CN114101686A - Treatment method of neodymium iron boron oxidation blank - Google Patents

Treatment method of neodymium iron boron oxidation blank Download PDF

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Publication number
CN114101686A
CN114101686A CN202111321672.9A CN202111321672A CN114101686A CN 114101686 A CN114101686 A CN 114101686A CN 202111321672 A CN202111321672 A CN 202111321672A CN 114101686 A CN114101686 A CN 114101686A
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neodymium
iron boron
neodymium iron
oxidized
boron
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CN114101686B (en
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韩海军
崔金玉
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Sino Magnetics Technology Co Ltd
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Sino Magnetics Technology Co Ltd
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    • 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
    • B22F9/023Hydrogen absorption
    • 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
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02Compacting only
    • 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
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/1017Multiple heating or additional steps
    • 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
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24After-treatment of workpieces or articles
    • 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
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24After-treatment of workpieces or articles
    • B22F2003/248Thermal after-treatment
    • 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
    • B22F2009/045Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by other means than ball or jet milling

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Hard Magnetic Materials (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

The invention relates to the field of neodymium iron boron magnetic materials, and discloses a method for processing a neodymium iron boron oxidized blank, which comprises the following steps: the oxidation blank and the same performance grade raw material are proportioned according to the proportion of 1:9, are smelted and cast into a neodymium-iron-boron alloy cast sheet, and then a certain proportion of blocky praseodymium and neodymium are added to carry out hydrogen crushing, jet milling, profiling and sintering to obtain the neodymium-iron-boron magnet. The treatment method can eliminate the oxidation substances in the oxidation blank, ensure the full hydrogen absorption, avoid the occurrence of large-size hard nucleus particles, reduce the average granularity of airflow milling, improve the formability of fine powder, avoid impurities, improve the product quality, effectively protect a feeder and a grading wheel of airflow milling equipment, and reduce the maintenance cost.

Description

Treatment method of neodymium iron boron oxidation blank
Technical Field
The invention relates to the field of neodymium iron boron magnetic materials, in particular to a method for processing a neodymium iron boron oxidized blank.
Background
The neodymium iron boron magnetic material has higher requirement on the oxygen content of the environment where the material is located in the production process, all production processes must be in an oxygen-free environment, otherwise, the neodymium iron boron magnetic material has an oxidation phenomenon and becomes an oxidation blank after being sintered. The handling of these oxidized blanks is then a problem that needs to be solved by the respective manufacturers of neodymium-iron-boron magnetic materials. At present, part of manufacturers realize recycling by a method of carrying out surface treatment, hydrogen crushing, airflow milling, powder pressing and sintering on unqualified products generated in the production process of the neodymium iron boron magnetic material into qualified blanks. However, if the oxidized boule is also treated exactly as above, the following problems may occur:
1. the oxidation blank in the prior art cannot be eliminated by the existing method, the produced product still can be influenced by the oxidation, and the product performance is low in qualification rate;
2. the inside oxide of oxidation blank hardly reacts with hydrogen and realizes the hydrogen breakage, makes crushing effect not good, and the air current crocus average particle size after the jet mill is big, and formability is poor, can appear impurity of certain degree, influences product quality.
3. Because the oxidized substances in the oxidized blank are difficult to be broken by hydrogen, large-size hard nucleus particles are easy to appear, the hard nucleus particles can damage a feeder and a grading wheel of the jet mill equipment, and the maintenance cost is high.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Disclosure of Invention
The invention aims to provide a neodymium iron boron oxidation blank processing method, which aims to solve the problem of processing the oxidation blank generated in the production process of the neodymium iron boron magnetic material at present.
In order to achieve the purpose, the invention provides a method for processing a neodymium iron boron oxidized blank, which is characterized by comprising the following steps of:
the first step is as follows: classifying the neodymium iron boron oxidized blanks according to the grade numbers of the neodymium iron boron, and storing the neodymium iron boron oxidized blanks respectively;
the second step is that: preparing raw material components corresponding to the grades according to the grades of the classified neodymium iron boron oxidized blanks;
the third step: adding neodymium iron boron oxidized blanks corresponding to the grades into a certain grade of raw material components, and then smelting and casting to prepare neodymium iron boron alloy cast sheets;
the fourth step: adding blocky praseodymium-neodymium into the neodymium-iron-boron alloy cast sheet, and then carrying out hydrogen crushing;
the fifth step: carrying out airflow milling on the hydrogen broken powder after hydrogen breaking to prepare powder, pressing and sintering the powder to obtain a neodymium iron boron magnet;
and a sixth step: and repeating the operation from the third step to the fifth step for other classified neodymium iron boron oxidized blanks.
In an embodiment of the present invention, in the third step, the neodymium iron boron oxidized blank accounts for 10% of the total mass of the neodymium iron boron oxidized blank and the corresponding grade raw material component.
In an embodiment of the present invention, in the fourth step, the mass of the added block praseodymium-neodymium is 1.0% to 2.0% of the sum of the mass of the ndfeb alloy cast sheet and the mass of the added block praseodymium-neodymium. Specifically, when the neodymium iron boron oxidation blank belongs to an H series number, the mass of the added block praseodymium neodymium is 1% -1.5% of the mass sum of the neodymium iron boron alloy cast sheet and the added block praseodymium neodymium, and taking 40H as an example, the added block praseodymium neodymium is 1.5% of the mass sum of the neodymium iron boron alloy cast sheet and the added block praseodymium neodymium; when the neodymium iron boron oxidation blank belongs to N series, the mass of the added block praseodymium neodymium is 1.5% -2.0% of the mass sum of the neodymium iron boron alloy cast sheet and the added block praseodymium neodymium.
In an embodiment of the present invention, the hydrogen fragmentation in the fourth step comprises: absorbing hydrogen for 6 hours in a hydrogen environment with the pressure of 0.04MPa, dehydrogenating in a temperature environment of 610 ℃, and finishing hydrogen crushing when the vacuum degree is more than 10 Pa.
In an embodiment of the present invention, the process of milling the powder by the gas flow in the fifth step comprises: the rotating speed of a grading wheel is 2400r/min, and a lubricant with a mass ratio of four parts per million is added into the powder for mixing for 6 hours in the air-flow milling process; the pressing process comprises the steps of placing mixed fine powder after air flow grinding in a magnetic field for orientation and isostatic pressing, wherein the magnetic field intensity is 1.2T, the isostatic pressing pressure is 220MPa, and the isostatic pressing time is 40 seconds; the sintering process comprises the following steps: firstly sintering at 1110 ℃, carrying out primary tempering at 940 ℃, and carrying out secondary tempering at 640 ℃ to obtain the neodymium iron boron magnet.
Compared with the prior art, the invention has the advantages that:
the method can eliminate the oxide inside the oxidized blank, ensure the full hydrogen absorption, avoid the occurrence of large-size hard core particles, reduce the average particle size of airflow milled powder, improve the formability of fine powder, avoid impurities and improve the product quality. Meanwhile, the feeder and the grading wheel of the jet mill equipment can be effectively protected, and the maintenance cost is reduced.
Drawings
Fig. 1 is a process flow diagram of a method for treating an oxidized blank of ndfeb according to an embodiment of the present invention.
Detailed Description
The following detailed description of the present invention is provided in conjunction with the accompanying drawings, but it should be understood that the scope of the present invention is not limited to the specific embodiments.
Throughout the specification and claims, unless explicitly stated otherwise, the word "comprise", or variations such as "comprises" or "comprising", will be understood to imply the inclusion of a stated element or component but not the exclusion of any other element or component.
Example 1
A neodymium iron boron oxidation blank treatment method is disclosed, the technological process is shown in figure 1, the neodymium iron boron oxidation blanks are classified according to neodymium iron boron brand, and are respectively stored, for example, the brand of a certain neodymium iron boron oxidation blank is 40H, the weight of the neodymium iron boron oxidation blank is 65 kg, 585 kg of raw material components with neodymium iron boron 9 times of mass is prepared according to the standard of 40H performance brand, the neodymium iron boron oxidation blank is added into the raw material components, 650 kg (10% of the raw material components of the neodymium iron boron oxidation blank and 90%) is added into a flail furnace according to the standard requirement to be smelted and cast into neodymium iron boron alloy cast sheets, the yield is considered, the cast neodymium iron boron alloy cast sheets are 640 kg, then 9.75 kg of blocky praseodymium neodymium is added according to the proportion of 1.5% of the mass, hydrogen absorption is carried out for 6 hours under the pressure hydrogen environment with the pressure of more than 0.04MPa, dehydrogenation is carried out under the high temperature environment with the temperature of 610 ℃, and finishing hydrogen crushing when the vacuum degree is more than 10 Pa. The powder after hydrogen crushing was sampled and observed, and hard core particles were not found. Then, the jet milling is carried out and the jet milling powder is detected, and the average granularity is found to be 2.7um, which is 0.5um smaller than that of the jet milling powder which is directly subjected to hydrogen crushing and jet milling without smelting, and the formability during the compression is improved and the quality of the product is improved.
The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.

Claims (6)

1. A treatment method of neodymium iron boron oxidation blanks is characterized by comprising the following steps:
the first step is as follows: classifying the neodymium iron boron oxidized blanks according to the grade numbers of the neodymium iron boron, and storing the neodymium iron boron oxidized blanks respectively;
the second step is that: preparing raw material components corresponding to the grades according to the grades of the classified neodymium iron boron oxidized blanks;
the third step: adding neodymium iron boron oxidized blanks corresponding to the grades into a certain grade of raw material components, and then smelting and casting to prepare neodymium iron boron alloy cast sheets;
the fourth step: adding blocky praseodymium-neodymium into the neodymium-iron-boron alloy cast sheet, and then carrying out hydrogen crushing;
the fifth step: carrying out airflow milling on the hydrogen broken powder after hydrogen breaking to prepare powder, pressing and sintering the powder to obtain a neodymium iron boron magnet;
and a sixth step: and repeating the operation from the third step to the fifth step for other classified neodymium iron boron oxidized blanks.
2. The method for processing the neodymium iron boron oxidized blank according to claim 1, wherein in the third step, the mass ratio of the neodymium iron boron oxidized blank to the corresponding grade raw material components is 1: 9.
3. the method for processing neodymium-iron-boron oxidized blanks according to claim 1, wherein in the fourth step, the mass of the added block praseodymium-neodymium is 1.0% -2.0% of the sum of the mass of the neodymium-iron-boron alloy cast sheet and the mass of the added block praseodymium-neodymium.
4. The method for processing the neodymium-iron-boron oxidized blank according to claim 1, wherein when the neodymium-iron-boron oxidized blank belongs to an H series number, the mass of the added block praseodymium-neodymium is 1% -1.5% of the mass sum of the neodymium-iron-boron alloy cast sheet and the added block praseodymium-neodymium; when the neodymium iron boron oxidation blank belongs to N series, the mass of the added block praseodymium neodymium is 1.5% -2.0% of the mass sum of the neodymium iron boron alloy cast sheet and the added block praseodymium neodymium.
5. The method of processing a neodymium iron boron oxidized blank according to claim 1,
the hydrogen crushing process in the fourth step comprises the following steps: absorbing hydrogen for 6 hours in a hydrogen environment with the pressure of 0.04MPa, dehydrogenating in a temperature environment of 610 ℃, and finishing hydrogen crushing when the vacuum degree is more than 10 Pa.
6. The method of processing a neodymium iron boron oxidized blank according to claim 1,
the process of the airflow milling powder in the fifth step comprises the following steps: the rotating speed of a grading wheel is 2400r/min, and a lubricant with a mass ratio of four parts per million is added into the powder for mixing for 6 hours in the air-flow milling process; the pressing process comprises the steps of placing mixed fine powder after air flow grinding in a magnetic field for orientation and isostatic pressing, wherein the magnetic field intensity is 1.2T, the isostatic pressing pressure is 220MPa, and the isostatic pressing time is 40 seconds; the sintering process comprises the following steps: firstly sintering at 1110 ℃, carrying out primary tempering at 940 ℃, and carrying out secondary tempering at 640 ℃ to obtain the neodymium iron boron magnet.
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Citations (14)

* Cited by examiner, † Cited by third party
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JPH06340902A (en) * 1993-06-02 1994-12-13 Shin Etsu Chem Co Ltd Production of sintered rare earth base permanent magnet
CN1227392A (en) * 1998-02-25 1999-09-01 潘树明 Rare-earth-Fe-B permanent magnetic material and its preparation technology
JP2002060855A (en) * 2000-08-22 2002-02-28 Shin Etsu Chem Co Ltd METHOD FOR RECYCLING Nd-BASED RARE EARTH METAL MAGNET SCRAP
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CN101952915A (en) * 2008-02-20 2011-01-19 株式会社爱发科 Method for regenerating scrap magnets
JP2011124394A (en) * 2009-12-10 2011-06-23 Daido Electronics Co Ltd Magnetic powder recovering method of rare-earth bonded magnet and magnet material for rare-earth bonded magnet
WO2014033004A1 (en) * 2012-08-30 2014-03-06 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Method for reclaiming neodymium oxide from a starting mixture
CN104190943A (en) * 2014-08-04 2014-12-10 中磁科技股份有限公司 Method for recycling sintered neodymium-iron-boron waste materials
CN104439256A (en) * 2014-11-24 2015-03-25 湖南航天磁电有限责任公司 Method for recycling and reusing sintered Nd-Fe-B oxidation blank
CN105957678A (en) * 2016-06-30 2016-09-21 中铝广西有色金源稀土有限公司 Method for recycling sintered NdFeB waste
CN107275029A (en) * 2016-04-08 2017-10-20 沈阳中北通磁科技股份有限公司 A kind of high-performance Ne-Fe-B permanent magnet produced with neodymium iron boron waste material and manufacture method
CN111180189A (en) * 2019-12-31 2020-05-19 慈溪市恒韵照明有限公司 Method for preparing N40M type sintered NdFeB magnetic material by adding 38M waste material
CN111192754A (en) * 2019-12-31 2020-05-22 慈溪市恒韵照明有限公司 Method for preparing N38M type sintered neodymium-iron-boron magnetic material at low cost
CN111341512A (en) * 2020-03-09 2020-06-26 钢铁研究总院 High-cost performance rare earth permanent magnet and preparation method thereof

Patent Citations (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06340902A (en) * 1993-06-02 1994-12-13 Shin Etsu Chem Co Ltd Production of sintered rare earth base permanent magnet
CN1227392A (en) * 1998-02-25 1999-09-01 潘树明 Rare-earth-Fe-B permanent magnetic material and its preparation technology
JP2002060855A (en) * 2000-08-22 2002-02-28 Shin Etsu Chem Co Ltd METHOD FOR RECYCLING Nd-BASED RARE EARTH METAL MAGNET SCRAP
CN101045256A (en) * 2006-03-31 2007-10-03 潘树明 Synthesizing process for regenerating rare earth permanent magnet alloy from waste alloy
CN101952915A (en) * 2008-02-20 2011-01-19 株式会社爱发科 Method for regenerating scrap magnets
JP2011124394A (en) * 2009-12-10 2011-06-23 Daido Electronics Co Ltd Magnetic powder recovering method of rare-earth bonded magnet and magnet material for rare-earth bonded magnet
WO2014033004A1 (en) * 2012-08-30 2014-03-06 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Method for reclaiming neodymium oxide from a starting mixture
CN104190943A (en) * 2014-08-04 2014-12-10 中磁科技股份有限公司 Method for recycling sintered neodymium-iron-boron waste materials
CN104439256A (en) * 2014-11-24 2015-03-25 湖南航天磁电有限责任公司 Method for recycling and reusing sintered Nd-Fe-B oxidation blank
CN107275029A (en) * 2016-04-08 2017-10-20 沈阳中北通磁科技股份有限公司 A kind of high-performance Ne-Fe-B permanent magnet produced with neodymium iron boron waste material and manufacture method
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CN111180189A (en) * 2019-12-31 2020-05-19 慈溪市恒韵照明有限公司 Method for preparing N40M type sintered NdFeB magnetic material by adding 38M waste material
CN111192754A (en) * 2019-12-31 2020-05-22 慈溪市恒韵照明有限公司 Method for preparing N38M type sintered neodymium-iron-boron magnetic material at low cost
CN111341512A (en) * 2020-03-09 2020-06-26 钢铁研究总院 High-cost performance rare earth permanent magnet and preparation method thereof

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