CN103122418B - A kind of α of elimination-Fe prepares the method for high performance sintered neodymium-iron-boron - Google Patents
A kind of α of elimination-Fe prepares the method for high performance sintered neodymium-iron-boron Download PDFInfo
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- CN103122418B CN103122418B CN201310045392.9A CN201310045392A CN103122418B CN 103122418 B CN103122418 B CN 103122418B CN 201310045392 A CN201310045392 A CN 201310045392A CN 103122418 B CN103122418 B CN 103122418B
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Abstract
The present invention relates to a kind of method that the α of elimination-Fe prepares high performance sintered neodymium-iron-boron, it is characterized in that, prepare main and auxiliary two kinds of alloys, respectively through melting, fragmentation, powder process.At master alloying crushing process, by the powder of rich α-Fe and qualified powder separation.Then auxiliary alloy to be added in auxiliary alloy according to the weight ratio of the 3-20% of master alloying and mix, then preparing neodymium iron boron magnetic body through die mould, sintering timeliness.
Description
Technical field
The present invention relates to field of powder metallurgy, particularly relate to a kind of method that the α of elimination-Fe prepares high performance sintered neodymium-iron-boron.
Background technology
Neodymium iron boron a kind ofly has high magnetic energy product and coercitive rareearth magnetic material, the advantage of high-energy-density makes neodymium-iron-boron magnetic material obtain a wide range of applications in modern industry and electronic technology simultaneously, thus makes the miniaturization of the equipment such as instrument, electroacoustic motor, magnetic separation magnetization, lightweight, slimming become possibility.Neodymium iron boron is divided into sintered NdFeB and Agglutinate neodymium-iron-boron two kinds, sintered Nd-Fe-B magnetic material has excellent magnetic property, be widely used in the fields such as electronics, electric machinery, medicine equipment, toy, packaging, hardware machinery, space flight and aviation, comparatively common are permanent-magnet machine, loud speaker, magnetic separator, computer disc driver, MR imaging apparatus instrument etc.
The magnetic property improving sintered NdFeB is one of important topic of numerous scholar and manufacturing enterprise's research always.α-Fe is the key factor that can produce decisive role to magnetism of material.The parameter influences such as the main acceptor's phase volume of the remanent magnetism of neodymium iron boron, magnetic energy product, composition, density.At fusion process, because neodymium iron boron is non-equilibrium process of cooling, therefore cause the generation of α-Fe, the appearance of α-Fe, decrease principal phase volume fraction, be degrading magnet border structure, thus cause magnetic property to decline.
Prior art solves the problem of α-Fe mainly through several aspect:
1) smelting technique is adopted.Adopt smelting technique, slow owing to cooling, the precipitation of α-Fe can only be reduced by improving total amount of rare earth, not only increasing cost, causing the decline of principal phase volume fraction simultaneously, thus can not obtain premium quality product; In addition, before fragmentation, increase homogenize treatment measures, although ingot casting can eliminate most of α-Fe after homogenize process, after pyroprocessing, grain growth, is degrading magnetic property equally.
2) rapid hardening technology is adopted.By improving alloy speed of cooling, cooling down with the speed surpassing 1000 DEG C/s when high temperature, reducing the generation of α-Fe.The method can produce the alloy of low α-Fe under low content of rare earth, has been widely used in the preparation of high performance magnet.But the method exists two problems, one is that disposable input is high, and high-performance rapid hardening furnace price all reaches 500-1000 ten thousand yuan, and maintenance cost is high, and the cost of common smelting furnace cost ability 30-50 ten thousand yuan, its Gao Mao is unfavorable for technology popularization; Two is that the Product processing of rapid hardening alloy production is poor, and when manufacturing complex shapes product, product scrap rate is high, and Application Areas is limited.
Summary of the invention
For above-mentioned deficiency, the invention provides a kind of method that the α of elimination-Fe prepares high performance sintered neodymium-iron-boron.
Said method comprising the steps of:
Step one, prepare master alloying and auxiliary alloy, starting material according to the composition of master alloying and auxiliary alloy respectively through melting, fragmentation, powder process, wherein in the shattering process of described master alloying, control the weight of bed material in airflow milling mill chamber and be separated: when alloy residuals weight is the 2-7% of total charging capacity in described airflow milling grinding system, this part material is as defective powder treatment, and all the other are as qualified powder treatment;
Step 2, adds to auxiliary alloy in described qualified powder in the ratio of the 3-20% of described qualified powder quality and mixes;
Step 3, compression moulding, through sintering oven sintering timeliness; Wherein
Consisting of of described master alloying: Ln
xb
yfe
100-X-Y, wherein
Ln is rare earth element, comprise La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y wherein one or more;
X, Y are each element weight percent content: wherein, 26.8≤X≤29.5,0.90≤Y≤1.20;
Described auxiliary alloy composition is: Ln α M β B γ Fe
100-alpha-beta-γ, wherein
Ln is rare earth element, comprise La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y wherein one or more;
M is Addition ofelements, comprises one or more in the elements such as Co, Cu, Nb, Zr, Ta, Ag, Au, Cr, Al, Ga, Sn, W, V, Mo, Ti;
α, β, γ are each element weight percent content: wherein, 35≤α≤60,5≤β≤15,0.90≤γ≤1.20.
Preferably, described method is further comprising the steps of, suppresses separately, sinters described defective powder, at fusion process as starting material regeneration.
Preferably, described method is further comprising the steps of, compression moulding, through 890-920 DEG C, 480-630 DEG C two-stage temper aging.
The method preparing high performance sintered neodymium-iron-boron according to elimination α-Fe of the present invention reduces the generation of α-Fe, provides the performance of sintered NdFeB.
Embodiment
The present invention is described in further detail below, can implement according to this with reference to specification sheets word to make those skilled in the art.
The method preparing high performance sintered neodymium-iron-boron according to elimination α-Fe of the present invention comprises the following steps:
Step one, prepares master alloying and auxiliary alloy.
Consisting of of master alloying: Ln
xb
yfe
100-X-Y, wherein
Ln is rare earth element, comprise La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y wherein one or more;
X, Y are each element weight percent content: wherein, 26.8≤X≤29.5,0.90≤Y≤1.20;
Described auxiliary alloy composition is: Ln
αm
βb
γfe
100-alpha-beta-γ, wherein
Ln is rare earth element, comprise La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, Y wherein one or more;
M is Addition ofelements, comprises one or more in the elements such as Co, Cu, Nb, Zr, Ta, Ag, Au, Cr, Al, Ga, Sn, W, V, Mo, Ti;
α, β, γ are each element weight percent content: wherein, 35≤α≤60,5≤β≤15,0.90≤γ≤1.20.
Starting material according to the composition of master alloying and auxiliary alloy, if master alloying composition is Ln
28.6b
1.01fe
70.39; Auxiliary alloying constituent is Ln
55b
0.98m
10fe
34.02in vacuum melting furnace, at 1450-1550 DEG C, high temperature forms the aluminium alloy of melting respectively, then aluminium alloy casting is cooled to the alloy pig that thickness is 0.2-25mm.Under nitrogen or protection of inert gas, undertaken that coarse breaking, hydrogen are broken by Mechanical Crushing method, alloy powder is broken into the powder of 3-5 μm by airflow milling, wherein in the shattering process of described master alloying, control the weight of bed material in airflow milling mill chamber and be separated: when alloy residuals weight is the 2-7% of total charging capacity in described airflow milling grinding system, this part material is as defective powder treatment, and all the other are as qualified powder treatment;
Step 2, adds to auxiliary alloy in described qualified powder in the ratio of the 3-20% of described qualified powder quality and mixes;
Step 3, compression moulding, through sintering oven sintering timeliness.
In pressing under magnetic field press, powder compression is become pressed compact, sinter timeliness afterwards, pressed compact is sintered 1000-1100 DEG C of temperature in vacuum sintering furnace, 480-630 DEG C of temper aging.In a preferred embodiment of the invention, through 890-920 DEG C, 480-630 DEG C two-stage temper aging.
Embodiment 1
Eliminate α-Fe and prepare the method for high performance sintered neodymium-iron-boron, prepare as follows:
Step one, prepares main and auxiliary two kinds of alloys.
Prepare burden described according to the form below 1, main and auxiliary alloy raw material forms the aluminium alloy of melting respectively in vacuum melting furnace through 1500 DEG C of high temperature, then pour into the main and auxiliary alloy that thickness is 15mm.
Table 1
| Master alloying | Nd28.6B1.01Fe70.39 |
| Auxiliary alloy | More than Nd55B0.98Al2Cu1Nb4Zr1Co5Ga1.6Fe |
Step 2, main and auxiliary alloy mixing.
Wherein, half is according to existing technique: master alloying is put in vacuum sintering furnace and at 1075 DEG C, carries out Homogenization Treatments 5 hours, then under nitrogen or protection of inert gas, respectively coarse breaking, hydrogen fragmentation are carried out to master alloying, auxiliary alloy, in airflow milling equipment, then grind to form the powder of 3-5 μm; Finally in auxiliary alloy: master alloying=7.2: the ratio of 92.8, add in master alloying by auxiliary alloy, mechanical overturn mixes.
Second half is according to technique of the present invention: respectively, directly carries out coarse breaking, hydrogen fragmentation, then at the powder that airflow milling equipment will grind to form 3-5 μm to master alloying, auxiliary alloy; According to the present invention, master alloying is pulverized in airflow milling equipment, and when in system, residual alloys weight is total weight alloy 6%, in system, residual powdered alloy is as defective powder, and all the other are as qualified powder.Especially, according to auxiliary alloy: the ratio of master alloying (qualified powder)=7.2: 92.8, added to by auxiliary alloy in the qualified powder of master alloying, mechanical overturn mixes.Underproof master alloying powder is then suppressed separately, is sintered, at fusion process as starting material regeneration.
Step 3, compression moulding, through sintering oven sintering timeliness.
Under the protection of nitrogen or rare gas element; the magnetic field medium-pressure type of the powder mixed at 1.7T in pressing under magnetic field press is shaping; then in vacuum sintering furnace, 4 hours are incubated at 1050 DEG C; through 920 DEG C, 500 DEG C difference tempering 2,4 hours after insulation terminates; after completing, magnetic property detection is carried out to blank, the results are shown in Table 2.
Table 2
Embodiment 2
Step one, prepares main and auxiliary two kinds of alloys.
Prepare burden described according to the form below 3, main and auxiliary alloy raw material forms the aluminium alloy of melting respectively in vacuum melting furnace through 1520 DEG C of high temperature, then pour into the main and auxiliary alloy that thickness is 18mm.
Table 3
| Master alloying | Nd29.2B1.00Fe69.8 |
| Auxiliary alloy | More than Nd30Dy6Tb6B0.98Al6Cu1.5Nb3Ta1Zr1.4Co14Ga1.4Fe |
Step 2, main and auxiliary alloy mixing.
Wherein, half is according to existing technique: directly under nitrogen or protection of inert gas, carry out coarse breaking, hydrogen fragmentation respectively to master alloying, auxiliary alloy, then grind to form the powder of 3-5 μm in airflow milling; Finally in auxiliary alloy: master alloying=15: the ratio of 85, add in master alloying by auxiliary alloy, mechanical overturn mixes.
Second half is according to the inventive method: respectively, directly carries out coarse breaking, hydrogen fragmentation to master alloying, auxiliary alloy, in airflow milling equipment, then grinds to form the powder of 3-5 μm; According to the present invention, master alloying is pulverized in airflow milling equipment, and when in system, residual alloys weight is total weight alloy 4%, in system, residual powdered alloy is as defective powder, and all the other are as qualified powder.Especially, according to auxiliary alloy: the ratio of master alloying (qualified powder)=15: 85, added to by auxiliary alloy in the qualified powder of master alloying, mechanical overturn mixes.Defective master alloying powder is then suppressed separately, is sintered, at fusion process as starting material regeneration.
Step 3, compression moulding, through sintering oven sintering timeliness.
Under the protection of nitrogen or rare gas element; the magnetic field medium-pressure type of the powder mixed at 2.0T in pressing under magnetic field press is shaping; then in vacuum sintering furnace, 3.5 hours are incubated at 1065 DEG C; through 900 DEG C, 480 DEG C difference tempering 2,3 hours after insulation terminates; after completing, magnetic property detection is carried out to blank, the results are shown in Table 4.
Table 4
Embodiment 3
Step one, prepares alloy.
Only produce the method for single alloy according to the present invention, prepare burden by the single alloying constituent in table 5, its composition is consistent with the mixed alloying constituent of the present invention.Raw material forms the aluminium alloy of melting in vacuum melting furnace through 1470 DEG C of high temperature, then pour into the alloy that thickness is 20mm.
Completely according to a method for invention, two alloying ingredient described according to the form below 5, in main and auxiliary alloy raw material difference vacuum melting furnace, at 1470 DEG C, high temperature forms the aluminium alloy of melting, then pours into the main and auxiliary alloy that thickness is 20mm.
Table 5
Step 2, main and auxiliary alloy mixing.
Alloy carries out coarse breaking under nitrogen or protection of inert gas, hydrogen is broken, in airflow milling equipment, then grind to form the powder of 3-5 μm;
Wherein, only produce the method for single alloy according to the present invention, single alloy is pulverized in airflow milling equipment, when system is when in system, residual alloys weight is total weight alloy 2.5%, in system, residual powdered alloy is as defective powder, and all the other are as qualified powder.Defective master alloying powder is then suppressed separately, is sintered, at fusion process as starting material regeneration.
Another kind of completely according to the method for invention, master alloying is pulverized in airflow milling equipment, and when in system, residual alloys weight is total weight alloy 2.5%, in system, residual powdered alloy is as defective powder, and all the other are as qualified powder.Especially, according to auxiliary alloy: the ratio of master alloying (qualified powder)=9: 91, added to by auxiliary alloy in qualified master alloying powder, mechanical overturn mixes.Defective master alloying powder is then suppressed separately, is sintered, at fusion process as starting material regeneration.
Step 3, compression moulding, through sintering oven sintering timeliness.
Under the protection of nitrogen or rare gas element; the magnetic field medium-pressure type of the powder mixed at 1.7T in pressing under magnetic field press is shaping; then in vacuum sintering furnace, 5 hours are incubated at 1045 DEG C; through 910 DEG C, 490 DEG C difference tempering 2.5,4.5 hours after insulation terminates; after completing, magnetic property detection is carried out to blank, the results are shown in Table 6.
Table 6
The method preparing high performance sintered neodymium-iron-boron according to elimination α-Fe of the present invention prepares two kinds of alloys.If only prepare a kind of alloy, after being separated later, composition can be caused to change.Prepare master alloying here, its composition is close to theoretical composition, even if after isolation, its rare earth composition is still constant, is conducive to the design of magnet.Adopt pairing gold in addition, can control grain boundaries composition, be conducive to preparing premium quality product.NdFeB rear-earth content is more close to rare earth theory content (26.8%wt), and performance is better.Need the rich neodymium of guarantee 2% could degaussing to be coupled mutually simultaneously, obtain high comprehensive magnetic energy.Also just more than theoretical rare earth (28.8%wt), rare earth more lower performance is higher.But the low meeting of rare earth causes α-Fe to occur, degradation.
As master alloying content of rare earth low (LN < 32), α-Fe is there will be at fusion process, auxiliary alloy content of rare earth high (LN > 32), therefore there will not be α-Fe, therefore here need to process master alloying specially, and auxiliary alloy does not need.Rich α-Fe composite material is higher than normal alloy composition iron content, and therefore toughness is large, utilizes airflow milling powder, is by ultrasonic air-flow, alloy to be collided mutually to realize fragmentation.Because rich α-Fe toughness is large, be difficult to be realized by collision broken, when also just meaning grinding more difficult fragmentation or the broken time longer, when its particle size after cracking does not reach separation condition, particle not by airflow milling separation system, thus stays system internal recycle.Present method utilizes this point exactly, by residuum doses in Controlling System, realizes rich α-Fe component powders and qualified powder separation.
Grind powder as qualified powder treatment; in auxiliary alloy: qualified powder=7.2 of master alloying: the ratio of 92.8; auxiliary alloy is added in the qualified powder of master alloying; mechanical overturn mixes; under the protection of nitrogen or rare gas element, the magnetic field medium-pressure type of powder at 1.7T in pressing under magnetic field press is shaping, then in vacuum sintering furnace 1050 DEG C of insulations 4 hours; through 920 DEG C, 500 DEG C difference tempering 2,4 hours after insulation terminates, after completing, magnetic property detection is carried out to blank.
After in grinding system, powdered alloy is clayed into power separately, compression moulding, be put in sintering oven 1080 DEG C insulation 3 hours, the blank after sintering is directly got back in smelting furnace as starting material and is recycled.
Although embodiment of the present invention are open as above, but it is not restricted to listed in specification sheets and embodiment utilization, it can be applied to various applicable the field of the invention completely, for those skilled in the art, can easily realize other amendment, therefore do not deviating under the universal that claim and equivalency range limit, the present invention is not limited to specific details and illustrates here and the embodiment described.
Claims (3)
1. eliminate the method that α-Fe prepares high performance sintered neodymium-iron-boron, it is characterized in that, said method comprising the steps of:
Step one, prepare master alloying and auxiliary alloy, starting material according to the composition of auxiliary alloy through melting, fragmentation, powder process, starting material are cooled to alloy pig that thickness is 0.2-25mm, fragmentation, powder process according to the composition of master alloying through melting, aluminium alloy casting, wherein in the shattering process of described master alloying, control the weight of bed material in airflow milling mill chamber and be separated: when alloy residuals weight is the 2-7% of total charging capacity in described airflow milling grinding system, this part material is as defective powder treatment, and all the other are as qualified powder treatment;
Step 2, adds to auxiliary alloy in described qualified powder in the ratio of the 3-20% of described qualified powder quality and mixes;
Step 3, compression moulding, through sintering oven sintering timeliness; Wherein,
Consisting of of described master alloying: Ln
xb
yfe
100-X-Y, wherein,
Ln is rare earth element, comprise La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu wherein one or more;
X, Y are each element weight percent content: wherein, 26.8≤X≤29.5,0.90≤Y≤1.20;
Described auxiliary alloy composition is: Ln
αm
βb
γfe
100-alpha-beta-γ, wherein,
Ln is rare earth element, comprise La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu wherein one or more;
M is Addition ofelements, comprise Co, Cu, Nb, Zr, Ta, Ag, Au, Cr, Al, Ga, Sn, W, V, Mo, Ti wherein one or more;
α, β, γ are each element weight percent content: wherein, 35≤α≤60,5≤β≤15,0.90≤γ≤1.20.
2. eliminate the method that α-Fe prepares high performance sintered neodymium-iron-boron as claimed in claim 1, described method is further comprising the steps of, suppresses separately, sinters described defective powder, at fusion process as starting material regeneration.
3. eliminate the method that α-Fe prepares high performance sintered neodymium-iron-boron as claimed in claim 1 or 2, described method is further comprising the steps of, compression moulding, through 890-920 DEG C, 480-630 DEG C two-stage temper aging.
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| JP2012204823A (en) * | 2011-03-28 | 2012-10-22 | Tdk Corp | Method for producing rare earth sintered magnet |
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| WO2010063142A1 (en) * | 2008-12-01 | 2010-06-10 | Zhejiang University | Sintered nd-fe-b permanent magnet with high coercivity for high temperature applications |
| WO2010063143A1 (en) * | 2008-12-01 | 2010-06-10 | Zhejiang University | Modified nd-fe-b permanent magnet with high corrosion resistance |
| JP2012204823A (en) * | 2011-03-28 | 2012-10-22 | Tdk Corp | Method for producing rare earth sintered magnet |
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