt sheet that will not introduce other foreign ions to electrode (CE).
Step B prepares SmCl3-CoCl2During-EMIC ionic liquid, weigh under room temperature, mix homogeneously, progressively heat up, at 120 DEG C, be incubated 2h remove moisture.
Purity of electrode described in step A is 99.0%.
In reference electrode described in step A, ionic liquid is close with extraneous ionic liquid composition, it is possible to the reference electrode current potential remained stable for.
In glove box described in step B, O2< 1ppm, H2O < 1ppm.
A second aspect of the present invention, it is provided that a kind of SmCo nano wire adopting any of the above-described method to prepare, described SmCo nano wire is black, and diameter is at 50��100nm, and length is at 5 ��m��30 ��m.
The invention has the advantages that:
1, ionic liquid electrodeposition purity is high, it does not have side reaction occurs.
Ionic liquid electrochemical window is big, and electrical conductivity is high, and vapour pressure almost can be ignored, and Heat stability is good during electro-deposition, and electrodeposition process is simple, does not contain other impurity in obtained alloy, and current efficiency is high.
2, simple to operate saving time, work efficiency is high.
This method does not use template, and direct potentiostatic electrodeposition obtains nano wire, saves and makes template and dissolve the process of template, simple and convenient, drastically increases work efficiency.
3, the pattern of alloy and composition are controlled.
When ionic liquid carries out electro-deposition, the composition of product and the pattern of alloy can be controlled by regulating the technological parameters such as the composition of electrolyte, sedimentation potential, sedimentation time and temperature.
4, SmCo nano wire is thinner.
The SmCo nano wire that direct electro-deposition goes out can be reduced to 50nm, and diameter is less, it is possible to reaches the level of template, and the nano wire obtained has obvious magnetic anisotropy.
Accompanying drawing explanation
Fig. 1 is the technology path of ionic liquid electrodeposition nano wire;
Fig. 2 is the electrochemistry cyclic voltammetry curve of ionic liquid electrodeposition nano wire;
Fig. 3 is that in ionic liquid, under different condition, electro-deposition goes out the SEM figure of the SmCo nano wire obtained;
Fig. 4 is the B-H loop of SmCo nano wire.
Detailed description of the invention
Below in conjunction with embodiment, detailed description of the invention provided by the invention is elaborated.
Embodiment 1:
One, electrode pre-treatment, working electrode (WE) is leaf, is cobalt sheet to electrode (CE), and reference electrode (RE) is Co2+/ Co electrode, it consists of cobalt silk and is immersed in 40:60mol%CoCl2In the porous glass tube of-EMIC ionic liquid. Before using, all electrode sand paperings are to minute surface, and cobalt sheet and the cobalt ultrasonic 20min of silk acetone wash away Organic substance, more standby with deionized water cleaning, drying. Working electrode leaf first to use 2MHNO3Ultrasonic 20min washes away oxide, then washes away Organic substance with the ultrasonic 20min of acetone, finally cleans post-drying with deionized water standby;
Two, preparation electrolyte, in glove box, the mol ratio according to 1.67:40:60 weighs SmCl3��CoCl2And EMIC, after mix homogeneously, with the heating rate of 0.5 DEG C/min, at 120 DEG C, it is incubated 2h removes moisture, blue-colored ionic liquid SmCl after stirring, can be obtained3-CoCl2-EMIC;
Three, SmCo alloy electrodeposition, when electro-deposition, is set in-0.68V by sedimentation potential, and sedimentation time is set to 1200s, and temperature range is 120 DEG C. After deposition terminates, close electrochemical workstation, take out working electrode, first clean three times in acetonitrile, deionizing liquid, then wash away acetonitrile with acetone, be then placed in glove box and dry, the nano wire pattern such as Fig. 3 a obtained.
Four, nano wire being carried out magnetism testing, B-H loop as shown in Figure 4, has obvious magnetic anisotropy, and direction of easy axis is parallel to nano wire long axis direction.
Embodiment 2:
One, electrode pre-treatment, working electrode (WE) is leaf, is cobalt sheet to electrode (CE), and reference electrode (RE) is Co2+/ Co electrode, it consists of cobalt silk and is immersed in 40:60mol%CoCl2In the porous glass tube of-EMIC ionic liquid. Before using, all electrode sand paperings are to minute surface, and cobalt sheet and the cobalt ultrasonic 20min of silk acetone wash away Organic substance, more standby with deionized water cleaning, drying. Working electrode leaf first to use 2MHNO3Ultrasonic 20min washes away oxide, then washes away Organic substance with the ultrasonic 20min of acetone, finally cleans post-drying with deionized water standby;
Two, preparation electrolyte, in glove box, the mol ratio according to 1.67:40:60 weighs SmCl3��CoCl2And EMIC, after mix homogeneously, with the heating rate of 0.5 DEG C/min, at 120 DEG C, it is incubated 2h removes moisture, blue-colored ionic liquid SmCl after stirring, can be obtained3-CoCl2-EMIC;
Three, SmCo alloy electrodeposition, when electro-deposition, is set in-0.68V by sedimentation potential, and sedimentation time is set to 1200s, and temperature range is 100 DEG C. After deposition terminates, close electrochemical workstation, take out working electrode, first clean three times in acetonitrile, deionizing liquid, then wash away acetonitrile with acetone, be then placed in glove box and dry, the nano wire pattern such as Fig. 3 b obtained.
Embodiment 3:
One, electrode pre-treatment, working electrode (WE) is leaf, is cobalt sheet to electrode (CE), and reference electrode (RE) is Co2+/ Co electrode, it consists of cobalt silk and is immersed in 40:60mol%CoCl2In the porous glass tube of-EMIC ionic liquid. Before using, all electrode sand paperings are to minute surface, and cobalt sheet and the cobalt ultrasonic 20min of silk acetone wash away Organic substance, more standby with deionized water cleaning, drying.Working electrode leaf first to use 2MHNO3Ultrasonic 20min washes away oxide, then washes away Organic substance with the ultrasonic 20min of acetone, finally cleans post-drying with deionized water standby;
Two, preparation electrolyte, in glove box, the mol ratio according to 1.67:40:60 weighs SmCl3��CoCl2And EMIC, after mix homogeneously, with the heating rate of 0.5 DEG C/min, at 120 DEG C, it is incubated 2h removes moisture, blue-colored ionic liquid SmCl after stirring, can be obtained3-CoCl2-EMIC;
Three, SmCo alloy electrodeposition, when electro-deposition, is set in-0.75V by sedimentation potential, and sedimentation time is set to 1200s, and temperature range is 120 DEG C. After deposition terminates, close electrochemical workstation, take out working electrode, first clean three times in acetonitrile, deionizing liquid, then wash away acetonitrile with acetone, be then placed in glove box and dry, the nano wire pattern such as Fig. 3 c obtained.
Below the preferred embodiment of the invention has been illustrated, but the invention is not limited to described embodiment, those of ordinary skill in the art it may also be made that under the premise without prejudice to the invention spirit all equivalent modification or replacement, these equivalent modification or replacement are all contained in the application claim limited range.
Claims (8)
1. the method without template electric-sedimentation SmCo nano wire, it is characterised in that specifically comprise the following steps that
A, employing three-electrode system, work electrode, cobalt sheet or graphite as to electrode, Co with tungsten, molybdenum, ferrum, noble metal platinum or gold2+/ Co electrode is reference electrode, and it consists of cobalt silk and is immersed in 40:60mol%CoCl2In the porous glass tube of-EMIC ionic liquid; Working electrode is before the use, it is necessary to sand paperings at different levels to minute surface, adopts 2M salpeter solution ultrasonic cleaning to remove oxide-film, adopts deionized water cleaning electrode post-drying afterwards; All electrodes ultrasonic cleaning organics removal in acetone;
B, ionic liquid preparation: in the glove box in argon gas atmosphere, to 1-ethyl-3-methylimidazolium chloride, namely in EMIC add SmCl3And CoCl2, heated and stirred, the blue new ionic liquid SmCl being uniformly mixed3-CoCl2-EMIC, SmCl3Molar percentage be 1.00-6.00%, CoCl2The molar percentage that molar percentage is 30.00-60.00%, EMIC be 34.00-69.00%;
C, SmCl in stepb3-CoCl2Carrying out potentiostatic electrodeposition, sedimentation potential-0.4V��-1.0V, time 100s��5000s in-EMIC ionic liquid, temperature range is 70��150 DEG C;
After D, electro-deposition terminate, the working electrode in step C is first cleaned three times with acetonitrile, wash ionic liquid off, then clean removal acetonitrile solution with acetone, dry and obtain solid product;
E, dry: baking step D to wash the solid product obtained, is SmCo nano wire;
F, magnetism testing, carry out B-H loop test to nano wire, has obvious magnetic anisotropy.
2. the method for the nano wire of SmCo without template electric-sedimentation according to claim 1, it is characterised in that described SmCo nano wire is black, diameter is at 50��100nm, and length is at 5 ��m��30 ��m.
3. the method for the nano wire of SmCo without template electric-sedimentation according to claim 1, it is characterised in that in described step A, working electrode is leaf, is cobalt sheet to electrode.
4. the method for the nano wire of SmCo without template electric-sedimentation according to claim 1, it is characterised in that prepare SmCl in step B3-CoCl2During-EMIC ionic liquid, weigh under room temperature, mix homogeneously, progressively heat up, at 120 DEG C, be incubated 2h remove moisture.
5. the method for the nano wire of SmCo without template electric-sedimentation according to claim 1, it is characterised in that the purity of electrode described in step A is 99.0%.
6. the method for the nano wire of SmCo without template electric-sedimentation according to claim 1, it is characterised in that in the reference electrode described in step A, ionic liquid is close with extraneous ionic liquid composition, it is possible to the reference electrode current potential remained stable for.
7. the method for the nano wire of SmCo without template electric-sedimentation according to claim 1, it is characterised in that in the glove box described in step B, O2< 1ppm, H2O < 1ppm.
8. adopting the SmCo nano wire that the arbitrary described method of claim 1-7 prepares, described SmCo nano wire is black, and diameter is at 50��100nm, and length is at 5 ��m��30 ��m.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107884693A (en) * | 2017-11-06 | 2018-04-06 | 武汉华星光电半导体显示技术有限公司 | Electrical characteristics test method |
| US9938628B2 (en) * | 2015-05-19 | 2018-04-10 | General Electric Company | Composite nanoparticles containing rare earth metal and methods of preparation thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104087976A (en) * | 2014-07-02 | 2014-10-08 | 河北工业大学 | Preparation method of Sm-Co alloy amorphous magnetic nanowire array |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104087976A (en) * | 2014-07-02 | 2014-10-08 | 河北工业大学 | Preparation method of Sm-Co alloy amorphous magnetic nanowire array |
Non-Patent Citations (1)
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| YUQI CHEN: "Electrodeposition of SmCo alloy nanowires with a large length-diameter ratio from SmCl3–CoCl2–1-ethyl-3-methylimidazolium chloride ionic liquid without template", 《RSC ADVANCES》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9938628B2 (en) * | 2015-05-19 | 2018-04-10 | General Electric Company | Composite nanoparticles containing rare earth metal and methods of preparation thereof |
| CN107884693A (en) * | 2017-11-06 | 2018-04-06 | 武汉华星光电半导体显示技术有限公司 | Electrical characteristics test method |
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