CN106887322B - A kind of method of high-efficiency production of nano crystalline substance rare earth permanent magnet powder - Google Patents

A kind of method of high-efficiency production of nano crystalline substance rare earth permanent magnet powder Download PDF

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CN106887322B
CN106887322B CN201710122712.4A CN201710122712A CN106887322B CN 106887322 B CN106887322 B CN 106887322B CN 201710122712 A CN201710122712 A CN 201710122712A CN 106887322 B CN106887322 B CN 106887322B
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rare earth
permanent magnet
earth permanent
liquation
smelting
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CN106887322A (en
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高学绪
牟星
包小倩
***
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University of Science and Technology Beijing USTB
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University of Science and Technology Beijing USTB
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22DCASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D11/00Continuous casting of metals, i.e. casting in indefinite lengths
    • B22D11/06Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars
    • B22D11/0611Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars formed by a single casting wheel, e.g. for casting amorphous metal strips or wires
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22DCASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D11/00Continuous casting of metals, i.e. casting in indefinite lengths
    • B22D11/06Continuous casting of metals, i.e. casting in indefinite lengths into moulds with travelling walls, e.g. with rolls, plates, belts, caterpillars
    • B22D11/0637Accessories therefor
    • B22D11/064Accessories therefor for supplying molten metal
    • B22D11/0642Nozzles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C45/00Amorphous alloys

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Power Engineering (AREA)
  • Nanotechnology (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Composite Materials (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Hard Magnetic Materials (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The invention belongs to technical field of magnetic materials, and in particular to a kind of method of high-efficiency production of nano crystalline substance rare earth permanent magnet powder.Its preparation process includes smelting furnace master alloy melting, holding furnace to the step such as the secondary smelting of foundry alloy and insulation, spray band, Crystallizing treatment and powder processed.Wherein, using hundreds of kilograms of foundry alloys of the disposable melting of smelting furnace, reduce melting batch, reduce multiple melting caused by time cost, improve the uniformity of foundry alloy;Using holding furnace secondary smelting and insulation, overturn by the flowing of liquation, promote the homogenization of foundry alloy liquation, improve the quality of foundry alloy liquation;The discharge of foundry alloy liquation is increased using jet rose, improves production efficiency.Finally, the good rare earth permanent magnet powder of high-volume, low cost, high efficiency production homogeneity can be achieved.

Description

A kind of method of high-efficiency production of nano crystalline substance rare earth permanent magnet powder
Technical field
The present invention principally falls into technical field of magnetic materials, and in particular to a kind of high-efficiency production of nano crystalline substance rare earth permanent magnet powder Method.
Background technology
Rare earth permanent-magnetic material is that the alloy formed by rare earth metal and magnesium-yttrium-transition metal is process, wherein Nd Fe B alloys It is comprehensive magnetic energy highest, the rare earth permanent-magnetic material that application is most wide, with the fastest developing speed.Nd-Fe-B permanent magnet material is from preparation It is main from the point of view of method to be divided to sintering and bond two major classes.Sintered Nd-Fe-B permanent magnetic material is manufactured using the method for powder metallurgy, bag Include the techniques such as rapid hardening slab, powder processed, shaping, sintering heat treatment, machining.Binding Nd-Fe-B permanent magnetic material is then by Nd-Fe-B powder End and binding agent mix by a certain percentage, then through being molded, injecting, extrusion calendaring the methods of technique be prepared.
Bonding process can prepare the Nd-Fe-B permanent magnet material that dimensional accuracy is high, complex-shaped or special, and production efficiency It is high.The magnetic property of binding Nd-Fe-B permanent magnetic material depends primarily on the microstructure and magnetic property of magnetic, and this and rare earth permanent magnet The preparation method of powder is closely related.It is to prepare to bond magnetic, prepared material property after permanent magnet ingot casting directly crushes in early days It is very poor, no industrialization value.Widely used method is quick quenching technique now, be U.S. GM (General Motors Corporation) concentrate strength on through Crossing the 6th generation equipment of the technological improvement of five essence just realizes the industrialization production of rapidly quenched magnetic powder.The technique is in vacuum In fast quenching equipment, protected with inert gas, melt foundry alloy in quartz ampoule, in the presence of argon pressure, foundry alloy Nozzle of the liquation through quartzy bottom of the tube is ejected at a high speed on the surface of the copper roller of rotation, with about 105~106DEG C/s cooling velocity Quick solidification, forms rare earth permanent magnet amorphous thin ribbon, then via being fabricated to nanocrystalline rare-earth permanent magnetism powder after Crystallizing treatment.But this method Yield and less efficient.
The efficiency of amorphous nano-crystalline neodymium iron boron strip is prepared for quick quenching technique in current industrial production and yield is relatively low asks Topic, the present invention propose a kind of method of high-efficiency production of nano crystalline substance rare earth permanent magnet powder.
The content of the invention
The present invention provides a kind of method of high-efficiency production of nano crystalline substance rare earth permanent magnet powder.Rare earth can be realized forever by this method The high-volume of magnetic, continuous production, the yield of rare earth permanent magnet powder is improved, reduce production cost, improve production efficiency.
To solve technical problem, the present invention adopts the following technical scheme that:
1. master alloy melting:Required raw material are arranged into smelting furnace B1 according to ratio requirement, smelting furnace B1 can Hundreds of kilograms of raw materials of disposable melting;1280~1580 DEG C of smelting temperature.
2. secondary smelting and the insulation of foundry alloy liquation:To improve the quality of foundry alloy liquation, foundry alloy liquation is carried out Secondary smelting;Foundry alloy liquation in smelting furnace B1 can be poured among holding furnace B2 via verting for smelting furnace B1;Smelting furnace B1 In foundry alloy can also enter holding furnace B2 by way of rising pouring;Holding furnace B2 temperature control is protected at 1250~1550 DEG C Warm 20~50min of time.
3. spray band:Foundry alloy liquation flows into tundish B4 via holding furnace B2, and the mode for flowing into tundish B4 can be via guarantor Warm stove B2's verts or is injected from holding furnace B2 bottoms, and two ways is required for entering tundish B4 by guiding gutter B3;Water conservancy diversion Groove B3 is provided with attemperator, ensures the temperature stabilization of foundry alloy liquation;Tundish B4 capacity limit in 10kg~100kg, with The fluctuation of melt flow is reduced, or melt flow is adjusted using argon gas control pressure;It is female using stopper C1 elevating control The bet of alloy melt;Tundish B4 divides into jet rose B5, each 10~20mm of aperture of jet rose B5;Mother alloy melt passes through The copper roller B6 of rotation at a high speed is flowed to by jet rose B5, controls roller 10~50m/s of speed, so as to which rare earth permanent magnet amorphous band be made.
4. crystallization and thermal treatment and powder processed:The rare earth permanent magnet amorphous nanocrystalline strip fallen in collecting vessel B7 is loaded into crystallization heat In treatment furnace, 550~750 DEG C of heat treatment temperature, 5~60min of soaking time;Powder processed is crushed after the completion of crystallization.
Because rare earth permanent magnet easily aoxidizes, above-mentioned steps need to carry out in vacuum environment A1.
The invention has the advantages that:
1. the present invention using smelting furnace can disposable hundreds of kilograms of melting rare earth permanent magnet raw material, can effectively subtract The time cost that band is once brought once is sprayed in few traditional handicraft melting, is the basis that high-volume efficiently produces rare earth permanent magnet powder.
2. present invention increase holding furnace carries out secondary smelting and insulation, turn by foundry alloy liquation from smelting furnace to holding furnace Flowing upset during shifting, can further remove the impurity among foundry alloy liquation, be more beneficial for obtaining the mother of high quality Alloy molten solution.
3. technique provided by the present invention can obtain the foundry alloy liquation of high quality, and using the centre of low capacity Bag, ensure the stabilization of melt flow during spray band.Therefore the quality of the rare earth permanent magnet powder prepared by the present invention is more stable, performance is consistent Property it is high.
4. present invention employs jet rose, it is more beneficial for improving the output in the unit interval.
5. the consumptive materials such as the tundish among the present invention can effectively reduce production cost with repeated multiple times utilization.
Brief description of the drawings
Fig. 1 is the schematic diagram of embodiment of the present invention.
Fig. 2 is the schematic diagram of jet rose in implementation case of the present invention.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention It is explained in further detail.It should be appreciated that specific embodiment described herein is used only for explaining the present invention, it is not used to Limit the present invention.
On the contrary, the present invention covers any replacement done in the spirit and scope of the present invention being defined by the claims, repaiied Change, equivalent method and scheme.Further, in order that the public has a better understanding to the present invention, below to the thin of the present invention It is detailed to describe some specific detail sections in section description.Part without these details for a person skilled in the art Description can also understand the present invention completely.
Embodiment 1:
A kind of method of high-efficiency production of nano crystalline substance rare earth permanent magnet powder, its step are as follows:
1. master alloy melting:Required raw material are arranged into smelting furnace B1 according to ratio requirement, smelting furnace B1's Raw material quality 500kg;To avoid rare earth permanent-magnetic material from being oxidized, the process of master alloy melting is needed under vacuum anaerobic environment Carry out;1480 DEG C of smelting temperature.
2. secondary smelting and the insulation of foundry alloy liquation:To improve the quality of foundry alloy liquation, foundry alloy liquation is carried out Secondary smelting;Foundry alloy liquation in smelting furnace B1 is poured among holding furnace B2 via verting for smelting furnace B1;Holding furnace B2's Temperature control is at 1450 DEG C, soaking time 25min.
3. spray band:Foundry alloy liquation enters tundish B4 via guiding gutter B3;Tundish B4 capacity is 50kg;Tundish B4 divides into jet rose B5, each aperture 10mm of jet rose B5;Lifting stopper C1 makes mother alloy melt bet;Mother alloy melt The copper roller B6 of rotation at a high speed is flowed to via jet rose B5, roller speed 20m/s is controlled, obtains rare earth permanent magnet amorphous band.
4. crystallization and thermal treatment and powder processed:The rare earth permanent magnet amorphous band fallen in collecting vessel B7 is loaded into Crystallizing thermal treatment furnace In, 650 DEG C of crystallization and thermal treatment temperature, soaking time 30min;Powder processed is crushed after the completion of crystallization.
Because rare earth permanent magnet easily aoxidizes, above-mentioned steps need to carry out in vacuum environment A1.
The time that the present embodiment prepares 500kg nanocrystalline rare-earth permanent magnetism powders is 305min, and traditional handicraft needs 950min.
Embodiment 2:
1. master alloy melting:Required raw material are arranged into smelting furnace B1 according to ratio requirement, in smelting furnace B1 Raw material quality 800kg;To avoid rare earth permanent-magnetic material from being oxidized, the process of master alloy melting is needed in vacuum anaerobic environment Lower progress;About 1450 DEG C of smelting temperature.
2. secondary smelting and the insulation of foundry alloy liquation:To improve the quality of foundry alloy liquation, foundry alloy liquation is carried out Secondary smelting;Foundry alloy in smelting furnace B1 enters holding furnace B2 by way of rising pouring;Holding furnace B2 temperature control exists 1420 DEG C, soaking time 50min.
3. spray band:Foundry alloy liquation flows into tundish B4 from holding furnace B2 bottoms via guiding gutter B3, and its inflow can pass through Stopper is added in holding furnace B2, by the elevating control of stopper;Tundish B4 capacity limit can use argon gas to control in 80kg Pressure controls melt flow;Tundish B4 divides into jet rose B5, each aperture 12mm of jet rose B5;Lifting stopper C1 makes Mother alloy melt is betted;Mother alloy melt flows to the copper roller B6 of rotation at a high speed via jet rose B5, controls roller speed 28m/s, from And rare earth permanent magnet amorphous band is made.
4. crystallization and thermal treatment and powder processed:The rare earth permanent magnet amorphous band fallen in collecting vessel B7 is loaded into Crystallizing thermal treatment furnace In, 700 DEG C of heat treatment temperature, soaking time 20min;Powder processed is crushed after the completion of crystallization.
Among the technique, all devices all use sealed connection, it is only necessary to each device are vacuumized, without providing Overall vacuum environment.
The time that the present embodiment prepares 800kg nanocrystalline rare-earth permanent magnetism powders is 390min, and traditional handicraft needs 1430min。

Claims (2)

  1. A kind of 1. method of high-efficiency production of nano crystalline substance rare earth permanent magnet powder, it is characterised in that:
    1) master alloy meltings:Required raw material are arranged into smelting furnace B1 according to ratio requirement, smelting furnace B1 is disposable Hundreds of kilograms of raw materials of melting;
    2) secondary smelting of foundry alloys liquation and insulation:Secondary smelting is carried out to foundry alloy liquation;Foundry alloy in smelting furnace B1 Liquation is poured among holding furnace B2 via verting for smelting furnace B1, or enters holding furnace B2 by way of rising pouring;
    3) sprays band:Foundry alloy liquation flows into tundish B4 via holding furnace B2, and the mode for flowing into tundish B4 is by holding furnace B2 Vert or injected from holding furnace B2 bottoms, two ways is required for entering tundish B4 by guiding gutter B3;Guiding gutter B3 is set There is attemperator, ensure the temperature stabilization of foundry alloy liquation;Tundish B4 capacity limit is molten to reduce in 10kg~100kg The fluctuation of rate of flow of fluid, or melt flow is adjusted using argon gas control pressure;Melted using stopper C1 elevating control foundry alloy The bet of body;Tundish B4 divides into jet rose B5, and mother alloy melt flows to the copper roller B6 of rotation at a high speed via jet rose B5, So as to which rare earth permanent magnet amorphous band be made;
    4) crystallization and thermal treatments and powder processed:The rare earth permanent magnet amorphous nanocrystalline strip fallen in collecting vessel B7 is loaded at crystallization heat Manage in stove, powder processed is crushed after the completion of crystallization;
    Described preparation process is required for carrying out in vacuum environment A1;
    1280~1580 DEG C of the smelting temperature of step 1) master alloy melting;
    Step 2) holding furnace B2 temperature control is at 1250~1550 DEG C, 20~50min of soaking time;
    Each 10~the 20mm of aperture of step 3) the jet rose B5;The copper roller B6 of rotation roller speed is 10~50m/s at a high speed.
  2. A kind of 2. method of high-efficiency production of nano crystalline substance rare earth permanent magnet powder as claimed in claim 1, it is characterised in that:Step 4) is described Heat treatment temperature is 550~750 DEG C, 5~60min of soaking time.
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WO2020097937A1 (en) * 2018-11-16 2020-05-22 青岛云路先进材料技术股份有限公司 Atomization comminuting apparatus and atomization comminuting method
CN112331468A (en) * 2020-10-14 2021-02-05 宁波韵升股份有限公司 Preparation method of high-remanence sintered neodymium-iron-boron magnet

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CN1442253A (en) * 2002-03-06 2003-09-17 北京有色金属研究总院 Equipment for quick cooling thick alloy belt and preparation method using said equipment and its product
CN102665962A (en) * 2009-12-01 2012-09-12 株式会社爱发科 Vacuum melting and casting device
CN102266924A (en) * 2011-07-09 2011-12-07 中国铝业股份有限公司 Continuous cast-rolling process for producing 5005 aluminum plastic strip billet
CN103111624A (en) * 2013-03-18 2013-05-22 江苏巨鑫磁业有限公司 Preparation method of iron-based low-rare earth NdFeB rapid quenching permanent magnetic powder
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CN106378428A (en) * 2016-10-08 2017-02-08 江苏国能合金科技有限公司 Mobile smelting furnace amorphous thin ribbon production overall machine system structure and control method thereof

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