CN108461272A - A technique for being used to form hydride nano-particle face coat - Google Patents
A technique for being used to form hydride nano-particle face coat Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
- H01F41/0293—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets diffusion of rare earth elements, e.g. Tb, Dy or Ho, into permanent magnets
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Abstract
A technique for it being used to form hydride nano-particle face coat, belongs to technical field of magnetic materials.The rare earth hydride particle and adhesive of variable grain size are dispersed in dispersant, dispersant is the volatile solution such as anhydrous propanone, and at least one of rare earth Pr, Nd, Tb, Dy, adhesive is PVP (polyvinylpyrrolidone) etc..Above-mentioned hydride particle is sprayed to by Sintered NdFeB rare-earth magnet surface using spraying method, is allowed to be formed uniformly, it is fine and close, do not fall off and the regulatable rare earth hydride nanoparticle coating of thickness.Rare earth hydride grain coating can be obviously improved the magnetic property of thicker size sintered rare-earth permanent magnetic body, the especially coercivity of magnet.The usage amount of heavy rare earth in sintered rare-earth permanent magnetic body can be reduced, to reduce the manufacturing cost of high-coercivity magnet under the premise of ensureing that magnet has good magnetic property using the method for the present invention.
Description
Technical field
The present invention relates to a kind of new methods forming rare earth hydride nanoparticle coating, and the present invention is for improving rare earth forever
The coercivity of magnetic sintered magnet, belongs to technical field of magnetic materials.
Background technology
Since NdFeB magnets have excellent comprehensive magnetic energy, computer, communication apparatus, aviation have been widely used in it
Space flight, the critical function device of the technical fields such as vehicles.As electric vehicle, hybrid vehicle, wind power generation etc. are low
Carbon economic industry is increasingly ripe, and the demand of high-coercivity magnet is more urgent.The magneto high speed operation temperature of its critical component
It spends at 200 DEG C or more, and, the Curie temperature of NdFeB magnets itself is relatively low, and thermal stability is poor, and operating temperature is usually less than 100
DEG C, heat demagnetization easily occurs under high temperature, therefore directly limit application of the magnet in fields such as high-temperature electric machines.So how to improve burning
Tying the thermal stability of NdFeB magnets becomes associated production and application field urgent problem to be solved.
In order to which sintered NdFeB magnet improves coercivity and improves temperature stability, major way is added by melting mode
Enter Dy or Tb to obtain (Nd, the Dy) of high anisotropy field2Fe14B or (Nd, Tb)2Fe14B main phases improve magnet coercivity, into
And improve the temperature characterisitic of alloy.But the introducing of the heavy rare earth elements such as melting mode Dy or Tb is used not only to significantly reduce magnetic
The remanent magnetism and magnetic energy product of body, and increased considerably due to the more addition of expensive Dy or Tb the cost of magnet.
In this regard, the purpose of the present invention is improve the magnetocrystalline anisotropy of main phase grain superficial layer by grain boundary decision method
, at the same by improve crystal boundary borderline properties and its with the interaction of main phase grain, to improve the interior of sintered NdFeB magnet
Coercivity is reported, while remanent magnetism to magnet and magnetic energy product generate minimum negative effect.
Patent CN101908397 discloses coating hydride nano-particle on sintered NdFeB magnet surface, but not at present
Uniformly, efficiency is low.Patent CN1035456208A is disclosed forms nanometer with the method for electro-deposition on sintered NdFeB magnet surface
The coating of hydride, but such method the problem of there is combination force differences between powder and magnet.
Patent CN107026003A disclose heavy rare earth and Ga mixed-powder be covered in magnet drying after be diffused place
Reason;CN103745823A, which is disclosed, to be coated the quality percentage of Dy that a layer thickness is 10~200 μm in Ar gas heat spraying methods and contains
DIFFUSION TREATMENT is carried out after the DyTb alloy-layers that amount is 60%~90%;CN107578912A is disclosed heavy rare earth powder and oxygen
DIFFUSION TREATMENT is carried out after being covered in magnet drying after agent, binder, organic solvent mixing;CN104134528A discloses surface
Spraying is containing suspension under heavy rare earth and room temperature, DIFFUSION TREATMENT after drying under an inert gas.Using micron in the above patent
Particle is coated, diffusion energy force difference, therefore handled magnet thickness is less than or equal to 4mm.
Invention content
The purpose of the present invention is for the rare earth permanent magnet sintered magnet of thicker size obtain high-coercive force one kind is provided can be with
Realize the technical method of mass production.
The present invention provides through the methods of spraying to form rare earth hydride nanoparticle coating on the surface of sintered magnet
Novel technical method.Another of the present invention to the effect that utilizes the above-mentioned place for being used to form rare earth hydride nanoparticle coating
Agent is managed, a kind of method forming rare earth hydride nanoparticle coating on the body surface for need surface coated treatment is provided.
Using this method, the surface for including rare earth hydride nanoparticle can be formed on the surface of blocky rare earth permanent magnet sintered magnet
Coating can be notable by carrying out two level heat treatment to the magnet for having formed rare earth hydride nanoparticle coating on surface
Improve the magnetic property of magnet, the especially coercivity of magnet.
A kind of technical method being used to form hydride nano-particle face coat, which is characterized in that include the following steps:
To after heating magnet surface spray rare earth hydride surface coating treatment, rare earth hydride surface coating treatment be containing
Then the acetone colloidal solution of rare earth nano hydride and binder forms rare earth hydride nanoparticle in magnet surface and applies
Layer, rare earth nano hydride are at least one of Pr, Nd, Tb, Dy hydride.Gained rare earth hydride nanoparticle coating is equal
It is even, fine and close, do not fall off and thickness is controllable;
The hydride nano-particle of face coat is made to be diffused into inside magnet to prepare by heat treatment process again
High magnetic characteristics sintered magnet.The weight ratio percentage of further requirement hydride nano-particle face coat is 0.1-1%, according to this
To determine thickness.The magnet of 10cm can be more than with diffusion thickness.
The method to form rare earth hydride nanoparticle coating is further prepared using above-mentioned inorganic agent, using spraying
Mode, specific steps include:It is ready for forming the inorganic agent of rare earth hydride nanoparticle face coat first, will handle
Agent is placed in spray gun pot, and is stirred continuously and is allowed to form suspension, it is ensured that the concentration in watering can is consistent.Magnetic after surface is polished
Body is cleaned with anhydrous propanone, and air-heater drying after weighing, is heated on warm table, then added with spray gun pair in closed container
Magnet after heat is sprayed, and surface obtains certain thickness rare earth hydride nanoparticle layer, weigh weight, 650 DEG C-
Level-one heat treatment is carried out at a temperature of 900 DEG C, then time 2-6 hour carries out at a temperature of 450 DEG C -550 DEG C at two level heat
Reason, time 2-4 hour.
The present invention is mainly used for forming the inorganic agent of rare earth hydride nanoparticle face coat, rare earth hydride surface
The preparation of coating treatment:It is molten that rare earth hydride nanoparticle is dispersed in the colloid formed in the easy volatile solvents such as acetone
Liquid, the range of the average particle diameter of rare earth hydride are and adhesive to be added in colloidal solution between 10-500 nanometers,
Adhesive is PVP (polyvinylpyrrolidone) etc., forms the inorganic agent for rare earth hydride nanoparticle face coat.Processing
The concentration of agent middle rare earth hydride is 0.2-0.5g/ml, the mass percent 0.5%-5% of binder;Further preferred PVP points
Subchain length is different, PVP model PVP k15-PVP k60;Further preferably in the average particle diameter 10- of rare earth hydride
Between 500 nanometers, as rare earth hydride average particle diameter increases, PVP models increase.It is selected not for different-thickness magnet
With the rare earth hydride particle disposal agent of granularity size.
Above-mentioned spraying is preferred, and small-sized agitating device is equipped in watering can and is stirred continuously, uniform suspension is made to be sprayed by spray gun
Go out.NdFeB magnets after polishing are cleaned with anhydrous propanone, and air-heater drying is put on a metal plate, is placed on warm table together
It is heated to 80-120 DEG C, time 2-5 minute carries out spray treatment, spray gun and magnet to the magnet after heating in closed container
Operating distance be 8-15cm, spray gun pressure 0.2-0.5MPa, the air extractor of closed container side is opened after spraying, is made
Air flows and recycles anhydrous propanone by end, while making the powder rapid precipitation in closed container and recycling.At magnet heat
The magnetic property of magnet can be significantly improved after reason, especially the coercivity of magnet is promoted apparent.
Involved magnet is the sintered magnet such as sintered NdFeB magnet of any material containing rare earth in the present invention.Below
Each embodiment is to be prepared such as NdFeB magnets, the magnet of difference weightening ratio by spray-on coating method under identical experiment condition
Every magnetic parameter of magnet is tested after being heat-treated by different process.
The advantage of the invention is that:
(1) present invention uses rare earth hydride nanoparticle inorganic agent, higher than micron particles activity using nano particle, more
The characteristics of easily spreading, can be more than such as NdFeB magnets of 10cm with diffusion thickness, and difference can be selected for different-thickness magnet
The rare earth hydride particle disposal agent of granularity size, and obtain preferable effect.
(2) rare earth hydride nanoparticle inorganic agent using the present invention, the magnetic property of handled magnet are significantly better than micro-
Rice grain.
(3) due to nano particle smaller, the particle of different sizes needs to be mixed with the different glue of molecular chain length
It closes, has better binding force to reach powder and magnet, the glue suitable for nano particle is had developed thus, using spraying method
Coating uniform, fine and close, not easily to fall off and controllable thickness can be formed on sintered NdFeB magnet surface.
(4) relative to micron particles, using the suspension not free settling of nano particle configuration, spraying evenly, magnet one
Cause property is more preferable.The follow-up diffusion temperature of magnet is relatively lower, and the time is shorter, advantageously reduces cost.
(5) magnets exhibit of the invention goes out good magnetic property, and simple process and low cost is honest and clean, it can be achieved that industrialization
Production.
Specific implementation mode
With reference to embodiment, the present invention will be further described, but the present invention is not limited to following embodiments.
Embodiment 1
300-500 nanometers of rare earth hydrogenation dysprosium particle 3g of particle diameter is uniformly mixed with the anhydrous propanone solution of 10ml,
Hydrogenation dysprosium is set to be uniformly dispersed in anhydrous propanone, and it is 60 that 0.4g PVP k values, which are added, subsequent heating water bath simultaneously uses glass bar
Stirring ensure glue uniform dissolution in the solution, prepare be used to form hydrogenation dysprosium grain coating suspension, a concentration of 0.25/
Ml (since the volume of gained suspension and dispersant is almost the same, similarly hereinafter).
Sintered NdFeB magnet is prepared into the small pieces of 10 × 10 × 8mm of appearance and size, and its surface is polished.It will
Magnet anhydrous propanone cleaning that treated, air-heater drying are put on a metal plate after weighing, and are placed on warm table and are added together
Heat is to 100 DEG C, 5 minutes time;Spray treatment, the working distance of spray gun and magnet are carried out in closed container to the magnet after heating
From for 10cm, spray gun pressure 0.3MPa, the evacuation device of air of closed container side is opened after spraying, makes the powder in closed container
Last rapid precipitation simultaneously recycles, and magnet surface obtains certain thickness rare earth hydrogenation dysprosium stratum granulosum, weighs weight.By NdFeB magnets
It is 1 × 10 to be placed in vacuum degree-4In the heat treatment furnace of pa, level-one heat treatment temperature is 850 DEG C, 2 hours;Two level heat treatment temperature
It is 550 DEG C, 4 hours.The final magnetic property parameter of treated magnet is shown in Table No. 2 magnets in 1.
Embodiment 2
300-500 nanometers of rare earth hydrogenation terbium particle 5g of particle diameter is uniformly mixed with the anhydrous propanone solution of 10ml,
Hydrogenation terbium is set to be uniformly dispersed in anhydrous propanone, and it is 60 that 0.3g PVP k values, which are added, subsequent heating water bath simultaneously uses glass bar
Stirring ensures glue uniform dissolution in the solution, prepares the suspension for being used to form hydrogenation terbium grain coating, a concentration of 0.5g/
ml。
Sintered NdFeB magnet is prepared into the small pieces of 10 × 10 × 10mm of appearance and size, and its surface is polished.It will
Magnet anhydrous propanone cleaning that treated, air-heater drying are put on a metal plate after weighing, and are placed on warm table and are added together
Heat is to 80 DEG C, 4 minutes time;Spray treatment, the working distance of spray gun and magnet are carried out in closed container to the magnet after heating
From for 15cm, spray gun pressure 0.5MPa, the evacuation device of air of closed container side is opened after spraying, makes the powder in closed container
Last rapid precipitation simultaneously recycles, and magnet surface obtains certain thickness rare earth hydrogenation terbium stratum granulosum, weighs weight.By NdFeB magnets
It is 1 × 10 to be placed in vacuum degree-4In the heat treatment furnace of pa, level-one heat treatment temperature is 900 DEG C, 3 hours;Two level heat treatment temperature
It is 500 DEG C, 3 hours.The final magnetic property parameter of treated magnet is shown in Table No. 3 magnets in 1.
Embodiment 3
10-100 nanometers of rare earth hydrogenation terbium particle 4g of particle diameter is uniformly mixed with the anhydrous propanone solution of 10ml, is made
Hydrogenation terbium is uniformly dispersed in anhydrous propanone, and it is 15 that 0.15g PVP k values, which are added, and subsequent heating water bath is simultaneously stirred with glass bar
Mixing ensures glue uniform dissolution in the solution, prepares the suspension for being used to form hydrogenation terbium grain coating, a concentration of 0.2g/
ml。
Sintered NdFeB magnet is prepared into the small pieces of 10 × 10 × 12mm of appearance and size, and its surface is polished.It will
Magnet anhydrous propanone cleaning that treated, air-heater drying are put on a metal plate after weighing, and are placed on warm table and are added together
Heat is to 120 DEG C, 4 minutes time;Spray treatment, the working distance of spray gun and magnet are carried out in closed container to the magnet after heating
From for 8cm, spray gun pressure 0.2MPa, the evacuation device of air of closed container side is opened after spraying, makes the powder in closed container
Last rapid precipitation simultaneously recycles, and magnet surface obtains certain thickness rare earth hydrogenation terbium stratum granulosum, weighs weight.By NdFeB magnets
It is 1 × 10 to be placed in vacuum degree-4In the heat treatment furnace of pa, level-one heat treatment temperature is 900 DEG C, 5 hours;Two level heat treatment temperature
It is 500 DEG C, 3 hours.The final magnetic property parameter of treated magnet is shown in Table No. 4 magnets in 1.
Embodiment 4
100-200 nanometers of rare earth praseodymium hydride particle 2g of particle diameter is uniformly mixed with the anhydrous propanone solution of 10ml,
Praseodymium hydride is set to be uniformly dispersed in anhydrous propanone, and it is 17 that 0.1g PVP k values, which are added, subsequent heating water bath simultaneously uses glass bar
Stirring ensures glue uniform dissolution in the solution, prepares the suspension for being used to form praseodymium hydride grain coating, a concentration of
0.25g/ml。
Sintered NdFeB magnet is prepared into the small pieces of 10 × 10 × 6mm of appearance and size, and its surface is polished.It will
Magnet anhydrous propanone cleaning that treated, air-heater drying are put on a metal plate after weighing, and are placed on warm table and are added together
Heat is to 100 DEG C, 4 minutes time;Spray treatment, the working distance of spray gun and magnet are carried out in closed container to the magnet after heating
From for 15cm, spray gun pressure 0.5MPa, the evacuation device of air of closed container side is opened after spraying, makes the powder in closed container
Last rapid precipitation simultaneously recycles, and magnet surface obtains certain thickness rare earth praseodymium hydride stratum granulosum, weighs weight.By NdFeB magnets
It is 1 × 10 to be placed in vacuum degree-4In the heat treatment furnace of pa, level-one heat treatment temperature is 770 DEG C, 4 hours;Two level heat treatment temperature
It is 450 DEG C, 2 hours.The final magnetic property parameter of treated magnet is shown in Table No. 5 magnets in 1.
Embodiment 5
200-300 nanometers of rare earth neodymium hydride particle 2g of particle diameter is uniformly mixed with the anhydrous propanone solution of 10ml,
Neodymium hydride is set to be uniformly dispersed in anhydrous propanone, and it is 30 that 0.25g PVP k values, which are added, subsequent heating water bath simultaneously uses glass bar
Stirring ensures glue uniform dissolution in the solution, prepares the suspension for being used to form neodymium hydride grain coating, a concentration of 0.5g/
ml。
Sintered NdFeB magnet is prepared into the small pieces of 10 × 10 × 6mm of appearance and size, and its surface is polished.It will
Magnet anhydrous propanone cleaning that treated, air-heater drying are put on a metal plate after weighing, and are placed on warm table and are added together
80 DEG C of heat, 3 minutes time;Spray treatment, the operating distance of spray gun and magnet are carried out in closed container to the magnet after heating
For 12cm, spray gun pressure 0.4MPa, the evacuation device of air of closed container side is opened after spraying, makes the powder in closed container
Rapid precipitation simultaneously recycles, and magnet surface obtains certain thickness rare earth hydride stratum granulosum, weighs weight.NdFeB magnets are set
In vacuum degree be 1 × 10-4In the heat treatment furnace of pa, level-one heat treatment temperature is 650 DEG C, 6 hours;Two level heat treatment temperature is
520 DEG C, 3 hours.The final magnetic property parameter of treated magnet is shown in Table No. 6 magnets in 1.
Table 1
Claims (10)
1. a kind of technical method being used to form hydride nano-particle face coat, which is characterized in that include the following steps:It is right
Magnet surface after heating sprays rare earth hydride surface coating treatment, and rare earth hydride surface coating treatment is containing dilute
Then the acetone colloidal solution of native nanometer hydride and binder forms rare earth hydride nanoparticle coating in magnet surface,
Rare earth nano hydride is at least one of Pr, Nd, Tb, Dy hydride.
2. a kind of technical method being used to form hydride nano-particle face coat described in accordance with the claim 1, feature
It is, then makes the hydride nano-particle of face coat be diffused into inside magnet to prepare high magnetic by heat treatment process
Performance sintered magnet.
3. a kind of technical method being used to form hydride nano-particle face coat described in accordance with the claim 1, feature
It is, it is desirable that the weight ratio percentage of hydride nano-particle face coat is 0.1-1%.
4. special according to a kind of technical method being used to form hydride nano-particle face coat as claimed in claim 1 or 2
Sign is that, with the mode of spraying, specific steps include:It is ready for forming rare earth hydride nanoparticle face coat first
Inorganic agent, inorganic agent is placed in spray gun pot, and be stirred continuously and be allowed to form suspension, it is ensured that the concentration in watering can is consistent;
Magnet after surface is polished is cleaned with anhydrous propanone, and air-heater drying after weighing, is heated on warm table, then closed
The magnet after heating is sprayed with spray gun in container, surface obtains certain thickness rare earth hydride nanoparticle layer, then
Weight is weighed, level-one heat treatment, time 2-6 hour, then at 450 DEG C -550 DEG C are carried out at a temperature of 650 DEG C -900 DEG C
At a temperature of carry out two level heat treatment, time 2-4 hour.
5. a kind of technical method being used to form hydride nano-particle face coat described in accordance with the claim 1, feature
It is, the concentration of inorganic agent middle rare earth hydride is 0.2-0.5g/ml, the mass percent 0.5%-5% of binder.
6. a kind of technical method being used to form hydride nano-particle face coat described in accordance with the claim 1, feature
It is, the range of the average particle diameter of rare earth hydride is between 10-500 nanometers;Can diffusion thickness more than 10cm
Magnet.
7. a kind of technical method being used to form hydride nano-particle face coat described in accordance with the claim 1, feature
It is, the preparation of rare earth hydride surface coating treatment:Rare earth hydride nanoparticle is dispersed in acetone etc. easily to wave
The colloidal solution formed in hair solvent, and adhesive is added in colloidal solution, adhesive PVP is formed and is hydrogenated for rare earth
The inorganic agent of object nano grain surface coating.
8. a kind of technical method being used to form hydride nano-particle face coat according to claim 7, feature
It is, further preferred PVP molecular chain lengths are different, PVP model PVP k15-PVP k60;Further preferably in rare earth hydrogen
Between 10-500 nanometers of the average particle diameter of compound, as rare earth hydride average particle diameter increases, PVP models increase.
9. a kind of technical method being used to form hydride nano-particle face coat described in accordance with the claim 1, feature
It is, using spraying, small-sized agitating device is installed in watering can and is stirred continuously, uniform suspension is made to be sprayed by spray gun;Polishing
Magnet afterwards is cleaned with anhydrous propanone, and air-heater drying puts on a metal plate, is placed on warm table is heated to 80-120 together
DEG C, time 2-5 minute.
10. a kind of technical method being used to form hydride nano-particle face coat described in accordance with the claim 1, feature
It is, spray treatment is carried out in closed container to the magnet after heating, the operating distance of spray gun and magnet is 8-15cm, spray
Rifle pressure is 0.2-0.5MPa, and the air extractor of closed container side is opened after spraying, so that air is flowed and is recycled by end
Anhydrous propanone, while making the powder rapid precipitation in closed container and recycling.
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CN109926297A (en) * | 2019-04-09 | 2019-06-25 | 江西理工大学 | A kind of preparation method of low heavy rare earth performance Nd Fe B sintered magnet |
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Application publication date: 20180828 Assignee: GANZHOU FORTUNE ELECTRONIC Ltd. Assignor: Beijing University of Technology Contract record no.: X2023990000051 Denomination of invention: A technology for forming surface coating of hydride nanoparticles Granted publication date: 20200522 License type: Common License Record date: 20230106 |