CN1046173C - Process for manufacturing rare-earth permanent magnet - Google Patents
Process for manufacturing rare-earth permanent magnet Download PDFInfo
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- CN1046173C CN1046173C CN92109915A CN92109915A CN1046173C CN 1046173 C CN1046173 C CN 1046173C CN 92109915 A CN92109915 A CN 92109915A CN 92109915 A CN92109915 A CN 92109915A CN 1046173 C CN1046173 C CN 1046173C
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Abstract
The present invention relates to a method for fabricating temperature resistant Fe-base rare-earth permanent magnets, and each temperature resistant Fe-base rare-earth permanent magnet is composed of ND, dysprosium, boron, ferrum, etc. The temperature resistant Fe-base rare-earth permanent magnet is characterized in that cobalt is not contained; a small amount of aluminum, gallium and plumbum can be added; components of the temperature resistant Fe-base rare-earth permanent magnet have the weight proportion according to atomic percentage: 1 % of Nd15 to 16, 0.1 to 1.2% of Dy, 6-7.9% of B, l0.5 to 1.6% of A and 0.1 to 0.4% of Ga, and the rest is Fe. The present invention is characterized in that the components are mixed in proportion and are melted into an ingot in a vacuum induction furnace with inert gas protection; after crushed, the ingot is ground into powder, the size of which is smaller than 100 um, in protective medium, such as gasoline, etc.; lead oxide powder is added for ball milling to obtain fine powder of 3 to 5 um; the fine powder is processed in the methods of baking, first pressing and isostatic shaping, and a shaping magnet is processed for secondary sintering and heat processing under vacuum and inert protection. The magnet has a positive magnetic induction temperature coefficient within 40 to 120 DEG C, use temperature is as high as 180 to 200 DEG C and price is low.
Description
The present invention relates to the magnet manufacture method, belong to H01F 41/02 class, a kind of manufacture method of rare-earth permanent magnet.
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 and methods such as Co, Dy mostly, improve the Curie temperature of magnet, improve the magnetic strength temperature coefficient, simultaneously also increase substantially the HCJ of magnet, 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.So other ways without cobalt (Co) have also put forward.On July 6th, 1987, " the clear 62-151541A of JP; the permanet magnet material of improvement " announced a application in Japan's special permission Room, think " at R-Fe-B is that various metallic elements are added in the alloy pilot scale; remanent magnetism, maximum magnetic energy product are improved; improve temperature characterisitic and produce effect, but coercive force does not almost improve ".Thereby propose " between the field trash of crystalline substance Jie R-Fe-B composition of alloy and interpolation reaction difficult, domain wall is moved be suppressed, improve coercive force and form so-called pinning effect.Inquire into the result of various additives, pointing out has extremely excellent effect as metal oxides such as the crystal of main component and non-crystal glass, lead oxide, bismuth oxide, silica.These materials can use separately or two or more merging is used." manufacturing process quoted of this article is: in vaccum sensitive stove,, be fused into ingot with inert gas shielding, broken then, the moulding in magnetic field of crystal Nd-Fe-B powder, carry out sintering, promptly conventional so-called powder metallurgic method is made anisotropic magnetic material.
The manufacture method that the purpose of this invention is to provide a kind 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 manufacture method of rare-earth permanent magnet of the present invention comprises the powder metallurgy process of making anisotropic magnetic material; Raw material is based on neodymium, iron, boron, it is characterized in that dysprosium is arranged, aluminium, gallium and plumbous oxide, and press atomic percent and prepare burden, Nd 15-16.1%, Dy 0.1-1.2%, B 6-7.9%, Al 0.5-1.6%, Ga 0.1-0.4%, surplus is Fe; Lead oxide is not included in the alloy total amount 100%, can add by weight 0-0.5% when ball milling.Mentioned component is mixed by proportioning, in the vaccum sensitive stove of blanketing with inert gas, be fused into ingot, operations such as warp slightly breaks, carefully breaks, in protective mediums such as gasoline or toluene, wear into powder less than 100 μ m, add the lead oxide powder bundle again, do protection with same medium and carry out ball milling, obtain the fine powder of 3-5 μ m; With the fine powder oven dry, in being not less than the magnetic field of 960KA/m, use 0.5-2t/cm
2The pressure pre-profiling, again through 2-4t/cm
2Static pressure such as pressure, the density that makes blank is greater than 5g/cm
3, 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 first time annealing at 800-900 ℃ then, the same sintering of condition carries out the heat treatment second time at 500-700 ℃ again, and low during the comparable sintering of vacuum condition, blanketing with inert gas is chilled to room temperature.
The performance of magnet is:
Br=1,1-1.2T Hcj＞19KOe
(BH)max＞26.5MGOe
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 element (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 temperature.
Embodiment:
| Example | Alloying element is formed % | Sintering and annealing process | Serviceability temperature (℃) | Remarks | ||||||
| Nd | Dy | Fe | B | Al | Ca | PbO | ||||
| 1 | 15.7 | 0.63 | 75.7 | 6.3 | 1.5 | 0.17 | 0 | 1080 ℃ * 1h cooling rate＞the same 700 ℃ * 1h of 900 ℃ * 1h of 300 ℃/min cooling rate＞500 ℃/min | 200 | Do not add PbO |
| 2 | 15.6 | 0.6 | 75 | 7.1 | 1.5 | 0.2 | 0.5wt | 1120 ℃ * 1h cooling rate＞the same 700 ℃ * 1h of 850 ℃ * 1h of 300 ℃/min cooling rate＞500 ℃/min | 205 | Add PbO |
| 3 | 16.1 | 0.1 | 75 | 7 | 1.5 | 0.3 | 0 | 1080 ℃ * 1h cooling rate＞the same 600 ℃ * 1h of 900 ℃ * 1.5h of 300 ℃/min cooling rate＞500 ℃/min | 200 | Do not add PbO |
| 4 | 15.7 | 0.7 | 76 | 6 | 1.4 | 0.2 | 0.2wt | 1100 ℃ * 1h cooling rate＞the same 600 ℃ * 1h of 900 ℃ * 1.5h of 300 ℃/min cooling rate＞500 ℃/min | 180 | Add PbO |
| 5 | 15 | 1.2 | 75 | 7.1 | 1.3 | 0.4 | 0 | 1120 ℃ * 1h cooling rate＞900 ℃ * 1h of 300 ℃/min cooling rate＞650 ℃ * 1h of 300 ℃/min cooling rate＞500 ℃/min | 200 | Do not add PbO |
The manufacture method of rare-earth permanent magnet of the present invention comprises the powder metallurgy process of making anisotropic magnetic material; Raw material is based on neodymium, iron, boron, it is characterized in that dysprosium is arranged, aluminium, gallium and plumbous oxide, and press atomic percent and prepare burden, Nd15-16.1%, Dy0.1-1.2%, B6-7.9%, Al0.5-1.6%, Ga0.1-0.4%, surplus is Fe; Lead oxide is not included in the alloy total amount 100%, can add by weight 0-0.5% when ball milling.Mentioned component is mixed by proportioning, in the vaccum sensitive stove of blanketing with inert gas, be fused into ingot,, in protective mediums such as gasoline or toluene, wear into powder, add lead oxide powder again less than 100 μ m through broken, thin operation such as broken slightly; Dysprosium in the mentioned component (Dy) both can be the simple metal element, also can be its oxide Dy
2O
3, use Dy instead Dy
2O
3The time should be when ball milling and lead add simultaneously, addition is as the criterion with the amount that the content of dysprosium in the oxide is equal to when adding pure dysprosium.Do protection with same medium and carry out ball milling, obtain the fine powder of 3-5 μ m; With the fine powder oven dry, in being not less than the magnetic field of 960kA/m, use 0.5-2t/cm
2The pressure pre-profiling, again through 2-4t/cm
2Static pressure such as pressure, the density that makes blank is greater than 5g/cm
3, 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, the same sintering of condition carries out the heat treatment second time again in 500-700 ℃.Low during the comparable sintering of vacuum condition, blanketing with inert gas is chilled to room temperature.
Said cold soon, cooling rate is greater than 300 ℃/min, said chilling, and cooling rate is 500-1200 ℃/min.
The cooling rate of described sintering and annealing and method: cold soon, be meant that cooling rate is greater than 300 ℃/min with air or water jacket cooling, described chilling is meant with air or nitrogen, and uses liquid medium, as coolings such as liquid nitrogen, cooling rate is 500-1200 ℃/min.
Claims (3)
1, a kind of manufacture method of rare-earth permanent magnet, comprise the powder metallurgy process of making anisotropic magnetic material: in the vaccum sensitive stove of blanketing with inert gas, raw material is fused into ingot, operations such as warp slightly breaks, carefully breaks, raw material is based on neodymium, iron, boron, it is characterized in that dysprosium is arranged, aluminium, gallium and plumbous oxide, press the atomic percent batching, Nd 15-16.1%, Dy 0.1-1.2%, B 6-7.9%, Al 0.5-1.6%, Ga 0.1-0.4%, surplus is Fe; Mentioned component is mixed by proportioning, be fused into ingot, add lead oxide powder again, do protection with same medium and carry out ball milling, obtain the fine powder of 3-5 μ m after jaw crushing and mill are worn into the powder less than 100 μ m in protective mediums such as gasoline or toluene; With the fine powder oven dry, in being not less than the magnetic field of 960KA/m, use 0.5-2t/cm
2The pressure pre-profiling, again through 2-4t/cm
2Static pressure such as pressure, the density that makes blank is greater than 5g/cm
3, 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 first time annealing at 800-900 ℃ then, the same sintering of condition carries out the heat treatment second time at 500-700 ℃ again, and low during the comparable sintering of vacuum condition, blanketing with inert gas is chilled to room temperature.
2, the manufacture method of rare-earth permanent magnet according to claim 1 is characterized in that lead oxide is not included in the alloy total amount 100%, can add by weight 0-0.5% when ball milling; Dysprosium Dy in the composition both can be the simple metal element, also can be its oxide Dy
2O
3Use Dy instead Dy
2O
3The time, the amount of the content of dysprosium when adding pure dysprosium is as the criterion in the oxide, and also should be when ball milling and lead add simultaneously.
3, the manufacture method of rare-earth 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 with air or nitrogen and uses liquid medium that as coolings such as liquid nitrogen, cooling rate is 500-1200 ℃/min.
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 |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN92109915A CN1046173C (en) | 1992-09-25 | 1992-09-25 | Process for manufacturing rare-earth permanent magnet |
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| Publication Number | Publication Date |
|---|---|
| CN1084668A CN1084668A (en) | 1994-03-30 |
| CN1046173C true CN1046173C (en) | 1999-11-03 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN92109915A Expired - Fee Related CN1046173C (en) | 1992-09-25 | 1992-09-25 | Process for manufacturing rare-earth permanent magnet |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP1762316B1 (en) | 2004-06-30 | 2014-07-16 | TDK Corporation | Method for producing a rare earth sintered magnet and its raw material and granules |
| 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 |
| CN102682949B (en) * | 2012-05-23 | 2013-11-27 | 钢铁研究总院 | High-resistivity permanent magnetic alloy and preparing method thereof |
Citations (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 |
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1992
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62151541A (en) * | 1985-12-25 | 1987-07-06 | S C M:Kk | Improved permanent magnet material |
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