CN107689292A - A kind of preparation method of the double principal phase MULTILAYER COMPOSITE permanent magnets of Ce bases - Google Patents
A kind of preparation method of the double principal phase MULTILAYER COMPOSITE permanent magnets of Ce bases Download PDFInfo
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- CN107689292A CN107689292A CN201711055269.XA CN201711055269A CN107689292A CN 107689292 A CN107689292 A CN 107689292A CN 201711055269 A CN201711055269 A CN 201711055269A CN 107689292 A CN107689292 A CN 107689292A
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- 239000002131 composite material Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 31
- 239000000956 alloy Substances 0.000 claims abstract description 31
- 230000005291 magnetic effect Effects 0.000 claims abstract description 27
- 238000002844 melting Methods 0.000 claims abstract description 20
- 230000008018 melting Effects 0.000 claims abstract description 20
- 238000010791 quenching Methods 0.000 claims abstract description 19
- 230000000171 quenching effect Effects 0.000 claims abstract description 19
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 17
- 238000005275 alloying Methods 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 241000282887 Suidae Species 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000000137 annealing Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000004544 sputter deposition Methods 0.000 claims description 9
- 229910052796 boron Inorganic materials 0.000 claims description 8
- 239000000470 constituent Substances 0.000 claims description 8
- 239000000446 fuel Substances 0.000 claims description 8
- 229910052742 iron Inorganic materials 0.000 claims description 8
- 229910052750 molybdenum Inorganic materials 0.000 claims description 8
- 229910052726 zirconium Inorganic materials 0.000 claims description 8
- 238000000151 deposition Methods 0.000 claims description 5
- 230000008021 deposition Effects 0.000 claims description 5
- 239000000696 magnetic material Substances 0.000 abstract description 4
- 238000004093 laser heating Methods 0.000 description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 230000005389 magnetism Effects 0.000 description 7
- 238000009413 insulation Methods 0.000 description 6
- 238000010792 warming Methods 0.000 description 6
- 229910052761 rare earth metal Inorganic materials 0.000 description 5
- 150000002910 rare earth metals Chemical class 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910001172 neodymium magnet Inorganic materials 0.000 description 2
- 229910000521 B alloy Inorganic materials 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000005381 magnetic domain Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
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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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/005—Ferrous alloys, e.g. steel alloys containing rare earths, i.e. Sc, Y, Lanthanides
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/10—Ferrous alloys, e.g. steel alloys containing cobalt
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/12—Ferrous alloys, e.g. steel alloys containing tungsten, tantalum, molybdenum, vanadium, or niobium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/14—Ferrous alloys, e.g. steel alloys containing titanium or zirconium
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets 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
- H01F1/04—Magnets 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
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
- H01F1/055—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
- H01F1/057—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
- H01F1/0571—Alloys 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
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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
- H01F41/14—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 applying magnetic films to substrates
- H01F41/18—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 applying magnetic films to substrates by cathode sputtering
- H01F41/183—Sputtering targets therefor
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Abstract
The invention discloses a kind of preparation method of the double principal phase MULTILAYER COMPOSITE permanent magnets of Ce bases, belong to technical field of magnetic materials.The preparation method includes：1）Each raw material is weighed according to CeFeB alloying components and is mixed, and mixed material is subjected to vacuum melting, then fast quenching gets rid of band and alloy thin band is made；2）Each raw material is weighed according to CeCo alloying components and is mixed, mixed material is subjected to vacuum melting, then will be poured into after melted CeCo alloy pigs fusing in magnetic control spattering target mould, is polished, cuts after cooling, obtain CeCo targets；3）Make step using magnetron sputtering technique（2）Obtained CeCo targets are in step 1）CeCo layers are sequentially formed on the scope of freedom and chilling face of obtained CeFeB strips；4）By step（3）The double principal phase MULTILAYER COMPOSITE permanent magnets of obtained Ce bases carry out vacuum heat, and the double principal phase MULTILAYER COMPOSITE permanent magnets of Ce bases of the present invention are made.The preparation method of the double principal phase MULTILAYER COMPOSITE permanent magnets of Ce bases of the present invention not only improves the temperature stability of magnet, and ensures higher magnetic property, realizes temperature stability and the matched well of magnetic property.
Description
Technical field
The present invention relates to a kind of preparation method of the double principal phase MULTILAYER COMPOSITE permanent magnets of Ce bases, and in particular to a kind of CeFeB/
The preparation method of CeCo composite nanocrystalline magnets, belongs to technical field of magnetic materials.
Background technology
Increased sharply with the yield and sales volume of third generation neodymium iron boron magnetic body, cause industry to sharp rise Nd demands, seek
Metal Nd alternative metals or exploration magnet of new generation have become one of problem of neodymium iron boron industry solution.Therefore, researcher
Also having attempted to substitute Nd elements using Rare-Earth Ce, and carrying out substantial amounts of research work.In 1985, many scholars were
Through the research for starting Ce systems rare earth permanent-magnetic material.In recent years, particularly after the appearance of rare earth treaty, rare earth price rises violently into one
Step has promoted the attention that domestic and foreign scholars are developed to Ce systems rare earth permanent-magnetic material.Meanwhile domestic and international study hotspot mainly passes through
Ce substitutes Nd elements completely, prepares the Ce-Fe-B alloys using Ce2Fe14B as unique principal phase.Particularly in Ce-Fe-B Ji Na
In the brilliant magnet of rice, its magnetic property is preferably developed, however, the development in terms of its temperature stability is but relatively more slow always
Slowly.And Ce-Co bases magnet has higher temperature stability and Curie point, but its intrinsic magnetic characteristic is relatively low.Therefore,
Two kinds of permanent magnets with performance complement feature are combined with each other as high-performance high temperature resistant NEW TYPE OF COMPOSITE permanent magnetism is prepared at present
The new way of body.But composite permanent magnet is due to the effect between the interface microstructure between each magnet, Hard Magnetic phase, preparation
Technology controlling and process etc., which can not be realized, preferably to be recognized and controls, and is made its combination property and is not up to required.
In view of the above-mentioned problems, the present invention is combined using quick quenching technique-magnetron sputtering technique-laser heating heat treatment, effectively
Compound Ce-Fe-B bases and Ce-Co base nanometer crystal magnet, by its magnet thickness, Interface Microstructure and the control of phase composition, realizing
The preparation of the nanocrystalline permanent magnet of the double principal phase MULTILAYER COMPOSITEs of Ce bases of high-temperature characteristic and high magnetic characteristics.
The content of the invention
The purpose of the present invention is for overcome the deficiencies in the prior art, there is provided a kind of magnetic for effectively improving nanocrystalline composite
The preparation method of the double principal phase MULTILAYER COMPOSITE permanent magnets of the Ce bases of performance and temperature characterisitic.
The preparation method of the double principal phase MULTILAYER COMPOSITE permanent magnets of Ce bases of the present invention, comprises the following steps：
1）Each raw material is weighed according to CeFeB alloying components and is mixed, and mixed material is subjected to vacuum melting, then fast quenching is got rid of
Alloy thin band is made in band；
2）Each raw material is weighed according to CeCo alloying components and is mixed, and mixed material is subjected to vacuum melting, then by melting
Poured into after good CeCo alloy pigs fusing in magnetic control spattering target mould, polish, cut after cooling, obtain CeCo targets；
3）Make step using magnetron sputtering technique（2）Obtained CeCo targets are in step 1）The scope of freedom of obtained CeFeB strips
With CeCo layers are sequentially formed on chilling face；
4）By step（3）The double principal phase MULTILAYER COMPOSITE permanent magnets of obtained Ce bases carry out vacuum heat, and the Ce bases of the present invention are made
Double principal phase MULTILAYER COMPOSITE permanent magnets.
Further, the constituent of the CeFeB alloys and mass percent are：Ce：32.2~38.2%、Fe： 60.5
~72.5%、B：0.8~1.6%、Mo：0.1~0.6%、Zr：0.1~0.8%、Co：0.1~0.5%.
Further, step（1）The FFR'S fuel assembly that middle fast quenching gets rid of band is 15 ~ 40m/s.
Further, described CeCo alloys are CeCo5Or CeCo7Type magnet.
Further, step 3）The process conditions of middle magnetron sputtering deposition CeCo layers are：Vacuum chamber vacuum in sputter procedure
Spend for 8 × 10-3Pa~3×10-2Pa, magnetron sputtering electric current are 15 ~ 25A, the scope of freedom of strip and the sputtering time phase in chilling face
Together, the magnetron sputtering time is 15 ~ 45min.
Further, described vacuum heat treatment process parameter is：40 ~ 110 DEG C/s of heating rate, annealing temperature 450 ~
850 DEG C, 15 ~ 60min of annealing time.
Compared with prior art, the invention has the advantages that and beneficial effect：Pass through quick quenching technique-magnetron sputtering skill
Art-laser heating heat treatment technics, which is combined, prepares the double principal phase MULTILAYER COMPOSITE permanent magnets of Ce bases, more by adjusting CeFeB and CeCo
The thickness of layer magnet, crystallite dimension, make Ce2Fe14B phases and CeCo5Or CeCo7Exchange-coupling interaction mutually occurs for two Hard Magnetics of phase, has
The magnetic domain that effect realizes double Hard Magnetic phases synchronously inverts, the magnetic property of the double principal phase nanocrystalline magnets of lifting Ce bases；Meanwhile pass through magnetic control
Sputtering adds CeCo magnets, effectively improves the high-temperature stability of the double principal phase nanocrystalline magnets of Ce bases.
Embodiment
With reference to embodiment and comparative example, the present invention is further elaborated.
Embodiment 1
1）Each raw material is weighed according to CeFeB alloying components and is mixed, and mixed material is subjected to vacuum melting, then fast quenching is got rid of
Alloy thin band is made in band；The constituent and mass percent of the CeFeB alloys be：Ce：35.4%、Fe： 62.9%、B：
1.1%、Mo：0.2%、Zr：0.3%、Co：0.1%；The FFR'S fuel assembly that described fast quenching gets rid of band is 25m/s；
2）Each raw material is weighed according to CeCo alloying components and is mixed, and mixed material is subjected to vacuum melting, then by melting
Poured into after good CeCo alloy pigs fusing in magnetic control spattering target mould, polish, cut after cooling, obtain CeCo targets；It is described
CeCo alloys be CeCo5Type magnet；
3）Make CeCo using magnetron sputtering technique5Target sequentially forms CeCo on the scope of freedom of CeFeB strips and chilling face5
Layer；Described magnetron sputtering deposition CeCo5Layer process conditions be：Vacuum degree in vacuum chamber is 9 × 10 in sputter procedure-3Pa, magnetic
Control sputtering current is 20A, and the scope of freedom of strip and the sputtering time in chilling face are 20min；
4）The double principal phase MULTILAYER COMPOSITE permanent magnets of Ce bases obtained above are put into laser heating anneal stove, control laser heating is moved back
Stove heating rate is 90 DEG C/s, is warming up to 600 DEG C and insulation annealing 30min and carries out vacuum heat, the Ce of the present invention is made
The double principal phase MULTILAYER COMPOSITE permanent magnets of base.
Comparative example
1）Each raw material is weighed according to CeFeB alloying components and is mixed, and mixed material is subjected to vacuum melting, then fast quenching is got rid of
Alloy thin band is made in band；The constituent and mass percent of the CeFeB alloys be：Ce：35.4%、Fe：62.9%、B：
1.1%、Mo：0.2%、Zr：0.3%、Co：0.1%；The FFR'S fuel assembly that described fast quenching gets rid of band is 25m/s；
2）CeFeB alloy thin strip magnets obtained above are put into laser heating anneal stove, control laser heating anneal stove liter
Warm speed is 90 DEG C/s, is warming up to 600 DEG C and insulation annealing 30min and carries out vacuum heat, Ce base list principal phase permanent magnetism is made
Body.
Test remanent magnetism, coercivity, magnetic energy product and the Curie temperature of above-mentioned two sample respectively by vibrating specimen magnetometer, it is right
Than result as shown in table 1.
Table 1
From table 1, compared with Ce base list principal phase permanent magnets, double principal phase MULTILAYER COMPOSITE permanent magnets of Ce bases prepared by the present invention, its
Magnetic energy product improves 20.9%, and Curie temperature improves 15.7%.
Embodiment 2
1）Each raw material is weighed according to CeFeB alloying components and is mixed, and mixed material is subjected to vacuum melting, then fast quenching is got rid of
Alloy thin band is made in band；The constituent and mass percent of the CeFeB alloys be：Ce：36.1 %、Fe： 61.7%、B：
1.2%、Mo：0.3%、Zr：0.5%、Co：0.2%；The FFR'S fuel assembly that described fast quenching gets rid of band is 32m/s；
2）Each raw material is weighed according to CeCo alloying components and is mixed, and mixed material is subjected to vacuum melting, then by melting
Poured into after good CeCo alloy pigs fusing in magnetic control spattering target mould, polish, cut after cooling, obtain CeCo targets；It is described
CeCo alloys be CeCo5Type magnet；
3）Make CeCo using magnetron sputtering technique5Target sequentially forms CeCo on the scope of freedom of CeFeB strips and chilling face5
Layer；Described magnetron sputtering deposition CeCo5Layer process conditions be：Vacuum degree in vacuum chamber is 9 × 10 in sputter procedure-3Pa, magnetic
Control sputtering current is 20A, and the scope of freedom of strip and the sputtering time in chilling face are 30min；
4）The double principal phase MULTILAYER COMPOSITE permanent magnets of Ce bases obtained above are put into laser heating anneal stove, control laser heating is moved back
Stove heating rate is 90 DEG C/s, is warming up to 625 DEG C and insulation annealing 30min and carries out vacuum heat, the Ce of the present invention is made
The double principal phase MULTILAYER COMPOSITE permanent magnets of base.
Comparative example
1）Each raw material is weighed according to CeFeB alloying components and is mixed, and mixed material is subjected to vacuum melting, then fast quenching is got rid of
Alloy thin band is made in band；The constituent and mass percent of the CeFeB alloys be：Ce：36.1 %、Fe： 61.7%、B：
1.2%、Mo：0.3%、Zr：0.5%、Co：0.2%；The FFR'S fuel assembly that described fast quenching gets rid of band is 32m/s；
2）CeFeB alloy thin strip magnets obtained above are put into laser heating anneal stove, control laser heating anneal stove liter
Warm speed is 90 DEG C/s, is warming up to 625 DEG C and insulation annealing 30min and carries out vacuum heat, Ce base list principal phase permanent magnetism is made
Body.
Test remanent magnetism, coercivity, magnetic energy product and the Curie temperature of above-mentioned two sample respectively by vibrating specimen magnetometer, it is right
It is more as shown in table 2 than result.
Table 2
From table 2, compared with Ce base list principal phase permanent magnets, double principal phase MULTILAYER COMPOSITE permanent magnets of Ce bases prepared by the present invention, its
Magnetic energy product improves 36.6%, and Curie temperature improves 15.0%.
Embodiment 3
1）Each raw material is weighed according to CeFeB alloying components and is mixed, and mixed material is subjected to vacuum melting, then fast quenching is got rid of
Alloy thin band is made in band；The constituent and mass percent of the CeFeB alloys be：Ce：37.8 %、Fe： 59.2%、B：
1.5%、Mo：0.4%、Zr：0.7%、Co：0.4%；The FFR'S fuel assembly that described fast quenching gets rid of band is 35m/s；
2）Each raw material is weighed according to CeCo alloying components and is mixed, and mixed material is subjected to vacuum melting, then by melting
Poured into after good CeCo alloy pigs fusing in magnetic control spattering target mould, polish, cut after cooling, obtain CeCo targets；It is described
CeCo alloys be CeCo5Type magnet；
3）Make CeCo using magnetron sputtering technique5Target sequentially forms CeCo on the scope of freedom of CeFeB strips and chilling face5
Layer；Described magnetron sputtering deposition CeCo5Layer process conditions be：Vacuum degree in vacuum chamber is 9 × 10 in sputter procedure-3Pa, magnetic
Control sputtering current is 20A, and the scope of freedom of strip and the sputtering time in chilling face are 40min；
4）The double principal phase MULTILAYER COMPOSITE permanent magnets of Ce bases obtained above are put into laser heating anneal stove, control laser heating is moved back
Stove heating rate is 90 DEG C/s, is warming up to 660 DEG C and insulation annealing 30min and carries out vacuum heat, the Ce of the present invention is made
The double principal phase MULTILAYER COMPOSITE permanent magnets of base.
Comparative example
1）Each raw material is weighed according to CeFeB alloying components and is mixed, and mixed material is subjected to vacuum melting, then fast quenching is got rid of
Alloy thin band is made in band；The constituent and mass percent of the CeFeB alloys be：Ce：37.8 %、Fe： 59.2%、B：
1.5%、Mo：0.4%、Zr：0.7%、Co：0.4%；The FFR'S fuel assembly that described fast quenching gets rid of band is 35m/s；
2）CeFeB alloy thin strip magnets obtained above are put into laser heating anneal stove, control laser heating anneal stove liter
Warm speed is 90 DEG C/s, is warming up to 660 DEG C and insulation annealing 30min and carries out vacuum heat, Ce base list principal phase permanent magnetism is made
Body.
Test remanent magnetism, coercivity, magnetic energy product and the Curie temperature of above-mentioned two sample respectively by vibrating specimen magnetometer, it is right
It is more as shown in table 2 than result.
Table 3
From table 3, compared with Ce base list principal phase permanent magnets, double principal phase MULTILAYER COMPOSITE permanent magnets of Ce bases prepared by the present invention, its
Magnetic energy product improves 31.9%, and Curie temperature improves 17.1%.
Claims (6)
1. the preparation method of the double principal phase MULTILAYER COMPOSITE permanent magnets of a kind of Ce bases, it is characterised in that comprise the following steps：
1）Each raw material is weighed according to CeFeB alloying components and is mixed, and mixed material is subjected to vacuum melting, then fast quenching is got rid of
Alloy thin band is made in band；
2）Each raw material is weighed according to CeCo alloying components and is mixed, and mixed material is subjected to vacuum melting, then by melting
Poured into after good CeCo alloy pigs fusing in magnetic control spattering target mould, polish, cut after cooling, obtain CeCo targets；
3）Make step using magnetron sputtering technique（2）Obtained CeCo targets are in step 1）The scope of freedom of obtained CeFeB strips
With CeCo layers are sequentially formed on chilling face；
4）By step（3）The double principal phase MULTILAYER COMPOSITE permanent magnets of obtained Ce bases carry out vacuum heat, and the Ce bases of the present invention are made
Double principal phase MULTILAYER COMPOSITE permanent magnets.
2. the preparation method of the double principal phase MULTILAYER COMPOSITE permanent magnets of Ce bases according to claim 1, it is characterised in that：It is described
The constituent and mass percent of CeFeB alloys be：Ce：32.2~38.2%、Fe： 60.5~72.5%、B：0.8~1.6%、Mo：
0.1~0.6%、Zr：0.1~0.8%、Co：0.1~0.5%.
3. the preparation method of the double principal phase MULTILAYER COMPOSITE permanent magnets of Ce bases according to claim 1, it is characterised in that：Step
（1）The FFR'S fuel assembly that middle fast quenching gets rid of band is 15 ~ 40m/s.
4. the preparation method of the double principal phase MULTILAYER COMPOSITE permanent magnets of Ce bases according to claim 1, it is characterised in that：It is described
CeCo alloys be CeCo5Or CeCo7Type magnet.
5. the preparation method of the double principal phase MULTILAYER COMPOSITE permanent magnets of Ce bases according to claim 1, it is characterised in that：Step
（3）The process conditions of middle magnetron sputtering deposition CeCo layers are：Vacuum degree in vacuum chamber is 8 × 10 in sputter procedure-3Pa~3×10- 2Pa, magnetron sputtering electric current are 15 ~ 25A, and the scope of freedom of strip is identical with the sputtering time in chilling face, the magnetron sputtering time be 15 ~
45min。
6. the preparation method of the double principal phase MULTILAYER COMPOSITE permanent magnets of Ce bases according to claim 1, it is characterised in that：It is described
Vacuum heat treatment process parameter be：40 ~ 110 DEG C/s of heating rate, 450 ~ 850 DEG C of annealing temperature, annealing time 15 ~
60min。
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| CN201711055269.XA CN107689292B (en) | 2017-11-01 | 2017-11-01 | A kind of preparation method of the double main phase MULTILAYER COMPOSITE permanent magnets of Ce base |
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| JP2012209442A (en) * | 2011-03-30 | 2012-10-25 | Hitachi Metals Ltd | Bulk magnet and method for manufacturing the same |
| CN102800454A (en) * | 2012-08-30 | 2012-11-28 | 钢铁研究总院 | Low-cost double-main phase Ce permanent-magnet alloy and preparation method thereof |
| CN104332262A (en) * | 2014-08-27 | 2015-02-04 | 安泰科技股份有限公司 | Nanometer double-phase composite permanent magnetic material with high magnetic energy product and preparation method thereof |
| CN104762519A (en) * | 2015-03-23 | 2015-07-08 | 北京工业大学 | A preparing method of a nanocrystal Sm<2>Co<17>/Co double-phase composite permanent magnetic alloy |
| CN105374485A (en) * | 2015-11-26 | 2016-03-02 | 宁波科星材料科技有限公司 | Multi-layer composite magnet and preparation method thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012209442A (en) * | 2011-03-30 | 2012-10-25 | Hitachi Metals Ltd | Bulk magnet and method for manufacturing the same |
| CN102800454A (en) * | 2012-08-30 | 2012-11-28 | 钢铁研究总院 | Low-cost double-main phase Ce permanent-magnet alloy and preparation method thereof |
| CN104332262A (en) * | 2014-08-27 | 2015-02-04 | 安泰科技股份有限公司 | Nanometer double-phase composite permanent magnetic material with high magnetic energy product and preparation method thereof |
| CN104762519A (en) * | 2015-03-23 | 2015-07-08 | 北京工业大学 | A preparing method of a nanocrystal Sm<2>Co<17>/Co double-phase composite permanent magnetic alloy |
| CN105374485A (en) * | 2015-11-26 | 2016-03-02 | 宁波科星材料科技有限公司 | Multi-layer composite magnet and preparation method thereof |
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Application publication date: 20180213 Assignee: ZHEJIANG ZHONGYUAN MAGNETIC MATERIAL Co.,Ltd. Assignor: China Jiliang University Contract record no.: X2021330000034 Denomination of invention: A preparation method of CE based double main phase multilayer composite permanent magnet Granted publication date: 20191001 License type: Common License Record date: 20210408 |