CN103871704A - Praseodymium iron nitrogen phosphorus permanent magnet material and preparing method thereof - Google Patents
Praseodymium iron nitrogen phosphorus permanent magnet material and preparing method thereof Download PDFInfo
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Abstract
The invention provides a praseodymium iron nitrogen phosphorus permanent magnet material and a preparing method of the praseodymium iron nitrogen phosphorus permanent magnet material. The alloy thin belt material has high residual magnetic flux density. The preparing method has the advantages that the process is simple, the production cost is low, and the method is applicable to industrial production. The praseodymium iron nitrogen phosphorus permanent magnet material comprises the following ingredients in percentage by weight: 0.3 to 0.6 percent of Sc, 1 to 3 percent of Zr, 1 to 5 percent of Si, 0.1 to 0.2 percent of Ce, 0.1 to 0.2 percent of Lu, 0.1 to 0.3 percent of Ge, 0.8 to 1.6 percent of V, 0.1 to 0.2 percent of N, 0.1 to 0.2 percent of C, 1 to 2 percent of B, 22 to 25 percent of Nd, 0.7 percent to 0.9 percent of Pb, 0.5 percent to 1.15 percent of P and the balance Fe.
Description
technical field:
The invention belongs to metal material field, relate to a kind of neodymium iron nitrogen phosphorus permanent magnetic material and preparation method.
background technology:
cN201210380046.1number application provides the preparation method of the thin brilliant sintered NdFeB of a kind of high-compactness, and its production method comprises: foundry alloy is smelted casting and made rapid hardening strip, breaks airflow milling powder by hydrogen, and be orientated after die mould, by HIP sintering densification, finally by crossing temper, obtain product.In the method, by apply the gas pressure that is not less than 0.5MPa in sintering process, not only make magnet density increase, and can reduce sintering temperature, shortening sintering time, make crystal grain obtain obvious refinement, the rich neodymium of intergranular distributes more even mutually, thereby improves remanent magnetism and the coercive force of magnet, and combination property significantly promotes.But the material remanent magnetism making is on the low side.
summary of the invention:
The present invention is directed to above-mentioned technological deficiency, a kind of neodymium iron nitrogen phosphorus permanent magnetic material is provided, this alloy thin band material has high residual magnetic flux density.
Another object of the present invention is to provide the preparation method of above-mentioned neodymium iron nitrogen phosphorus permanent magnetic material, and this preparation method's technique is simple, and production cost is low, is suitable for suitability for industrialized production.
the object of the invention is to be achieved through the following technical solutions:
A kind of neodymium iron nitrogen phosphorus permanent magnetic material, in this material, the weight percentage of composition is: Sc 0.3-0.6%, Zr1-3%, Si 1-5%, Ce 0.1-0.2%, Lu 0.1-0.2%, Ge 0.1-0.3%, V 0.8-1.6%, N 0.1-0.2%, C 0.1-0.2%, B 1-2%, Nd 22-25%, Pb 0.7%～0.9%, P 0.5%～1.15%, all the other are Fe.
The preparation method of above-mentioned material comprises the following steps:
1) first prepare burden according to above-mentioned composition, the purity of raw material Sc, Zr, Si, Ce, Lu, Ge, Nd, Pb, P, Fe is all greater than 99.9%; The ferrorphosphorus form that it is 24% that P adopts containing P percentage by weight adds; V, N, the C VN alloy form take weight ratio as V:N:C=8:1:1 adds; B is to add as 24% ferro-boron form containing B percentage by weight;
2) raw material is put into vaccum sensitive stove melting, smelting temperature is 1550～1580 ℃, obtains master alloy ingot; Then adopt disintegrating machine that master alloy ingot is broken into alloy fragment;
3) alloy fragment is placed in liquid nitrogen and carries out K cryogenic treatment, locates temperature and is-196 ℃, is incubated 20～25 minutes; Taking-up is put at ambient temperature and is left standstill 0.5～2 hour; Alloy fragment being put into vacuum degree is again 0.05～0.0.8Pa, and it is broken that the hydrogen crushing furnace that stove internal gas pressure is 0.6～1.0atm carries out hydrogen, and temperature is heated to 250～320 ℃, and hydrogen makes fragment become meal after broken 40～60 minutes;
4) then meal is put into airflow milling and wear into fine powder, airflow milling powder pressure 6～7atm; Then fine powder is put into mould briquet, briquetting pressure is 0.02～0.06MPa;
5) take out molded part and pack sintering basin into, it is 0.01～0.04Pa that molded part is sent into vacuum degree in company with sintering basin, and temperature is the interior sintering of the sintering electric furnace of 1070～1100 ℃, is incubated power-off after 80～120 minutes, naturally cool to 800～900 ℃ with stove, then meet electricity insulation 2～3h; After again power-off be cooled to 490～500 ℃, then meet electricity insulation 3～5h, then cool to room temperature with the furnace and come out of the stove, obtain neodymium iron nitrogen phosphorus permanent magnetic material.
Further design of the present invention is:
Step 2) in disintegrating machine by master alloy ingot fragmentation to 3～6mm size alloy fragment.
In step 3), coarse granularity is 20～40 microns.
In step 4), powder particle size is 3～5 microns.
the present invention has following beneficial effect:
Ge, Pb in material of the present invention can reduce the angle of wetting of rich Nd phase and principal phase, suppresses growing up of principal phase, and principal phase interface defect density is reduced, and magnetic reversal farmland is in interface forming core difficulty.Therefore improved the remanent magnetism of material.The present invention adds Pr and N in Fe, can form PrFe12NX permanent magnetism principal phase; In Fe, add Nd and B, can form permanent magnetism principal phase Nd2Fe14B.These two compound existence of principal phase, have strengthened the permanent magnetism performance of alloy.
Pb, P in material replaces part B atom.In alloy material, Ce, Lu element enter principal phase.This is because the element that is dissolved in principal phase has reduced effective demagnetizing factor and refinement principal phase, and these all can effectively improve the magnetic property of magnet.The reason that Sc, Zr, C improve HCJ is the intercrystalline parafacies forming, and has suppressed growing up of crystal grain intersection particle, refinement main phase grain, therefore just suppressed their enhancings of stray magnetic field around, and then improved HCJ.
Products obtained therefrom of the present invention has excellent magnetic energy.In the present invention's preparation, other cost of material of rare element trace used is lower; Prepare in addition alloy in kind and, through cooling fast, guaranteed the uniformity of alloying component, tissue and performance, guaranteed the quality of alloy.This alloy preparation technology is easy, and process is simple, and the alloy of production has good performance, is convenient to very much suitability for industrialized production.In preparation method of the present invention, raw material is put into vaccum sensitive stove melting, then adopt disintegrating machine by master alloy ingot fragmentation to 3-6mm size, be placed in liquid nitrogen and carry out K cryogenic treatment, then it is broken that alloy fragment is carried out to hydrogen.The broken hydrogen absorption characteristic that utilizes rare earth intermetallic compound of hydrogen, is placed in alloy under hydrogen environment, and hydrogen enters alloy along phase thin layer, makes it expansion explosion and fragmentation, along rich neodymium layer place cracking mutually.The broken fritter that makes of hydrogen becomes meal.The present invention adopts alloying component optimization and deep cooling combination.The feature of the application's technique is effectively to make crystal grain obtain refinement, easily obtains high performance product.Material property of the present invention is in table 1.
This case technology is applicable to electromechanics trade, is also suitable for other electrical apparatus industry.
accompanying drawing explanation:
Fig. 1 is neodymium iron nitrogen phosphorus permanent magnetic material prepared by the embodiment of the present invention one.
As seen from Figure 1, the even tissue densification of this material.
embodiment:
embodiment mono-:
Neodymium iron nitrogen phosphorus permanent magnetic material of the present invention, preparation method comprise the following steps:
1) according to weight percentage be first: Sc 0.3%, Zr 1%, Si 1%, Ce 0.%, Lu 0.1%, Ge 0.1%, V 0.8%, N 0.1%, C 0.1%, B 1%, Nd 22%, Pb 0.7%, P 0.5%, all the other are prepared burden for Fe, and the purity of raw material Sc, Zr, Si, Ce, Lu, Ge, Nd, Pb, P, Fe is all greater than 99.9%; The ferrorphosphorus form that it is 24% that P adopts containing P percentage by weight adds; V, N, the C VN alloy form take weight ratio as V:N:C=8:1:1 adds; B is to add as 24% ferro-boron form containing B percentage by weight;
2) raw material is put into vaccum sensitive stove melting, smelting temperature is 1550 ℃, obtains master alloy ingot; Then adopt disintegrating machine by master alloy ingot fragmentation to 3～6mm size alloy fragment;
3) alloy fragment is placed in liquid nitrogen and carries out K cryogenic treatment, locates temperature and is-196 ℃, is incubated 20 minutes; Taking-up is put at ambient temperature and is left standstill 0.5 hour; Alloy fragment being put into vacuum degree is again 0.05Pa, and it is broken that the hydrogen crushing furnace that stove internal gas pressure is 0.6atm carries out hydrogen, and temperature is heated to 250 ℃, and hydrogen makes fragment become meal after broken 40 minutes, and coarse granularity is 20～40 microns;
Utilize the hydrogen absorption characteristic of rare earth intermetallic compound, Nd Fe B alloys is placed under hydrogen environment, hydrogen enters alloy along rich neodymium phase thin layer, makes it expansion explosion and fragmentation, along rich neodymium layer place cracking mutually.
4) then meal is put into airflow milling and wears into fine powder, with high pressure draught by stir after meal blow afloat, by collision each other, dynamics is diminished, powder particle size is 3～5 microns.Airflow milling powder pressure 6atm; Then fine powder is put into mould briquet, briquetting pressure is 0.02MPa;
5) take out molded part and pack sintering basin into, it is 0.01Pa that molded part is sent into vacuum degree in company with sintering basin, and temperature is the interior sintering of the sintering electric furnace of 1070 ℃, is incubated power-off after 80 minutes, naturally cools to 800 ℃ with stove, then meets electricity insulation 2h; After again power-off be cooled to 490 ℃, then meet electricity insulation 3h, then cool to room temperature with the furnace and come out of the stove, obtain neodymium iron nitrogen phosphorus permanent magnetic material.
embodiment bis-:
Neodymium iron nitrogen phosphorus permanent magnetic material of the present invention, preparation method comprise the following steps:
1) according to weight percentage be first: Sc 0.6%, Zr 3%, Si 5%, Ce 0.2%, Lu 0.2%, Ge 0.3%, V 1.6%, N 0.2%, C 0.2%, B 2%, Nd 25%, Pb 0.9%, P 1.15%, all the other are prepared burden for Fe, and the purity of raw material Sc, Zr, Si, Ce, Lu, Ge, Nd, Pb, P, Fe is all greater than 99.9%; The ferrorphosphorus form that it is 24% that P adopts containing P percentage by weight adds; V, N, the C VN alloy form take weight ratio as V:N:C=8:1:1 adds; B is to add as 24% ferro-boron form containing B percentage by weight;
2) raw material is put into vaccum sensitive stove melting, smelting temperature is 1580 ℃, obtains master alloy ingot; Then adopt disintegrating machine by master alloy ingot fragmentation to 3～6mm size alloy fragment;
3) alloy fragment is placed in liquid nitrogen and carries out K cryogenic treatment, locates temperature and is-196 ℃, is incubated 25 minutes; Taking-up is put at ambient temperature and is left standstill 2 hours; Alloy fragment being put into vacuum degree is again 0.0.8Pa, and it is broken that the hydrogen crushing furnace that stove internal gas pressure is 1.0atm carries out hydrogen, and temperature is heated to 320 ℃, and hydrogen makes fragment become meal after broken 60 minutes, and coarse granularity is 20～40 microns;
Utilize the hydrogen absorption characteristic of rare earth intermetallic compound, Nd Fe B alloys is placed under hydrogen environment, hydrogen enters alloy along rich neodymium phase thin layer, makes it expansion explosion and fragmentation, along rich neodymium layer place cracking mutually.
4) then meal is put into airflow milling and wears into fine powder, with high pressure draught by stir after meal blow afloat, by collision each other, dynamics is diminished, powder particle size is 3～5 microns.Airflow milling powder pressure 7atm; Then fine powder is put into mould briquet, briquetting pressure is 0.06MPa;
5) take out molded part and pack sintering basin into, it is 0.04Pa that molded part is sent into vacuum degree in company with sintering basin, and temperature is the interior sintering of the sintering electric furnace of 1100 ℃, is incubated power-off after 120 minutes, naturally cools to 900 ℃ with stove, then meets electricity insulation 3h; After again power-off be cooled to 500 ℃, then meet electricity insulation 5h, then cool to room temperature with the furnace and come out of the stove, obtain neodymium iron nitrogen phosphorus permanent magnetic material.
embodiment tri-:
Neodymium iron nitrogen phosphorus permanent magnetic material of the present invention, preparation method comprise the following steps:
1) according to weight percentage be first: Sc 0.5%, Zr 2%, Si 3%, Ce 0.15%, Lu 0.15%, Ge 0.2%, V 1.2%, N 0.15%, C 0.15%, B 1.5%, Nd 24%, Pb 0.8%, P 0.8%, all the other are prepared burden for Fe, and the purity of raw material Sc, Zr, Si, Ce, Lu, Ge, Nd, Pb, P, Fe is all greater than 99.9%; The ferrorphosphorus form that it is 24% that P adopts containing P percentage by weight adds; V, N, the C VN alloy form take weight ratio as V:N:C=8:1:1 adds; B is to add as 24% ferro-boron form containing B percentage by weight;
2) raw material is put into vaccum sensitive stove melting, smelting temperature is 1560 ℃, obtains master alloy ingot; Then adopt disintegrating machine by master alloy ingot fragmentation to 3～6mm size alloy fragment;
3) alloy fragment is placed in liquid nitrogen and carries out K cryogenic treatment, locates temperature and is-196 ℃, is incubated 25 minutes; Taking-up is put at ambient temperature and is left standstill 1 hour; Alloy fragment being put into vacuum degree is again 0.06Pa, and it is broken that the hydrogen crushing furnace that stove internal gas pressure is 0.8atm carries out hydrogen, and temperature is heated to 300 ℃, and hydrogen makes fragment become meal after broken 50 minutes, and coarse granularity is 20～40 microns;
Utilize the hydrogen absorption characteristic of rare earth intermetallic compound, Nd Fe B alloys is placed under hydrogen environment, hydrogen enters alloy along rich neodymium phase thin layer, makes it expansion explosion and fragmentation, along rich neodymium layer place cracking mutually.
4) then meal is put into airflow milling and wears into fine powder, with high pressure draught by stir after meal blow afloat, by collision each other, dynamics is diminished, powder particle size is 3～5 microns.Airflow milling powder pressure 6atm; Then fine powder is put into mould briquet, briquetting pressure is 0.05MPa;
5) take out molded part and pack sintering basin into, it is 0.03Pa that molded part is sent into vacuum degree in company with sintering basin, and temperature is the interior sintering of the sintering electric furnace of 1000 ℃, is incubated power-off after 100 minutes, naturally cools to 850 ℃ with stove, then meets electricity insulation 2h; After again power-off be cooled to 500 ℃, then meet electricity insulation 4h, then cool to room temperature with the furnace and come out of the stove, obtain neodymium iron nitrogen phosphorus permanent magnetic material.
embodiment tetra-: (proportioning components is not in design of the present invention)
Each composition percentage composition by weight: Sc 0.2% in neodymium iron nitrogen phosphorus permanent magnetic material, Zr 0.5%, Si 3%, Ce 0.15%, Lu 0.15%, Ge 0.2%, V 0.4%, N 0.05%, C 0.05%, B 0.5%, Nd 21%, Pb 0.5%, P 0.4%, all the other Fe prepare burden, and preparation process is with embodiment mono-.
embodiment five: (proportioning components is not in design of the present invention)
Each composition percentage composition by weight: Sc 0.8% in neodymium iron nitrogen phosphorus permanent magnetic material, Zr 4%, Si 6%, Ce 0.3%, Lu 0.3%, Ge 0.4%, V 2.4%, N 0.3%, C 0.3%, B 3%, Nd 26%, Pb 1.2%, P 1.3%, all the other Fe prepare burden, and preparation process is with embodiment mono-.
Table 1
As can be seen from the above table, in material, add Sc, Zr, Si, Ce, Lu, Ge, V, N,, B, Nd, Pb, P element contribute to alloy to have the raising of soft magnet performance.But exceed the scope of the application's design, not only no raising of soft magnet performance, reduce on the contrary.Reason is that these elements are too much, can form non-magnetic compound, has also reduced the useful effect of element.Sc, Nd, Ce, Lu, Ge element are too much, no longer work, and waste on the contrary raw material.
Claims (5)
1. a neodymium iron nitrogen phosphorus permanent magnetic material, is characterized in that: in this material, the weight percentage of composition is: Sc 0.3-0.6%, Zr1-3%, Si 1-5%, Ce 0.1-0.2%, Lu 0.1-0.2%, Ge 0.1-0.3%, V 0.8-1.6%, N 0.1-0.2%, C 0.1-0.2%, B 1-2%, Nd 22-25%, Pb 0.7%～0.9%, P 0.5%～1.15%, all the other are Fe.
2. the preparation method of neodymium iron nitrogen phosphorus permanent magnetic material described in claim 1, is characterized in that: the method comprises the following steps:
1) first prepare burden according to above-mentioned composition, the purity of raw material Sc, Zr, Si, Ce, Lu, Ge, Nd, Pb, P, Fe is all greater than 99.9%; The ferrorphosphorus form that it is 24% that P adopts containing P percentage by weight adds; V, N, the C VN alloy form take weight ratio as V:N:C=8:1:1 adds; B is to add as 24% ferro-boron form containing B percentage by weight;
2) raw material is put into vaccum sensitive stove melting, smelting temperature is 1550～1580 ℃, obtains master alloy ingot; Then adopt disintegrating machine that master alloy ingot is broken into alloy fragment;
3) alloy fragment is placed in liquid nitrogen and carries out K cryogenic treatment, locates temperature and is-196 ℃, is incubated 20～25 minutes; Taking-up is put at ambient temperature and is left standstill 0.5～2 hour; Alloy fragment being put into vacuum degree is again 0.05～0.0.8Pa, and it is broken that the hydrogen crushing furnace that stove internal gas pressure is 0.6～1.0atm carries out hydrogen, and temperature is heated to 250～320 ℃, and hydrogen makes fragment become meal after broken 40～60 minutes;
4) then meal is put into airflow milling and wear into fine powder, airflow milling powder pressure 6～7atm; Then fine powder is put into mould briquet, briquetting pressure is 0.02～0.06MPa;
5) take out molded part and pack sintering basin into, it is 0.01～0.04Pa that molded part is sent into vacuum degree in company with sintering basin, and temperature is the interior sintering of the sintering electric furnace of 1070～1100 ℃, is incubated power-off after 80～120 minutes, naturally cool to 800～900 ℃ with stove, then meet electricity insulation 2～3h; After again power-off be cooled to 490～500 ℃, then meet electricity insulation 3～5h, then cool to room temperature with the furnace and come out of the stove, obtain neodymium iron nitrogen phosphorus permanent magnetic material.
3. preparation method according to claim 2, is characterized in that: step 2) in disintegrating machine by master alloy ingot fragmentation to 3～6mm size alloy fragment.
4. preparation method according to claim 2, is characterized in that: in step 3), coarse granularity is 20～40 microns.
5. preparation method according to claim 2, is characterized in that: in step 4), powder particle size is 3～5 microns.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109473271A (en) * | 2018-11-08 | 2019-03-15 | 浙江嘉兴南湖电子器材集团有限公司 | A kind of magnet orientation compression moulding technique |
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Effective date of registration: 20181205 Address after: 224000 Area B of Fucheng Industrial Park, Funing County, Yancheng City, Jiangsu Province Patentee after: Jiangsu Fusheng Environmental Protection Group Co., Ltd. Address before: 210044 Ning six road, Pukou District, Nanjing, Jiangsu Province, No. 219 Patentee before: Nanjing University of Information Science and Technology |