CN102400143A - Machinery galvanizing surface treatment method of neodymium iron boron permanent magnetic material - Google Patents
Machinery galvanizing surface treatment method of neodymium iron boron permanent magnetic material Download PDFInfo
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Abstract
The invention provides a machinery galvanizing surface treatment method of a neodymium iron boron permanent magnetic material. The method comprises the following steps of: (1) chamfering and polishing; (2) degreasing and removing oil; (3) pickling and removing rust; (4) strike plating copper; and (5) galvanizing on the neodymium iron boron permanent magnetic material by using a galvanizing solution, wherein the galvanizing solution contains a base liquid, a dispersant, an impact media and a metal powder. By the adoption of the machinery galvanizing method, the neodymium iron boron permanent magnetic material can be endowed with excellent corrosion resistance, and high temperature demagnetizing factor of the neodymium iron boron permanent magnetic material can be greatly reduced.
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 zinc-plating of Nd-Fe-Bo permanent magnet material.
Background technology
Application of neodymium iron boron (NdFeB) permanent magnet material in recent years and development very rapidly, and the protection of Nd-Fe-Bo permanent magnet material is to be related to one of gordian technique that can Nd-Fe-Bo permanent magnet material apply.Nd-Fe-Bo permanent magnet material mainly is prepared from through powder metallurgical technique elements such as rare earth metal neodymium (Nd), iron and boron.As the strongest present magneticsubstance, Nd-Fe-Bo permanent magnet material has been widely used in fields such as electroplating device, machinery, medical treatment, automobile, and application prospect is very wide.
The prerequisite that Nd-Fe-Bo permanent magnet material is used is at first to resolve the anticorrosion problem of Nd-Fe-Bo permanent magnet material.As a kind of porous material that is prepared from powder metallurgical technique, rich neodymium phase, neodymium iron boron principal phase and borderline phase in the Nd-Fe-Bo permanent magnet material are easy to form intergranular corrosion.Because the character of the rear earth element nd in the neodymium iron boron powder alloy is active; Thereby the corrosion resisting property that makes whole Nd-Fe-B alloys becomes very poor; Particularly very easily corrosion in damp and hot environment; And, had a strong impact on the work-ing life of Nd-Fe-Bo permanent magnet material because of corrosion failure causes the decline or the damage of magnetic property, reduced the stability and the safety of product.The magnetic property of Nd-Fe-Bo permanent magnet material and its weave construction have very big relation.The principal phase of Nd-Fe-Bo permanent magnet material is the main source of its magnetic property, and to coercive force contribution maximum be rich neodymium phase.After Nd-Fe-Bo permanent magnet material corrodes, huge variation will take place in its magnetic property.Therefore, the anticorrosion problem of Nd-Fe-Bo permanent magnet material is the subject matter that Nd-Fe-Bo permanent magnet material need solve always.
At present, the anti-corrosion method of Nd-Fe-Bo permanent magnet material has a variety of, for example electronickelling, electro-galvanizing (CN1421547A, CN1056133A), plating MULTI-LAYER NICKEL, copper facing (CN1514889A), phosphatization, electrocoating paint etc.Electro-galvanizing is under the effect of direct supply, and the 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, deposition zinc on metal parts.Concrete grammar is: in the cylinder of rotation, put into by plating part, granulated glass sphere, water, chemical promoter and zinc powder, after cylinder reached certain rotating speed, piece surface just generated the good continuous zinc layer of bonding force.It is thus clear that mechanical zinc-plating is due to the effect of physics and chemical two aspects.
Application number is that 02110408.5 Chinese invention patent application discloses a kind of mechanical zinc-plating process.This mechanical zinc-plating process is a raw material with industrial zinc powder (150～300 order); Activation by means of special use disperses plating assistant agent; With glass microballon as impact media; Can carry out mechanical zinc-plating to ferrous metals workpiece such as hardware, standardized component, cast iron pipelines, obtain appearance have silvery white glossy evenly, fine and close, slick pure zinc coating.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 film forming Nd-Fe-Bo permanent magnet material, after under 150 ℃ this Nd-Fe-Bo permanent magnet material placement being cooled to normal temperature after 1 hour, so repeating 2-3 time, measure the flux value of this Nd-Fe-Bo permanent magnet material more then.Flux value according to this twice measurement can calculate the high temperature demagnetize.High temperature demagnetize through the Nd-Fe-Bo permanent magnet material after the surface treatment method processing of the prior art is generally 2-15%.
Summary of the invention
The object of the present invention is to provide a kind of surface treatment method of mechanical zinc-plating of Nd-Fe-Bo permanent magnet material, said method comprises the steps:
(1) chamfering polishing: adopt mechanical vibration or barreling chamfering method that Nd-Fe-Bo permanent magnet material is carried out the routine polishing;
(2) degreasing degreasing: use sodium phosphate, yellow soda ash or sodium hydroxide to carry out conventional degreasing degreasing;
(3) acid pickling and rust removing: use salpeter solution that said Nd-Fe-Bo permanent magnet material is carried out conventional acid pickling and rust removing, washing, sulfuric acid activation then;
(4) flash copper: use copper plating bath to carry out copper plate at neodymium-iron-boron permanent magnetic material surface; Said copper plating bath comprises the copper sulfate of 0.03～0.5 mol; 0.05 the S-WAT of the YD 30 of～0.7 mol and 0.02～0.3 mol, and the pH of said copper plating bath is 6.5～7.5; With
(5) mechanical zinc-plating: adopt galvanizing flux that Nd-Fe-Bo permanent magnet material is carried out zinc coating, said galvanizing flux comprises basal liquid, dispersion agent, impact media and metal-powder; Wherein, said basal liquid comprises 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 the tensio-active agent 0P-10 of 0.1-0.5 grams per liter, and the pH of said basal liquid is 5.0-6.0; Said dispersion agent is the polyoxyethylene glycol aqueous solution of 1.0-5.0 grams per liter; Said impact media is a granulated glass sphere; Said metal-powder is the zinc metal-powder.
Preferably, the copper facing time is 1 minute.The thickness of said copper layer is the 3-5 micron.
Preferably, the volume ratio of said basal liquid and said dispersion agent is 1: 1-3.
Preferably, the diameter of said granulated glass sphere is the 0.5-5 micron, and the weight ratio of granulated glass sphere and magnet is 1: 1-4.
Preferably, the particle diameter of said zinc metal-powder is the 3-10 micron.
Preferably, the thickness of said zinc layer is the 8-20 micron.
Preferably, said Nd-Fe-Bo permanent magnet material is sintered Nd-Fe-B permanent magnetic material or binding Nd-Fe-B permanent magnetic material.
In mechanical zinc-plating method of the present invention, at first Nd-Fe-Bo permanent magnet material is carried out surface treatment, this surface treatment can adopt currently known methods of the prior art to carry out.For example, at first use mechanical vibration or barreling chamfering method that Nd-Fe-Bo permanent magnet material is polished.Use basic soln that Nd-Fe-Bo permanent magnet material is carried out degreasing degreasing then, for example Nd-Fe-Bo permanent magnet material is put into the basic soln that sodium hydroxide that the sodium phosphate that risen by 20g/, yellow soda ash that 10g/ rises and 10g/ rise forms and carry out degreasing degreasing.Then this Nd-Fe-Bo permanent magnet material is carried out acid pickling and rust removing, for example use the salpeter solution of 1% (volume ratio) to clean the oxide compound of removing this neodymium-iron-boron permanent magnetic material surface.Final rinse water falls the acid and the impurity of neodymium-iron-boron permanent magnetic material surface.
Compare with hot dip process with plating of the prior art, mechanical zinc-plating method of the present invention can saves energy reach 80%, and electroplate liquid formulation is nontoxic, and liquid waste disposal is easy.Therefore, mechanical zinc-plating method of the present invention has that production cost is low, technology simply is convenient to grasp and advantage such as environmental protection.
The mechanical zinc-plating method of the application of the invention can make Nd-Fe-Bo permanent magnet material obtain the superior corrosion resistance ability, and makes the no hydrogen embrittlement of Nd-Fe-Bo permanent magnet material and the annealing softening phenomenon of hot dip process.
Compare with the surface treatment method of prior art, another beneficial effect of mechanical zinc-plating method of the present invention is the high temperature demagnetizing factor that greatly reduces Nd-Fe-Bo permanent magnet material, and the high temperature demagnetizing factor is controlled at below 0.15%.
Embodiment
In order further to understand structure of the present invention, characteristic and other purposes, combine appended preferred embodiment to specify as follows at present, illustrated preferred embodiment only is used to technical scheme of the present invention is described, and non-limiting the present invention.
Embodiment 1
2.3 kilograms of elder generations of sintered Nd-Fe-B permanent magnetic material of
18mm were polished in vibrating ball mill 2 hours.Through sodium phosphate 20g/ liter, yellow soda ash 10g/ liter, after sodium hydroxide 10g/ rose degreasing degreasing, oxide on surface was removed in pickling in 1% nitric acid, washed 3 times, after 5% sulfuric acid activation, carried out copper facing again.The Nd-Fe-Bo permanent magnet material that above-mentioned pre-treatment is intact is put into copper plating bath, copper plating bath consist of copper sulfate 0.03 mol, S-WAT 0.02 mol, the EDTA0.15 mol, pH is 6.5.Reaction is 1 minute in drum, forms the copper layer at neodymium-iron-boron permanent magnetic material surface.Copper layer thickness is 3 microns.The basal liquid composition is: manganous phosphate 20 grams per liters, tin protochloride 5 grams per liters, Potassium monofluoride 0.2 grams per liter and tensio-active agent 0P-10 0.1 grams per liter, pH=5.0.The dispersion agent composition is: the aqueous solution of 1 polyoxyethylene glycol, 5.0 grams per liters.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).After the magnet washing that forms the copper layer, 2.3 kilograms granulated glass spherees, 1 kilogram 3 microns the zinc powder drum of packing into is immersed in the trough of the basal liquid for preparing in advance and dispersion liquid, barrel plating 30 minutes, coat-thickness are 8 microns.After barrel plating finishes pearl and workpiece are separated drying, packing.Carry out cross file test, salt-fog test, humid heat test and high temperature demagnetize then and measure, do not rise through coating and peel off, non-scale, bonding force is fine, referring to table 1.
Embodiment 2
The binding Nd-Fe-B permanent magnetic material of
18mm is pressed the polishing of embodiment 1 method for 3.5 kilograms; Degreasing degreasing, acid-wash activation.The Nd-Fe-Bo permanent magnet material that above-mentioned pre-treatment is intact is put into copper plating bath, copper plating bath consist of copper sulfate 0.5 mol, S-WAT 0.30 mol, the EDTA0.7 mol, pH is 7.5.Reaction is 1 minute in drum, forms copper layer, 5 microns of copper layer thickness at neodymium-iron-boron permanent magnetic material surface.The basal liquid composition is: manganous phosphate 80 grams per liters, tin protochloride 0.5 grams per liter, Potassium monofluoride 10 grams per liters and tensio-active agent 0P-100.5 grams per liter, pH=6.0.The dispersion agent composition is: the aqueous solution of polyoxyethylene glycol 1.0 grams per liters.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).After the magnet washing that forms the copper layer, 0.5 kilogram magnet and 2.0 kilograms granulated glass sphere, 0.5 kilogram 10 microns zinc powder to be packed in the trough of basal liquid that the drum immersion prepares in advance and dispersion liquid, barrel plating 60 minutes, coat-thickness are 20 microns.After barrel plating finishes pearl and workpiece are separated drying, packing.Carry out cross file test, salt-fog test, humid heat test and high temperature demagnetize then and measure, do not rise through coating and peel off, non-scale, bonding force is fine, referring to table 1.
Embodiment 3
The sintered Nd-Fe-B permanent magnetic material of
18mm is pressed the polishing of embodiment 1 method for 3.5 kilograms; Degreasing degreasing, acid-wash activation.The Nd-Fe-Bo permanent magnet material that above-mentioned pre-treatment is intact is put into copper plating bath, copper plating bath consist of copper sulfate 0.25 mol, S-WAT 0.10 mol, the EDTA0.47 mol, pH is 6.8.Reaction is 1 minute in drum, forms the copper layer at neodymium-iron-boron permanent magnetic material surface, and copper layer thickness is 3.5 microns.The basal liquid composition is: manganous phosphate 60 grams per liters, tin protochloride 2.5 grams per liters, Potassium monofluoride 7 grams per liters and tensio-active agent 0P-100.35 grams per liter, pH=5.5.The dispersion agent composition is: the aqueous solution of polyoxyethylene glycol 3.5 grams per liters.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).After the magnet washing that forms the copper layer, 1 kilogram magnet and 3.0 kilograms granulated glass sphere, 1.2 kilograms 5 microns zinc powder to be packed in the trough of basal liquid that the drum immersion prepares in advance and dispersion liquid, barrel plating 60 minutes, coat-thickness are 12 microns.After barrel plating finishes pearl and workpiece are separated drying, packing.Carry out cross file test, salt-fog test, humid heat test and high temperature demagnetize then and measure, do not rise through coating and peel off, non-scale, bonding force is fine, referring to table 1.
Embodiment 4
The Nd-Fe-Bo permanent magnet material of
18mm is pressed the polishing of embodiment 1 method for 3.5 kilograms; Degreasing degreasing, acid-wash activation.The Nd-Fe-Bo permanent magnet material that above-mentioned pre-treatment is intact is put into copper plating bath, copper plating bath consist of copper sulfate 0.4 mol, S-WAT 0.16 mol, the EDTA0.36 mol, pH is 7.0.Reaction is 30 seconds in drum, forms the copper layer at neodymium-iron-boron permanent magnetic material surface, and copper layer thickness is 4.0 microns.The basal liquid composition is: manganous phosphate 55 grams per liters, tin protochloride 2.8 grams per liters, Potassium monofluoride 1 grams per liter and tensio-active agent 0P-10 0.4 grams per liter, pH=5.5.The dispersion agent composition is: the aqueous solution of polyoxyethylene glycol 2.0 grams per liters.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).After the magnet washing that forms the copper layer, 1.5 kilograms magnets and 3.0 kilograms granulated glass sphere, 1.2 kilograms 8 microns zinc powder to be packed in the trough of basal liquid that the drum immersion prepares in advance and dispersion liquid, barrel plating 60 minutes, coat-thickness are 15 microns.After barrel plating finishes pearl and workpiece are separated drying, packing.Carry out cross file test, salt-fog test, humid heat test and high temperature demagnetize then and measure, do not rise through coating and peel off, non-scale, bonding force is fine, referring to table 1.
Embodiment 5
The sintered Nd-Fe-B permanent magnetic material of
18mm is pressed the polishing of embodiment 1 method for 3.5 kilograms; Degreasing degreasing, acid-wash activation.The Nd-Fe-Bo permanent magnet material that above-mentioned pre-treatment is intact is put into copper plating bath, copper plating bath consist of copper sulfate 0.35 mol, S-WAT 0.23 mol, the EDTA0.09 mol, pH is 6.8.Reaction is 15 seconds in drum, forms the copper layer at neodymium-iron-boron permanent magnetic material surface.Copper layer thickness is 5.0 microns.The basal liquid composition is: manganous phosphate 55 grams per liters, tin protochloride 1.5 grams per liters, Potassium monofluoride 0.8 grams per liter and tensio-active agent 0P-100.2 grams per liter, pH=6.0.The dispersion agent composition is: the aqueous solution of polyoxyethylene glycol 4.0 grams per liters.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).After the magnet washing that forms the copper layer, 2.0 kilograms magnets and 2.0 kilograms granulated glass sphere, 0.5 kilogram 7 microns zinc powder to be packed in the trough of basal liquid that the drum immersion prepares in advance and dispersion liquid, barrel plating 70 minutes, coat-thickness are 17 microns.After barrel plating finishes pearl and workpiece are separated drying, packing.Carry out cross file test, salt-fog test, humid heat test and high temperature demagnetize then and measure, do not rise through coating and peel off, non-scale, bonding force is fine, referring to table 1.
The comparative example 1
2.3 kilograms of elder generations of binding Nd-Fe-B permanent magnetic material of
18mm were polished in vibrating ball mill 2 hours.Through sodium phosphate 20g/ liter, yellow soda ash 10g/ liter, after sodium hydroxide 10g/ rose degreasing degreasing, oxide on surface was removed in pickling in 1% nitric acid, and washing dries up.Electro-galvanizing, 10 microns of zinc coating thickness.Carry out cross file test, salt-fog test, humid heat test and high temperature demagnetize then and measure, Corrosion Protection is referring to table 1.
Table 1
Can be found out that by table 1 coating surface of the present invention is even, solidity to corrosion is high, the humid heat test (85 ℃ of temperature, humidity 80, relative humidity 100%) of salt-fog test 48 hours and 200 hours.And the high temperature demagnetizing factor of surface treatment method of the present invention is below 0.15%, and the also corresponding high temperature demagnetizing factor that is lower than the prior art like product is 2～5%.
Need to prove that foregoing invention content and embodiment are intended to prove the practical application of technical scheme provided by the present invention, should not be construed as qualification protection domain of the present invention.Those skilled in the art are in spirit of the present invention and principle, when doing various modifications, being equal to replacement or improvement.Protection scope of the present invention is as the criterion with appended claims.
Claims (8)
1. the surface treatment method of the mechanical zinc-plating of a Nd-Fe-Bo permanent magnet material, said method comprises the steps:
(1) chamfering polishing: adopt mechanical vibration or barreling chamfering method that Nd-Fe-Bo permanent magnet material is carried out the routine polishing;
(2) degreasing degreasing: use sodium phosphate, yellow soda ash or sodium hydroxide to carry out conventional degreasing degreasing;
(3) acid pickling and rust removing: use salpeter solution that said Nd-Fe-Bo permanent magnet material is carried out conventional acid pickling and rust removing, washing, sulfuric acid activation then;
(4) flash copper: use copper plating bath to carry out copper plate at neodymium-iron-boron permanent magnetic material surface; Said copper plating bath comprises the copper sulfate of 0.03～0.5 mol; 0.05 the S-WAT of the YD 30 of～0.7 mol and 0.02～0.3 mol, and the pH of said copper plating bath is 6.5～7.5; With
(5) mechanical zinc-plating: adopt galvanizing flux that Nd-Fe-Bo permanent magnet material is carried out zinc coating, said galvanizing flux comprises basal liquid, dispersion agent, impact media and metal-powder; Wherein, said basal liquid comprises 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 the tensio-active agent 0P-10 of 0.1-0.5 grams per liter, and the pH of said basal liquid is 5.0-6.0; Said dispersion agent is the polyoxyethylene glycol aqueous solution of 1.0-5.0 grams per liter; Said impact media is a granulated glass sphere; Said metal-powder is the zinc metal-powder.
2. method according to claim 1 is characterized in that, the copper facing time is 1 minute.
3. method according to claim 1 is characterized in that, the thickness of said copper layer is the 3-5 micron.
4. method according to claim 1 is characterized in that, the volume ratio of said basal liquid and said dispersion agent is 1: 1-3.
5. method according to claim 1 is characterized in that, the diameter of said granulated glass sphere is the 0.5-5 micron, and the weight ratio of granulated glass sphere and magnet is 1: 1-4.
6. method according to claim 1 is characterized in that the particle diameter of said zinc metal-powder is the 3-10 micron.
7. method according to claim 1 is characterized in that, the thickness of said zinc layer is the 8-20 micron.
8. method according to claim 1 is characterized in that, said 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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Cited By (3)
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| CN106521586A (en) * | 2016-11-28 | 2017-03-22 | 宁波韵升股份有限公司 | Electrogalvanizing method of neodymium iron boron magnet |
| CN107313080A (en) * | 2017-06-30 | 2017-11-03 | 钢铁研究总院 | Electroplate liquid, preparation method and the electro-plating method of neodymium iron boron product Direct Electroplating copper |
| CN110205623A (en) * | 2019-06-24 | 2019-09-06 | 杨澎 | It is a kind of without using sulfuric acid, hydrochloric acid, phosphoric acid high-strength steel nailing mechanical zinc-plating process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110205623A (en) * | 2019-06-24 | 2019-09-06 | 杨澎 | It is a kind of without using sulfuric acid, hydrochloric acid, phosphoric acid high-strength steel nailing mechanical zinc-plating process |
| CN110205623B (en) * | 2019-06-24 | 2021-05-18 | 杨澎 | Mechanical galvanizing process for high-strength steel nail without using sulfuric acid, hydrochloric acid and phosphoric acid |
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