CN102400144B - A kind of surface treatment method of mechanical plating zinc-nickel of Nd-Fe-Bo permanent magnet material - Google Patents
A kind of surface treatment method of mechanical plating zinc-nickel of Nd-Fe-Bo permanent magnet material Download PDFInfo
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Abstract
The invention provides a kind of surface treatment method of mechanical plating zinc-nickel of Nd-Fe-Bo permanent magnet material, described method comprises the steps: that (1) chamfering is polished; (2) degreasing degreasing; (3) acid pickling and rust removing; (4) flash copper and (5) mechanical plating zinc-nickel: adopt zinc-plated nickel liquid to carry out zinc-plated nickel dam to Nd-Fe-Bo permanent magnet material, described zinc-plated nickel liquid comprises basal liquid, dispersion agent, impact media and metal-powder.The mechanical plating zinc-nickel method of the application of the invention can make Nd-Fe-Bo permanent magnet material obtain excellent corrosion resistance nature, and greatly reduces the high temperature demagnetizing factor of Nd-Fe-Bo permanent magnet material.
Description
Technical field
The present invention relates to a kind of surface treatment method of Nd-Fe-Bo permanent magnet material, particularly a kind of surface treatment method of mechanical plating zinc-nickel of Nd-Fe-Bo permanent magnet material.
Background technology
The application and development of neodymium iron boron (NdFeB) permanent magnet material is very rapid in recent years, and the protection of Nd-Fe-Bo permanent magnet material is related to one of gordian technique that can Nd-Fe-Bo permanent magnet material apply.Nd-Fe-Bo permanent magnet material is mainly prepared from by powder metallurgical technique by elements such as rare earth metal neodymium (Nd), iron and boron.As magneticsubstance the strongest at present, Nd-Fe-Bo permanent magnet material has been widely used in the fields such as electroplating device, machinery, medical treatment, automobile, and application prospect is very wide.
The prerequisite of Nd-Fe-Bo permanent magnet material application first to resolve the Anticorrosion of Nd-Fe-Bo permanent magnet material.As a kind of porous material be prepared from by powder metallurgical technique, the rich neodymium phase in Nd-Fe-Bo permanent magnet material, neodymium iron boron principal phase and border are easy to form intergranular corrosion mutually.Because the character of the rear earth element nd in neodymium iron boron powder metallurgy is active, thus the corrosion resisting property of whole Nd-Fe-B alloys is made to become very poor, particularly very easily corrosion in damp and hot environment, and cause decline or the damage of magnetic property because of corrosion failure, have a strong impact on the work-ing life of Nd-Fe-Bo permanent magnet material, reduce stability and the reliability of product.The magnetic property of Nd-Fe-Bo permanent magnet material and its weave construction have very large relation.The principal phase of Nd-Fe-Bo permanent magnet material is the main source of its magnetic property, and maximum to coercive force contribution be rich neodymium phase.After Nd-Fe-Bo permanent magnet material corrodes, will there is huge change in its magnetic property.Therefore, the Anticorrosion of Nd-Fe-Bo permanent magnet material is the subject matter that Nd-Fe-Bo permanent magnet material needs to solve always.
At present, the anti-corrosion method of Nd-Fe-Bo permanent magnet material has a variety of, such as electronickelling, electro-galvanizing (CN1421547A, CN1056133A), shooting of multi-layer nickel electroplating, copper facing (CN1514889A), phosphatization, electrocoating paint etc.Electro-galvanizing is under the effect of direct supply, and metallic zinc ion is reduced into metallic zinc on negative electrode, and mechanical zinc-plating does not then need direct supply, utilizes the effect of mechanical energy and chemical promoter, on metal parts deposition zinc.Concrete grammar is: in the cylinder rotated, put into plated part, granulated glass sphere, water, chemical promoter and zinc powder, after cylinder reaches certain rotating speed, piece surface just generates the good continuous zinc layers of bonding force.Visible mechanical zinc-plating is caused by the effect of physics and chemistry two aspect.
Application number be 02110408.5 Chinese invention patent application disclose a kind of mechanical zinc-plating process.This mechanical zinc-plating process with industrial zinc power (150 ~ 300 order) for raw material, by means of special activation dispersion plating assistant agent, with glass microballon as impact media, mechanical zinc-plating can be carried out to ferrous metals workpiece such as hardware, standardized component, cast iron pipelines, obtain even, fine and close, the smooth pure zinc coating that appearance has silvery white gloss.This pure zinc coating has good corrosion resisting property and stability.
On the other hand, how to reduce the flux loss of Nd-Fe-Bo permanent magnet material in surface treatment process and more and more become a sharp-pointed problem.Measure the magnetic flux of the Nd-Fe-Bo permanent magnet material of film forming, after then this Nd-Fe-Bo permanent magnet material being placed 1 hour at 150 DEG C, cool to normal temperature, after so repeating 2-3 time, then measure the flux value of this Nd-Fe-Bo permanent magnet material.Flux value according to this twice measurement can calculate high temperature demagnetize.The high temperature demagnetize of the Nd-Fe-Bo permanent magnet material after surface treatment method process of the prior art is generally 2-15%.
Summary of the invention
The object of the present invention is to provide a kind of mechanical plating zinc-nickel method of Nd-Fe-Bo permanent magnet material, described method comprises the steps:
(1) chamfering polishing: adopt mechanical vibration or barreling chamfering method to carry out routine polishing to Nd-Fe-Bo permanent magnet material;
(2) degreasing degreasing: use sodium phosphate, sodium carbonate or sodium hydroxide to carry out conventional degreasing degreasing;
(3) acid pickling and rust removing: then use salpeter solution to carry out conventional acid pickling and rust removing, washing, sulfuric acid activated to described Nd-Fe-Bo permanent magnet material;
(4) flash copper: use copper plating bath to carry out copper plate at neodymium-iron-boron permanent magnetic material surface, described copper plating bath comprises the copper sulfate of 0.03 ~ 0.5 mol/L, the ethylenediamine tetraacetic acid (EDTA) of 0.05 ~ 0.7 mol/L and the S-WAT of 0.02 ~ 0.3 mol/L, and the pH of described copper plating bath is 6.5 ~ 7.5; With
(5) mechanical plating zinc-nickel: adopt zinc-plated nickel liquid to carry out zinc-plated nickel dam to Nd-Fe-Bo permanent magnet material, described zinc-plated nickel liquid comprises basal liquid, dispersion agent, impact media and metal-powder; Wherein, described basal liquid comprises the tensio-active agent 0P-10 of the manganous phosphate of 20-80 grams per liter, the tin protochloride of 0.5-5 grams per liter, the Potassium monofluoride of 0.2-10 grams per liter and 0.1-0.5 grams per liter, and the pH of described basal liquid is 5.0-6.0; Described dispersion agent is the Aqueous Solutions of Polyethylene Glycol of 1.0-5.0 grams per liter; Described impact media is granulated glass sphere; Described metal-powder is zinc and nickel metal powder.
Preferably, the copper facing time is 1 minute.The thickness of described layers of copper is 3-5 micron.
Preferably, the volume ratio of described basal liquid and described dispersion agent is 1: 1-3.
Preferably, the diameter of described granulated glass sphere is 0.5-5 micron, is 1: 1-4 with the weight percent of magnet.
Preferably, the particle diameter of described zinc and nickel metal powder is 3-10 micron.
Preferably, the mass ratio of described zinc and nickel metal powder is 2-10: 1.
Preferably, the thickness of described zinc-nickel layer is 8-20 micron.
Preferably, described Nd-Fe-Bo permanent magnet material is sintered Nd-Fe-B permanent magnetic material or binding Nd-Fe-B permanent magnetic material.
In mechanical plating zinc-nickel method of the present invention, first carry out surface treatment to Nd-Fe-Bo permanent magnet material, this surface treatment can adopt currently known methods of the prior art to carry out.Such as, mechanical vibration or barreling chamfering method is first used to polish Nd-Fe-Bo permanent magnet material.Then use basic solution to carry out degreasing degreasing to Nd-Fe-Bo permanent magnet material, such as, Nd-Fe-Bo permanent magnet material is put into sodium carbonate that the sodium phosphate, the 10g/ that are risen by 20g/ rise and the basic solution that forms of sodium hydroxide that 10g/ rises carries out degreasing degreasing.Then acid pickling and rust removing is carried out to this Nd-Fe-Bo permanent magnet material, such as, use the oxide compound of this neodymium-iron-boron permanent magnetic material surface of salpeter solution cleaning removing of 1% (volume ratio).Final rinse water falls acid and the impurity of neodymium-iron-boron permanent magnetic material surface.
Compare with hot dip process with plating of the prior art, mechanical plating zinc-nickel method of the present invention saves energy can reach 80%, and electroplate liquid formulation is nontoxic, and liquid waste disposal is easy.Therefore, mechanical plating zinc-nickel method of the present invention has that production cost is low, technique is simply convenient to grasp and environmental advantages.The mechanical plating zinc-nickel method of the application of the invention can make Nd-Fe-Bo permanent magnet material obtain excellent corrosion resistance nature, and makes the annealing softening phenomenon without hydrogen embrittlement and hot dip process of Nd-Fe-Bo permanent magnet material.
Compared with the surface treatment method of prior art, another beneficial effect of mechanical plating zinc-nickel method of the present invention is the high temperature demagnetizing factor greatly reducing Nd-Fe-Bo permanent magnet material, and is controlled below 0.15% by high temperature demagnetizing factor.
Embodiment
In order to understand structure of the present invention, feature and other objects further, the appended preferred embodiment of existing combination is described in detail as follows, and illustrated preferred embodiment is only for illustration of technical scheme of the present invention, and non-limiting the present invention.
Embodiment 1
Will
nd-Fe-Bo permanent magnet material 2.3 kilograms of elder generations of 18mm polish 2 hours in vibrating ball mill.Through sodium phosphate 20g/ liter, sodium carbonate 10g/ liter, after sodium hydroxide 10g/ rises degreasing degreasing, in 1% nitric acid pickling removing oxide on surface, wash 3 times, more sulfuric acid activated through 5% after carry out copper facing.Nd-Fe-Bo permanent magnet material complete for above-mentioned pre-treatment is put into copper plating bath, copper plating bath consist of copper sulfate 0.03 mol/L, S-WAT 0.02 mol/L, EDTA0.15 mol/L, pH is 6.5.React 1 minute in drum, form layers of copper at neodymium-iron-boron permanent magnetic material surface, copper layer thickness 3.0 microns.Basal liquid composition is manganous phosphate 20 grams per liter, tin protochloride 5 grams per liter, Potassium monofluoride 0.2 grams per liter and tensio-active agent 0P-100.1 grams per liter, pH=5.0.Dispersion agent composition is the aqueous solution of polyoxyethylene glycol 5.0 grams per liter.Wherein the volume ratio of basal liquid and dispersion liquid is 1: 1.Impact media is the granulated glass sphere of D0.5 (diameter is 0.5 micron).The mass ratio adding two kinds of metal-powders of zinc-nickel is 10: 1.After the magnet forming layers of copper is washed, by the granulated glass sphere of 2.3 kilograms, the zinc powder of 1 kilogram 3 microns and the nickel powder of 3 microns.Loading drum immerses in the trough of basal liquid and the dispersion liquid prepared in advance, barrel plating 30 points, coat-thickness 8 microns.After barrel plating, pearl and workpiece are separated, dry, packaging.Then carry out cross file test, salt-fog test, humid heat test and high temperature demagnetize to measure, do not rise and peel off, non-scale through coating, bonding force is fine, see table 1.
Embodiment 2
Will
the Nd-Fe-Bo permanent magnet material 3.5 kilograms of 18mm polishes by embodiment 1 method, degreasing degreasing, acid-wash activation.Nd-Fe-Bo permanent magnet material complete for above-mentioned pre-treatment is put into copper plating bath, copper plating bath consist of copper sulfate 0.5 mol/L, S-WAT 0.30 mol/L, EDTA0.7 mol/L, pH is 7.5.React 1 minute in drum, form layers of copper at neodymium-iron-boron permanent magnetic material surface, copper layer thickness 4.0 microns.Basal liquid composition is: manganous phosphate 80 grams per liter, tin protochloride 0.5 grams per liter, Potassium monofluoride 10 grams per liter and tensio-active agent 0P-10 0.5 grams per liter, pH=6.0.Dispersion agent composition is the aqueous solution of polyoxyethylene glycol 1.0 grams per liter.Wherein the volume ratio of basal liquid and dispersion liquid is 1: 3.Impact media is the granulated glass sphere of D5 (diameter is 5 microns).The mass ratio of two kinds of metal-powders of zinc-nickel is 2: 1.After the magnet forming layers of copper is washed, the magnet of 0.5 kilogram and the granulated glass sphere of 2.0 kilograms, the zinc powder of 0.5 kilogram 10 microns and nickel powder are loaded drum and immerses in the trough of basal liquid and the dispersion liquid prepared in advance, barrel plating 60 points, coat-thickness 20 microns.After barrel plating, pearl and workpiece are separated, dry, packaging.Then carry out cross file test, salt-fog test, humid heat test and high temperature demagnetize to measure, do not rise and peel off, non-scale through coating, bonding force is fine, see table 1.
Embodiment 3
Will
the Nd-Fe-Bo permanent magnet material 3.5 kilograms of 18mm polishes by embodiment 1 method, degreasing degreasing, acid-wash activation.Nd-Fe-Bo permanent magnet material complete for above-mentioned pre-treatment is put into copper plating bath, copper plating bath consist of copper sulfate 0.25 mol/L, S-WAT 0.10 mol/L, EDTA0.47 mol/L, pH is 6.8.React 1 minute in drum, form layers of copper at neodymium-iron-boron permanent magnetic material surface, copper layer thickness 5.0 microns.Basal liquid composition is: manganous phosphate 60 grams per liter, tin protochloride 2.5 grams per liter, Potassium monofluoride 7 grams per liter and tensio-active agent 0P-10 0.35 grams per liter, pH=5.5.Dispersion agent composition is the aqueous solution of polyoxyethylene glycol 3.5 grams per liter.Wherein the volume ratio of basal liquid and dispersion liquid is 1: 2.Impact media is the granulated glass sphere of D3 (diameter is 3 microns).The mass ratio of two kinds of metal-powders of zinc-nickel is 5: 1.By form layers of copper magnet washing after, the magnet of 1 kilogram and the granulated glass sphere of 3.0 kilograms, the zinc powder of 1.2 kilograms 5 microns and nickel powder are mixed in proportion and load drum and immerse in the trough of basal liquid and the dispersion liquid prepared in advance, barrel plating 60 points, coat-thickness 12 microns.After barrel plating, pearl and workpiece are separated, dry, packaging.Then carry out cross file test, salt-fog test, humid heat test and high temperature demagnetize to measure, do not rise and peel off, non-scale through coating, bonding force is fine, see table 1.
Embodiment 4
Will
the Nd-Fe-Bo permanent magnet material 3.5 kilograms of 18mm polishes by embodiment 1 method, degreasing degreasing, acid-wash activation.Nd-Fe-Bo permanent magnet material complete for above-mentioned pre-treatment is put into copper plating bath, copper plating bath consist of copper sulfate 0.4 mol/L, S-WAT 0.16 mol/L, EDTA0.36 mol/L, pH is 7.0.React 30 seconds in drum, form copper layer thickness 3.5 microns at neodymium-iron-boron permanent magnetic material surface.Basal liquid composition is: manganous phosphate 55 grams per liter, tin protochloride 2.8 grams per liter, Potassium monofluoride 1 grams per liter and tensio-active agent 0P-10 0.4 grams per liter, pH=5.5.Dispersion agent composition is the aqueous solution of polyoxyethylene glycol 3.0 grams per liter.Wherein the volume ratio of basal liquid and dispersion liquid is 1: 1.Impact media is the granulated glass sphere of D2 (diameter is 2 microns).The mass ratio of two kinds of metal-powders of zinc-nickel is 8: 1.After the magnet forming layers of copper is washed, the magnet of 1.5 kilograms and the granulated glass sphere of 3.0 kilograms, the zinc powder of 1.2 kilograms 10 microns and the nickel powder of 3 microns are loaded drum and immerses in the trough of basal liquid and the dispersion liquid prepared in advance, barrel plating 60 points, coat-thickness 15 microns.After barrel plating, pearl and workpiece are separated, dry, packaging.Then carry out cross file test, salt-fog test, humid heat test and high temperature demagnetize to measure, do not rise and peel off, non-scale through coating, bonding force is fine, see table 1.
Embodiment 5
Will
the Nd-Fe-Bo permanent magnet material 3.5 kilograms of 18mm polishes by embodiment 1 method, degreasing degreasing, acid-wash activation.Nd-Fe-Bo permanent magnet material complete for above-mentioned pre-treatment is put into copper plating bath, copper plating bath consist of copper sulfate 0.35 mol/L, S-WAT 0.23 mol/L, EDTA0.05 mol/L, pH is 6.8.React 15 seconds in drum, form layers of copper at neodymium-iron-boron permanent magnetic material surface, copper layer thickness 4.5 microns.Basal liquid composition is: manganous phosphate 55 grams per liter, tin protochloride 1.5 grams per liter, Potassium monofluoride 0.8 grams per liter and tensio-active agent 0P-10 0.2 grams per liter, pH=6.0.Dispersion agent composition is the aqueous solution of polyoxyethylene glycol 4.0 grams per liter.Wherein the volume ratio of basal liquid and dispersion liquid is 1: 3.Impact media is the granulated glass sphere of D4 (diameter is 4 microns).The mass ratio of two kinds of metal-powders of zinc-nickel is 7: 1.After the magnet forming layers of copper is washed, the magnet of 2.0 kilograms and the granulated glass sphere of 2.0 kilograms, the zinc powder of 0.5 kilogram 3 microns and the nickel powder of 10 microns are loaded drum and immerses in the trough of basal liquid and the dispersion liquid prepared in advance, barrel plating 70 points, coat-thickness 17 microns.After barrel plating, pearl and workpiece are separated, dry, packaging.Then carry out cross file test, salt-fog test, humid heat test and high temperature demagnetize to measure, do not rise and peel off, non-scale through coating, bonding force is fine, see table 1.
Comparative example 1
Will
nd-Fe-Bo permanent magnet material 2.3 kilograms of elder generations of 18mm polish 2 hours in vibrating ball mill.Through sodium phosphate 20g/ liter, sodium carbonate 10g/ liter, after sodium hydroxide 10g/ rises degreasing degreasing, pickling removing oxide on surface in 1% nitric acid, washing dries up.Electro-galvanizing, zinc coating thickness 10 microns.Then carry out cross file test, salt-fog test, humid heat test and high temperature demagnetize to measure, Corrosion Protection is see table 1.
Comparative example 2
Will
nd-Fe-Bo permanent magnet material 2.3 kilograms of elder generations of 18mm polish 2 hours in vibrating ball mill.Through sodium phosphate 20g/ liter, sodium carbonate 10g/ liter, after sodium hydroxide 10g/ rises degreasing degreasing, pickling removing oxide on surface in 1% nitric acid, washing dries up.Nd-Fe-Bo permanent magnet material complete for above-mentioned pre-treatment is put into copper plating bath, copper plating bath consist of copper sulfate 0.03 mol/L, S-WAT 0.02 mol/L, EDTA0.15 mol/L, pH is 6.5.React 1 minute in drum, form layers of copper at neodymium-iron-boron permanent magnetic material surface.Basal liquid composition is: manganous phosphate 20 grams per liter, tin protochloride 5 grams per liter, Potassium monofluoride 0.2 grams per liter and tensio-active agent 0P-10 0.1 grams per liter, pH5.0.Dispersion agent composition is the aqueous solution of 1 polyoxyethylene glycol 5.0 grams per liter.Wherein the volume ratio of basal liquid and dispersion liquid is 1: 1.Impact media is the granulated glass sphere of D0.5.After the magnet forming layers of copper is washed, the magnet of 2.0 kilograms and the granulated glass sphere of 2.0 kilograms, the zinc powder of 0.5 kilogram 7 microns are loaded drum and immerses in the trough of basal liquid and the dispersion liquid prepared in advance, barrel plating 70 points, coat-thickness 20 microns.After barrel plating, pearl and workpiece are separated, dry, packaging.Then carry out cross file test, salt-fog test, humid heat test and high temperature demagnetize to measure, Corrosion Protection is see table 1.
Table 1
As can be seen from Table 1, coating surface of the present invention is even, and solidity to corrosion is high, the humid heat test (temperature 85 DEG C, humidity 80, relative humidity 100%) of salt-fog test 72 hours and 300 hours.And the high temperature demagnetizing factor of surface treatment method of the present invention is below 0.15%, also the corresponding high temperature demagnetizing factor lower than prior art like product is 2 ~ 5%.
It should be noted that, foregoing invention content and embodiment are intended to the practical application proving technical scheme provided by the present invention, should not be construed as limiting the scope of the present invention.Those skilled in the art in spirit of the present invention and principle, when doing various amendment, equivalent replace or improve.Protection scope of the present invention is as the criterion with appended claims.
Claims (6)
1. a surface treatment method for the mechanical plating zinc-nickel of Nd-Fe-Bo permanent magnet material, described method comprises the steps:
(1) chamfering polishing: adopt mechanical vibration or barreling chamfering method to carry out routine polishing to Nd-Fe-Bo permanent magnet material;
(2) degreasing degreasing: use sodium phosphate, sodium carbonate or sodium hydroxide to carry out conventional degreasing degreasing;
(3) acid pickling and rust removing: then use salpeter solution to carry out conventional acid pickling and rust removing, washing, sulfuric acid activated to described Nd-Fe-Bo permanent magnet material;
(4) flash copper: use copper plating bath to carry out copper plate at neodymium-iron-boron permanent magnetic material surface, the copper facing time is 1 minute, described copper plating bath comprises the copper sulfate of 0.03 ~ 0.5 mol/L, the ethylenediamine tetraacetic acid (EDTA) of 0.05 ~ 0.7 mol/L and the S-WAT of 0.02 ~ 0.3 mol/L, and the pH of described copper plating bath is 6.5 ~ 7.5; With
(5) mechanical plating zinc-nickel: adopt zinc-plated nickel liquid to carry out zinc-plated nickel dam to Nd-Fe-Bo permanent magnet material, described zinc-plated nickel liquid comprises basal liquid, dispersion agent, impact media and metal-powder; Wherein, described basal liquid comprises the tensio-active agent 0P-10 of the manganous phosphate of 20-80 grams per liter, the tin protochloride of 0.5-5 grams per liter, the Potassium monofluoride of 0.2-10 grams per liter and 0.1-0.5 grams per liter, and the pH of described basal liquid is 5.0-6.0; Described dispersion agent is the Aqueous Solutions of Polyethylene Glycol of 1.0-5.0 grams per liter; The volume ratio of described basal liquid and described dispersion agent is 1: 1-3; Described impact media is granulated glass sphere; Described metal-powder is zinc and nickel metal powder, and the particle diameter of described zinc and nickel metal powder is 3-10 micron.
2. surface treatment method according to claim 1, is characterized in that, the thickness of described layers of copper is 3-5 micron.
3. surface treatment method according to claim 1, is characterized in that, the diameter of described granulated glass sphere is 0.5-5 micron, and the weight ratio of itself and Nd-Fe-Bo permanent magnet material is 1: 1-4.
4. surface treatment method according to claim 1, is characterized in that, the mass ratio of described zinc and nickel metal powder is 2-10: 1.
5. surface treatment method according to claim 1, is characterized in that, the thickness of described zinc-nickel layer is 8-20 micron.
6. surface treatment method according to claim 1, is characterized in that, described Nd-Fe-Bo permanent magnet material is sintered Nd-Fe-B permanent magnetic material or binding Nd-Fe-B permanent magnetic material.
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| CN107937948A (en) * | 2017-11-17 | 2018-04-20 | 烟台首钢磁性材料股份有限公司 | A kind of neodymium iron boron magnetic body and its preparation process for having composite deposite |
| CN109030550A (en) * | 2018-06-04 | 2018-12-18 | 安徽天宇磁业股份有限公司 | A kind of Nd-Fe-B permanent magnet material coating determination method |
| CN110699572A (en) * | 2019-09-26 | 2020-01-17 | 江苏兴洋管业股份有限公司 | Large-diameter nickel-based composite pipe fitting and preparation method thereof |
| CN115198272B (en) * | 2022-06-20 | 2023-11-07 | 包头市英思特稀磁新材料股份有限公司 | Method for forming composite coating by directly electroplating copper on surface of neodymium iron boron |
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