CN107564723A - The preparation method of high-coercive force neodymium iron boron magnetic body - Google Patents
The preparation method of high-coercive force neodymium iron boron magnetic body Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of high-coercive force neodymium iron boron magnetic body, by by a certain amount of Dy82.3Co17.7Alloy powder is dissolved in appropriate solvent, and then magnet is dipped in the solution, and one layer of Dy is coated in magnet surface82.3Co17.7Alloy-layer, then it is heat-treated, is finally made high-coercive force neodymium iron boron magnetic body.Significantly improved by neodymium iron boron magnetic body coercivity made of the preparation method, and heavy rare earth utilization rate is higher, compared with preparing the magnet of equal performance, reduces cost and the consumption of raw material.
Description
Technical field
The present invention relates to magnetic material preparing technical field, more particularly to a kind of preparation side of high-coercive force neodymium iron boron magnetic body
Method.
Background technology
Sintered NdFeB magnet is because the premium properties such as its high saturated magnetic induction, high-coercive force and high energy product are in wind-force
Generating, satellite communication, communications and transportation, medical treatment and health and fitness facilities etc. are used widely, and are especially led in hybrid vehicle
Domain, the demand sharp increase of Sintered NdFeB magnet.But the Curie temperature of sintering Sintered NdFeB magnet is not high, only
312 DEG C, worked under higher than 200 DEG C environment, it is easy to cause the high-temp magnetic performance degradation of magnet, influence motor uses the longevity
Life.To ensure motor normal work, it is desirable to which magnet must have the coercive higher than 2000KA/m (25kOe) at normal temperatures
Power.According to the literature, the coercivity of Sintered NdFeB magnet is controlled by Nucleation Mechanism, if each of crystal boundary near zone can be improved
Anisotropy field just can effectively suppress the formation of nuclei of reversed domain, so as to improve coercivity.
Heavy rare earth element terbium (Tb) and dysprosium (Dy) meet the requirements, and they can substitute principal phase Nd2Fe14After neodymium (Nd) in B,
Generate cenotype (Nd, Dy)2Fe14B and (Nd, Tb)2Fe14B, its corresponding magnetocrystalline anisotropy field be respectively 17600KA/m and
12000KA/m, much larger than Nd2Fe14B anisotropy field 5600KA/m.Wherein heavy rare earth Tb is due to its very expensive former material
Expect that price is seldom applied to the large-scale production of Sintered NdFeB magnet, and relatively relatively inexpensive Dy elements can be used as research pair
As.But because Dy and Fe are that anti-ferromagnetism couples, being greatly reduced for magnet remanent magnetism can be caused using the method for conventional alloys, and
In view of melting scaling loss, it is necessary to which adding a large amount of Dy can be only achieved high-coercive force, the increase of magnet generation cost is caused.
Another method is that grain boundary structure optimization prepares high-coercive force neodymium iron boron magnetic body, generally Dy2O3、DyF3And DyHx
It is added to Deng powder by way of alloying in main phase grain and carries out mixing compacting, sintering and timeliness to prepare neodymium-iron-boron
Body, or coated in magnet surface, coercivity is improved by way of heat treatment.And Dy2O3、DyF3And DyHxThese chemical combination
The fusing point of thing is all of a relatively high, and under production temperature condition of heat treatment used, they are still unfused, are unfavorable for the sintering of magnet
Densification, be also unfavorable for heavy rare earth element crystal boundary circulation spread, in addition, the oxygen (O) that left behind in magnet, fluorine (F) and
Hydrogen (H) atom can also deteriorate the magnetic property of magnet.
The content of the invention
It is an object of the invention to solve at least the above, and provide the advantages of at least will be described later.
It is a still further object of the present invention to provide a kind of preparation method of high-coercive force neodymium iron boron magnetic body, by by neodymium iron boron
Magnet is placed in the Dy of configuration82.3Co17.7Ultrasound is coated and sintered in mixed solution so that manufactured neodymium iron boron magnetic body coercivity shows
Write and improve, and heavy rare earth utilization rate is higher, compared with preparing the magnet of equal performance, reduces cost and the consumption of raw material.
In order to realize according to object of the present invention and further advantage, there is provided following technical scheme:
A kind of preparation method of high-coercive force neodymium iron boron magnetic body, is mainly included the following steps that:
Step 1, the surface of neodymium iron boron magnetic body cleaned;
Step 2, by Dy82.3Co17.7Alloy powder 15-55g, alcohol 100-500ml and cosolvent 1-8g mixing, stirring are equal
It is even to obtain Dy82.3Co17.7Mixed solution;
Step 3, by step 1 clean after neodymium iron boron magnetic body be placed in the Dy82.3Co17.7In mixed solution, and coordinate super
Sound coating makes neodymium iron boron magnetic body surface form Dy82.3Co17.7Alloy-layer, and dry, obtain prefabricated high-coercive force neodymium iron boron magnetic body;
Step 4, the prefabricated high-coercive force neodymium iron boron magnetic body is placed in vacuum sintered, and carry out diffusion heat treatments, i.e.,
Obtain the high-coercive force neodymium iron boron magnetic body.
Preferably, in the preparation method of described high-coercive force neodymium iron boron magnetic body, to the table of neodymium iron boron magnetic body in step 1
The specific method that face is cleaned is:To the surface degreasing of neodymium iron boron magnetic body, rust and washing and drying.
Preferably, in the preparation method of described high-coercive force neodymium iron boron magnetic body,
Oil removing is carried out to the surface of neodymium iron boron magnetic body using alkali lye, the alkali lye is the carbon that mass concentration is 15-20g/L
Sour sodium, sodium hydroxide, the one or more of tertiary sodium phosphate press quality with mass concentration for 1-3g/L APES
Than for 1:1 mixed liquor being mixed to get;
The surface of neodymium iron boron magnetic body is derusted using rust removing solution, the rust removing solution is mass fraction 3-5% nitric acid
Solution.
Preferably, in the preparation method of described high-coercive force neodymium iron boron magnetic body, the temperature of the alkali liquor oil removing is 50-
60 DEG C, the oil removing time is 80-100s;The derusting time of the rust removing solution is 15-30s.
Preferably, in the preparation method of described high-coercive force neodymium iron boron magnetic body, Dy described in step 282.3Co17.7Close
Granularity≤the 100nm at bronze end;Mass fraction >=99.5% of the alcohol;The cosolvent is mass fraction >=99.8%
Polyethylene glycol 400 moisturizing solubilizer.
Preferably, in the preparation method of described high-coercive force neodymium iron boron magnetic body, the Dy82.3Co17.7Alloy powder
Preparation method is:The metallic cobalt melting acquisition in induction melting furnace for being 99.9% by rare earth dysprosium and purity that purity is 99.9%
Dy82.3Co17.7Alloy cast ingot, then carry out hydrogen and crush, and the high-energy ball milling under ethanol medium protection, produce described
Dy82.3Co17.7Alloy powder.
Preferably, in the preparation method of described high-coercive force neodymium iron boron magnetic body, the time that ultrasound coats in step 3 is
3-10min。
Preferably, in the preparation method of described high-coercive force neodymium iron boron magnetic body, drying temperature is described in step 3
80-100 DEG C, drying time 15-30min.
Preferably, in the preparation method of described high-coercive force neodymium iron boron magnetic body, diffusion heat treatments bag described in step 4
Include one-level temper and second annealing processing;
Wherein, the temperature of the one-level temper is 800-950 DEG C, soaking time 3-5h;At the second annealing
The temperature of reason is 450-650 DEG C, soaking time 2-4h.
The present invention comprises at least following beneficial effect:
The present invention is by by a certain amount of Dy82.3Co17.7Alloy powder is dissolved in appropriate solvent, is then dipped in magnet
In the solution, one layer of Dy is coated in magnet surface82.3Co17.7Alloy-layer, then it is heat-treated so that manufactured neodymium-iron-boron
The coercivity of body significantly improves, and heavy rare earth utilization rate is higher, compared with preparing the magnet of equal performance, reduces raw material
Cost and consumption.
The present invention chooses the Dy of low melting point82.3Co17.7Alloy, in the case where not introducing the nonmagnetic elements such as hydrogen, oxygen, fluorine
Promote effective diffusion of Dy elements.In heat treatment process, the Dy coated in magnet top layer82.3Co17.7Alloy can diffuse into magnetic
Surface layer region, the heavy rare earth element in coat can be diffused into inside magnet, the common microstructure for improving magnet and excellent
Change the border structure of magnetic phase, reach and improve coercitive purpose.
Further advantage, target and the feature of the present invention embodies part by following explanation, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Embodiment
The present invention is described in further detail below, to make those skilled in the art being capable of evidence with reference to specification word
To implement.
It should be appreciated that such as " having ", "comprising" and " comprising " term used herein do not allot one or more
The presence or addition of individual other elements or its combination.
A kind of preparation method of high-coercive force neodymium iron boron magnetic body, is mainly included the following steps that:
Step 1, the surface of neodymium iron boron magnetic body cleaned.
Step 2, by Dy82.3Co17.7Alloy powder 15-55g, alcohol 100-500ml and cosolvent 1-8g mixing, stirring are equal
It is even to obtain Dy82.3Co17.7Mixed solution.
Step 3, by step 1 clean after neodymium iron boron magnetic body be placed in the Dy82.3Co17.7In mixed solution, and coordinate super
Sound coating makes neodymium iron boron magnetic body surface form Dy82.3Co17.7Alloy-layer, and dry, obtain prefabricated high-coercive force neodymium iron boron magnetic body.
Step 4, the prefabricated high-coercive force neodymium iron boron magnetic body is placed in vacuum sintered, and carry out diffusion heat treatments, i.e.,
Obtain the high-coercive force neodymium iron boron magnetic body.
In one preferred scheme, the specific method cleaned in step 1 to the surface of neodymium iron boron magnetic body is:To neodymium iron boron
Surface degreasing, rust and washing and the drying of magnet.
In one preferred scheme, oil removing is carried out to the surface of neodymium iron boron magnetic body using alkali lye, the alkali lye is mass concentration
It is the alkyl phenol of 15-20g/L sodium carbonate, sodium hydroxide, the one or more of tertiary sodium phosphate with mass concentration for 1-3g/L
APEO is 1 in mass ratio:1 mixed liquor being mixed to get.The surface of neodymium iron boron magnetic body is derusted using rust removing solution,
The rust removing solution is mass fraction 3-5% salpeter solution.
In one preferred scheme, the temperature of the alkali liquor oil removing is 50-60 DEG C, and the oil removing time is 80-100s;The derusting
The derusting time of liquid is 15-30s.
In one preferred scheme, Dy described in step 282.3Co17.7Granularity≤100nm of alloy powder;The matter of the alcohol
Measure fraction >=99.5%;The cosolvent is the polyethylene glycol 400 moisturizing solubilizer of mass fraction >=99.8%.
In one preferred scheme, the Dy82.3Co17.7The preparation method of alloy powder is:By the rare earth that purity is 99.9%
The metallic cobalt that dysprosium and purity are 99.9% melting in induction melting furnace obtains Dy82.3Co17.7Alloy cast ingot, then carry out hydrogen
It is broken, and the high-energy ball milling under ethanol medium protection, produce the Dy82.3Co17.7Alloy powder.
In one preferred scheme, the time of ultrasound coating is 3-10min in step 3.
In one preferred scheme, drying temperature described in step 3 is 80-100 DEG C, drying time 15-30min.
In one preferred scheme, diffusion heat treatments described in step 4 include one-level temper and second annealing is handled.
Wherein, the temperature of the one-level temper is 800-950 DEG C, soaking time 3-5h;At the second annealing
The temperature of reason is 450-650 DEG C, soaking time 2-4h.
Embodiment 1
A kind of preparation method of high-coercive force neodymium iron boron magnetic body, is mainly included the following steps that:
Step 1, from the Sintered NdFeB magnet (size D10*6mm) that the trade mark is 44H sample is used as, and to its surface
Cleaned.
Specifically clean method is:First, sample is placed in into ultrasonic 90s progress degreasing in the alkaline solution that temperature is 50 DEG C to remove
Oil, then using flowing clear water cleaning, untill last process residual solution cleans up.
Then, the sample after oil removing is put into ultrasonic 15s in the salpeter solution that mass fraction is 3% and removes removing rust and oxidation
Layer, then using flowing clear water cleaning, untill last process residual solution cleans up.
Finally, the neodymium iron boron magnetic body obtained after removing iron rust and oxide layer is put into ultrasonic tank and carries out ultrasonic washing,
The loose particle in surface and impurity are washed away, is dried up after taking-up with hair-dryer, obtains the Sintered NdFeB magnet of surface cleaning.
The component of wherein alkaline solution is:Mass concentration is 18g/L tertiary sodium phosphate, 18g/L sodium carbonate, 15g/L
The emulsifying agent APES OP-10 of sodium hydroxide and 2g/L, it is 0.33 according to mass ratio:0.33:0.33:1 mixing.
Step 2, the Dy by particle diameter for 80nm82.3Co17.7Alloy powder 20g, with the wine that 300ml mass fractions are 99.8%
Essence and the polyethylene glycol 400 (PEG-400) that 5g mass fractions are 99.9% mix, and are uniformly mixing to obtain Dy82.3Co17.7Mixing
Solution.
Step 3, by step 1 clean after sample be placed in the Dy82.3Co17.7In mixed solution, ultrasound coating 3min,
It is placed in toasting 15min in the drying box that temperature is 80 DEG C, obtains prefabricated high-coercive force neodymium iron boron magnetic body.
Step 4, the prefabricated high-coercive force neodymium iron boron magnetic body is placed in vacuum sintered, in 900 DEG C of insulation heat treatment 4h,
Argon gas is air-cooled to room temperature, then heats to 520 DEG C of insulation heat treatment 3h, argon gas is air-cooled to room temperature again, produces the high coercive
Power neodymium iron boron magnetic body.
Embodiment 2
A kind of preparation method of high-coercive force neodymium iron boron magnetic body, is mainly included the following steps that:
Step 1, from the Sintered NdFeB magnet (size D10*6mm) that the trade mark is 38SH sample is used as, and to its table
Cleaned in face.
Specifically clean method is:First, sample is placed in into ultrasonic 90s progress degreasing in the alkaline solution that temperature is 50 DEG C to remove
Oil, then using flowing clear water cleaning, untill last process residual solution cleans up.
Then, the sample after oil removing is put into ultrasonic 15s in the salpeter solution that mass fraction is 3% and removes removing rust and oxidation
Layer, then using flowing clear water cleaning, untill last process residual solution cleans up.
Finally, the neodymium iron boron magnetic body obtained after removing iron rust and oxide layer is put into ultrasonic tank and carries out ultrasonic washing,
The loose particle in surface and impurity are washed away, is dried up after taking-up with hair-dryer, obtains the Sintered NdFeB magnet of surface cleaning.
The component of wherein alkaline solution is:Mass concentration is 15g/L tertiary sodium phosphate, 15g/L sodium carbonate, 15g/L
The OP-10 of sodium hydroxide and 2g/L, it is 0.33 according to mass ratio:0.33:0.33:1 mixing.
Step 2, the Dy by particle diameter for 80nm82.3Co17.7Alloy powder 30g, with the wine that 380ml mass fractions are 99.7%
Essence and the polyethylene glycol 400 (PEG-400) that 6g mass fractions are 99.8% mix, and are uniformly mixing to obtain Dy82.3Co17.7Mixing
Solution.
Step 3, by step 1 clean after sample be placed in the Dy82.3Co17.7In mixed solution, ultrasound coating 5min,
It is placed in toasting 20min in the drying box that temperature is 80 DEG C, obtains prefabricated high-coercive force neodymium iron boron magnetic body.
Step 4, the prefabricated high-coercive force neodymium iron boron magnetic body is placed in vacuum sintered, in 900 DEG C of insulation heat treatment 4h,
Argon gas is air-cooled to room temperature, then heats to 570 DEG C of insulation heat treatment 3h, argon gas is air-cooled to room temperature again, produces the high coercive
Power neodymium iron boron magnetic body.
Comparative example 1
The uncoated direct tempering of 44H sintered state magnets prepared using conventional smelting technology, obtains No. 1 neodymium-iron-boron
Body.
Comparative example 2
The uncoated direct tempering of 42SH sintered state magnets prepared using conventional smelting technology, obtains No. 2 neodymium-iron-borons
Body.
Comparative example 3
The uncoated direct tempering of 38SH sintered state magnets prepared using conventional smelting technology, obtains No. 3 neodymium-iron-borons
Body.
Comparative example 4
The uncoated direct tempering of 35EH sintered state magnets prepared using conventional smelting technology, obtains No. 4 neodymium-iron-borons
Body.
No. 1 neodymium iron boron magnetic body and contrast that the high-coercive force neodymium iron boron magnetic body and comparative example 1 obtained to embodiment 1 obtains
No. 2 neodymium iron boron magnetic bodies that example 2 obtains carry out plasma spectrum Dy content analysis respectively, and lossless with NIM-10000H rare earth permanent magnets
Tester carries out magnetism testing, and test result is referring to table 1 below.
Heavy rare earth content and the magnetic property contrast of neodymium iron boron magnetic body prepared by the embodiment 1 of table 1 and comparative example 1,2
As shown in Table 1, contrasted with conventional smelting technology, for the neodymium iron boron magnetic body of the same trade mark, Dy82.3Co17.7Alloy-coated
For the neodymium iron boron magnetic body of preparation compared with No. 1 neodymium iron boron magnetic body that comparative example 1 obtains, its HCJ has significant raising,
And for using the trade mark prepared by conventional smelting technology as 42SH No. 2 neodymium iron boron magnetic bodies, the neodymium iron boron magnetic body that embodiment 1 obtains
While high remanent magnetism and magnetic energy product is maintained, the size of HCJ and No. 2 neodymium iron boron magnetic bodies also has essentially no difference, but
Compared in the equal coercitive smelting neodymium-iron-boron technique of manufacture, significantly reduce heavy rare earth Dy use content, effectively reduce
Production cost.
No. 3 neodymium iron boron magnetic bodies and contrast that the high-coercive force neodymium iron boron magnetic body and comparative example 3 obtained to embodiment 2 obtains
No. 4 neodymium iron boron magnetic bodies that example 4 obtains carry out plasma spectrum Dy content analysis respectively, and lossless with NIM-10000H rare earth permanent magnets
Tester carries out magnetism testing, and test result is referring to table 2 below.
Heavy rare earth content and the magnetic property contrast of neodymium iron boron magnetic body prepared by the embodiment 2 of table 2 and comparative example 3,4
As shown in Table 2, contrasted with conventional smelting technology, for the neodymium iron boron magnetic body of the same trade mark, Dy82.3Co17.7Alloy-coated
For the neodymium iron boron magnetic body of preparation compared with No. 3 neodymium iron boron magnetic bodies that comparative example 3 obtains, its HCJ has significant raising,
And for using the trade mark prepared by conventional smelting technology as 35EH No. 4 neodymium iron boron magnetic bodies, the neodymium iron boron magnetic body that embodiment 2 obtains
While high remanent magnetism and magnetic energy product is maintained, the size of HCJ and No. 4 neodymium iron boron magnetic bodies also has essentially no difference, but
Compared in the equal coercitive smelting neodymium-iron-boron technique of manufacture, significantly reduce heavy rare earth Dy use content, effectively reduce
Production cost.
Although embodiment of the present invention is disclosed as above, it is not restricted in specification and embodiment listed
With it can be applied to various suitable the field of the invention completely, can be easily for those skilled in the art
Other modification is realized, therefore under the universal limited without departing substantially from claim and equivalency range, it is of the invention and unlimited
In specific details.
Claims (9)
1. a kind of preparation method of high-coercive force neodymium iron boron magnetic body, wherein, mainly include the following steps that:
Step 1, the surface of neodymium iron boron magnetic body cleaned;
Step 2, by Dy82.3Co17.7Alloy powder 15-55g, alcohol 100-500ml and cosolvent 1-8g mixing, stir
To Dy82.3Co17.7Mixed solution;
Step 3, by step 1 clean after neodymium iron boron magnetic body be placed in the Dy82.3Co17.7In mixed solution, and coordinate ultrasonic painting
Covering makes neodymium iron boron magnetic body surface form Dy82.3Co17.7Alloy-layer, and dry, obtain prefabricated high-coercive force neodymium iron boron magnetic body;
Step 4, the prefabricated high-coercive force neodymium iron boron magnetic body is placed in vacuum sintered, and carry out diffusion heat treatments, produce institute
State high-coercive force neodymium iron boron magnetic body.
2. the preparation method of high-coercive force neodymium iron boron magnetic body as claimed in claim 1, wherein, to neodymium iron boron magnetic body in step 1
The specific method that is cleaned of surface be:To the surface degreasing of neodymium iron boron magnetic body, rust and washing and drying.
3. the preparation method of high-coercive force neodymium iron boron magnetic body as claimed in claim 2, wherein,
Oil removing is carried out to the surface of neodymium iron boron magnetic body using alkali lye, the alkali lye is the carbonic acid that mass concentration is 15-20g/L
Sodium, sodium hydroxide, tertiary sodium phosphate one or more with mass concentration be 1-3g/L APES in mass ratio
For 1:1 mixed liquor being mixed to get;
The surface of neodymium iron boron magnetic body is derusted using rust removing solution, the rust removing solution is mass fraction 3-5% salpeter solution.
4. the preparation method of high-coercive force neodymium iron boron magnetic body as claimed in claim 3, wherein, the temperature of the alkali liquor oil removing is
50-60 DEG C, the oil removing time is 80-100s;The derusting time of the rust removing solution is 15-30s.
5. the preparation method of high-coercive force neodymium iron boron magnetic body as claimed in claim 1, wherein, Dy described in step 282.3Co17.7
Granularity≤100nm of alloy powder;Mass fraction >=99.5% of the alcohol;The cosolvent is mass fraction >=99.8%
Polyethylene glycol 400 moisturizing solubilizer.
6. the preparation method of high-coercive force neodymium iron boron magnetic body as claimed in claim 5, wherein, the Dy82.3Co17.7Alloyed powder
End preparation method be:The metallic cobalt melting in induction melting furnace for being 99.9% by rare earth dysprosium and purity that purity is 99.9%
Obtain Dy82.3Co17.7Alloy cast ingot, then carry out hydrogen and crush, and the high-energy ball milling under ethanol medium protection, produce described
Dy82.3Co17.7Alloy powder.
7. the preparation method of high-coercive force neodymium iron boron magnetic body as claimed in claim 1, wherein, in step 3 ultrasound coating when
Between be 3-10min.
8. the preparation method of high-coercive force neodymium iron boron magnetic body as claimed in claim 1, wherein, drying temperature described in step 3
For 80-100 DEG C, drying time 15-30min.
9. the preparation method of high-coercive force neodymium iron boron magnetic body as claimed in claim 1, wherein, described in step 4 at diffusion heat
Reason includes one-level temper and second annealing processing;
Wherein, the temperature of the one-level temper is 800-950 DEG C, soaking time 3-5h;The second annealing processing
Temperature is 450-650 DEG C, soaking time 2-4h.
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XIAOFENG ZHANG ET.AL: "Improvement of the thermal stability of sintered Nd-Fe-B magnets by intergranular addition of Dy82.3Co17.7", 《JOURNAL OF APPLIED PHYSICS》 * |
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Application publication date: 20180109 |