CN1084668A - A kind of manufacture method of rare-earth permanent magnet - Google Patents
A kind of manufacture method of rare-earth permanent magnet Download PDFInfo
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- CN1084668A CN1084668A CN 92109915 CN92109915A CN1084668A CN 1084668 A CN1084668 A CN 1084668A CN 92109915 CN92109915 CN 92109915 CN 92109915 A CN92109915 A CN 92109915A CN 1084668 A CN1084668 A CN 1084668A
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Abstract
A kind of manufacture method of rare-earth permanent magnet is made up of neodymium, dysprosium, boron, iron etc., it is characterized in that not containing cobalt, can add a spot of aluminium, gallium, lead.Its component is Nd15-16,1% by atomic percent, Dy0.1-1.2%, and B6-7.9%, Al0.5-1.6%, Ga0.1-0.4%, all the other are Fe.Method is that mentioned component is mixed by proportioning; in the vaccum sensitive stove of blanketing with inert gas, be fused into ingot; the powder less than 100um is worn in broken back in protective mediums such as gasoline; add lead oxide powder again and make ball milling; obtain the fine powder of 3-5um; drying, first pressing, isostatic compaction, moulding magnet again under the protection of vacuum and inertia through first and second sintering, heat treatment.This magnet has positive magnetic strength temperature coefficient in 40-120 ℃, serviceability temperature is up to 180-200 ℃, low price.
Description
Since iron-base rare-earth permanent-magnet alloy came out from nineteen eighty-three, because its superior performance is drawn materials easily, moderate cost had obtained develop rapidly.Yet there are the low and corrosion-resistant two big shortcomings of serviceability temperature in this kind alloy.For this reason, there are a lot of patents to propose solution; Aspect raising ferrous rare earth permanent magnet thermal endurance, adopt compound interpolation Co_Al mostly, methods such as Co_Dy, improve the Curie temperature of magnet, improve the magnetic strength temperature coefficient, also increase substantially the HCJ of magnet simultaneously, thereby make magnet be applicable to higher serviceability temperature.As everyone knows, the low main cause of iron-based rare-earth permanent magnetism NdFeB serviceability temperature is its Curie temperature low (312 ℃), and add the Curie temperature that cobalt (Co) can greatly improve magnet, but cause coercitive reduction again, can increase substantially coercitive element so use, as aluminium (Al), dysprosium (Dy) and the compound interpolation of cobalt (Co) also can use niobium (Nb), molybdenum (Mo), vanadium (V), gallium (Ga), tin (Sn), bismuth (Bl) etc. and cobalt (Co) compound.In a word, method in the past all is to be the thermal endurance that main means remove to improve magnet to add cobalt Co.But cobalt (Co) is a precious metal, can not be extensive use of.
The objective of the invention is to propose a kind of manufacture method of rare-earth permanent magnet, the magnet according to this method is made has positive magnetic strength temperature coefficient in 40-120 ℃ of temperature range, and serviceability temperature is up to 180-200 ℃, and price comparison is cheap.
The composition of rare-earth permanent magnet of the present invention by atomic percent is; Nd15-16.1%, Dy0.1-1.2%, B6-7.9%, remainder is Fe, wherein the Ga of the Al of available 0.5-1.6% and 0.1-0.4% substitutes Fe.Lead oxide PbO is not included in the alloy total amount 100%, can add by weight 0-0.5% when ball milling.The manufacture method of magnet is: mentioned component is connect proportioning mix, be fused into ingot in the vaccum sensitive stove of blanketing with inert gas; Through thick broken, thin operation such as broken, in protective mediums such as gasoline or toluene, wear into powder then, add the lead oxide powder again, do to protect with same medium and carry out ball milling, obtain the fine powder of 3-5 μ m less than 100 μ m; With the fine powder oven dry, with the pressure pre-profiling of 0.5-2t/cm, again through the static pressure such as pressure of 2-4t/cm, the density that makes blank block is greater than 5g/cm in being not less than the magnetic field boundary of 960kA/cm; The moulding magnet in 1050-1120 ℃ of sintering 1-3 hour, is chilled to room temperature soon under vacuum and inert gas shielding, carry out the annealing first time at 800-900 ℃ then, and the same sintering of condition carries out the heat treatment second time at 500-700 ℃ again.Low during the comparable sintering of vacuum condition, blanketing with inert gas is chilled to room temperature.
The magnetic property of magnet is:
The irreversible loss W of Br=1.1-1.2T Hcj＞19KOe (BH) max＞26.5MGOe magnet is not: when the draw ratio L/D=1 of magnet 210 ℃
W is not=10.7%
226 ℃ of W are not=20.4%
202 ℃ of W are not=4.63% during L/D=1.06
226 ℃ of W are not=15.8%
197 ℃ of W are not=22.45% during L/D=0.545
202 ℃ of W are not=33%
180 ℃ of W are not=71.6% during L/D=0.095
Standard code, magnet are when L/D=1.04, and the temperature of irreversible loss＜5% o'clock is called the serviceability temperature of magnet.Thus, serviceability temperature of the present invention is 180-200 ℃.
The magnetic strength temperature coefficient of magnet:
In the time of 40-120 ℃, for just, i.e. value when the magnetic flux density of this temperature range inner magnet is not less than room temperature.
Characteristics of the present invention are fully without cobalt (Co), and the addition of heavy rare earth element dysprosium (Dy) is minimum, and noble element gallium (Ga) is to add as trace element, and the addition of plumbous (Pb) is also very little, so cost is low, promote easily.Generally add aluminium (Al) in magnet, the serviceability temperature of magnet is no more than 150 ℃, when serviceability temperature＞150 ℃, finds that its performance is also poorer than the magnet that does not add aluminium.But when Dy, Al, Ga and time spent, this shortcoming of aluminium has obtained inhibition, and the Curie temperature of magnet and intrinsic stupid power all increase substantially.Therefore, the serviceability temperature of magnet almost be doubled (serviceability temperature of normal temperature neodymium iron boron magnetic body is 80-100 ℃).The adding of plumbous (Pb) has improved the toughness of magnet, and is also favourable to improving serviceability temperature.
Embodiment:
The manufacture method of heatproof iron-base permanent-magnet body is that the dysprosium in the composition (DY) both can be the simple metal element, also can be its oxide DY
2O
3And dysprosia should add when ball milling.When using DY
2O
3The time, the addition of neodymium Nd will correspondingly strengthen, and the addition of heavy rare earth element is less than 0.2%.
| Select and edit and want number | Alloying element is formed % | Sintering and annealing process | The serviceability temperature remarks (℃) |
| ?Nd????Dy????Fe????B????Al????Ga????PbO | |||
| ??1 | ?15.6??0.6???75????6.9??1.5???0.4 | 1080 ℃ * 1h cooling rate＞900 ℃ * 1h of 300 ℃/min " 700 ℃ * 1h cooling rate＞500 ℃/min | ?200??????L/D＝1.04 |
| ??2 | ?15.6??0.6???75????7.1??1.5???0.2???0.3Wt | 1120 ℃ * 1h cooling rate＞850 ℃ * 1h of 300 ℃/min " 700 ℃ * 1h cooling rate＞500 ℃ of min | ?205??????L/D＝1.04 |
| ??3 | ?15.7??0.65??75.5??6.7??1.5???0.4 | 1100 ℃ * 1h cooling rate＞900 ℃ * 1.5h of 300 ℃/min " 650 ℃ * 1h cooling rate＞500 ℃/min | ?180??????L/D＝0.41 |
| ??4 | ?15.7??0.7???76????6????1.4???0.2???0.2Wt | 1100 ℃ * 1h cooling rate＞300 ℃ of min 900 ℃ * 1.5 " 600 ℃ * 1h cooling rates＞500 ℃/min | ?180??????L/D＝0.095 |
| ??5 | ?16.1??0?????75.6??6.6??1.5???0.2 | 1120 ℃ * 1h cooling rate＞900 ℃ * 1h of 300 ℃/min " 650 ℃ * 1h cooling rate＞500 ℃/min | 150 do not add Dy |
| ??6 | ?15.6??0?????77.6??6.6??0?????0.2 | 1120 ℃ * 1h cooling rate＞900 ℃ * 1.5h of 300 ℃/min " 600 ℃ * 1h cooling rate＞300 ℃/min | Do not add Dy and Al 140 L/D=1.04 |
| ??7 | " 600 ℃ * 1h of L/D=1.04 cooling rate＞500 ℃/min that 1120 ℃ * 1h＞cooling rate＞300 ℃/min 150 does not add 15.6 0.6 75.7 6.6 1.5 0 900 ℃ * 1.5h of Ga | ||
The cooling rate and the method for described sintering and annealing are: cold soon, be meant that cooling rate is greater than 300c/min with air or water jacket cooling, described chilling, be meant with air or argon gas, and with liquid medium, as coolings such as liquid nitrogen, cooling rate is 500-1200c/min.
Claims (5)
1, a kind of manufacture method of rare-earth permanent magnet, be made up of neodymium, iron, boron etc., be characterized in dysprosium, aluminium, gallium and plumbous oxide, manufacture method is that above-mentioned composition is cooperated by a certain percentage, in vaccum sensitive stove,, be fused into ingot with inert gas shielding; Through jaw crushing and mill, in protective mediums such as gasoline or toluene, make meal then, add lead oxide powder again, do protection with same medium and carry out ball milling, obtain the fine powder of 3-5um less than 100um; With the fine powder oven dry, with the pressure forming of 0.5-2t/cm, again through the static pressure such as pressure of 2-4t/cm, the density that makes blank is greater than 5g/cm in being not less than the magnetic field boundary of 960KA/m; The moulding magnet in 1050-1120 ℃ of sintering 1-3 hour, is chilled to room temperature soon under vacuum and inert gas shielding, carry out the annealing first time then in 800-900 ℃, and the same sintering of condition carries out the heat treatment second time at 500-700 ℃ again.Vacuum is low when requiring comparable sintering, and blanketing with inert gas is chilled to room temperature.
2, the manufacture method of heatproof iron-base permanent-magnet body according to claim 1 is characterized in that described composition proportion by atomic percent 15-16.1% Nd, 0.2-1.2% Dy, and 6-7.9% B, surplus is Fe; Wherein in the total amount of Fe, the replacement amount of Al is 0.5-1.6%, G
2Replacement amount be 0.1-0.4%.
3, the manufacture method of heatproof iron-base permanent-magnet body according to claim 1 is characterized in that the dysprosium (Dy) in the composition both can be the simple metal element, also can be its oxide Dy
2O
3, and dysprosia should add when ball milling; When using Dy
2O
3The time, the addition of Nd will correspondingly increase.The addition of heavy rare earth element is less than 0.2%.
4, the manufacture method of permanent magnet according to claim 1 is characterized in that lead oxide is to add when ball milling, addition is the 0.1-0.5% of alloy total amount, to improve Curie temperature, HCJ and the toughness of magnet.
5, the manufacture method of permanent magnet according to claim 1 is characterized in that the cooling rate of sintering and annealing and method are: described fast cold being meant with air or water jacket cooled off, and cooling rate is greater than 300 ℃/min; Described chilling is meant that the cold speed of unloading is 500-1200 ℃/min with air or argon gas and with liquid medium, as coolings such as liquid nitrogen.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN92109915A CN1046173C (en) | 1992-09-25 | 1992-09-25 | Process for manufacturing rare-earth permanent magnet |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN92109915A CN1046173C (en) | 1992-09-25 | 1992-09-25 | Process for manufacturing rare-earth permanent magnet |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1084668A true CN1084668A (en) | 1994-03-30 |
| CN1046173C CN1046173C (en) | 1999-11-03 |
Family
ID=4944466
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN92109915A Expired - Fee Related CN1046173C (en) | 1992-09-25 | 1992-09-25 | Process for manufacturing rare-earth permanent magnet |
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|---|---|
| CN (1) | CN1046173C (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7858023B2 (en) | 2004-06-30 | 2010-12-28 | Tdk Corporation | Method for producing raw material powder for rare earth sintered magnet, method for producing rare earth sintered magnet, granule and sintered body |
| CN101190548B (en) * | 2007-10-15 | 2011-06-01 | 淄博工陶耐火材料有限公司 | Method for isostatic pressing rotary tube |
| CN102682949A (en) * | 2012-05-23 | 2012-09-19 | 钢铁研究总院 | High-resistivity permanent magnetic alloy and preparing method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62151541A (en) * | 1985-12-25 | 1987-07-06 | S C M:Kk | Improved permanent magnet material |
-
1992
- 1992-09-25 CN CN92109915A patent/CN1046173C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7858023B2 (en) | 2004-06-30 | 2010-12-28 | Tdk Corporation | Method for producing raw material powder for rare earth sintered magnet, method for producing rare earth sintered magnet, granule and sintered body |
| CN101190548B (en) * | 2007-10-15 | 2011-06-01 | 淄博工陶耐火材料有限公司 | Method for isostatic pressing rotary tube |
| CN102682949A (en) * | 2012-05-23 | 2012-09-19 | 钢铁研究总院 | High-resistivity permanent magnetic alloy and preparing method thereof |
| CN102682949B (en) * | 2012-05-23 | 2013-11-27 | 钢铁研究总院 | High-resistivity permanent magnetic alloy and preparing method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1046173C (en) | 1999-11-03 |
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