CN114899004A - Multiphase coupling method and apparatus for preparing high abundance cerium magnet N38SH - Google Patents
Multiphase coupling method and apparatus for preparing high abundance cerium magnet N38SH Download PDFInfo
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- 229910052684 Cerium Inorganic materials 0.000 title claims abstract description 22
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000010168 coupling process Methods 0.000 title claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 59
- RZJQYRCNDBMIAG-UHFFFAOYSA-N [Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Zn].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn] Chemical class [Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Cu].[Zn].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Ag].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn].[Sn] RZJQYRCNDBMIAG-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000000843 powder Substances 0.000 claims abstract description 40
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000001257 hydrogen Substances 0.000 claims abstract description 21
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 21
- 229910000640 Fe alloy Inorganic materials 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 239000006247 magnetic powder Substances 0.000 claims abstract description 12
- 238000005245 sintering Methods 0.000 claims abstract description 11
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 9
- 239000000956 alloy Substances 0.000 claims abstract description 9
- 230000008569 process Effects 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 239000011261 inert gas Substances 0.000 claims abstract description 5
- 238000002360 preparation method Methods 0.000 claims abstract description 5
- 230000001681 protective effect Effects 0.000 claims abstract description 5
- 238000010902 jet-milling Methods 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 58
- 239000000463 material Substances 0.000 claims description 21
- 238000007664 blowing Methods 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 10
- GSVIBLVMWGSPRZ-UHFFFAOYSA-N cerium iron Chemical compound [Fe].[Fe].[Fe].[Fe].[Fe].[Fe].[Fe].[Fe].[Fe].[Fe].[Fe].[Fe].[Fe].[Fe].[Fe].[Fe].[Fe].[Ce].[Ce] GSVIBLVMWGSPRZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000004020 conductor Substances 0.000 claims description 6
- 238000009694 cold isostatic pressing Methods 0.000 claims description 4
- 238000006356 dehydrogenation reaction Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 238000007670 refining Methods 0.000 claims description 4
- 238000005496 tempering Methods 0.000 claims description 4
- RDTHZIGZLQSTAG-UHFFFAOYSA-N dysprosium iron Chemical compound [Fe].[Dy] RDTHZIGZLQSTAG-UHFFFAOYSA-N 0.000 claims description 3
- 238000003801 milling Methods 0.000 claims description 3
- 238000009987 spinning Methods 0.000 claims description 2
- 238000013467 fragmentation Methods 0.000 claims 1
- 238000006062 fragmentation reaction Methods 0.000 claims 1
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 19
- 230000000694 effects Effects 0.000 description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 9
- 238000010008 shearing Methods 0.000 description 8
- 150000002910 rare earth metals Chemical class 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000009471 action Effects 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 230000008878 coupling Effects 0.000 description 4
- 238000005859 coupling reaction Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- 229910001172 neodymium magnet Inorganic materials 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 230000005514 two-phase flow Effects 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910052777 Praseodymium Inorganic materials 0.000 description 2
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000013013 elastic material Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- -1 neodymium iron boron rare earth Chemical class 0.000 description 2
- 229910052758 niobium Inorganic materials 0.000 description 2
- 150000002895 organic esters Chemical class 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000000737 periodic effect Effects 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910052692 Dysprosium Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000013421 nuclear magnetic resonance imaging Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 229910000938 samarium–cobalt magnet Inorganic materials 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
Images
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus 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
- H01F41/02—Apparatus 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
- H01F41/0253—Apparatus 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus 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
- H01F41/02—Apparatus 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
- H01F41/0253—Apparatus 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
- H01F41/0266—Moulding; Pressing
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The invention discloses a multiphase coupling method for preparing high abundance cerium magnet N38SH, comprising the following steps: separate preparation of the first and second main phase alloys: respectively burdening, and respectively adding the raw materials into a vacuum rapid hardening and flaying furnace to carry out a strip throwing process after burdening to obtain two rapid hardening slices; carrying out hydrogen fracture on the Dy-Fe alloy and the first main phase rapid hardening tablet; respectively carrying out jet milling on the hydrogen-broken first main phase alloy rapid hardening sheet and the second main phase alloy rapid hardening sheet to obtain two kinds of magnetic powder with approximate granularity; mixing powder in a powder mixing device, and performing orientation forming on the mixed magnetic powder magnetic field of the first main phase alloy and the second main phase alloy in the inert gas protective atmosphere to prepare a blank; and sintering the prepared blank in a sintering furnace. The invention realizes the composition of 2-14-1 type main phases with different rare earth elements in the alloy by mixing the powder prepared by the rapid hardening belts with different components, thereby obtaining better comprehensive magnetic performance.
Description
Technical Field
The present invention relates to the field of methods for making high abundance cerium magnets, and in particular to a multiphase coupling method and apparatus for making high abundance cerium magnet N38 SH.
Background
At present, the neodymium iron boron rare earth permanent magnet material is a permanent magnet material with the strongest magnetic property discovered so far, and has wide application in more and more fields with excellent magnetic property, such as medical nuclear magnetic resonance imaging, computer hard disk drives, acoustic mobile phones, wind power generation, aerospace fields and the like. Along with the demand of people for low carbon and energy conservation, the neodymium iron boron rare earth permanent magnet material is increasingly applied to the fields of automobile motors, energy-saving electric appliances and the like.
At present, the yield of the neodymium iron boron in China is the first in the world. Although the neodymium iron boron has certain cost advantage compared with the second generation SmCo series material, the cost is still higher. As rare earth elements, the abundance of Ce element is far higher than that of Nd element, and the price of the Ce element is about one tenth of that of the Nd element. On one hand, the addition of Ce can greatly save the cost of raw materials; on the other hand, the adverse effect on the environment in the rare earth separation process can be effectively reduced. However, the conventional Ce-containing rare earth permanent magnet has poor comprehensive magnetic performance, and the application of the Ce-containing permanent magnet is limited.
Disclosure of Invention
Aiming at the problems, the invention provides a multiphase coupling method for preparing cerium-iron-containing magnet N38SH with high abundance, and solves the defects that the existing prepared rare earth permanent magnet containing Ce has poor comprehensive magnetic performance and limits the application of the rare earth permanent magnet containing Ce.
The technical scheme adopted by the invention is as follows:
a multiphase coupling method of making high abundance cerium magnet N38SH, comprising the steps of:
s1, separate preparation of first and second main phase alloys: respectively burdening according to the composition of the first main phase alloy and the second main phase alloy, respectively adding the burdened raw materials into a vacuum rapid hardening and flailing furnace to carry out a strip throwing process, refining for 18-25 minutes, then standing for 5-8 minutes, and pouring to obtain two rapid hardening slices, namely a first main phase alloy rapid hardening slice and a second main phase alloy rapid hardening slice;
s2, hydrogen breaking Dy-Fe alloy of Dy80/Fe20 and the first main phase alloy quick-setting slice;
s3, adding the dysprosium-iron alloy of the hydrogen-broken Dy80/Fe20 into the hydrogen-broken first main phase alloy quick-setting sheet, and respectively carrying out airflow milling on the mixture and the second main phase alloy quick-setting sheet to obtain two kinds of magnetic powder with the particle size being close to each other;
s4, mixing powder in a powder mixing device, then under the protective atmosphere of inert gas, orienting and forming the mixed magnetic powder of the first main phase alloy and the second main phase alloy in a magnetic field with the magnetic field intensity of 1.5-2.5T, and then carrying out cold isostatic pressing to prepare a blank;
s5, sintering the prepared blank in a sintering furnace, preserving heat for 0.5-10 hours at 400-800 ℃ for dehydrogenation, preserving heat for 2-6 hours at 1030-1080 ℃ for cooling, and then performing secondary tempering treatment for 2-6 hours at 750-750 ℃ and 550-750 ℃ respectively.
The invention realizes the composition of 2-14-1 type main phases with different rare earth elements in the alloy by mixing the powder prepared by the rapid hardening belts with different components, thereby obtaining better comprehensive magnetic performance.
Optionally, the temperature of the tape-spinning process in the step S1 is 1430-1480 ℃.
Optionally, the particle size of the two kinds of magnetic powder obtained in step S3 is between 1 μm and 6 μm.
Optionally, the rotation speed of the sorting wheel during the air jet milling in the step S3 is controlled to be 2500 r/min-4500 r/min.
Optionally, in step S2, Dy-Fe alloy of Dy80/Fe20 is added to the first main phase rapid hardening tablet for hydrogen fracture.
Optionally, in step S2, hydrogen crushing is separately performed on the dysprosium-iron alloy of Dy80/Fe20 and the rapid hardening sheet of the first main phase alloy; and then mixing the first main phase alloy coarse powder after hydrogen crushing and the Dy-Fe alloy coarse powder of Dy80/Fe20 after hydrogen crushing according to the proportion.
The invention also discloses powder mixing equipment for preparing the high-abundance cerium magnet N38SH, which comprises a mixing tank body, wherein a stirring device is arranged in the mixing tank body, and the stirring device comprises a motor and a stirring rod driven by the motor, which are arranged at the upper end of the mixing tank body; the stirring rod is provided with a first stirring blade; the lower part of the mixing tank body is provided with a blowing nozzle, and the blowing nozzle is connected with an external blowing part and used for blowing air to the inner cavity of the mixing tank body; and a feeding port is arranged at the top of the mixing tank body. The invention relates to a two-phase flow coupling mixing method under the shearing coaction of a stirring rod and gas (argon or nitrogen); the first stirring blade rolls the powder from bottom to top, airflow is transversely broken up, and the high-speed impact and the shearing force generated by the airflow can fully disperse and mix the materials.
Optionally, a cross rod is installed at the upper part of the stirring rod, a fixing sleeve is installed at the middle part of the cross rod, a limiting ring is installed on the stirring rod below the fixing sleeve, the fixing sleeve is sleeved in the stirring rod, and a fixing disc is installed at the bottom of the stirring rod; the stirring rod below the cross rod is provided with a first stirring blade, the cross rod is provided with a movable block sleeved on the cross rod, a spring sleeved on the cross rod is arranged between the fixed sleeve and the movable block, one end of the spring is connected with the movable block, and the other end of the spring is connected with the fixed sleeve. The outside of movable block is equipped with the stopper of installing on the horizontal pole. The bottom of the movable block is provided with a telescopic rod made of elastic materials, the fixed disk is provided with a sliding groove, and the bottom of the telescopic rod is slidably connected with the sliding groove.
Optionally, a conducting ring made of a conducting material is arranged on the outer side of the outer side wall of the fixed disk, a conducting rod electrically connected with the conducting ring is arranged at the bottom of the conducting ring, a conducting ball made of a conducting material is rotatably mounted at the bottom of the conducting rod, a conducting plate is arranged on the inner wall of the bottom of the mixing tank body, a brush piece with a width larger than that of the conducting plate is arranged at the tail end of the conducting plate, and the brush piece is continuously contacted with the conducting ring; the bottom of the material mixing tank body is provided with a circular wedge-shaped disc, the upper width and the lower width of the electric brush piece are larger than the maximum thickness of the wedge-shaped disc, the wedge-shaped disc is provided with a resistance arc piece, the resistance arc piece comprises a plurality of resistance pieces, the resistance pieces are arranged along one direction, and the resistances of the resistance pieces are sequentially increased; the resistance piece is electrically connected with one pole of the mobile power supply, the electric brush piece is electrically connected with the other pole of the mobile power supply, and a second stirring blade is arranged on the outer side of the telescopic rod; the second stirring blade is arranged between two adjacent first stirring blades.
Optionally, an ammeter is further arranged between the resistor and the mobile power supply, the ammeter is electrically connected with an external control unit, and the control unit is electrically connected with the driving motor.
Optionally, the top of the sliding groove protrudes towards the middle to form a limiting flange, and the bottom of the telescopic rod protrudes outwards to form a clamping piece.
Optionally, the cross section of the spring is an ellipse vertically arranged.
Advantageous effects
1. The invention realizes the composition of 2-14-1 type main phases with different rare earth elements in the alloy by mixing the powder prepared by the rapid hardening belts with different components, thereby obtaining better comprehensive magnetic performance.
2. The invention controls the type and distribution of the rare earth elements in the main phase by adjusting the type, quantity and proportion of the rare earth elements in the rapid hardening tablets, can conveniently realize the adjustment and optimization of the content and distribution of the heavy rare earth elements in the magnet by adjusting the content of the heavy rare earth elements in the rapid hardening zone and the proportion of the heavy rare earth elements in the rapid hardening zone without the heavy rare earth elements, and realizes the high-efficiency utilization of the heavy rare earth elements.
3. The invention adopts 2-4 quick-setting belts which are combined according to different proportions, can basically realize the production of magnets with various brands, reduces the production cost and improves the production efficiency by efficiently utilizing heavy rare earth and reducing the sintering temperature, and can realize large-scale production without modifying equipment.
4. The invention relates to a two-phase flow coupling mixing method under the shearing coaction of a stirring rod and gas (argon or nitrogen); the first stirring blade rolls the powder from bottom to top, airflow is transversely broken up, and the high-speed impact and the shearing force generated by the airflow can fully disperse and mix the materials.
5. The invention relates to a two-phase flow coupling mixing method under the shearing combined action of a stirring rod and gas (argon or nitrogen); the first stirring blade rolls the powder from bottom to top, airflow is transversely broken up, and the high-speed impact and the shearing force generated by the airflow can fully disperse and mix the materials. When the puddler rotational speed difference is, the effect sliding block of effect at centrifugal force removes along the horizontal pole effect, drives the telescopic link and slides along the effect of fixed disk for second stirring vane has axial rotation simultaneously, also has up-and-down and side-to-side movement, and it has improved mixing efficiency, avoids appearing obvious layering at the faster effect of rotational speed material down.
The electric conduction rod machine and the electric conduction ball which are electrically connected with the conducting ring rotate along the wedge-shaped disc and push the cross rod and periodically contact with the resistance arc piece, the electric brush piece is continuously contacted with the conducting ring and is electrically connected with one pole of the mobile power supply through the resistance piece, the electric brush piece is electrically connected with the other pole of the mobile power supply, so that the ammeter in the closed circuit continuously changes, the control unit receives a current signal of the ammeter and controls the periodic change of the output power of the driving motor, the first stirring blade and the second stirring blade periodically change, the material does not drip down and is rolled up, and obvious layering of the material under the action of the rotating speed is avoided.
6. The sliding block moves along the cross rod under the action of centrifugal force to drive the spring to move, and the spring with the oval section also plays a role in pushing the material to move left and right.
Description of the drawings:
fig. 1 is a sectional structural view of a powder mixing apparatus for producing a high abundance cerium magnet N38SH according to example 6 of the present invention;
fig. 2 is a partially enlarged view of a portion a of fig. 1 of the powder mixing apparatus for producing a high abundance cerium magnet N38SH according to example 6 of the present invention;
fig. 3 is a partially enlarged view of a portion B of fig. 1 of the powder mixing apparatus for producing a high abundance cerium magnet N38SH according to example 6 of the present invention;
fig. 4 is a top view of the fixed disk of fig. 3 of the powder mixing apparatus for producing high abundance cerium magnets N38SH according to example 6 of the present invention;
fig. 5 is a sectional view of the chute of fig. 3 of the powder mixing apparatus for producing a high abundance cerium magnet N38SH according to example 6 of the present invention;
fig. 6 is a flowchart of a control unit of a powder mixing apparatus for producing a high abundance cerium magnet N38SH according to example 6 of the present invention;
fig. 7 is a sectional structural view of a spring of the powder mixing apparatus for producing a high abundance cerium magnet N38SH according to example 7 of the present invention.
The figures are numbered:
1. the mixing tank comprises a mixing tank body, 2, a stirring device, 3, a motor, 4, a stirring rod, 5, a blowing nozzle, 6, a feeding port, 7, a cross rod, 8, a fixing sleeve, 9, a limiting ring, 10, a fixing disk, 11, a first stirring blade, 12, a movable block, 13, a spring, 14, a buckling piece, 15, a limiting block, 16, a telescopic rod, 17, a sliding chute, 18, a conducting ring, 19, a conducting rod, 20, a conducting ball, 21, a conducting sheet, 22, an electric brush sheet, 23, a wedge-shaped disk, 24, a resistance arc sheet, 25, a resistance piece, 26, a mobile power supply, 27, a current meter, 28, a control unit, 29, a stirring blade, 30 and a limiting flange.
The specific implementation formula is as follows:
the following detailed description of embodiments of the present invention is provided in connection with the accompanying drawings and examples. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
In the description of the present invention, "a plurality" means two or more unless otherwise specified; the terms "upper", "lower", "left", "right", "inner", "outer", "front", "rear", "head", "tail", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are only for convenience in describing and simplifying the description, and do not indicate or imply that the device or element referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus, should not be construed as limiting the invention. Furthermore, the terms "first," "second," "third," and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance. In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "connected" and "connected" are to be interpreted broadly, e.g., as being fixed or detachable or integrally connected; may be mechanically coupled, directly coupled, or indirectly coupled through an intermediary. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Example 1
The technical scheme adopted by the invention is as follows:
the invention discloses a high abundance cerium magnet N38SH, comprising: the dual-main-phase alloy method is characterized in that two different main-phase alloys are prepared, the components of a first main-phase alloy are (Cex, Re1-x) aFe100-a-b-cBbTMc in percentage by mass, wherein x is more than or equal to 10 and less than or equal to 15, a is more than or equal to 29 and less than or equal to 32, b is more than or equal to 0.9 and less than or equal to 1.2, c is more than or equal to 1.0 and less than or equal to 2.5, Re is one or more of Nd, Pr and La elements, TM is one or more of Co, Cu, Nb, Al, Zr and Ti, the components of a second main-phase alloy in percentage by mass are (Cex, Re1-x) aFe100-a-b-cBbTMc, wherein x is more than or equal to 10 and less than or equal to 13, a is more than or equal to 30 and less than or equal to 33, b is more than or equal to 0.9 and less than or equal to 1.2, c is more than or equal to 2.5, Re is one or equal to Pr, Dy, one or more of Co, Cu, Nb, Al, Zr and Ti, and two raw materials are respectively prepared.
| Example 1 | Example 2 | Example 3 | |
| First main phase | 49％+1％DyFe | 48％+2％DyFe | 47％+3％DyFe |
| Second main phase | 50％ | 50％ | 50％ |
And (3) detection results:
example 4
The invention discloses a multiphase coupling method for preparing high abundance cerium magnet N38SH, comprising the following steps:
s1, separate preparation of first and second main phase alloys: respectively burdening according to the composition of a first main phase alloy and a second main phase alloy, respectively adding the burdening raw materials into a vacuum rapid-hardening sheet-throwing furnace for a strip throwing process, wherein the temperature T is 1430 and 1480 ℃, the refining T is 18-25 minutes, then standing for 5-8 minutes, and pouring to obtain two rapid-hardening sheets (respectively a first main phase alloy rapid-hardening sheet and a second main phase alloy rapid-hardening sheet) with the average thickness of 0.1-0.5 mm;
s2, adding the Dy-Fe alloy of Dy80/Fe20 into the first main phase rapid hardening tablet according to the proportion of 1-3% to perform hydrogen crushing (in a hydrogen crushing furnace to obtain fine powder, wherein the hydrogen content in the powder is 800-1000ppm, the oxygen content in the powder is 1000-1500ppm), and after the hydrogen crushing, usually adding a lubricant such as organic ester;
s3, obtaining two kinds of magnetic powder with the grain size of 1-6 μm and the grain size close to each other by an air flow mill, wherein the rotating speed of a sorting wheel during the air flow mill is controlled to be 2500 r/min-4500 r/min (an antioxidant is usually added in the air flow mill process);
and S4, mixing powder in a powder mixing machine, carrying out orientation molding on the mixed magnetic powder of the first main phase alloy and the second main phase alloy in a magnetic field with the magnetic field intensity of 1.5-2.5T under the inert gas protective atmosphere (the density of a primary molding blank is rho & lt 4.0-4.2), and carrying out cold isostatic pressing (190 plus 240Mpa) to prepare the blank (the density is rho & lt 4.2-4.4).
S5, sintering in a sintering furnace, preserving heat for 0.5-10 hours at 400-800 ℃ for dehydrogenation, preserving heat for 2-6 hours at 1030-1080 ℃ for water cooling (adopting water cooling in small experiments) or air cooling (adopting air cooling in production and directly blowing by a fan); the secondary tempering treatment is carried out for 2-6 hours at 750-950 ℃ and 550-750 ℃ respectively.
The articles of the examples of the present invention achieve a cerium iron magnet magnetic energy product of 36MGOe or more and an intrinsic coercive force of 21KOe or more when cerium oxide content is 30% or more in total rare earth.
Example 5
The invention discloses a multiphase coupling method for preparing high abundance cerium magnet N38SH, comprising the following steps:
s1, separate preparation of first and second main phase alloys: respectively burdening according to the composition of a first main phase alloy and a second main phase alloy, respectively adding the burdening raw materials into a vacuum rapid-hardening sheet-throwing furnace for a strip throwing process, wherein the temperature T is 1430 and 1480 ℃, the refining T is 18-25 minutes, then standing for 5-8 minutes, and pouring to obtain two rapid-hardening sheets (respectively a first main phase alloy rapid-hardening sheet and a second main phase alloy rapid-hardening sheet) with the average thickness of 0.1-0.5 mm;
s2, in the step S2, hydrogen breaking is separately carried out on the Dy-Fe alloy of Dy80/Fe20 and the first main phase alloy quick-setting sheet (in a hydrogen breaking furnace, fine powder is obtained, the hydrogen content in the powder is 800-1000ppm, and the oxygen content is 1000-1500 ppm); then mixing the first main phase alloy coarse powder after hydrogen crushing and the Dy-Fe alloy coarse powder of Dy80/Fe20 after hydrogen crushing according to a proportion; after the hydrogen milling, a lubricant, such as an organic ester, is usually added.
S3, obtaining two kinds of magnetic powder with the grain size of 1-6 μm and the grain size close to each other by an air flow mill, wherein the rotating speed of a sorting wheel during the air flow mill is controlled to be 2500 r/min-4500 r/min (an antioxidant is usually added during the air flow mill process);
and S4, mixing powder in a powder mixing machine, carrying out orientation molding on the mixed magnetic powder of the first main phase alloy and the second main phase alloy in a magnetic field with the magnetic field intensity of 1.5-2.5T under the inert gas protective atmosphere (the density of a primary molding blank is rho & lt 4.0-4.2), and carrying out cold isostatic pressing (190 plus 240Mpa) to prepare the blank (the density is rho & lt 4.2-4.4).
S5, sintering in a sintering furnace, preserving heat for 0.5-10 hours at 400-800 ℃ for dehydrogenation, preserving heat for 2-6 hours at 1030-1080 ℃ for water cooling (adopting water cooling in small experiments) or air cooling (adopting air cooling in production and directly blowing by a fan); the secondary tempering treatment is carried out for 2-6 hours at 750-950 ℃ and 550-750 ℃ respectively.
Example 6
As shown in fig. 1, 2, 3, 4, 5 and 6, the invention also discloses a mixing device for preparing the cerium magnets N38SH with high abundance, which comprises a mixing tank body 1, wherein a stirring device 2 is arranged in the mixing tank body, and the stirring device comprises a motor 3 arranged at the upper end of the mixing tank body and a stirring rod 4 driven by the motor; the lower part of the mixing tank body is provided with a blowing nozzle 5, and the blowing nozzle is connected with an external blowing part to blow air to the inner cavity of the mixing tank body. And a feeding port 6 is arranged at the top of the mixing tank body. The blowing component is externally connected with an argon or nitrogen gas source.
A cross rod 7 is arranged at the upper part of the stirring rod, a fixing sleeve 8 is arranged in the middle of the cross rod, a limiting ring 9 is arranged on the stirring rod below the fixing sleeve, the fixing sleeve is sleeved in the stirring rod, and a fixing disc 10 is arranged at the bottom of the stirring rod; the stirring rod below the cross rod is provided with a first stirring blade 11, the cross rod is provided with a movable block 12 sleeved on the cross rod, a spring 13 sleeved on the cross rod is arranged between the fixed sleeve and the movable block, one end of the spring is connected with the movable block, and the other end of the spring is connected with the fixed sleeve. The outside of movable block is equipped with the stopper 15 of installing on the horizontal pole. The bottom of the movable block is provided with a telescopic rod 16 made of elastic materials, the fixed disk is provided with a sliding groove 17, and the bottom of the telescopic rod is slidably connected with the sliding groove.
The outer side of the outer side wall of the fixed disk is provided with a conducting ring 18 made of conducting materials, the bottom of the conducting ring is provided with a conducting rod 19 which is electrically connected with the conducting rod, the bottom of the conducting rod is rotatably provided with a conducting ball 20 made of conducting materials, the inner wall of the bottom of the mixing tank body is provided with a conducting strip 21, the tail end of the conducting strip is provided with a brush piece 22 with the width larger than that of the conducting strip, and the brush piece is continuously contacted with the conducting ring; the bottom of the material mixing tank body is provided with a circular wedge-shaped disc 23, the upper width and the lower width of each electric brush piece are larger than the maximum thickness of the wedge-shaped disc, a resistance arc piece 24 is arranged on the wedge-shaped disc and comprises a plurality of resistance pieces 25, the resistance pieces are arranged along one direction, and the resistances of the resistance pieces are sequentially increased; the resistance piece is electrically connected with one pole of a mobile power supply 26, the electric brush piece is electrically connected with the other pole of the mobile power supply, an ammeter 27 is further arranged between the resistance piece and the mobile power supply, the ammeter is electrically connected with an external control unit 28, and the control unit is electrically connected with a driving motor; a second stirring blade 29 is arranged on the outer side of the telescopic rod; the second stirring blade is arranged between two adjacent first stirring blades. The top of the sliding groove protrudes towards the middle to form a limiting flange 30, and the bottom of the telescopic rod protrudes outwards to form a clamping piece 14. The control unit of the present invention may employ a computer system or a PLC (programmable logic controller).
In the implementation of the embodiment, the mixing method of two-phase flow coupling is implemented by shearing and coaction of the stirring rod and gas (argon or nitrogen); the first stirring blade rolls the powder from bottom to top, airflow is transversely broken up, and the high-speed impact and the shearing force generated by the airflow can fully disperse and mix the materials. When the puddler rotational speed difference is, the effect sliding block of effect at centrifugal force removes along the horizontal pole effect, drives the telescopic link and slides along the effect of fixed disk for second stirring vane has axial rotation simultaneously, also has up-and-down and side-to-side movement, and it has improved mixing efficiency, avoids appearing obvious layering at the faster effect of rotational speed material down.
The cross rod is driven to rotate along with the rotation of the stirring rod, the conductive rod machine and the conductive ball which are electrically connected with the conductive ring rotate along the wedge-shaped disc at the moment, the cross rod is pushed to be in contact with the resistance arc piece periodically, the electric brush piece is continuously contacted with the conductive ring and is electrically connected with one pole of the mobile power supply through the resistance piece, the electric brush piece is electrically connected with the other pole of the mobile power supply, so that the current meter in the closed circuit continuously changes, the control unit receives a current signal of the current meter and controls the periodic change of the output power of the driving motor, the first stirring blade and the second stirring blade periodically change (the current is increased, the rotation speed is reduced when the current is reduced or broken), the material does not drip and then is rolled up, and obvious layering of the material under the action of the rotation speed is avoided.
Example 7
As shown in fig. 7, the present embodiment 6 differs from embodiment 7 in that the cross section of the spring is an oval shape arranged vertically.
When this embodiment was implemented, the effect sliding block of centrifugal force removed along the horizontal pole effect, drove the spring and removed, and the spring of oval section still plays the effect that the removal was moved to the promotion material.
The above description is only for the preferred embodiment of the present invention and is not intended to limit the scope of the present invention, and all equivalent structural changes made by using the contents of the present specification and the drawings can be directly or indirectly applied to other related technical fields and are included in the scope of the present invention.
Claims (10)
1. A multiphase coupling method for making high abundance cerium magnet N38SH, comprising the steps of:
s1, separate preparation of first and second main phase alloys: respectively burdening according to the composition of the first main phase alloy and the second main phase alloy, respectively adding the burdened raw materials into a vacuum rapid hardening and flailing furnace to carry out a strip throwing process, refining for 18-25 minutes, then standing for 5-8 minutes, and pouring to obtain two rapid hardening slices, namely a first main phase alloy rapid hardening slice and a second main phase alloy rapid hardening slice;
s2, hydrogen breaking Dy-Fe alloy of Dy80/Fe20 and the first main phase alloy quick-setting slice;
s3, adding the dysprosium-iron alloy of the hydrogen-broken Dy80/Fe20 into the hydrogen-broken first main phase alloy quick-setting sheet, and respectively carrying out airflow milling on the mixture and the second main phase alloy quick-setting sheet to obtain two kinds of magnetic powder with the particle size being close to each other;
s4, mixing powder in a powder mixing device, then under the protective atmosphere of inert gas, orienting and forming the mixed magnetic powder of the first main phase alloy and the second main phase alloy in a magnetic field with the magnetic field intensity of 1.5-2.5T, and then carrying out cold isostatic pressing to prepare a blank;
s5, sintering the prepared blank in a sintering furnace, preserving heat for 0.5-10 hours at 400-800 ℃ for dehydrogenation, preserving heat for 2-6 hours at 1030-1080 ℃ for cooling, and then performing secondary tempering treatment for 2-6 hours at 750-750 ℃ and 550-750 ℃ respectively.
2. The multiphase coupling method for producing high abundance cerium magnet N38SH, as claimed in claim 1, wherein the temperature of the strip spinning process in step S1 is 1430-1480 ℃.
3. The multiphase coupling method for producing high abundance cerium magnet N38SH according to claim 1, wherein the step S3 yields two magnetic powders having a particle size between 1-6 μm.
4. The multiphase coupling method according to claim 3, wherein the rotation speed of the classifying wheel during jet milling in step S3 is controlled to be 2500 r/min-4500 r/min.
5. The multiphase coupling method for preparing high abundance cerium-iron magnet N38SH as claimed in claim 1 or 2 or 3 or 4, wherein Dy-iron alloy of Dy80/Fe20 is added to the first main phase rapid solidified sheet for hydrogen fragmentation in step S2.
6. The multiphase coupling method for preparing high abundance cerium-iron magnet N38SH as claimed in claim 1 or 2 or 3 or 4, wherein Dy-iron alloy of Dy80/Fe20 and the first main phase alloy rapidly solidified sheet are separately subjected to hydrogen fracturing in step S2; and then mixing the first main phase alloy coarse powder after hydrogen crushing and the Dy-Fe alloy coarse powder of Dy80/Fe20 after hydrogen crushing according to the proportion.
7. A powder mixing apparatus for making high abundance cerium magnet N38SH, comprising: the stirring device comprises a motor and a stirring rod driven by the motor, wherein the motor is arranged at the upper end of the material mixing tank body; the stirring rod is provided with a first stirring blade; the lower part of the mixing tank body is provided with a blowing nozzle, and the blowing nozzle is connected with an external blowing part and used for blowing air to the inner cavity of the mixing tank body; and a feeding port is arranged at the top of the mixing tank body.
8. The powder mixing apparatus for preparing high-abundance cerium iron bodies N38SH according to claim 7, wherein a cross bar is installed on the upper part of the stirring rod, a fixing sleeve is installed in the middle of the cross bar, a limiting ring is installed on the stirring rod below the fixing sleeve, the fixing sleeve is sleeved in the stirring rod, and a fixing disc is installed at the bottom of the stirring rod; a first stirring blade is arranged on a stirring rod below the cross rod, a movable block sleeved on the cross rod is arranged on the cross rod, a spring sleeved on the cross rod is arranged between the fixed sleeve and the movable block, one end of the spring is connected with the movable block, and the other end of the spring is connected with the fixed sleeve; the outside of movable block is equipped with the stopper of installing on the horizontal pole. The bottom of the movable block is provided with a telescopic rod, the fixed disk is provided with a sliding chute, and the bottom of the telescopic rod is slidably connected with the sliding chute.
9. The powder mixing equipment for preparing the cerium iron magnet N38SH with high abundance according to claim 8, wherein a conductive ring made of conductive material is arranged on the outer side of the outer side wall of the fixed disk, a conductive rod is electrically connected to the bottom of the conductive ring, a conductive ball made of conductive material is rotatably installed at the bottom of the conductive rod, a conductive sheet is arranged on the inner wall of the bottom of the material mixing tank, a brush piece with a width larger than that of the conductive sheet is arranged at the tail end of the conductive sheet, and the brush piece is continuously contacted with the conductive ring; the bottom of the material mixing tank body is provided with a circular wedge-shaped disc, the upper width and the lower width of the electric brush piece are larger than the maximum thickness of the wedge-shaped disc, the wedge-shaped disc is provided with a resistance arc piece, the resistance arc piece comprises a plurality of resistance pieces, the resistance pieces are arranged along one direction, and the resistances of the resistance pieces are sequentially increased; the resistance piece is electrically connected with one pole of the mobile power supply, the electric brush piece is electrically connected with the other pole of the mobile power supply, and a second stirring blade is arranged on the outer side of the telescopic rod; the second stirring blade is arranged between two adjacent first stirring blades.
10. The powder mixing apparatus for preparing the cerium iron magnet N38SH according to claim 8, wherein an ammeter is further disposed between the resistive member and the mobile power source, and is electrically connected to a control unit, and the control unit is electrically connected to a driving motor; the top of the sliding groove protrudes towards the middle to form a limiting flange, and the bottom of the telescopic rod protrudes outwards to form a clamping piece; the cross section of the spring is in an oval shape which is vertically arranged.
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