CN100484666C - Nd-Fe-B magnet inorganic sealing hole adhesion and cathode electrophoresis composite surface protection technique - Google Patents

Nd-Fe-B magnet inorganic sealing hole adhesion and cathode electrophoresis composite surface protection technique Download PDF

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Publication number
CN100484666C
CN100484666C CNB2006101665296A CN200610166529A CN100484666C CN 100484666 C CN100484666 C CN 100484666C CN B2006101665296 A CNB2006101665296 A CN B2006101665296A CN 200610166529 A CN200610166529 A CN 200610166529A CN 100484666 C CN100484666 C CN 100484666C
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China
Prior art keywords
magnet
hole
cathode electrophoresis
composite surface
sealing
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CN101015858A (en
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邱大健
肖祥定
倪晓雪
赵定义
谢鸽平
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WUHAN INST OF MATERIAL PROTECTION
Wuhan Research Institute of Materials Protection
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WUHAN INST OF MATERIAL PROTECTION
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Abstract

The invention relates to a method for adhering neodymium iron boron inorganic hole and cathode electrophoresis composite surface protection, wherein the invention uses inorganic hole agent of potassium metasilicate, liquid glass or lithium silicate whose modules are 3.3-5.4, 3.3 and 4.5, added with inhibitor additive as 0.5-2% hexamethylene tetramine, 0.2-1% bioquin and 0.5-3% sodium molybdatem, under vacuum condition to seal the holes of neodymium iron boron magnet, then processes composite surface protection of electrophoresis coat. The invention has simple operation and semi-automatic operation, to obtain uniform thickness and better insulation property.

Description

A kind of Nd-Fe-B magnet inorganic sealing hole adhesion and cathode electrophoresis composite surface protection technique
Technical field
A kind of Nd-Fe-B magnet inorganic sealing hole adhesion of the present invention and cathode electrophoresis composite surface protection technique belong to the surface protection technique field of porous magnet, particularly the process for protecting surface of bonded neodymium-iron-boron magnet and technology.
Background technology
Neodymium iron boron has excellent magnetism energy and high cost performance as third generation rare earth permanent-magnetic material, has therefore all obtained high speed development in scientific research, production, application facet in recent years.Be widely used in high-tech areas such as electronic apparatus, machinery and medicine equipment, automobile, aviation, along with improving constantly of its performance, new application growth point continues to bring out, be the development of the kownledge economy of representative particularly, constantly bring new purposes to functional materials such as rare earth permanent magnets with the information industry.
But the neodymium chemism in the neodymium iron boron magnetic body is strong, easily oxidizedly get rusty, magnet is made up of heterogeneous structure, is easy to produce grain boundary corrosion, and its short texture, the porosity height, easily pretreatment liquids such as residual acid, alkali cause the long-term corrosion to magnet.A large amount of holes are easy to cause inhales the hydrogen efflorescence, and magnetic property is descended.So need take appropriate measures magnet is protected.
At present, the main means of defence of NdFeB material has: metal coating and organic coating method.For metal coating, because the porous of magnet, easy residual plating bath in the hole causes the long-term corrosion to magnet.For bonded magnet, owing to the inhomogeneities of surface conductance, cause the inhomogeneities of coating, even phenomenon appears not plating in some areas especially.
The organic coating method comprises methods such as NdFeB material surface spraying, dip-coating and ability cathode electrophoresis.With regard to the used spraying method of toroidal magnet, the coating material loss is big; And need the tow sides upset, thereby the processing step that relates to is many; And the shortcoming that has the film thickness uniformity difference.Adopt dip-coating method because drippage and other problems of coating material, be difficult to obtain the coating of uniform thickness, and the porous magnet, its hole can not get abundant filling, will cause expansion in the dry run and so on problem.Even for the ability cathode electrophoresis coating, and the good favor that more and more is subjected to the user in neodymium iron boron magnetic body protection field of adhesive force.But the particularity that neodymium iron boron magnetic body had such as the high resistance of magnet, high porosity, surface electrophoresis poor activity does not reach greatly and cause the foreign ion accumulation after magnet gathers in tank liquor, electrical conductivity of solution increases, limited the raising of electrophoretic voltage in the coating process, make coating thickness low (≤20um) and be difficult to guarantee evenly, and easily cause the defectives such as producing flake, bubble of filming.Japan Patent Jp005428/2000 has introduced the method for sealing of silicate base slaine inorganic sealing hole agent to magnet surface coating, it is earlier magnet to be carried out the electrodeposited coating protection, then mushy electrodeposited coating being carried out sealing of hole handles, the hole of its magnet surface protection electrodeposited coating that has been shutoff, and the hole of magnet itself does not obtain effective shutoff, and, in hole sealing agent, do not add and improve corrosion proof additive, so the effect of shutoff neodymium iron boron magnetic body hole is not remarkable.Japan Patent JP2002088402 has introduced the vegetalitas medium and has mixed the method for magnet being carried out sealing of hole with metal dust, but the technology more complicated, poor practicability.
How further to improve the corrosion stability of neodymium-iron-boron magnetic material, make Nd-Fe-Bo permanent magnet material, be common concern in the industry and problem to be solved is arranged to adapt to multiple use.
Summary of the invention
The purpose of this invention is to provide a kind of Nd-Fe-B magnet inorganic sealing hole adhesion and cathode electrophoresis composite surface protection technique, at bonded neodymium-iron-boron magnet loose structure characteristics, to the bonded neodymium-iron-boron magnet sealing of hole of going ahead of the rest, carry out the composite surface guard technology that ability cathode electrophoresis is filmed with the inorganic sealing hole agent again.
Another object of the present invention is to provide a kind of inorganic sealing hole and the ability cathode electrophoresis combination technological method of filming at bonded neodymium-iron-boron magnet.
The objective of the invention is to be achieved through the following technical solutions:
The composite surface guard technology of this Nd-Fe-B magnet inorganic sealing hole adhesion and ability cathode electrophoresis, be to adopt the inorganic base metal silicate systems hole sealing agent that is added with functional additive, under vacuum condition, to the bonded neodymium-iron-boron magnet sealing of hole of going ahead of the rest, adopt the ability cathode electrophoresis technology to the bonded neodymium-iron-boron magnet of sealing of hole then, the composite surface guard technology that the electrophoresis of going is again filmed.
Bonded neodymium-iron-boron magnet immersed to be selected from modulus be that 3.3~5.4 potassium silicate or modulus are that 3.3 sodium metasilicate or modulus are the alkali silicate of 4.5 lithium metasilicate and add corresponding corrosion inhibiter hexa 0.5%~2%, 8-hydroxy-quinoline 0.2%~1%, in the inorganic sealing hole agent of sodium molybdate 0.5%~3%, in the vacuum still, be evacuated to more than the 750mmHg, continuity 10~15min, through washing, after 100 ℃~140 ℃ baking 2h~4h solidify, magnet is carried out after phosphatization handles, again will be through the magnet of the reason of sealing of hole herein as negative electrode, solid part is 18%~22% weight, conductance 1200 ± 600 μ s/cm, PH 5.8~6.5, in the ability cathode electrophoresis liquid of pigment 1:3~4, with initial voltage 80~90V, deposition voltage 140~160V, electrophoresis temperature are under 28~30 ℃ the condition, electrophoresis 150~180s, form the electrophoresis rete, use washed with de-ionized water, in baking oven,, finish curing in 170 ℃ of baking 30min again in 80 ℃ of baking 20~30min.Thereby obtain with inorganic sealing hole of the present invention and the ability cathode electrophoresis neodymium iron boron magnetic body that the composite surface guard technology handles of filming.
Inorganic sealing hole and ability cathode electrophoresis technology according to the bonded neodymium-iron-boron magnet of the composite surface guard technology of this Nd-Fe-B magnet inorganic sealing hole adhesion and ability cathode electrophoresis are as follows:
1, bonded neodymium-iron-boron magnet vacuum sealing of hole
Bonded neodymium-iron-boron magnet is immersed in the hole sealing agent prescription of pressing column weight amount percentage:
A kind of alkali silicate is selected from the potassium silicate of modulus 3.3~5.4, the silicic acid of modulus 3.3
Sodium or modulus 4.5 lithium metasilicates 94%~98.8%
Hexa 0.5%~2%
8-hydroxy-quinoline 0.2%~1%
Sodium molybdate 0.5%~3%
Place in the vacuum still, be evacuated to more than the 750mmHg, continuity 10~15min carries out sealing of hole and handles;
2, water drenches and cleans;
3,100 ℃~140 ℃ curing 2h~4h in baking oven;
4, phosphatization is handled;
5, pure water is cleaned;
6, ability cathode electrophoresis is filmed:
To by following ability cathode electrophoresis formula of liquid and process conditions, carry out electrophoretic coating through the magnet of above-mentioned processing as negative electrode, form the electrophoresis rete,
Electrophoresis liquid prescription and condition are as follows:
Electrophoresis liquid solid part 18%~22% weight
Electrical conductivity 1200 ± 600 μ s/cm
PH value 5.8~6.5
Pigment 1:3~4
Initial voltage 80~90V
Deposition voltage 140~160V
28~30 ℃ of electrophoresis temperatures
Electrophoresis time 150~180s;
7, deionized water is cleaned;
8, solidify: the phase I in 80 ℃, is toasted 20~30min in baking oven;
In 170 ℃, baking 30min finishes curing to second stage in baking oven.
By method of the present invention, can effectively solve the problem of the neodymium iron boron surface protection technique that causes because of hole.Hole-sealing technology is simple, and is easy to operate, and the cost performance height can design semi-automatic, clearance-type and carry out.By method of the present invention, can make that bonded neodymium-iron-boron magnet obtains that thickness is even, corrosion resisting property is good, the protective coating of aesthetic appearance and good insulation preformance.
The specific embodiment
Below in conjunction with specific embodiment, the present invention is further described
Embodiment 1
It is in 3.3 the potassium silicate inorganic material that the bonded neodymium-iron-boron material 1Kg of ф 25 * 15 is immersed modulus, put into the vacuum still, be evacuated to the above continuity of 750mmHg 10~15min, it is clean that test specimen is taken out water wash, in baking oven 100 ℃~140 ℃ solidify 2h~4h after, through phosphatization, washing, carrying out ability cathode electrophoresis again films: ability cathode electrophoresis initial voltage 80~90V, deposition voltage 140~160V, electrophoresis temperature is 28~30 ℃, and electrophoresis time is 150~180s, solidifies after washing again, i.e. 80 ℃ of bakings of elder generation 20~30min, 170 ℃ of baking 30min finish curing again.Promptly obtain handling and the film bonded neodymium-iron-boron magnet product of composite protective of ability cathode electrophoresis through inorganic sealing hole.This magnetic Nd-Fe-B ring protective coating is carried out corrosion resistant test, and its result satisfies following index:
The saline solution soaking at room temperature of 3% weight 80 hours is no abnormal;
Warm and humid heat test in being undertaken by GBT1740,860h does not have and gets rusty, expands;
Carry out salt spray test by GB/T1771, nothing was got rusty, is expanded in 200 hours.
Embodiment 2
It is in 4.8 the potassium silicate inorganic material that the bonded neodymium-iron-boron material 1Kg of ф 25 * 15 is immersed modulus, put into the vacuum still, be evacuated to the above continuity of 750mmHg 10~15min, it is clean that test specimen is taken out water wash, in baking oven 100 ℃-140 ℃ solidify 2h~4h after, through phosphatization, washing, carrying out ability cathode electrophoresis again films: ability cathode electrophoresis initial voltage 80~90V, deposition voltage 140~160V, electrophoresis temperature is 28~30 ℃, and electrophoresis time is 150~180s, solidifies after washing again, i.e. 80 ℃ of bakings of elder generation 20~30min, 170 ℃ of baking 30min finish curing again.Promptly obtain handling and the film bonded neodymium-iron-boron magnet product of composite protective of ability cathode electrophoresis through inorganic sealing hole.This magnetic Nd-Fe-B ring protective coating is carried out corrosion resistant test, and its result satisfies following index:
The saline solution soaking at room temperature of 3% weight 96 hours is no abnormal;
Warm and humid heat test in being undertaken by GBT1740,960h does not have and gets rusty, expands;
Carry out salt spray test by GB/T1771, nothing was got rusty, is expanded in 240 hours.
Embodiment 3
It is in 4.8 the potassium silicate inorganic sealing hole agent that the NdFeB material 1Kg that ф 25 * 15 is bonding immerse moduluses, add hexa 1% in the hole sealing agent, 8-hydroxy-quinoline 0.6%, put into the vacuum still, be evacuated to the above continuity of 750mmHg 10~15min, it is clean that test specimen is taken out water wash, in baking oven 100 ℃~140 ℃ solidify 2h~4h after, through phosphatization, washing, carrying out ability cathode electrophoresis again films: ability cathode electrophoresis initial voltage 80~90V, and deposition voltage 140~160V, electrophoresis temperature are 28~30 ℃, electrophoresis time is 150~180s, after washing, solidify again, i.e. 80 ℃ of bakings of elder generation, 20~30min, 170 ℃ of baking 30min finish curing again.Promptly obtain containing the inorganic sealing hole processing of corrosion inhibition additive and the bonded neodymium-iron-boron magnet product of ability cathode electrophoresis composite protective.This magnetic Nd-Fe-B ring protective coating is carried out corrosion resistant test, and its result satisfies following index:
The saline solution soaking at room temperature of 3% weight 96 hours is no abnormal;
Warm and humid heat test in being undertaken by GBT1740,1080h does not have and gets rusty, expands;
Carry out salt spray test by GB/T1771, nothing was got rusty, is expanded in 300 hours.
Embodiment 4
It is in 4.8 the potassium silicate inorganic sealing hole agent that the bonded neodymium-iron-boron material 1Kg of ф 25 * 15 is immersed modulus, add hexa 1% in the hole sealing agent, 8-hydroxy-quinoline 0.2%, sodium molybdate 0.5% is put into the vacuum still, be evacuated to the above continuity of 750mmHg 10~15min, it is clean that test specimen is taken out water wash, in baking oven 100 ℃~140 ℃ solidify 2h~4h after, through phosphatization, washing, carrying out ability cathode electrophoresis again films: ability cathode electrophoresis initial voltage 80~90V, deposition voltage 140~160V, electrophoresis temperature is 28~30 ℃, and electrophoresis time is 150~180s, solidifies after washing again, i.e. 80 ℃ of bakings of elder generation 20~30min, 170 ℃ of baking 30min finish curing again.Promptly obtain containing the inorganic sealing hole processing of corrosion inhibition additive and the bonded neodymium-iron-boron magnet product of ability cathode electrophoresis composite protective.This magnetic Nd-Fe-B ring protective coating is carried out corrosion resistant test, and its result satisfies following index:
The saline solution soaking at room temperature of 3% weight 120 hours is no abnormal;
Warm and humid heat test in being undertaken by GBT1740,1200h does not have and gets rusty, expands;
Carry out salt spray test by GB/T1771, nothing was got rusty, is expanded in 300 hours.
Comparative example 1
Bonded neodymium-iron-boron material 1Kg with ф 25 * 15, after oil removing → washing → phosphatization → washing, promptly carrying out ability cathode electrophoresis films: ability cathode electrophoresis initial voltage 80~90V, deposition voltage 140~160V, electrophoresis temperature is 28~30 ℃, and electrophoresis time is 150~180s, through washing, solidify: 80 ℃ are toasted 20~30min earlier again, again 170 ℃ of baking 30min.Obtain bonded neodymium-iron-boron magnet product without the single ability cathode electrophoresis coating protection of sealing of hole processing.This magnetic Nd-Fe-B ring protective coating is carried out corrosion resistant test, and its result satisfies following index:
The saline solution soaking at room temperature of 3% weight 48 hours is no abnormal;
Warm and humid heat test in being undertaken by GBT1740,576h does not have and gets rusty, expands;
Carry out salt spray test by GB/T1771, nothing was got rusty, is expanded in 180 hours.
Bonded neodymium-iron-boron magnet sealing of hole of the present invention and ability cathode electrophoresis composite protective technology protection domain are not limited to above-mentioned example.The present invention is equally applicable to Sintered NdFeB magnet.

Claims (2)

1, the composite surface means of defence of a kind of Nd-Fe-B magnet inorganic sealing hole adhesion and ability cathode electrophoresis, it is characterized in that adopting the method for sealing of the inorganic base metal silicate hole sealing agent that is added with corresponding corrosion inhibition additive, to the bonded neodymium-iron-boron magnet sealing of hole of going ahead of the rest, adopt the ability cathode electrophoresis coating method that the bonded neodymium-iron-boron magnet of sealing of hole is gone the composite surface protective treatment that ability cathode electrophoresis films again then, it is 3.3~5.4 potassium silicate that the inorganic base metal silicate of this hole sealing agent is selected from modulus, modulus is 3.3 sodium metasilicate, or modulus is 4.5 lithium metasilicate; The corrosion inhibition additive that is added is hexa 0.5%~2%, 8-hydroxy-quinoline 0.2%~1% and sodium molybdate 0.5%~3% by mass percent.
2, composite surface means of defence according to claim 1 is characterized in that the ability cathode electrophoresis coating method is to adopt low relatively initial voltage earlier, adopts high relatively deposition voltage then.
CNB2006101665296A 2006-12-28 2006-12-28 Nd-Fe-B magnet inorganic sealing hole adhesion and cathode electrophoresis composite surface protection technique Expired - Fee Related CN100484666C (en)

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Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102314990A (en) * 2010-07-08 2012-01-11 赵立文 Magnet and preparation method thereof
CN102776547B (en) * 2012-08-23 2015-01-21 安泰科技股份有限公司 Method for preparing rare earth permanent magnetic material
CN108048829B (en) * 2017-12-11 2019-06-25 宁波韵升股份有限公司 A kind of electrophoresis method of neodymium iron boron magnetic body
CN110983416A (en) * 2019-12-31 2020-04-10 枣阳市旺前电泳涂料有限公司 Electrophoretic paint painting process
CN112725806B (en) * 2020-12-29 2023-03-21 宁德师范学院 Neodymium-iron-boron composite corrosion inhibitor and application thereof

Citations (4)

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Publication number Priority date Publication date Assignee Title
CN1085963A (en) * 1993-11-03 1994-04-27 胡景云 The swimming of neodymium-iron-boron magnetic material cathode of surface applies production technique
CN1336672A (en) * 2000-07-31 2002-02-20 冲微型技研株式会社 High corrosion-resistant type Nd-Fe-B magnetic iron
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Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1085963A (en) * 1993-11-03 1994-04-27 胡景云 The swimming of neodymium-iron-boron magnetic material cathode of surface applies production technique
CN1336672A (en) * 2000-07-31 2002-02-20 冲微型技研株式会社 High corrosion-resistant type Nd-Fe-B magnetic iron
CN1528952A (en) * 2003-09-27 2004-09-15 沈阳工业学院 Neodymium-iron-boron magnet zinc plating and cathode electrophoresis composite protection process
CN1619718A (en) * 2003-11-17 2005-05-25 上海核工业第八研究所 Binding neodybium iron boron magnet surface cathode electrophoresis production technology

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* Cited by examiner, † Cited by third party
Title
粘接钕铁硼磁体阴极电泳涂装工艺研究. 肖祥定,邱大健,倪晓雪,梁晓东,李先成.材料保护,第5期. 2006
粘接钕铁硼磁体阴极电泳涂装工艺研究. 肖祥定,邱大健,倪晓雪,梁晓东,李先成.材料保护,第5期. 2006 *

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