CN103632791B - A kind of high-coercivity neodymium-iron-boronpermanent-magnet permanent-magnet material and preparation method thereof - Google Patents
A kind of high-coercivity neodymium-iron-boronpermanent-magnet permanent-magnet material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a kind of high-coercivity neodymium-iron-boronpermanent-magnet permanent-magnet material and preparation method thereof, this material has higher coercivity; This preparation method's technique is simple, and production cost is low, is suitable for suitability for industrialized production.Does is each composition by weight percent content of this material: La 3-8%, Ce 2-4%, Nd 22-25%; Co 0.5-1%, Cr 0.3-0.6%, Pb 0.5-1%, Sb 0.5-0.9%, B 0.5-1%, Si 0.5-0.7%, Sc 0.3-0.6%, all the other are Fe.
Description
Technical field
The invention belongs to metal material field, be specifically related to a kind of high-coercivity neodymium-iron-boronpermanent-magnet permanent-magnet material and preparation method thereof.
Background technology
No. CN201310218161.3 application discloses the preparation method of the shaping sintered Nd-Fe-B permanent magnetic material of a kind of carbon-dioxide protecting, and step comprises: namely the processing of batching, rejection tablet be evacuated to 0.05 ~ 0.1Pa and be heated to 1700 ~ 1800 DEG C of meltings 4 ~ 6 minutes; Namely the broken powder process of hydrogen vacuumize 0.05 ~ 0.1Pa, is heated to 100-300 DEG C, hydrogen crushing furnace internal gas pressure 0.8 ~ 1.2atm, broken 1.5 ~ 2.5 hours of hydrogen; Namely airflow milling powder controls abrasive dust pressure 5-7atm, granularity 2-5 μm; Namely shaping protection compacting is closed shaping in magnetic field, magnetic field intensity 16000-25000 oersted, and filling CO 2 gas to pressure is that 0.02-0.05MPa is shaping; Sintering and vacuum degree 0.01 ~ 0.04Pa, temperature 1020-1120 DEG C, 280 ~ 320 minutes time obtained neodymium iron boron magnetic body.
The method that compaction moulding in above-mentioned preparation method adopts cannot ensure the uniformity of material, obtained neodymium iron boron magnetic body, and its coercive force is 11.9kOe, and coercive force is lower.
Summary of the invention
Object of the present invention is exactly for above-mentioned technological deficiency, provides a kind of high-coercivity neodymium-iron-boronpermanent-magnet permanent-magnet material, and this material has higher coercive force.
Another object of the present invention is to provide a kind of high-coercivity neodymium-iron-boronpermanent-magnet permanent-magnet material preparation method, 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 high-coercivity neodymium-iron-boronpermanent-magnet permanent-magnet material, is characterized in that: in this material, the weight percentage of each composition is: La3-8%, Ce2-4%, Nd22-25%; Co0.5-1%, Cr0.3-0.6%, Pb0.5-1%, Sb0.5-0.9%, B0.5-1%, Si0.5-0.7%, Sc0.3-0.6%, all the other are Fe.
The preparation method of above-mentioned high-coercivity neodymium-iron-boronpermanent-magnet permanent-magnet material, the steps include:
(1) get La, Ce, Nd, Co, Cr, Pb, Sb, B, Si, Sc and Fe respectively according to above-mentioned percentage by weight to prepare burden, the purity of each raw material is all greater than 99.9%;
(2) raw material is put into vaccum sensitive stove melting, smelting temperature is 1660-1780 DEG C, leaves standstill and obtains foundry alloy liquid after 2-4 minute;
(3) by the transfer roller below foundry alloy liquid cast to induction furnace tapping hole, foundry alloy liquid runs into the transfer roller of rotation, is pulled form Cast Strip by transfer roller wheel rim;
(4) Cast Strip is cooled 5-10 minute naturally, then Cast Strip being put into hydrogen crushing furnace, to carry out hydrogen broken, and the vacuum degree of hydrogen crushing furnace is 0.05 ~ 0.1Pa, and stove internal gas pressure is 0.8 ~ 1.2atm; Temperature is 100-300 DEG C, and the broken 60-80 minute of hydrogen, obtains meal;
(5) meal is put into airflow milling, blown afloat by meal with high pressure draught, become fine powder, airflow milling powder pressure 5-7atm by collision each other, jet mill sorting wheel rotating speed is 3000 ~ 3300r/min;
(6) fine powder is put into the mould being provided with vibration generator, use press device to be pressed into required form, the vibration frequency of vibration generator is 15-80Hz;
(7) compressing rear taking-up molded part, load sintering basin, it is 0.01 ~ 0.04Pa that molded part is sent into vacuum degree in company with sintering basin, temperature is sinter in the sintering furnace of 1020-1120 DEG C, sinter after 280 ~ 320 minutes, after naturally cooling with stove, taking-up sinters shaped piece into and namely obtains neodymium iron boron magnetic body.
Wherein, the linear velocity of step (3) transfer running roller edge is 12-16m/s; The thickness of Cast Strip is 200-600 μm, and width is 10-30mm.In step 4, coarse granularity is 50-100 μm.In step (5), powder particle size is 2-5 μm.
In step 6, the briquetting pressure of press device is 0.02-0.05MPa; Vibration generator in step (6) comprises iron core, solenoid, armature and spring.
Material prepared by the present invention can be applicable to manufacture the fields such as instrument and meter, communication equipment, rotating machinery, magnetotherapy appliance.
the present invention has following beneficial effect compared to existing technology:
In permanent magnetic material of the present invention, La and Ce element enters in Nd matrix phase in the mode of doping or replacement.Sb, Co, La, Ce and Sc element in material is the important Addition ofelements of a class, and it can significantly improve the coercive force of sintered Nd-Fe-B permanent magnet, and it is can suppress grain growth, crystal grain thinning that these elements improve coercitive main cause, the coupling of isolation crystal grain.Pb replaces part B atom, can crystal grain thinning, improves material remanent magnetism.Si and Cr element can improve Curie temperature, oxidation resistance and corrosion resistance.
Preparation method of the present invention adopts material composition optimization and the molded mode that combines of shaking.Mould is provided with vibration generator, and vibration generator comprises iron core, solenoid, armature and spring.When energized, produce electromagnetic force at unshakable in one's determination and armature residual gap, the sheet iron strip that shakes on attraction base plate unshakable in one's determination moves base plate and moves upward, and spring is compressive state.When coil losing electricity, the magnetic field dissipate of calutron, shake iron and base plate whereabouts under spring force, spring reset, micro-vibration when realizing shaping.The tightness degree of material at compaction moulding can be ensured like this, ensure that the homogenization of composition of permanent magnetic material and the homogeneity of performance.
In preparation process of the present invention, rare element trace used, cost of material is lower; Adopt material composition optimization and molded combining of shaking in addition, ensure that the uniformity of permanent magnetic material composition, structure and properties, ensure that the quality of permanent magnetic material, products obtained therefrom has high-coercive force.Permanent magnetic material preparation technology of the present invention is simple, and the permanent magnetic material of production has good performance, is very convenient to suitability for industrialized production.
Material prepared by the present invention can be applicable to manufacture the fields such as instrument and meter, communication equipment, rotating machinery, magnetotherapy appliance.
Accompanying drawing explanation
Fig. 1 is the organization chart of permanent magnetic material of the present invention.
As seen from Figure 1, high-coercivity neodymium-iron-boronpermanent-magnet permanent-magnet material dense structure of the present invention is even.
Embodiment
embodiment one:
High-coercivity neodymium-iron-boronpermanent-magnet permanent-magnet material preparation method of the present invention, concrete steps are as follows:
(1) La3% is got respectively according to following weight percentage, Ce2%, Nd22%; Co0.5%, Cr0.3%; Pb0.5%, B0.5%, Si0.5%, Sc0.3%, Sb0.5%, all the other are prepared burden for Fe; Wherein the purity of La, Ce, Nd, Co, Cr, Pb, Sb, B, Si, Sc and Fe is all greater than 99.9%;
(2) raw material is put into vaccum sensitive stove melting, smelting temperature is 1660 DEG C, leaves standstill and obtains foundry alloy liquid after 2 minutes;
(3) by the transfer roller below foundry alloy liquid cast to induction furnace tapping hole, foundry alloy liquid runs into the transfer roller of rotation, is pulled form Cast Strip by transfer roller wheel rim; The linear velocity of transfer roller wheel rim is 12m/s; The thickness of Cast Strip is about 200 μm, and width is about 10mm;
(4) Cast Strip is cooled 5 minutes naturally, then Cast Strip being put into hydrogen crushing furnace, to carry out hydrogen broken, and the vacuum degree of hydrogen crushing furnace is 0.05Pa, and stove internal gas pressure is 0.8atm; Temperature is 100 DEG C, broken 60 minutes of hydrogen, and obtain meal, granularity is about 50 μm;
(5) meal is put into airflow milling, blown afloat by meal with high pressure draught, become fine powder, airflow milling powder pressure 5atm by collision each other, jet mill sorting wheel rotating speed is 3000r/min; Powder particle size is about 2 μm;
(6) fine powder is put into the mould being provided with vibration generator, use press device to be pressed into required form, the vibration frequency of vibration generator is 15Hz, and the briquetting pressure of press device is 0.02MPa; Vibration generator comprises iron core, solenoid, armature and spring, when energized, electromagnetic force is produced at unshakable in one's determination and armature residual gap, the sheet iron strip that shakes on attraction base plate unshakable in one's determination moves base plate and moves upward, spring is compressive state, when coil losing electricity, and the magnetic field dissipate of calutron, shake iron and base plate whereabouts under spring force, spring reset;
(7) compressing rear taking-up molded part, load sintering basin, it is 0.01Pa that molded part is sent into vacuum degree in company with sintering basin, and temperature is sinter in the sintering furnace of 1020 DEG C, sinter after 280 minutes, after naturally cooling with stove, taking-up sinters shaped piece into and namely obtains neodymium iron boron magnetic body.
embodiment two:
High-coercivity neodymium-iron-boronpermanent-magnet permanent-magnet material preparation method of the present invention, concrete steps are as follows:
(1) La8% is got respectively according to following weight percentage, Ce4%, Nd25%, Co1%, Cr0.6%; Pb1%, B1%, Si0.7%, Sc0.6%, Sb0.9%, all the other are prepared burden for Fe; Wherein the purity of La, Ce, Nd, Co, Cr, Pb, Sb, B, Si, Sc and Fe is all greater than 99.9%;
(2) raw material is put into vaccum sensitive stove melting, smelting temperature is 1700 DEG C, leaves standstill and obtains foundry alloy liquid after 3 minutes;
(3) by the transfer roller below foundry alloy liquid cast to induction furnace tapping hole, foundry alloy liquid runs into the transfer roller of rotation, is pulled form Cast Strip by transfer roller wheel rim; The linear velocity of transfer roller wheel rim is 14m/s; The thickness of Cast Strip is about 400 μm, and width is about 20mm;
(4) Cast Strip is cooled 8 minutes naturally, then Cast Strip being put into hydrogen crushing furnace, to carry out hydrogen broken, and the vacuum degree of hydrogen crushing furnace is 0.07Pa, and stove internal gas pressure is 1.0atm; Temperature is 200 DEG C, broken 70 minutes of hydrogen, and obtain meal, granularity is about 80 μm;
(5) meal is put into airflow milling, blown afloat by meal with high pressure draught, become fine powder, airflow milling powder pressure 6atm by collision each other, jet mill sorting wheel rotating speed is 3100r/min; Powder particle size is about 4 μm;
(6) fine powder is put into the mould being provided with vibration generator, use press device to be pressed into required form, the vibration frequency of vibration generator is 50Hz, and the briquetting pressure of press device is 0.03MPa; Vibration generator comprises iron core, solenoid, armature and spring, when energized, electromagnetic force is produced at unshakable in one's determination and armature residual gap, the sheet iron strip that shakes on attraction base plate unshakable in one's determination moves base plate and moves upward, spring is compressive state, when coil losing electricity, and the magnetic field dissipate of calutron, shake iron and base plate whereabouts under spring force, spring reset.
(7) compressing rear taking-up molded part, load sintering basin, it is 0.02Pa that molded part is sent into vacuum degree in company with sintering basin, and temperature is sinter in the sintering furnace of 1080 DEG C, sinter after 300 minutes, after naturally cooling with stove, taking-up sinters shaped piece into and namely obtains neodymium iron boron magnetic body.
embodiment three:
High-coercivity neodymium-iron-boronpermanent-magnet permanent-magnet material preparation method of the present invention, concrete steps are as follows:
(1) get La5% respectively according to following weight percentage, Ce3%, Nd23%, Co0.8%, Cr0.5%, Pb0.7%, B0.8%, Si0.6%, Sc0.4%, Sb0.7%, all the other are prepared burden for Fe; Wherein the purity of La, Ce, Nd, Co, Cr, Pb, Sb, B, Si, Sc and Fe is all greater than 99.9%;
(2) raw material is put into vaccum sensitive stove melting, smelting temperature is 1780 DEG C, leaves standstill and obtains foundry alloy liquid after 4 minutes;
(3) by the transfer roller below foundry alloy liquid cast to induction furnace tapping hole, foundry alloy liquid runs into the transfer roller of rotation, is pulled form Cast Strip by transfer roller wheel rim; The linear velocity of transfer roller wheel rim is 16m/s; The thickness of Cast Strip is about 600 μm, and width is about 30mm.
(4) Cast Strip is cooled 10 minutes naturally, then Cast Strip being put into hydrogen crushing furnace, to carry out hydrogen broken, and the vacuum degree of hydrogen crushing furnace is 0.1Pa, and stove internal gas pressure is 1.2atm; Temperature is 300 DEG C, broken 80 minutes of hydrogen, and obtain meal, granularity is about 100 μm;
(5) meal is put into airflow milling, blown afloat by meal with high pressure draught, become fine powder, airflow milling powder pressure 7atm by collision each other, jet mill sorting wheel rotating speed is 3300r/min; Powder particle size is about 5 μm.
(6) fine powder is put into the mould being provided with vibration generator, use press device to be pressed into required form, the vibration frequency of vibration generator is 80Hz, and the briquetting pressure of press device is 0.05MPa; Vibration generator comprises iron core, solenoid, armature and spring, when energized, electromagnetic force is produced at unshakable in one's determination and armature residual gap, the sheet iron strip that shakes on attraction base plate unshakable in one's determination moves base plate and moves upward, spring is compressive state, when coil losing electricity, and the magnetic field dissipate of calutron, shake iron and base plate whereabouts under spring force, spring reset.
(7) compressing rear taking-up molded part, load sintering basin, it is 0.04Pa that molded part is sent into vacuum degree in company with sintering basin, and temperature is sinter in the sintering furnace of 1120 DEG C, sinter after 320 minutes, after naturally cooling with stove, taking-up sinters shaped piece into and namely obtains neodymium iron boron magnetic body.
embodiment four:(composition proportion not the present invention relates in proportion)
Each Ingredients Weight percentage composition in high-coercivity neodymium-iron-boronpermanent-magnet permanent-magnet material of the present invention: La2%, Ce1%, Nd20%; Co0.4%, Cr0.2%, Pb0.2%, B0.3%, Si0.2%, Sc0.1%, Sb0.3%, all the other are prepared burden for Fe; Its preparation process is with embodiment one.
embodiment five:(composition proportion not the present invention relates in proportion)
Each Ingredients Weight percentage composition in high-coercivity neodymium-iron-boronpermanent-magnet permanent-magnet material of the present invention: La9%, Ce6%, Nd29%; Co2%, Cr0.9%, Pb1.1%, B1.2%, Si0.8%, Sc0.7%, Sb1%, all the other are prepared burden for Fe; Its preparation process is with embodiment one.
Table one
As can be seen from the above table, add La, Ce, Nd, Co, Cr, Pb, Sb, B, Si, Sc element to contribute to alloy there is coercitive raising.But exceed the scope that this case specifies, not only coercive force does not improve, and reduces on the contrary.Reason is these element meetings and the formation non-magnetic compound that reacts to each other, and reduces the useful effect of element itself.
Claims (7)
1. a high-coercivity neodymium-iron-boronpermanent-magnet permanent-magnet material, is characterized in that: in this material, the weight percentage of each composition is: La3-8%, Ce2-4%, Nd22-25%; Co0.5-1%, Cr0.3-0.6%, Pb0.5-1%, Sb0.5-0.9%, B0.5-1%, Si0.5-0.7%, Sc0.3-0.6%, all the other are Fe.
2. the preparation method of high-coercivity neodymium-iron-boronpermanent-magnet permanent-magnet material described in claim 1, the steps include:
(1) get La, Ce, Nd, Co, Cr, Pb, Sb, B, Si, Sc and Fe respectively according to percentage by weight to prepare burden, the purity of each raw material is all greater than 99.9%;
(2) raw material is put into vaccum sensitive stove melting, smelting temperature is 1660-1780 DEG C, leaves standstill and obtains foundry alloy liquid after 2-4 minute;
(3) by the transfer roller below foundry alloy liquid cast to induction furnace tapping hole, foundry alloy liquid runs into the transfer roller of rotation, is pulled form Cast Strip by transfer roller wheel rim;
(4) Cast Strip is cooled 5-10 minute naturally, then Cast Strip being put into hydrogen crushing furnace, to carry out hydrogen broken, and the vacuum degree of hydrogen crushing furnace is 0.05 ~ 0.1Pa, and stove internal gas pressure is 0.8 ~ 1.2atm; Temperature is 100-300 DEG C, and the broken 60-80 minute of hydrogen, obtains meal;
(5) meal is put into airflow milling, blown afloat by meal with high pressure draught, become fine powder, airflow milling powder pressure 5-7atm by collision each other, jet mill sorting wheel rotating speed is 3000 ~ 3300r/min;
(6) fine powder is put into the mould being provided with vibration generator, use press device to be pressed into required form, the vibration frequency of vibration generator is 15-80Hz;
(7) compressing rear taking-up molded part, load sintering basin, it is 0.01 ~ 0.04Pa that molded part is sent into vacuum degree in company with sintering basin, temperature is sinter in the sintering furnace of 1020-1120 DEG C, sinter after 280 ~ 320 minutes, after naturally cooling with stove, taking-up sinters shaped piece into and namely obtains neodymium-iron-boron permanent magnetic material.
3. preparation method according to claim 2, is characterized in that: the linear velocity of described step (3) transfer running roller edge is 12-16m/s; The thickness of Cast Strip is 200-600 μm, and width is 10-30mm.
4. the preparation method according to Claims 2 or 3, is characterized in that: in step 4, coarse granularity is 50-100 μm.
5. the preparation method according to Claims 2 or 3, is characterized in that: in step (5), powder particle size is 2-5 μm.
6. the preparation method according to Claims 2 or 3, is characterized in that: in step 6, the briquetting pressure of press device is 0.02-0.05MPa.
7. preparation method according to claim 6, is characterized in that: the vibration generator in described step (6) comprises iron core, solenoid, armature and spring.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1056599A (en) * | 1990-05-14 | 1991-11-27 | 北京科瑞德特钕磁体有限公司 | The prescription of Cd rare-earth permanent-magnet alloy and manufacture method thereof |
| CN103377820A (en) * | 2013-07-17 | 2013-10-30 | 烟台首钢磁性材料股份有限公司 | R-T-B-M sintered magnet and production method thereof |
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| CN1056599A (en) * | 1990-05-14 | 1991-11-27 | 北京科瑞德特钕磁体有限公司 | The prescription of Cd rare-earth permanent-magnet alloy and manufacture method thereof |
| CN103377820A (en) * | 2013-07-17 | 2013-10-30 | 烟台首钢磁性材料股份有限公司 | R-T-B-M sintered magnet and production method thereof |
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Denomination of invention: High-coercivity neodymium-iron-boron permanent-magnet material and preparation method thereof Effective date of registration: 20180724 Granted publication date: 20160120 Pledgee: Sichuan Jiang copper rare earth magnet Co., Ltd. Pledgor: Zhang Zuozhou|Jiangsu Nanfang Permanent Magnetic Technology Co., Ltd. Registration number: 2018990000587 |
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Date of cancellation: 20190823 Granted publication date: 20160120 Pledgee: Sichuan Jiang copper rare earth magnet Co., Ltd. Pledgor: Jiangsu Nanfang Permanent Magnetic Technology Co., Ltd. Registration number: 2018990000587 |