CN101901657B - Sintered NdFeB (neodymium iron boron) permanent magnet material and preparation method thereof - Google Patents
Sintered NdFeB (neodymium iron boron) permanent magnet material and preparation method thereof Download PDFInfo
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- CN101901657B CN101901657B CN2009101076492A CN200910107649A CN101901657B CN 101901657 B CN101901657 B CN 101901657B CN 2009101076492 A CN2009101076492 A CN 2009101076492A CN 200910107649 A CN200910107649 A CN 200910107649A CN 101901657 B CN101901657 B CN 101901657B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
- H01F1/0575—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
- H01F1/0577—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F3/087—Compacting only using high energy impulses, e.g. magnetic field impulses
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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
- H01F41/0266—Moulding; Pressing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/10—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure
- H01F1/11—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure in the form of particles
Abstract
The invention provides an NdFeB (neodymium iron boron) permanent magnet material, which contains an NdFeB alloy and a cobalt ferrite. The invention also provides a method for preparing the NdFeB permanent magnet material. The method comprises the following steps of: performing magnetic field-oriented compression moulding on a mixture of the NdFeB alloy and the cobalt ferrite; and sintering and tempering the mixture under the condition of vacuum or inert gas protection so as to obtain the NdFeB permanent magnet material. The method can prepare a sintered NdFeB permanent magnet material which has the advantages of corrosion resistance and high working temperature.
Description
Technical field
The invention relates to a kind of sintered Nd-Fe-B permanent magnetic material and preparation method thereof.
Background technology
The eighties of last century the eighties, the SUMITOMO CHEMICAL metal company has been invented Nd-Fe-Bo permanent magnet material first.Since coming out, Nd-Fe-Bo permanent magnet material has been widely used in various fields such as automobile, computer, electronics, machinery, the energy, medicine equipment owing to have advantages such as high energy product, high-coercive force, cheap relatively price and sufficient resources deposit.Therefore particularly neodymium iron boron has the very high ratio of performance to price, becomes to make that usefulness is high, volume is little, the ideal material of the magnetic function device of light weight, and many applications are produced revolutionary impacts.But continuous expansion and technological progress along with application.Performance requirement to permanent magnetic material raises day by day, aspects such as working temperature, corrosion resistance.
Because Nd-Fe-Bo permanent magnet material itself comprises highly reactive rare earth element; Institute is so that neodymium iron boron is easy to oxidized and in environment, be corroded; And in the situation about under not using any surface treatment, using; Corrosion trends towards carrying out from the surface when a spot of acidity or alkaline matter or water exist, and produces corrosion, and this can cause the degeneration of magnetic and passive.In addition, be embedded in the situation of magnetic circuit and similar device iron rust diffusion, the assembly around may polluting at this magnet that gets rusty.Simultaneously, because the Curie temperature of sintered NdFeB has only 310 ℃, temperature coefficient is bigger; The temperature coefficient of remanent magnetism is generally-0.09～-0.12%; The ratio of the percentage of the reversible variation of residual magnetic flux density and the variations in temperature number of degrees is called the remanence temperature coefficient when changing within the specific limits, and the remanent magnetism temperature coefficient is big more; The resistance to elevated temperatures that shows material is good more, and common magnetic material generally can only worked below 160 ℃.So along with the demand of rare-earth permanent magnet at automobile starter motor, motor in electric automobile etc. increases, to the new challenge of high temperature resistant and decay resistance proposition of permanent magnet.
A kind of technical scheme that improves the sintered Nd-Fe-B permanent magnetic material decay resistance is disclosed in the prior art; This method comprises Nd Fe B alloys powder and the 4at% that accounts for the sintered NdFeB powder; Make mixed-powder, then mixed-powder is pressed under the condition that protective gas exists, sintering magnetizes then; The interpolation that obtains the sintered Nd-Fe-B permanent magnetic material of cobalt; Though this sintered Nd-Fe-B permanent magnetic material has improved the decay resistance of permanent magnet, this permanent magnetic material non-refractory, working temperature has only 170 ℃.
Summary of the invention
Technical problem to be solved by this invention is to overcome the permanent magnetic material corrosion resistance that exists in the prior art, the shortcoming that heat-resisting quantity can improve simultaneously; A kind of corrosion resistance and good that has is provided, sintered Nd-Fe-B permanent magnetic material that resistance to elevated temperatures is good and preparation method thereof.
To achieve these goals, the invention provides a kind of sintered Nd-Fe-B permanent magnetic material, this permanent magnetic material contains Nd Fe B alloys and Conjugate ferrite.
The present invention also provides a kind of preparation method of Nd-Fe-Bo permanent magnet material; This method comprises that the mixture with Nd Fe B alloys and Conjugate ferrite carries out magnetic field orientating compression moulding; Under the condition of vacuum or inert gas shielding, carry out sintering and tempering then, obtain Nd-Fe-Bo permanent magnet material.
The sintered Nd-Fe-B permanent magnetic material that Nd-Fe-Bo permanent magnet material preparation method provided by the invention can make, corrosion resistance and good, and can be high temperature resistant.
Embodiment
Nd-Fe-Bo permanent magnet material provided by the invention contains Nd Fe B alloys and Conjugate ferrite.
The inventor is through a large amount of experiments; Find through interpolation Conjugate ferrite particle, and make them be evenly distributed on the crystal boundary place of neodymium iron boron, can suppress the overgrowth of neodymium iron boron crystal grain and domain size; It is pinning effect; Thereby effectively improve working temperature, the interpolation itself of cobalt element simultaneously just can generate stable intergranular additional tissue with neodymium, increases corrosion resistance and has the sintered Nd-Fe-B permanent magnetic material than elevated operating temperature simultaneously.The present invention is because reduced the content of heavy metal cobalt when adding the nanometer Conjugate ferrite to a certain extent than normal the interpolation; Reduced cost; And an amount of oxygen can improve the anti-resistance to elevated temperatures of permanent magnetic material in the Conjugate ferrite; Simultaneously because the existence of Conjugate ferrite makes the decay resistance of sintered Nd-Fe-B permanent magnetic material improve greatly.
Wherein, in the present invention, the content of Conjugate ferrite is the 0.1-20% weight % of said Nd Fe B alloys, is preferably 0.5-10%.
And the Nd Fe B alloys of being mentioned among the present invention has following composition:
Nd
aRe
bFe
(100-a-b-c-d)B
cM
d，
Wherein, a, b, c, d represent atomic percentage.1≤a≤10,5≤b≤12,5≤d≤8,0≤d≤15, surplus are Fe, and Re is at least a element among Pr, Dy, Tb, Ho, Gd, La, Ce, the Y, and M is selected among Co, Al, Cu, Zr, Ga, Nb, the Mo one or more.
Said interpolation Conjugate ferrite is dispersed in the material of main part, and the general formula of described Conjugate ferrite is Co
nFe
3-nO
4Wherein the n value is 0.1～2.0 arbitrary value.
Said Conjugate ferrite average particulate diameter is preferably the 20-60 nanometer.Make the evengranular crystal boundary place that is distributed in the neodymium iron boron principal phase of Conjugate ferrite through suitable technology, so that form pinning effect.And the content of cobalt can not surpass 20% of sintered NdFeB total weight, can cause coercitive serious decline if surpass.
To achieve these goals, the present invention also provides a kind of method for preparing sintered Nd-Fe-B permanent magnet, and this method comprises: the preparation alloy cast ingot, and wherein, this alloy cast ingot comprises Nd Fe B alloys, and this alloy cast ingot is ground into powder; Add cobalt ferrite powder, be orientated this powder in the outside magnetic field, and mixed powder compaction is become block pressed compact, under the condition of vacuum or inert gas shielding, carry out sintering and tempering then, obtain Nd-Fe-Bo permanent magnet material.
The technological process of adopting sintering process to make Nd-Fe-Bo permanent magnet material generally has prescription, melting, fragmentation, powder process, the compression moulding of magnetic orientation, vacuum-sintering, machine work and plating.Among the present invention after powder process, before the compression moulding of magnetic orientation, need Nd Fe B alloys powder and cobalt ferrite powder are mixed.
Concrete steps are following:
1) the broken and grinding with Nd Fe B alloys obtains the alloy material powder.The method that Nd Fe B alloys is broken can be quick-fried method of hydrogen or the method through crusher in crushing, and the method for said powder process can be processed the powder that average diameter is the 2-10 micron for through airflow milling or protective atmosphere ball milling abrasive material.
Said Nd Fe B alloys can be neodymium iron boron alloy of ingot and neodymium iron boron rapid hardening thin slice, can also can adopt casting technique to process the neodymium iron boron alloy of ingot through being purchased acquisition, or adopts rapid hardening thin slice technology to process neodymium iron boron rapid hardening thin slice, and its composition is:
Nd
aRe
bFe
(100-a-b-c-d)B
cM
d，
Wherein, a, b, c, d represent atomic percentage.1≤a≤10,5≤b≤12,5≤d≤8,0≤d≤15, surplus are Fe, and Re is at least a element among Pr, Dy, Tb, Ho, Gd, La, Ce, the Y, and M is selected among Co, Al, Cu, Zr, Ga, Nb, the Mo one or more.
The method that said casting technique is processed alloy of ingot is conventionally known to one of skill in the art; Can the alloy liquation after the melting be cast in the water-cooled copper mould; The neodymium iron boron alloy of ingot mainly constitutes with column crystal; Separated by rich neodymium phase thin layer between the column crystal, distance is about the 100-1500 micron between the adjacent rich neodymium phase layer.
The method that said rapid hardening thin slice technology is processed the rapid hardening thin slice is conventionally known to one of skill in the art; Can the alloy liquation after the melting be watered the copper roller rotating surface; About the rotational line speed 1-2 meter per second of copper roller surface; The alloy liquation cools off rapidly, form thickness between the 0.2-0.5 millimeter, the thin slice that differs in size of width, the brilliant width of thin slice cylindrical is the 5-25 micron.
Said is conventionally known to one of skill in the art through the broken method of hydrogen crushing furnace hydrogen, for example, and the Nd Fe B alloys that will have the unsalted surface rustless steel container of packing into; After vacuumizing; Charge into high-purity hydrogen, reach about an atmospheric pressure, after 20-30 minute, will hear that the cracker of alloy and the temperature of container raise; This is to form hydride behind the absorption hydrogen and explosion, vacuumizes dehydrogenase 12-10 hour at 400-600 ℃ then.
Said is conventionally known to one of skill in the art through disintegrating machine with neodymium iron boron alloy of ingot or the broken method of neodymium iron boron rapid hardening thin slice, for example adopts jaw crusher to carry out coarse crushing, carries out middle fragmentation through middle disintegrating machine then.
The method of said airflow milling powder process is conventionally known to one of skill in the art, utilizes air-flow that powder particle is accelerated to supersonic speed, makes it head-on collision each other and fragmentation.
2) this Nd Fe B alloys powder and Conjugate ferrite are mixed, obtain mixed-powder.
Said Conjugate ferrite should pass through dispersion treatment earlier, and addition is the 0.5-10% of neodymium iron boron main body powder total weight.The average particle diameter of Conjugate ferrite is the 10-150 nanometer, and ferritic average particulate diameter is the 20-60 nanometer under the preferable case.
Under preferable case, said preparation process of mixture comprises mixes Nd Fe B alloys and Conjugate ferrite in the presence of oxidation inhibitor, perhaps Nd Fe B alloys and Conjugate ferrite are mixed in the presence of oxidation inhibitor and lubricant; The consumption of said oxidation inhibitor is the 0.1-5 weight % of said material of main part, and the consumption of said lubricant is the 0-5 weight % of said material of main part.The not special restriction of said oxidation inhibitor; The kind of oxidation inhibitor and usage are conventionally known to one of skill in the art; As can be in polyethylene oxide alkyl ethers, PEO list fatty ester, the PEO alkylene ether one or more, can be to foreignize the oxidation inhibitor that the worker produces deeply particularly.The not special restriction of said lubricant, the kind of lubricant and usage are conventionally known to one of skill in the art, as being in gasoline, oleic acid, stearic acid, polyalcohol and polyethylene glycol, anhydro sorbitol, the tristerin one or more.
The mode of said mixing is conventionally known to one of skill in the art, can in batch mixer, evenly mix.
3) with the mixed-powder magnetic field orientating compression moulding that obtains, obtain parison spare.
With the method for mixed-powder compression moulding blank in magnetic field is conventional method, under the preferable case, in the magnetic field orientating moulding press, is compressed to parison spare, and condition does, moulding alignment magnetic field 1.2-3T, and moulded blank is through waiting static pressure 10-200 MPa compacting 10-60 second.Further increase the degree of orientation that magnetic can be improved in magnetic field.The compression moulding of parison spare is accomplished in the glove box of sealing fully, makes the magnetic air-isolation, has avoided on the one hand the danger of catching fire because of magnet oxidation heating, has reduced the oxygen content of final magnet on the other hand again.
4) parison spare is carried out sintering and tempering under the condition of vacuum or inert gas shielding, make Nd-Fe-Bo permanent magnet material.
The method of sintering and tempering is a conventional method; Under the preferable case, with parison spare under the condition of vacuum or inert gas shielding 1030-1120 ℃ sintering 2-8 hour, passed through again 800-920 ℃ of tempering heat treatment 1-3 hour; Through 500-650 ℃ of tempering 2-4 hour, make sintered Nd-Fe-B permanent magnetic material again.Carry out the tempering second time and can further improve coercive force.Because the fusing point of said Conjugate ferrite is all more than 1200 ℃, therefore, when said temperature sintering, said Conjugate ferrite can not decompose and melt.
Said inert gas can be any gas of not participating in reacting, and is preferably one or more of helium, argon gas, neon, krypton gas, xenon.
Embodiment 1
This embodiment is used to explain Nd-Fe-Bo permanent magnet material provided by the present invention and preparation method thereof.
1) Nd Fe B alloys adopts rapid hardening thin slice technology, and copper roller linear resonance surface velocity is 1.5 meter per seconds, and composition is (PrNd)
10.61Dy
3.5Fe
77.55B
5.87Co
1.68Al
0.5Cu
0.16Ga
0.13(a%), get rid of strap thickness and be about 0.3 millimeter.
2) broken through hydrogen crushing furnace hydrogen, inhale hydrogen under the room temperature to saturated, the hydrogen flour was processed in 550 ℃ of dehydrogenations in 6 hours, then under nitrogen protection the employing airflow milling to process average particulate diameter be 3.5 microns powder.
3) with average particulate diameter be the CoFe of 50 nanometers
2O
4Add in the Nd Fe B alloys powder, and add oxidation inhibitor (foreignizing the worker deeply produces).The consumption of Conjugate ferrite is 1% of a Nd Fe B alloys powder weight, and the consumption that oxidation inhibitor gathers is to account for 0.5% of Nd Fe B alloys powder weight.
4) in being full of the glove box of nitrogen, mixed powder is pressed into blank through Magnetic field press, the moulding alignment magnetic field is 1.6T, and pressure is 100 MPas, and the press time is 30 seconds.
5) to put into vacuum degree be 2 * 10 to the blank after the compacting
-2Sintering in the vacuum sintering furnace of handkerchief, 1080 ℃ of following sintering 3 hours, again through 850 ℃ of tempering heat treatment 2 hours, and 500 ℃ of double temperings 3 hours, make Nd-Fe-Bo permanent magnet material T1.
Comparative Examples 1
This Comparative Examples is not added the nanometer Conjugate ferrite, and all the other technologies and embodiment 1 are just the same, make Nd-Fe-Bo permanent magnet material CT1.
Embodiment 2
This embodiment is used to explain Nd-Fe-Bo permanent magnet material provided by the present invention and preparation method thereof.
Carry out according to embodiment 1, different is the Co of employing
2Fe
1O
4Conjugate ferrite in the Conjugate ferrite alternative embodiment 1, and the addition of Conjugate ferrite to account for Nd Fe B alloys powder weight be 5%.Make Nd-Fe-Bo permanent magnet material T2.
Embodiment 3
This embodiment is used to explain Nd-Fe-Bo permanent magnet material provided by the present invention and preparation method thereof.
Carry out according to embodiment 1, that different is CoFe
2O
4Average particulate diameter be that 100 nanometers make Nd-Fe-Bo permanent magnet material T3.
Embodiment 4
This embodiment is used to explain Nd-Fe-Bo permanent magnet material provided by the present invention and preparation method thereof.
Carry out according to embodiment 1, that different is CoFe
2O
4Consumption be 10 weight % of Nd Fe B alloys, make Nd-Fe-Bo permanent magnet material T4.
Comparative Examples 2
This embodiment is used to explain Nd-Fe-Bo permanent magnet material provided by the present invention and preparation method thereof.
Prepare sample T5 according to embodiment 1 described method, different is that the Conjugate ferrite among the embodiment 1 is replaced with Co, and wherein, the Co average particulate diameter is 50 nanometers, obtains Nd-Fe-Bo permanent magnet material CT2.
Embodiment 5-10
These embodiment are used to detect the Nd-Fe-Bo permanent magnet material T1-4 that adopts the present invention's preparation; And the Nd-Fe-Bo permanent magnet material CT1 of Comparative Examples 1-2 preparation, the magnetic property of CT2, adopt the permanent magnetic material different temperatures curve measurement system NIM200C of China National Measuring Science Research Inst. that test piece is carried out magnetic property and measure.
There are not preparation method's exclusive rights of implementing corresponding no antioxidant
Corrosion resistance test
With the Nd-Fe-Bo permanent magnet material T1-4 of preparation, and the Nd-Fe-Bo permanent magnet material of Comparative Examples 1-2 preparation to process diameter be 10mm, length is the cylindrical sample of 7mm; Carry out the HAST test at the unsaturated accelerated life test machine of the HAS-70CP of Terchy Environmental Technology Ltd. type; Experimental condition is 130 ℃, humidity 95%, steam pressure 2.7bar; Time is 10 days, with T1-4 and CT1, CT2 loss magnet quality record in subordinate list.
The maximum operating temperature test
Nd-Fe-Bo permanent magnet material T1-4 with preparation; And CT1, CT2 to process diameter be 10mm; Length is the cylindrical sample of 7mm, and the permanent magnetic material different temperatures curve measurement system NIM200C of employing China National Measuring Science Research Inst. from 60 ℃, is that unit gradually increase with 2 ℃ to test piece; Intrinsic demagnetization is bent by straight line when giving birth to a certain temperature, and the maximum operating temperature that reaches this NdFeB material is described.Test result is as shown in table 1:
Table 1
| Project | W Loss(mg/cm2) | Inflection temperature |
| T1 | 2.1 | 190℃ |
| T2 | 1.8 | 186℃ |
| T3 | 2.5 | 186℃ |
| T4 | 1.5 | 188℃ |
| T5 | 2.0 | 182℃ |
| CT1 | 8.2 | 160℃ |
| CT2 | 2.7 | 170℃ |
From table 1, can find out; The loss magnet quality of the sintered Nd-Fe-B permanent magnetic material sample T1 of embodiment 1 preparation that is provided among the present invention is 2.1; And the loss magnet quality of the CT2 of preparation is 2.7 in the Comparative Examples 2, and the inflection temperature of T1 is 190 ℃, and the inflection temperature of CT2 is 170 ℃; This shows that sintered Nd-Fe-B permanent magnetic material provided by the present invention has corrosion resistance and good, the advantage that resistance to elevated temperatures is good.
Claims (10)
1. sintered Nd-Fe-B permanent magnetic material, this permanent magnetic material contains Nd Fe B alloys and Conjugate ferrite, and wherein, the content of said Conjugate ferrite is the 0.5-10 weight % of said Nd Fe B alloys.
2. sintered Nd-Fe-B permanent magnetic material according to claim 1, wherein, the average particulate diameter of said Conjugate ferrite is the 10-150 nanometer.
3. sintered Nd-Fe-B permanent magnetic material according to claim 1, wherein, said Conjugate ferrite is Co
nFe
3-nO
4, wherein the n value is 0.1～2.0 arbitrary value.
4. sintered Nd-Fe-B permanent magnetic material according to claim 1, wherein, said Nd Fe B alloys has the composition shown in the following formula:
Nd
aRe
bFe
(100-a-b-c-d)B
cM
d
Wherein, a, b, c, d represent atomic percentage, 1≤a≤10; 5≤b≤12,5≤c≤8,0≤d≤15; Surplus is Fe, and Re is at least a element among Pr, Dy, Tb, Ho, Gd, La, Ce, the Y, and M is selected among Co, Al, Cu, Zr, Ga, Nb, the Mo one or more.
5. the preparation method of the described sintered Nd-Fe-B permanent magnetic material of claim 1; This method comprises carries out magnetic field orientating compression moulding with the mixture that contains Nd Fe B alloys and Conjugate ferrite; Under the condition of vacuum or inert gas shielding, carry out sintering and tempering then; Obtain Nd-Fe-Bo permanent magnet material; Wherein, the preparation process of mixture of said Nd Fe B alloys and Conjugate ferrite comprises Nd Fe B alloys and Conjugate ferrite is being mixed in the presence of the oxidation inhibitor or in the presence of oxidation inhibitor and lubricant; The consumption of said oxidation inhibitor is the 0.1-5 weight % of said Nd Fe B alloys, and the consumption of said lubricant is the 0-5 weight % of said Nd Fe B alloys.
6. according to the preparation method of the said sintered Nd-Fe-B permanent magnetic material of claim 5, wherein, the consumption of said Conjugate ferrite is the 0.5-10 weight % of said Nd Fe B alloys.
7. the preparation method of sintered Nd-Fe-B permanent magnetic material according to claim 5, wherein, said Conjugate ferrite is Co
nFe
3-nO
4Wherein the n value is 0.1～2.0 arbitrary value.
8. the preparation method of sintered Nd-Fe-B permanent magnetic material according to claim 5, wherein, said Nd Fe B alloys has the composition shown in the following formula:
Nd
aRe
bFe
(100-a-b-c-d)B
cM
d
Wherein, a, b, c, d represent atomic percentage, 1≤a≤10; 5≤b≤12,5≤c≤8,0≤d≤15; Surplus is Fe, and Re is at least a element among Pr, Dy, Tb, Ho, Gd, La, Ce, the Y, and M is selected among Co, Al, Cu, Zr, Ga, Nb, the Mo one or more.
9. the preparation method of sintered Nd-Fe-B permanent magnetic material according to claim 5, wherein, the average particulate diameter of said Conjugate ferrite is the 10-150 nanometer, the average particulate diameter of said Nd Fe B alloys is the 2-5 micron.
10. the preparation method of sintered Nd-Fe-B permanent magnetic material according to claim 5, wherein, the condition of said magnetic field orientating compression moulding comprises that magnetic field intensity is 1.2-3.0T, and pressure is the 10-200 MPa, and the press time is 10-60 second; The condition of said sintering comprises that sintering temperature is 1030-1120 ℃, and sintering time is 2-8 hour; Said tempering comprises double tempering, and the condition of tempering for the first time comprises that temperature is 800-920 ℃, and tempering time is 1-3 hour; Tempered condition comprises that temperature is 500-650 ℃ for the second time, and tempering time is 2-4 hour.
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101076492A CN101901657B (en) | 2009-05-27 | 2009-05-27 | Sintered NdFeB (neodymium iron boron) permanent magnet material and preparation method thereof |
| EP10780039.3A EP2436016B1 (en) | 2009-05-27 | 2010-05-17 | Nd-fe-b permanent magnetic material and preparation method thereof |
| PCT/CN2010/072854 WO2010135958A1 (en) | 2009-05-27 | 2010-05-17 | Nd-fe-b permanent magnetic material and preparation method thereof |
| US13/319,674 US20120058003A1 (en) | 2009-05-27 | 2010-05-17 | Nd-Fe-B PERMANENT MAGNETIC MATERIAL AND PREPARATION METHOD THEREOF |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101076492A CN101901657B (en) | 2009-05-27 | 2009-05-27 | Sintered NdFeB (neodymium iron boron) permanent magnet material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101901657A CN101901657A (en) | 2010-12-01 |
| CN101901657B true CN101901657B (en) | 2012-06-20 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2009101076492A Active CN101901657B (en) | 2009-05-27 | 2009-05-27 | Sintered NdFeB (neodymium iron boron) permanent magnet material and preparation method thereof |
Country Status (4)
| Country | Link |
|---|---|
| US (1) | US20120058003A1 (en) |
| EP (1) | EP2436016B1 (en) |
| CN (1) | CN101901657B (en) |
| WO (1) | WO2010135958A1 (en) |
Families Citing this family (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101853723B (en) | 2009-03-31 | 2012-11-21 | 比亚迪股份有限公司 | Composite magnetic material and preparation method thereof |
| CN102228760A (en) * | 2011-06-29 | 2011-11-02 | 无锡光旭新材料科技有限公司 | Permanent magnet filter stick and method for preparing permanent magnet material thereof |
| CN102361359B (en) * | 2011-11-04 | 2015-02-11 | 无锡天宝电机有限公司 | Corrosion-resistant neodymium iron boron permanent magnet for motor |
| CN102510176B (en) * | 2011-11-04 | 2014-11-26 | 无锡天宝电机有限公司 | Preparation method of heat-proof Nd-Fe-B permanent magnet for motor |
| CN102969111B (en) * | 2012-11-30 | 2015-09-30 | 钢铁研究总院 | Low-cost high-resistivity cerium magnet and preparation method thereof |
| CN102976738A (en) * | 2012-12-20 | 2013-03-20 | 南通万宝磁石制造有限公司 | Process for manufacturing permanent magnetic ferrite with high compression strength |
| CN105499557A (en) * | 2016-01-28 | 2016-04-20 | 河南中硬合金有限公司 | Hard alloy large-product holding-up hammer multi-component forming agent and preparation method |
| CN105957674B (en) * | 2016-05-13 | 2018-09-14 | 桂林电子科技大学 | A kind of Nd-Ce-Pr-Fe-B alloy thin band permanent-magnet materials of high-coercive force and preparation method thereof |
| CN106373688B (en) * | 2016-08-31 | 2019-03-29 | 浙江东阳东磁稀土有限公司 | A method of preparing rare earth permanent-magnetic material |
| RU2642508C1 (en) * | 2016-11-21 | 2018-01-25 | федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский ядерный университет "МИФИ" (НИЯУ МИФИ) | METHOD FOR PRODUCING HIGH-COERCIVITY MAGNETS FROM ALLOYS ON BASIS OF Nd-Fe-B |
| CN106747392B (en) * | 2017-03-03 | 2019-12-06 | 中国地质大学（北京） | Preparation method of Ho/Co composite doped Ni-Zn ferrite ceramic |
| CN107931598A (en) * | 2017-11-16 | 2018-04-20 | 浙江中杭新材料科技有限公司 | The preparation method of hybrid exciting synchronous motor magnet steel |
| CN107931621A (en) * | 2017-11-16 | 2018-04-20 | 浙江中杭新材料科技有限公司 | The preparation method of high temperature resistant synchronous motor magnet steel |
| RU2690867C1 (en) * | 2018-12-13 | 2019-06-06 | Акционерное общество "Научно-производственное объединение "Магнетон" | Mixture for producing thermostable magnetic alloys with rare-earth metals based on nd-fe-b system |
| CN110491614B (en) * | 2019-08-21 | 2022-06-24 | 南通成泰磁材科技有限公司 | Magnetic material with high compressive strength and preparation method thereof |
| CN110534281A (en) * | 2019-09-27 | 2019-12-03 | 江苏南方永磁科技有限公司 | A kind of permanent-magnet material and preparation method thereof |
| CN110571008A (en) * | 2019-09-27 | 2019-12-13 | 江苏南方永磁科技有限公司 | Magnetic composite material and preparation method thereof |
| CN112750586B (en) * | 2020-12-28 | 2024-03-29 | 包头稀土研究院 | Mixed rare earth sintered NdFeB permanent magnet and preparation method thereof |
| CN112863844A (en) * | 2021-03-24 | 2021-05-28 | 陈凯华 | Preparation process of corrosion-resistant neodymium iron boron magnet |
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| JP2005159054A (en) * | 2003-11-26 | 2005-06-16 | Tdk Corp | Method of manufacturing r-t-b-based permanent magnet |
| CN1688000A (en) * | 2005-06-06 | 2005-10-26 | 浙江大学 | Method for increasing sintering Nd-Fe-B coercive force by adding nano-oxide in crystal boundary phase |
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| JP3604853B2 (en) * | 1996-03-29 | 2004-12-22 | 株式会社Ｎｅｏｍａｘ | Manufacturing method of anisotropic bonded magnet |
| JP2002164205A (en) * | 2000-09-12 | 2002-06-07 | Hitachi Metals Ltd | Composite bonded magnet, rotating machine, and magnet roll |
| US6721144B2 (en) * | 2001-01-04 | 2004-04-13 | International Business Machines Corporation | Spin valves with co-ferrite pinning layer |
| US8465453B2 (en) * | 2003-12-03 | 2013-06-18 | Mayo Foundation For Medical Education And Research | Kits, apparatus and methods for magnetically coating medical devices with living cells |
| US20100261038A1 (en) * | 2007-11-02 | 2010-10-14 | Nobuyoshi Imaoka | Composite magnetic material for magnet and method for manufacturing such material |
-
2009
- 2009-05-27 CN CN2009101076492A patent/CN101901657B/en active Active
-
2010
- 2010-05-17 EP EP10780039.3A patent/EP2436016B1/en active Active
- 2010-05-17 US US13/319,674 patent/US20120058003A1/en not_active Abandoned
- 2010-05-17 WO PCT/CN2010/072854 patent/WO2010135958A1/en active Application Filing
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005159054A (en) * | 2003-11-26 | 2005-06-16 | Tdk Corp | Method of manufacturing r-t-b-based permanent magnet |
| CN1688000A (en) * | 2005-06-06 | 2005-10-26 | 浙江大学 | Method for increasing sintering Nd-Fe-B coercive force by adding nano-oxide in crystal boundary phase |
Also Published As
| Publication number | Publication date |
|---|---|
| EP2436016A4 (en) | 2012-10-31 |
| EP2436016B1 (en) | 2017-03-29 |
| WO2010135958A1 (en) | 2010-12-02 |
| US20120058003A1 (en) | 2012-03-08 |
| EP2436016A1 (en) | 2012-04-04 |
| CN101901657A (en) | 2010-12-01 |
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