CN101560671A - Method for preparing high entropy nanometer magnetic material containing magnesium, neodymium, cobalt, nickel and manganese - Google Patents

Method for preparing high entropy nanometer magnetic material containing magnesium, neodymium, cobalt, nickel and manganese Download PDF

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Publication number
CN101560671A
CN101560671A CNA2009100392257A CN200910039225A CN101560671A CN 101560671 A CN101560671 A CN 101560671A CN A2009100392257 A CNA2009100392257 A CN A2009100392257A CN 200910039225 A CN200910039225 A CN 200910039225A CN 101560671 A CN101560671 A CN 101560671A
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ion
neodymium
cobalt
nickel
manganese
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童叶翔
张鹏
刘萌
叶剑清
李高仁
刘鹏
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Sun Yat Sen University
National Sun Yat Sen University
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National Sun Yat Sen University
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Abstract

The invention discloses a method for preparing a high entropy nanometer magnetic material containing magnesium, neodymium, cobalt, nickel and manganese. The method adopts a cathodic electrodeposition process, and comprises the following steps: firstly, preparing organic system solution containing magnesium ions, neodymium ions, cobalt ions, nickel ions and manganese ions; secondly, adding supporting electrolyte into the organic system solution; using copper matrix or titanium matrix as a working electrode; adding an external electric field into the mixture to obtain the high entropy nanometer magnetic material containing magnesium, neodymium, cobalt, nickel and manganese. The preparation method has mild condition, can be carried out at normal temperature, and has simple production process, cheap and economic raw materials and high utilization rate. The preparation method belongs to non-linear process and can obtain even coating by depositing on matrix with complicated shape; the obtained magnetic materials have the advantages of soft magnetism and permanent magnetism and the invention has high utilization value and wide market prospect.

Description

A kind of preparation method who contains the high entropy nanometer magnetic material of magnesium, neodymium, cobalt, nickel and manganese
Technical field
The present invention relates to contain many pivots of magnesium lightweight high-entropy alloy material field, be specifically related to a kind of preparation method who contains the magnesium, neodymium, cobalt, nickel and manganese high entropy nanometer magnetic material.
Background technology
Magneticsubstance is used and is related to every field.The exploitation of novel magnetic material has important pushing effect to the development of new high-tech material industry.
After Nd-Fe-B the 4th generation permanent magnet material be the key subjects in present scientific research field.Obtain low-symmetry, high magnetocrystalline anisotropy, the permanent magnet material of high energy product is the basic characteristics and the requirement of this research.Simultaneously because the high saturation and magnetic intensity of soft magnetic materials, soft magnetism and permanent magnetism are carried out the permanent magnet material that Compound Machining and then acquisition have the two advantage concurrently at nanoscale has important meaning for the performance requriements that solves type material, has caused scientist and entrepreneur's interest at present.
The alloy of being made up of rare earth element and magnesium-yttrium-transition metal has good magnetic performance.In order to improve the alloy material magnetic performance, can metal alloy or particulate be uniformly dispersed by nano-crystallization, thereby obtain high performance magneticsubstance to reach practical purpose.
Many pivots high-entropy alloy is a kind of new nano material design concept, contains 5 kinds and above element in many pivots high-entropy alloy.High entropy is the characteristic of many pivots alloy, because high entropy effect suppresses the appearance of intermetallic compound, helps to form simple crystallization phases, and makes microstructure tend to nanometer, obtains nano structural material easily.
The preparation method of high-entropy alloy mainly adopts the electric arc melting method at present.The problem that has apparatus expensive and complicated operation causes the material cost height, has hindered application.
Summary of the invention
The objective of the invention is to overcome the deficiency that prior art exists, a kind of preparation method who contains the magnesium, neodymium, cobalt, nickel and manganese high entropy nanometer magnetic material is provided, utilize this method can under the condition of gentleness, prepare the high entropy material of nanostructure.
To achieve these goals, the present invention adopts following technical scheme:
The preparation method who contains the high entropy nanometer magnetic material of magnesium, neodymium, cobalt, nickel and manganese of the present invention adopts the cathode electrodeposition method.
Cathode electrodeposition is to utilize the extra electric field effect, at negative electrode generation chemical reaction, makes metal ion in negative electrode generation reduction reaction, and then deposits on matrix.Concrete steps are as follows:
(1) configuration contains the organic system solution of magnesium ion, neodymium ion, cobalt ion, nickel ion, mn ion;
(2) add supporting electrolyte, as working electrode, extra electric field carries out galvanic deposit promptly with copper matrix/titanium matrix.
In the above-mentioned steps (1), the volumetric molar concentration of magnesium ion or neodymium ion preferably is controlled between the 0.01mol/L to 0.1mol/L; Except that magnesium ion and neodymium ion, the volumetric molar concentration of other any metal ions is controlled between the 0.002mol/L to 0.05mol/L; Except that magnesium ion, other metal ions are neodymium ion (rare earth ion), cobalt ion, nickel ion and mn ion.
In the above-mentioned steps (2), the supporting electrolyte of adding is preferably indifferent electrolyte.
In the above-mentioned steps (2), extra electric field is to be reference electrode with the Ag/AgCl electrode, cathode potential between-2.2V between-the 2.7V.
In cathode electrodeposition, the reaction that negative electrode takes place is M N++ ne=M, deposition process relates to the diffusion and the reallocation of multielement, and the nucleation and the growth of precipitate are suppressed, and make microstructure tend to nanometer and noncrystallineization, help the formation of nanophase.
Compared with prior art, the present invention has following beneficial effect: can (1) temperature of the present invention take place not play a decisive role for this reaction, because many pivots characteristic of high-entropy alloy, therefore the factor that influences the alloy appearance structure is more, and control at room temperature changes other mode of deposition such as concentration, sedimentation potential, ionogen etc. and is prepared.Therefore preparation method of the present invention can carry out at normal temperatures, and production process is simple, and the required investment of plant and instrument is lower; (2) preparation method of the present invention belongs to non-linear process, can deposit on complex-shaped matrix and obtain uniform coating; (3) the used cheap economy of raw material of the present invention, the utilization ratio height.
Description of drawings
Fig. 1 is the Electronic Speculum result of 1 time prepared high-entropy alloy of embodiment;
Fig. 2 is the power spectrum result of 1 time prepared high-entropy alloy of embodiment.
Embodiment
Embodiment 1
Configuration contains the dimethyl sulfoxide (DMSO) organic system solution of 0.01mol/L magnesium ion, 0.01mol/L neodymium ion, 0.01mol/L cobalt ion, 0.01mol/L nickel ion, 0.01mol/L mn ion, the lithium perchlorate that adds 0.3mol/L, with the copper matrix as working electrode,-2.7V current potential deposit 5 minutes, can obtain containing the high entropy nanometer soft magnetic materials of magnesium, neodymium, cobalt, nickel and manganese.As shown in Figure 1, Fig. 1 is the Electronic Speculum figure as a result of high-entropy alloy.The power spectrum result of high-entropy alloy is shown in Fig. 2 and table 1.
The content of each element of table 1 (weight ratio and atom number ratio)
Figure A20091003922500061
Embodiment 2
Configuration contains the dimethyl sulfoxide (DMSO) organic system solution of 0.01mol/L magnesium ion, 0.01mol/L neodymium ion, 0.01mol/L cobalt ion, 0.01mol/L nickel ion, 0.01mol/L mn ion, the lithium perchlorate that adds 0.3mol/L, with the copper matrix as working electrode,-2.2V current potential deposit 5 minutes, can obtain containing the high entropy nanometer soft magnetic materials of magnesium, neodymium, cobalt, nickel and manganese.
Embodiment 3
Configuration contains the dimethyl sulfoxide (DMSO) organic system solution of 0.01mol/L magnesium ion, 0.01mol/L neodymium ion, 0.01mol/L cobalt ion, 0.01mol/L nickel ion, 0.01mol/L mn ion, the lithium perchlorate that adds 0.3mol/L, with the titanium matrix as working electrode,-2.7V current potential deposit 5 minutes, can obtain containing the high entropy nanometer soft magnetic materials of magnesium, neodymium, cobalt, nickel and manganese.
Embodiment 4
Configuration contains the dimethyl sulfoxide (DMSO) organic system solution of 0.01mol/L magnesium ion, 0.01mol/L neodymium ion, 0.05mol/L cobalt ion, 0.05mol/L nickel ion, 0.05mol/L mn ion, the lithium perchlorate that adds 0.3mol/L, with copper sheet as working electrode,-2.7V current potential deposit 5 minutes, can obtain containing the high-entropy alloy soft magnetic materials of magnesium, neodymium, cobalt, nickel and manganese.
Embodiment 5
Configuration contains the dimethyl sulfoxide (DMSO) organic system solution of 0.01mol/L magnesium ion, 0.01mol/L neodymium ion, 0.002mol/L cobalt ion, 0.002mol/L nickel ion, 0.002mol/L mn ion, the lithium perchlorate that adds 0.3mol/L, with copper sheet as working electrode,-2.7V current potential deposit 5 minutes, can obtain containing the high-entropy alloy soft magnetic materials of magnesium, neodymium, cobalt, nickel and manganese.
Embodiment 6
Configuration contains the dimethyl sulfoxide (DMSO) organic system solution of 0.1mol/L magnesium ion, 0.1mol/L neodymium ion, 0.01mol/L cobalt ion, 0.01mol/L nickel ion, 0.01mol/L mn ion, the lithium perchlorate that adds 0.3mol/L, with copper sheet as working electrode,-2.7V current potential deposit 5 minutes, can obtain containing the high-entropy alloy soft magnetic materials of magnesium, neodymium, cobalt, nickel and manganese.
Embodiment 7
Configuration contains the dimethyl sulfoxide (DMSO) organic system solution of 0.1mol/L magnesium ion, 0.1mol/L neodymium ion, 0.05mol/L cobalt ion, 0.05mol/L nickel ion, 0.05mol/L mn ion, the lithium perchlorate that adds 0.3mol/L, with copper sheet as working electrode,-2.7V current potential deposit 5 minutes, can obtain containing the high-entropy alloy soft magnetic materials of magnesium, neodymium, cobalt, nickel and manganese.
Embodiment 8
Configuration contains the dimethyl sulfoxide (DMSO) organic system solution of 0.1mol/L magnesium ion, 0.03mol/L neodymium ion, 0.05mol/L cobalt ion, 0.05mol/L nickel ion, 0.05mol/L mn ion, the lithium perchlorate that adds 0.3mol/L, with copper sheet as working electrode,-2.7V current potential deposit 5 minutes, can obtain containing the high-entropy alloy soft magnetic materials of magnesium, neodymium, cobalt, nickel and manganese.
Embodiment 9
Configuration contains the dimethyl formamide organic system solution of 0.01mol/L magnesium ion, 0.01mol/L neodymium ion, 0.01mol/L cobalt ion, 0.01mol/L nickel ion, 0.01mol/L mn ion, the lithium perchlorate that adds 0.3mol/L, with copper sheet as working electrode,-2.7V current potential deposit 5 minutes, can obtain containing the high-entropy alloy soft magnetic materials of magnesium, neodymium, cobalt, nickel and manganese.
Embodiment 10
Configuration contains the dimethyl formamide organic system solution of 0.01mol/L magnesium ion, 0.01mol/L neodymium ion, 0.01mol/L cobalt ion, 0.01mol/L nickel ion, 0.01mol/L mn ion, the tetraethyl-ammonium hexafluorophosphate that adds 0.3mol/L, with the copper matrix as working electrode,-2.7V current potential deposit 5 minutes, can obtain containing the high entropy nanometer soft magnetic materials of magnesium, neodymium, cobalt, nickel and manganese.
Embodiment 11
Configuration contains the dimethyl formamide organic system solution of 0.01mol/L magnesium ion, 0.01mol/L neodymium ion, 0.01mol/L cobalt ion, 0.01mol/L nickel ion, 0.01mol/L mn ion, the tetraethyl-ammonium hexafluorophosphate that adds 0.3mol/L, with the titanium matrix as working electrode,-2.7V current potential deposit 5 minutes, can obtain containing the high entropy nanometer soft magnetic materials of magnesium, neodymium, cobalt, nickel and manganese.

Claims (5)

1, a kind of preparation method who contains the high entropy nanometer magnetic material of magnesium, neodymium, cobalt, nickel and manganese is characterized in that comprising following steps:
(1) preparation contains the organic system solution of magnesium ion, neodymium ion, cobalt ion, nickel ion and mn ion;
(2) add supporting electrolyte, as working electrode, extra electric field carries out galvanic deposit promptly with copper matrix or titanium matrix.
2, preparation method according to claim 1 is characterized in that the volumetric molar concentration of described magnesium ion or neodymium ion is controlled between the 0.01mol/L to 0.1mol/L in the step (1).
3, preparation method according to claim 1 and 2 is characterized in that in the step (1), except that magnesium ion and neodymium ion, the volumetric molar concentration of other any metal ions is controlled between the 0.002mol/L to 0.05mol/L.
4, preparation method according to claim 1 is characterized in that in the step (2), described supporting electrolyte is an indifferent electrolyte.
5, preparation method according to claim 1 is characterized in that in the step (2), and described extra electric field is to be reference electrode with the Ag/AgCl electrode, the current potential of galvanic deposit between-2.2V between-the 2.7V.
CNA2009100392257A 2009-05-05 2009-05-05 Method for preparing high entropy nanometer magnetic material containing magnesium, neodymium, cobalt, nickel and manganese Pending CN101560671A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107675059A (en) * 2016-07-28 2018-02-09 龙岩紫荆创新研究院 Application of the magnetic high-entropy alloy film and preparation method thereof with high-entropy alloy film
CN108133799A (en) * 2017-12-20 2018-06-08 江西理工大学 A kind of high performance nano-crystal thermal deformation Nd-Fe-B permanent magnet and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107675059A (en) * 2016-07-28 2018-02-09 龙岩紫荆创新研究院 Application of the magnetic high-entropy alloy film and preparation method thereof with high-entropy alloy film
CN107675059B (en) * 2016-07-28 2019-06-21 龙岩紫荆创新研究院 Application of the magnetic high-entropy alloy film and preparation method thereof with high-entropy alloy film
CN108133799A (en) * 2017-12-20 2018-06-08 江西理工大学 A kind of high performance nano-crystal thermal deformation Nd-Fe-B permanent magnet and preparation method thereof

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