CN1035737A - Rare-earth permanent magnet and manufacture method thereof - Google Patents
Rare-earth permanent magnet and manufacture method thereof Download PDFInfo
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- CN1035737A CN1035737A CN88100001A CN88100001A CN1035737A CN 1035737 A CN1035737 A CN 1035737A CN 88100001 A CN88100001 A CN 88100001A CN 88100001 A CN88100001 A CN 88100001A CN 1035737 A CN1035737 A CN 1035737A
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Abstract
The Nd-Fe-B that the invention provides a kind of cheapness is permanent magnetic alloy and manufacture method thereof, is that Nd in the alloy replaces with portion C e with Nd-Fe-B, reaches the purpose that reduces cost.Add Al simultaneously and adopt three-stage sintering and the Technology for Heating Processing of timeliness-back burning, the permanent magnetism performance of alloy is increased substantially, the high performance Nd-Ce-Fe-B that has obtained a kind of cheapness is a permanent-magnet alloy, and corresponding method of manufacture is provided.
Description
The invention belongs to a kind of permanent magnetic alloy and manufacture method thereof, mainly be that a kind of to contain price the most cheap, the Nd-Ce-Fe-B of the rare earth metal Ce that reserves are the abundantest is the permanent magnetic alloy of the cheap high magnetic energy of iron-based and utilizes powder metallurgy method to make the method for this kind magnet.
From nineteen eighty-three R-Fe-B(R is rare earth metal) be since permanent magnetic alloy comes out, particularly Nd-Fe-B is an alloy, because its maximum magnetic energy product (BH) max has surpassed any in the past permanent magnet material, and the main component in the alloy is that reserves are abundant in the rare earth metal, the neodymium metal that price is more cheap, replaced the expensive cobalt metal that often contained in the former permanent-magnet alloy with iron, the alloy materials cost descends significantly, field and the result of use used are more and more wider, become better and better, at various magnetic separators, direct current machine, field such as thin speaker and electronic watch has all obtained satisfied effect, thereby caused permanent-magnet alloy worker's very big attention, dropped into a large amount of research and production, comprised that with regard to alloy middle rare earth metallic element whole 16 kinds of rare earth metals of Y have all been done a large amount of work.Add the 4th kind of metallic element such as V, Ta, Nb, Al etc. have also delivered a lot of articles and patent.But maximum with regard to reserves in its rare earth metal, the interpolation of the cerium that price is the most cheap, its particular study and achievement are very few.Also be all to have proposed a very wide scope just with regard to 16 kinds of rare earth metals as Chinese patent CN-GK85101455 the model model, and in the article main application be Nd, Pr, Dy, Tb and Ho, more concentrated is that Nd-Fe-B is, Ce is not had special argumentation.Also provide a kind of Nd-Pr-Ce-Fe-B permanent-magnet alloy and manufacture method thereof among the clear 62-93337 of day disclosure special permission communique, though added Ce in the alloy, but contain the price height, the Pr element that reserves are few, and the final tempering of alloy need be adopted from sintering temperature to 400 ℃, every 1 hour multistage aging system of 100 ℃ of insulations, whole temper aging takes very long.In order further to reduce Nd-Fe-B is the cost of permanent-magnet alloy, the present invention chooses a kind of from the very wide Nd-Fe-B set member scope that prior art provided and replaces part Nd with Ce, and add a small amount of Al, thereby the Nd-Ce-Fe-B that obtains a kind of cheapness is a permanent-magnet alloy, and by the permanent-magnet alloy that this concrete narrower one-tenth is grouped into, effective technology of providing a kind of suitable industrialization to make has reached the purpose that alloy has higher permanent magnetism performance.
The Nd-Ce-Fe-B that the purpose of this invention is to provide a kind of cheapness is a permanent magnetic alloy, rare earth metal in the alloy is except that Nd, it is maximum only to contain reserves, the rare earth metal cerium that price is the most cheap, and this is provided is that alloy obtains the industrialization production method that burn high permanent magnetism performance three-stage sintering and timeliness-back.
The present invention realizes like this, in order further to reduce Nd-Fe-B is the cost of permanent-magnet alloy, it is maximum only to choose in the rare earth metal reserves from many prior aries of having delivered in the applied rare earth metal, the rare earth metal cerium that price is the most cheap replaces the part neodymium, and adding along with cerium, add a spot of aluminium again and adjust the permanent magnetism performance, the last tempering system that adopts three-stage sintering and final timeliness-back burning at this concrete narrower composition range, descend significantly thereby obtained cost, and the Nd-Ce-Fe-B with very high permanent magnetism performance is a permanent-magnet alloy.
Nd-Ce-Fe-B of the present invention is in the permanent-magnet alloy, except that neodymium, only contains rare earth metal cerium, the content of each composition (atom %, following herein identical) as follows, the R(rare earth metal) be 15-19, B5-8, Al0.2-1.0, Yu Tie, the content of Ce accounts for the 5-37 of R total amount among the R.Coming the instead of part neodymium with rare earth metal cerium is in order to reduce the cost of this permanent-magnet alloy fully, because cerium is the abundantest element of reserves in the rare earth metal, the price of cerium is lower three times than neodymium, and like this, this Nd-Ce-Fe-B is that the cost of alloy just reduces 3-25% than Nd-Fe-B.But, adding after the cerium, the HCJ of alloy descends to some extent, readjusts up for the coercive force alloy again, adds a spot of aluminium again in alloy.It is effective that experiment is found.At this moment, the aluminium of interpolation is to have replaced the iron of part in the alloy, and experiment is found to replace iron with aluminium, can make the magnetocrystalline anisotropy of the inferior dot matrix of iron maximum occur, and the coercive force of alloy has been enhanced up as a result.In addition, owing to added cerium and aluminium simultaneously in the alloy, occur the decline contradiction of remanence strength Br again, the reduction of Br must make (BH) max also descend.For with the Br of alloy and (BH) max improve up, the present invention finds to adopt the three-stage sintering system Br can be improved, the main effect of three-stage sintering is the density that has improved press body, makes it to reach the 98-99% of alloy theory density, and makes it solid solution fully and be the homogenizing state.First section is that 1030-1070 ℃ of insulation fully exitted press body in 20-40 minute in a vacuum; this is the prerequisite that obtains desirable sintered density; second section is insulation 15-25 minute under 1070-1100 ℃ the high temperature under argon shield; sintering reaches desirable density; the 3rd section be in argon gas 1040-1060 ℃ the insulation 0.5-1.0 hour; be for the solid solution homogenizing, obtain the uniform tissue state.
After the three-stage sintering, in order further to improve performance at the permanent-magnet alloy of composition of the present invention, particularly the approach of the squareness ratio by improving HCJ and demagnetization curve improves the permanent magnetism performance of alloy, the invention provides the heat treating regime of timeliness-back burning.Ageing Treatment be in argon gas 530-620 ℃ the insulation 0.8-1.0 hour, burn the back is 650-950 ℃ of insulation 0.5-1.0 hour in argon gas, when heat treatment was burnt in this timeliness-back, the effect of alloy structure state mainly was the phase structure state that obtains best high-coercive force.
The present invention is cheap, and Nd-Ce-Fe-B is a permanent-magnet alloy, as being main purpose to reach cost low, guarantees the permanent magnetism performance simultaneously on a quite high level, and its best composition (atom %) is: Nd10.3Ce5.7B
6(Fe1-0.005Al0.005) 78, this alloy 1060 ℃ of sintering 30 minutes in vacuum, 1080 ℃ of sintering were reduced in 1050 ℃ of argon gas after 0.8 hour the best three-stage sintering of sintering in 20 minutes at last in the argon gas, again in argon gas in 600 ℃ of insulations 1 hour and argon gas after 1 hour best timeliness of 900 ℃ of insulations-back burning heat treatment, the Br of alloy reaches 11850Gs as a result, jHc be 8650Oe and (BH) max be the permanent magnetism performance of 29.5M.G.Oe, and the cost of alloy reduces by 25% than Nd-Fe-B alloy, the present invention is cheap, and Nd-Ce-Fe-B is a permanent-magnet alloy, as to have very high permanent magnetism performance be main purpose to provide one, guarantee that simultaneously this Nd-Fe-B is that cost of alloy is low, its optimal components is Nd15.2Ce0.8B
6(Fe1-0.005Al0.005) 78, this alloy 1060 ℃ of sintering 30 minutes in vacuum, 1080 ℃ of sintering are 20 minutes in the argon gas, cool in 1050 ℃ of argon gas sintering at last after 0.8 hour, in argon gas in 600 ℃ of insulations 1 hour and argon gas after 1 hour best timeliness of 900 ℃ of insulations-back burning heat treatment, the Br of its alloy reaches 13300Gs again, and jHc is 8000Oe, (BH) max is 41.7M.G.O, and the cost of alloy reduces by 3% than Nd-Fe-B system simultaneously.The cheap Nd-Ce-Fe-B of the present invention be in the alloy with Ce instead of part Nd, Ce accounts for the 5-37 of rare earth metal R total amount, is 5 o'clock at Ce, this is that alloy permanent magnetism performance is the highest, Ce be 37 o'clock this be that cost of alloy is minimum, and other composition optimum contents are B
6, Fe77.61, Al0.39.Promptly this moment, alloy promptly had cheap characteristics, had high permanent magnetism performance again.
It is to guarantee that the cheap Nd-Ce-Fe-B of the present invention is the industrialization production method that permanent-magnet alloy has high permanent magnetism performance that Technology for Heating Processing is burnt in three-stage sintering system of the present invention and timeliness-back, first section of three-stage sintering is 1030-1070 ℃ of insulation 20-40 minute under vacuum, it mainly acts on is that the gas in the pressing blank is emitted fully, thereby the 98-99% that reaches solid density for the high temperature sintering of next section lays the foundation, the temperature of this section can not be low excessively, too low must prolong temperature retention time, can cause the volatilization of rare earth element, temperature can not be too high, too high temperature also will cause a large amount of losses of rare earth element, optimum temperature is 1050 ℃, and Best Times is 30 minutes.Second section be under argon gas 1070-1100 ℃ the insulation 15-25 minute, carry out high temperature sintering, temperature is lower than 1070 ℃ does not have agglomeration, the density of promptly burning the back magnet does not reach requirement, temperature is higher than 1100 ℃ can make grain growth, cause the alloy coercive force to reduce, optimum temperature is 1080 ℃, and Best Times is 20 minutes.The 3rd section is 1040-1060 ℃ of insulation 0.5-1 hour under argon gas, and main effect is tissue and the homogenization of composition that makes magnet, and best system is 1050 ℃ of insulations 0.8 hour.The main effect of timeliness-back firing technique is the HCJ that the former can improve alloy, the latter can improve the squareness ratio of demagnetization curve, usually timeliness is 580-620 ℃ of insulation 0.8-1.5 hour, best system is 600 ℃ of insulations one hour, burn the back is 850-950 ℃ of insulation 0.5-1.5 hour, and best system is 900 ℃ of insulations 1 hour in the argon gas.
Implementing alloy of the present invention is that employing purity is 99% pure iron, and 99% metallic cerium, 99% neodymium metal, boron content are ferro-boron and the metallic aluminium of 10-20%, with raw material melting under the argon shield in electric induction furnace.Alloy pig is crushed to 60 order meal, and vibrating ball is worn into the fine powder about 3 μ m then, and fine powder is orientated in magnetic field and gives moldedly, and magnetic field intensity 13KOe, pressure are 100kg/cm
2, give molded after, static pressure, pressure 4T/cm such as impose again
2, then press body through three-stage sintering of the present invention and timeliness-after burn heat treatment and be chilled to room temperature soon, promptly having obtained cheap Nd-Ce-Fe-B of the present invention is the permanent-magnet alloy body.
With existing Nd-Fe-B is that permanent-magnet alloy is compared, cheap Nd-Ce-Fe-B of the present invention is that cost of alloy has reduced 3-25%, and because the Technology for Heating Processing that adopts three-stage sintering and timeliness-back to burn makes the permanent magnetism performance of this alloy have very high horizontal Br=11.8-13.3KG(1.18-1.33T), jH
C=8.0-11.2KOe(636.8-891.5Am
-1), (BH) max=29.5-41.7MGOe(234.8-331.9KJm
-3).
Further specify the present invention with embodiment below.
Atomic ratio is respectively the steel ingot of each composition shown in the table 1 and smelts acquisition under the argon shield in vacuum induction furnace; steel ingot is crushed to 60 order meal; meal is worn into the fine powder of 3 μ m again through vibrating ball; fine powder is placed the magnetic field orientation and gives molded; the magnetic field orientating direction is vertical with pressure direction; alignment magnetic field is 13KOe, gives pressure pressure 100kg/cm
2, give and press the back blank to impose hydrostatic pressure 4T/cm again
2Make the press body that is of a size of φ 10 * 10mm, this press body in a vacuum through 1050 ℃ 30 minutes, following 1080 ℃ of argon gas 20 minutes, following 1050 ℃ of three-stage sinterings of 0.8 hour of argon gas, after in 600 ℃ of 1 hour argon gas timeliness and the 900 ℃ of 1 hour argon gas back burn and handle, be chilled to room temperature soon, through Magnetic Measurement must table 1 shown in all values.As seen, at Nd-Ce-Fe-B of the present invention is in the alloy component range, not only cost of alloy has reduction (3-25% scope) in various degree, and through best three-stage sintering provided by the present invention and timeliness-after burn heat treatment after, the performance of each permanent-magnet alloy has all reached actual applicable level in the industry, and (BH) max can to reach this numerical value of 41.7MGOe be quite high for a kind of RE permanent magnetic alloy of cheapness.
It is Nd that table 2 shows atomic ratio
15.2Ce
0.8B
6(Fe
1-0.005Al
0.005)
78Permanent-magnet alloy, three-stage sintering and timeliness in scope provided by the present invention-after burn heat treatment, after its concrete practice three-stage sintering system as shown in table 2, be as cold as the temperature of Ageing Treatment soon, carry out the back then and burn, the back is chilled to room temperature after burning soon, measures each permanent magnetism performance such as table 2 at last and shows.Because adopt three-stage sintering of the present invention and timeliness-back to burn Technology for Heating Processing, this alloy all has quite high permanent magnetism performance, maximum magnetic energy product is all more than 41.0MGOe.
Claims (5)
1, a kind of cheapness contains R (R is a rare earth metal), Fe, the rare-earth permanent magnet alloy of B and Al, it is characterized in that containing among the R two kinds of rare earth metals of Ce and Nd, and the chemical composition of each component (atom %, below identical) is R15-19, B5-8, Al0.2-1.0, surplus Fe, the content of Ce accounts for the 5-37 of R total amount among the R.
2, rare earth permanent magnet ferroalloy according to claim 1 is characterized in that the minimum alloy composition of cost is Nd10.3Ce5.7B
6(Fe1-0.005Al0.005) 78.
3, rare earth permanent magnet ferroalloy according to claim 1, the chemical composition that it is characterized in that having the alloy of the highest permanent magnetism performance is Nd15.2Ce0.8B
6(Fe1-0.005Al0.005) 78.
4; the cheap R15-19 that contains; B5-8; Al0.2-1.0; surplus Fe; and the content of Ce accounts for the manufacture method of rare-earth permanent magnet alloy of the 5-37 of R total amount among the R; comprising smelting; pulverize; die mould, sintering and final tempering is characterized in that adopting the three-stage sintering system; first section in a vacuum 1030-1070 ℃ the insulation 20-40 minute; second section 1070-1100 ℃ of insulation 15-25 minute in argon gas, the 3rd section is after reducing temperature in argon gas 1040-1060 ℃, is incubated 0.5-1.0 hour; under argon shield, carry out timeliness-back behind the cool to room temperature again and burn heat treatment; Ageing Treatment is incubated 0.8-1.5 hour at 580-620 ℃, and the back is burnt and handled 850-950 ℃ of insulation 0.5-1.5 hour.
5, the manufacture method of rare-earth permanent magnet alloy according to claim 4; it is characterized in that the best system that three-stage sintering and timeliness-back burning is handled is as follows; the 1050 ℃ of insulations 30 minutes in a vacuum of first section of three-stage sintering, are incubated 20 minutes by second section in argon gas 1080 ℃; the 3rd section in argon gas 1050 ℃; be incubated 0.8 hour,, be incubated Ageing Treatment in 1 hour argon gas then through 600 ℃; at last again under argon shield, burnt 1 hour after 900 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN88100001A CN1035737A (en) | 1988-01-03 | 1988-01-03 | Rare-earth permanent magnet and manufacture method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN88100001A CN1035737A (en) | 1988-01-03 | 1988-01-03 | Rare-earth permanent magnet and manufacture method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN1035737A true CN1035737A (en) | 1989-09-20 |
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ID=4831110
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|---|---|---|---|
| CN88100001A Withdrawn CN1035737A (en) | 1988-01-03 | 1988-01-03 | Rare-earth permanent magnet and manufacture method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102012222751A1 (en) | 2011-12-15 | 2013-06-20 | Central Iron And Steel Research Institute | High-performance magnet with little neodymium and without heavy rare earth and a method for its production |
| DE102013206940A1 (en) | 2012-08-30 | 2014-03-06 | Central Iron And Steel Research Institute | Cost-effective dual-phase Ce permanent magnet alloy and method of making the same |
-
1988
- 1988-01-03 CN CN88100001A patent/CN1035737A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102012222751A1 (en) | 2011-12-15 | 2013-06-20 | Central Iron And Steel Research Institute | High-performance magnet with little neodymium and without heavy rare earth and a method for its production |
| DE102013206940A1 (en) | 2012-08-30 | 2014-03-06 | Central Iron And Steel Research Institute | Cost-effective dual-phase Ce permanent magnet alloy and method of making the same |
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