CN113903539A - High-precision sintering molding process for rubidium-iron-boron magnet - Google Patents

High-precision sintering molding process for rubidium-iron-boron magnet Download PDF

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Publication number
CN113903539A
CN113903539A CN202111360741.7A CN202111360741A CN113903539A CN 113903539 A CN113903539 A CN 113903539A CN 202111360741 A CN202111360741 A CN 202111360741A CN 113903539 A CN113903539 A CN 113903539A
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CN
China
Prior art keywords
rubidium
iron
boron magnet
oxide
boron
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Pending
Application number
CN202111360741.7A
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Chinese (zh)
Inventor
苏轩宏
叶臣哲
王光伟
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Suzhou Yuange Electronic Co Ltd
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Suzhou Yuange Electronic Co Ltd
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Priority to CN202111360741.7A priority Critical patent/CN113903539A/en
Publication of CN113903539A publication Critical patent/CN113903539A/en
Pending legal-status Critical Current

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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/04Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
    • H01F1/047Alloys characterised by their composition
    • H01F1/053Alloys characterised by their composition containing rare earth metals
    • H01F1/055Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • H01F1/0571Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes
    • H01F1/0575Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together
    • H01F1/0577Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B in the form of particles, e.g. rapid quenched powders or ribbon flakes pressed, sintered or bonded together sintered
    • 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
    • B22F3/1003Use of special medium during sintering, e.g. sintering aid
    • B22F3/1007Atmosphere
    • 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
    • B22F3/12Both compacting and sintering
    • B22F3/14Both compacting and sintering simultaneously
    • 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

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Power Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Hard Magnetic Materials (AREA)
  • Manufacturing Cores, Coils, And Magnets (AREA)

Abstract

The invention discloses a high-precision sintering molding process of a rubidium-iron-boron magnet, which comprises the following steps of grinding rubidium oxide, iron oxide and boron oxide respectively to prepare mixed powder; step two, sequentially carrying out rapid hardening and strip throwing, hydrogen explosion and jet milling on the mixed powder in the step 1 to prepare magnetic powder; step three, putting the magnetic powder obtained in the step 2 into a hot-pressing forming machine; and step four, putting the obtained rubidium-iron-boron magnet pressed blank into a vacuum sintering furnace, and performing three-time stepped sintering and cooling in the vacuum sintering furnace by taking rubidium oxide, iron oxide and boron oxide as main raw materials to obtain a high-magnetic-performance, high-density and anti-oxidation rubidium-iron-boron magnet finished product.

Description

High-precision sintering molding process for rubidium-iron-boron magnet
Technical Field
The invention relates to the technical field of rubidium-iron-boron magnet preparation, in particular to a high-precision sintering forming process for rubidium-iron-boron magnet.
Background
The rubidium iron boron magnet has extremely high magnetic energy product, coercive force and high energy density, and is widely used in the fields of modern industry, electronic technology and the like. The manufacturing process of the rubidium iron boron magnet comprises the following steps: alloy smelting → hydrogen crushing to prepare coarse powder → air flow grinding to prepare fine powder → shaping → isostatic pressing → sintering → surface treatment → magnetizing. The sintering is a key step, and the performance and the qualification rate of the rubidium-iron-boron magnet are directly determined by the quality of the sintering process.
Because the rubidium, iron and boron powder adsorbs a large amount of substances such as nitrogen, oxygen, carbon and the like, the substances are released at different temperature sections in the sintering process, the released substances need to be timely pumped out or diluted, otherwise, rubidium-rich phase in the rubidium, iron and boron magnet is consumed to cause material oxidation. In addition, the sintering process curve is complex, a higher vacuum degree needs to be kept in the sintering process, the sintering time is long, the energy consumption is high, and the cost is higher. The sintering time is shortened, a large amount of energy consumption can be saved, so that the manufacturing cost is effectively reduced, and the method has good economic and social significance.
Disclosure of Invention
The invention aims to provide a high-precision sintering and forming process of rubidium-iron-boron magnet, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a high-precision sintering molding process for rubidium-iron-boron magnet comprises the following steps:
step 1, respectively grinding rubidium oxide, iron oxide and boron oxide, and mixing the rubidium oxide, the iron oxide and the boron oxide after impurities are removed to prepare mixed powder;
step 2, sequentially carrying out rapid hardening and strip throwing, hydrogen explosion and jet milling on the mixed powder in the step 1 to prepare magnetic powder;
step 3, putting the magnetic powder obtained in the step 2 into a hot-press forming machine to obtain a green body with a required specification, performing a static pressure secondary forming process to improve the density of the green body, and putting the green body into a prepared high-temperature-resistant material model to obtain a rubidium-iron-boron magnet green body;
step 4, putting the obtained rubidium iron boron magnet pressed compact into a vacuum sintering furnace, vacuumizing the vacuum sintering furnace to 0.1Pa, heating to the first temperature of 550-700 ℃ within 90-150 minutes, and preserving heat for 30-40 minutes;
step 5, heating the rubidium iron boron magnet treated in the step 4 to a second temperature of 700 ℃ and 900 ℃ for 50-80 minutes, and preserving heat for 15-45 minutes;
step 6, heating the rubidium iron boron magnet treated in the step 5 to a third temperature of 900-1200 ℃ for 10-20 minutes, and preserving the heat for 200-245 minutes;
and 7, placing the rubidium iron boron magnet treated in the step 6 in an environment filled with inert gas for cooling to obtain a finished rubidium iron boron magnet product.
As a further scheme of the invention: and (3) when the jet mill is carried out in the step (2), inert gas is adopted for protection, and the oxygen content in the jet mill device is lower than 40 ppm.
As a further scheme of the invention: and 2, adding an antioxidant during jet milling.
As a further scheme of the invention: and 3, filling protective gas in the process of preparing the rubidium-iron-boron magnet pressed compact.
As a further scheme of the invention: and 7, placing the furnace body in inert gas for cooling, namely filling the inert gas for quenching and cooling to the temperature of 550-.
As a further scheme of the invention: and a temperature sensor and a pressure sensor are arranged on the vacuum sintering furnace.
As a further scheme of the invention: the inert gas and the protective gas are both argon or nitrogen.
As a further scheme of the invention: and (4) the finished product of the rubidium-iron-boron magnet prepared in the step (7) is plate-shaped.
Compared with the prior art, the invention has the beneficial effects that: the method comprises the steps of taking rubidium oxide, iron oxide and boron oxide as main raw materials, grinding the three raw materials respectively, removing impurities, mixing the ground materials into mixed powder, sequentially carrying out rapid hardening and strip throwing, hydrogen explosion and jet milling on the mixed powder to obtain magnetic powder, putting the magnetic powder into a hot-press forming machine to obtain a green body with a required specification, carrying out a static pressure secondary forming process to improve the density of the green body, putting the green body into a prepared high-temperature-resistant material model to obtain a rubidium-iron-boron magnet green body, finally putting the rubidium-iron-boron magnet green body into a vacuum sintering furnace to carry out vacuum sintering, carrying out three-time stepped sintering in the vacuum sintering furnace, cooling to obtain a rubidium-iron-boron magnet finished product with high magnetic performance, high density and oxidation resistance, and adopting a mode of combining gas quenching and natural cooling during cooling, so that the energy-saving effect is good.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A high-precision sintering molding process for rubidium-iron-boron magnet comprises the following steps:
step 1, respectively grinding rubidium oxide, iron oxide and boron oxide, and mixing the rubidium oxide, the iron oxide and the boron oxide after impurities are removed to prepare mixed powder;
step 2, sequentially carrying out rapid hardening and strip throwing, hydrogen explosion and jet milling on the mixed powder in the step 1 to prepare magnetic powder;
step 3, putting the magnetic powder obtained in the step 2 into a hot-press forming machine to obtain a green body with a required specification, performing a static pressure secondary forming process to improve the density of the green body, and putting the green body into a prepared high-temperature-resistant material model to obtain a rubidium-iron-boron magnet green body;
step 4, putting the obtained rubidium iron boron magnet pressed compact into a vacuum sintering furnace, vacuumizing the vacuum sintering furnace to 0.1Pa, heating to the first temperature of 550-700 ℃ within 90-150 minutes, and preserving heat for 30-40 minutes;
step 5, heating the rubidium iron boron magnet treated in the step 4 to a second temperature of 700 ℃ and 900 ℃ for 50-80 minutes, and preserving heat for 15-45 minutes;
step 6, heating the rubidium iron boron magnet treated in the step 5 to a third temperature of 900-1200 ℃ for 10-20 minutes, and preserving the heat for 200-245 minutes;
and 7, placing the rubidium iron boron magnet treated in the step 6 in an environment filled with inert gas for cooling to obtain a finished rubidium iron boron magnet product.
And (3) when the jet mill is carried out in the step (2), inert gas is adopted for protection, and the oxygen content in the jet mill device is lower than 40 ppm.
And 2, adding an antioxidant during jet milling.
And 3, filling protective gas in the process of preparing the rubidium-iron-boron magnet pressed compact.
And 7, placing the furnace body in inert gas for cooling, namely filling the inert gas for quenching and cooling to the temperature of 550-.
And a temperature sensor and a pressure sensor are arranged on the vacuum sintering furnace.
The inert gas and the protective gas are both argon or nitrogen.
And (4) the finished product of the rubidium-iron-boron magnet prepared in the step (7) is plate-shaped.
The method comprises the steps of taking rubidium oxide, iron oxide and boron oxide as main raw materials, grinding the three raw materials respectively, removing impurities, mixing the ground materials into mixed powder, sequentially carrying out rapid hardening and strip throwing, hydrogen explosion and jet milling on the mixed powder to obtain magnetic powder, putting the magnetic powder into a hot-press forming machine to obtain a green body with a required specification, carrying out a static pressure secondary forming process to improve the density of the green body, putting the green body into a prepared high-temperature-resistant material model to obtain a rubidium-iron-boron magnet green body, finally putting the rubidium-iron-boron magnet green body into a vacuum sintering furnace to carry out vacuum sintering, carrying out three-time stepped sintering in the vacuum sintering furnace, cooling to obtain a rubidium-iron-boron magnet finished product with high magnetic performance, high density and oxidation resistance, and adopting a mode of combining gas quenching and natural cooling during cooling, so that the energy-saving effect is good.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.

Claims (8)

1. A high-precision rubidium-iron-boron magnet sintering forming process is characterized by comprising the following steps:
step 1, respectively grinding rubidium oxide, iron oxide and boron oxide, and mixing the rubidium oxide, the iron oxide and the boron oxide after impurities are removed to prepare mixed powder;
step 2, sequentially carrying out rapid hardening and strip throwing, hydrogen explosion and jet milling on the mixed powder in the step 1 to prepare magnetic powder;
step 3, putting the magnetic powder obtained in the step 2 into a hot-press forming machine to obtain a green body with a required specification, performing a static pressure secondary forming process to improve the density of the green body, and putting the green body into a prepared high-temperature-resistant material model to obtain a rubidium-iron-boron magnet green body;
step 4, putting the obtained rubidium iron boron magnet pressed compact into a vacuum sintering furnace, vacuumizing the vacuum sintering furnace to 0.1Pa, heating to the first temperature of 550-700 ℃ within 90-150 minutes, and preserving heat for 30-40 minutes;
step 5, heating the rubidium iron boron magnet treated in the step 4 to a second temperature of 700 ℃ and 900 ℃ for 50-80 minutes, and preserving heat for 15-45 minutes;
step 6, heating the rubidium iron boron magnet treated in the step 5 to a third temperature of 900-1200 ℃ for 10-20 minutes, and preserving the heat for 200-245 minutes;
and 7, placing the rubidium iron boron magnet treated in the step 6 in an environment filled with inert gas for cooling to obtain a finished rubidium iron boron magnet product.
2. The high-precision rubidium-iron-boron magnet sintering molding process of claim 1, wherein inert gas is used for protection when the jet mill is performed in the step 2, and the oxygen content in a jet mill device is lower than 40 ppm.
3. The high-precision rubidium-iron-boron magnet sintering molding process as claimed in claim 2, wherein an antioxidant is added during the jet milling in step 2.
4. The high-precision rubidium-iron-boron magnet sintering molding process according to claim 3, wherein the rubidium-iron-boron magnet green compact prepared in the step 3 is filled with protective gas.
5. The high-precision rubidium-iron-boron magnet sintering molding process as claimed in claim 4, wherein the step 7 of placing in inert gas for cooling is that inert gas is filled for quenching and cooling to 550-600 ℃, then natural cooling to 300-420 ℃, and then gas quenching and cooling to room temperature are carried out and then furnace tapping is carried out.
6. The high-precision rubidium-iron-boron magnet sintering molding process of claim 5, wherein a temperature sensor and a pressure sensor are mounted on the vacuum sintering furnace.
7. The high-precision rubidium-iron-boron magnet sintering molding process of claim 6, wherein the inert gas and the protective gas are argon or nitrogen.
8. The high-precision sintering molding process of the rubidium-iron-boron magnet according to claim 7, wherein the finished rubidium-iron-boron magnet prepared in the step 7 is plate-shaped.
CN202111360741.7A 2021-11-17 2021-11-17 High-precision sintering molding process for rubidium-iron-boron magnet Pending CN113903539A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111360741.7A CN113903539A (en) 2021-11-17 2021-11-17 High-precision sintering molding process for rubidium-iron-boron magnet

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111360741.7A CN113903539A (en) 2021-11-17 2021-11-17 High-precision sintering molding process for rubidium-iron-boron magnet

Publications (1)

Publication Number Publication Date
CN113903539A true CN113903539A (en) 2022-01-07

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Application Number Title Priority Date Filing Date
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Application publication date: 20220107

Assignee: Yisheng Global Co.,Ltd.

Assignor: SUZHOU YUANGE ELECTRONIC Co.,Ltd.

Contract record no.: X2023990000746

Denomination of invention: A high-precision sintering process for rubidium iron boron magnet

License type: Common License

Record date: 20230810