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Process of electricity sedimentation in aqueous solution for producing rare earth magnetic film alloy material

An electrodeposition method and transition metal technology, applied in the field of rare earth permanent magnetic thin film alloy materials, can solve the problems that ultrafine powder cannot be in contact with air, cannot meet the production of permanent magnetic materials, and does not mention magnetic materials, etc. The effects of separation and film thickness control, easy composition and film thickness, and bright coating surface without cracks

Inactive Publication Date: 2005-08-31
湖南英才科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that the prepared ultrafine powder cannot be in contact with air, otherwise it is very easy to oxidize and spontaneously ignite, and the process is harsh.
However, Sm, Dy, and Gd, which are commonly used as rare earth permanent magnet materials, have not been reported.
And in the alloy of Nd and Fe, the percentage content of Nd is mostly 3.4% (mass percentage), and the maximum is no more than 7.5%, which cannot meet the requirements of producing permanent magnet materials
The patent document does not mention the production of magnetic materials

Method used

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  • Process of electricity sedimentation in aqueous solution for producing rare earth magnetic film alloy material
  • Process of electricity sedimentation in aqueous solution for producing rare earth magnetic film alloy material
  • Process of electricity sedimentation in aqueous solution for producing rare earth magnetic film alloy material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Embodiment 1: prepare Nd-Fe-B alloy

[0049] Plating solution: 0.08mol / L FeCl 2 +0.8mol / L Glycine+0.5mol / L NdCl 3 +0.8mol / LCaCl 2 +H 3 BO 3 0.5mol / L+additive II, wherein additive II is benzylamine 0.4g / L+H 3 BO 3 0.2g / L, pH=6.0, D=20mA / cm 2 , T=30℃

[0050] Coating composition: weight ratio Fe%=87.46, Nd=11.5%, B%=1.04

[0051] Coating test method: After dissolving the sample with 1:1 HCl, set it to 50ml, measure the content of Fe by atomic absorption method, measure the content of Nd and B respectively by spectrophotometry, heat-treat the obtained coating, and heat-treat the material The magnetic properties were measured with a vibrating sample magnetometer, and the results are shown in Figure 11 . It can be seen that the Bs of this material is 2×10 4 Gs. Br=Hc is 1600Oe, which is a permanent magnetic film material with excellent magnetic properties.

Embodiment 2

[0052] Embodiment 2: another group of electroplating solution components are, FeCl 2 (0.08mol / L)+Glycine(0.9mol / L)+CaCl 2 (0.8mol / L)+RE(0.5mol / L)+Additive I(0.2g / L)+Additive II+H 3 BO 3 (0.5mol / L); Wherein additive I is any one in polyethylene glycol 20000, dextran, gelatin, OP, EDTA, polyacrylamide, KI; Additive II is any in benzylamine, mannitol, ammoniacal liquor A (0.2g / L) and H 3 BO 3 (0.4g / L) mixed, or any one of dimethylaniline, benzylamine, methanol (0.4g / L) and NaBH 4 (0.2g / L) mixed.

Embodiment 3

[0053] Embodiment 3: technological process

[0054] ①Preparation of solution

[0055] Raw materials: rare earth oxide + hydrochloric acid or rare earth chloride, Fe powder + HCl or ferrous chloride, complexing agent, CaCl 2 , Additive I, H 3 BO 3 , Additive II.

[0056] The preparation process is as follows:

[0057] Solution A: After dissolving the rare earth oxide with hydrochloric acid, add some complexing agent.

[0058] Solution B: The transition metal chloride is dissolved and another part of the complexing agent is added.

[0059] Solution C: After mixing solution A and solution B, add CaCl 2 and H 3 BO 3 .

[0060] Adjust the pH value to 1-6.5

[0061] Solution D: Solution C + Additive I + Additive II.

[0062] Then adjust the pH to 1-6.5

[0063] ②Electrodeposition

[0064] Electrode: The anode uses an inert anode, a transition metal anode or a double anode, and the anode is an electrodeposited substrate material.

[0065] Plating treatment:

[0066] Br...

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Abstract

The electroplating solution of the invention comprises rare earth chloride, FeCl2, complexe agent, additive I, II, CaCl2. The process comprises, an inert anode or transition metal anode or two anodes; introducing pure argon or nitrogen to dispel oxygen, the whole electroplating process conducting in the protective environment of pure argon or nitrogen, the working current density is 20mA / cm2-200mA / cm2, the time is 15min-48hours, the temperature is 0-70degree C, taking out of the electroplated members, washing ,drying and sealing; placing the electroplated film in the protective environment of pure argon or nitrogen, heating at 700-800 degree C for 15min-20hours, sealing and storing. The electroplating solution is stable and has a wide range of working conditions. The rare earth alloy has more than 11% of rare earth.

Description

technical field [0001] The invention relates to a process for producing rare earth permanent magnetic film alloy materials by electrodeposition in aqueous solution. Background technique [0002] Alloys of rare earth metals and transition metals Fe, Co, and Ni are very good magnetic materials, and are widely used in aviation, aerospace, automobiles, electrical appliances, computers, communications, automatic control, and military affairs. The technologies currently used to prepare such materials are: 1. Melt rapid quenching method, that is, the master alloy is prepared by vacuum induction melting method, and the master alloy is melted in the quartz tube under the protection of inert gas in the vacuum rapid quenching equipment , under the action of argon pressure, the alloy solution is shot onto the high-speed rotating copper roller through the nozzle at the bottom of the quartz tube, and the 5 -10 6 The speed of ℃ / s is rapidly solidified into an amorphous, and then heat-tre...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25D3/56
Inventor 何凤娇
Owner 湖南英才科技有限公司
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