CN108878091A - A kind of preparation method of the Mn-Bi permanent magnet with ceramic protection layer - Google Patents
A kind of preparation method of the Mn-Bi permanent magnet with ceramic protection layer Download PDFInfo
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- CN108878091A CN108878091A CN201810704772.1A CN201810704772A CN108878091A CN 108878091 A CN108878091 A CN 108878091A CN 201810704772 A CN201810704772 A CN 201810704772A CN 108878091 A CN108878091 A CN 108878091A
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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
- H01F1/059—Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and Va elements, e.g. Sm2Fe17N2
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C12/00—Alloys based on antimony or bismuth
-
- 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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
- C23C4/11—Oxides
-
- 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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/134—Plasma spraying
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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
- H01F41/32—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 conductive, insulating or magnetic material on a magnetic film, specially adapted for a thin magnetic film
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Power Engineering (AREA)
- Plasma & Fusion (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Coating By Spraying Or Casting (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
Abstract
The invention discloses a kind of preparation method of Mn-Bi permanent magnet with ceramic protection layer, permanent-magnet material made from this method has excellent, stable permanent magnetism performance, and can be obtained by simple and easy preparation method；The present invention can guarantee magnet matrix and Al2O3Being connected firmly between-NiO composite ceramic coat, Al2O3- NiO composite ceramic coat is less prone to bubble and falls, while preparing Al using plasma spraying technology2O3- NiO composite ceramic coat so as to realize magnet surface high quality protect.
Description
Technical field
The present invention relates to magnetic material manufacturing fields, and in particular to a kind of system of the Mn-Bi permanent magnet with ceramic protection layer
Preparation Method.
Background technique
Rare earth permanent-magnetic material refers to alloy that rare earth metal and magnesium-yttrium-transition metal are formed through permanent magnetism made of certain technique
Material.Rare earth permanent-magnetic material is a kind of highest permanent-magnet material of currently known comprehensive performance, the magnetic that it is used than 90th century
The magnetic property of steel is more than 100 times high, and much than ferrite, alnico superior performance, the magnetic property than expensive platinum cobalt alloy is also high
One times.Due to the use of rare earth permanent-magnetic material, permanent magnet devices are not only promoted to miniaturization, improve the performance of product,
And promote the generation of certain particular devices, so rare earth permanent-magnetic material one occurs, cause greatly to pay attention to immediately, develop extremely fast
Speed.Rare earth permanent-magnetic material is applied widely in fields such as machinery, electronics, instrument and medical treatment.
Low-temperature phase (LTP) MnBi alloy has high magnetic anisotropy (11.6 × 106Erg/cc), Curie temperature is about
633K has positive coercive force temperature coefficient within the temperature range of 150K~550K, therefore MnBi alloy is considered to have
The high temperature permanent magnetic material of wide application prospect.The ferromagnetic property of MnBi is mainly derived from its low-temperature phase.MnBi alloy is at normal temperature
Multiple phases being closely connected can be formed, such as there are also cenotypes for low-temperature phase, high-temperature-phase, this largely constrains MnBi
The development of alloy brings great difficulty to the MnBi alloy of preparation high-purity low-temperature phase content.
Due to magnet phase alloy, processing technology is powder metallurgy or sinter molding.Short texture is porous, the electricity between each phase
Potential difference is larger, is easy to constitute the serious intercrystalline corrosion of primary battery generation under gentle environment, seriously affects performance and the longevity of magnet
Life.Currently, most commonly seen magnet surface guard technology is plating and chemical plating, however utilize plating and chemical plating process in magnetic
Body matrix surface prepares protective layer, and table, which mediates reason and plating process, can all make liquid substance enter substrate, so that in the later period
It blisters inside protective layer in use process, the failure phenomenons such as peeling.
Summary of the invention
The present invention provides a kind of preparation method of Mn-Bi permanent magnet with ceramic protection layer, permanent magnetism material made from this method
Material has excellent, stable permanent magnetism performance, and can be obtained by simple and easy preparation method；The present invention can guarantee magnetic
Body matrix and Al2O3Being connected firmly between-NiO composite ceramic coat, Al2O3- NiO composite ceramic coat is less prone to bubble
With fall, while using plasma spraying technology prepare Al2O3- NiO composite ceramic coat is so as to realizing that magnet surface is high-quality
Amount protection.
To achieve the goals above, above-mentioned purpose is realized, the present invention provides a kind of manganese bismuth with ceramic protection layer is forever
The preparation method of magnet, the Components Chemical formula of the permanent-magnet material matrix are Mn100-x-yBixCoy, wherein x=42-45, y=1-3；
This method comprises the following steps：
（1）Each element, which is weighed, according to mentioned component chemical formula carries out ingredient；
（2）Ingredient is placed in smelting furnace, at least up to 5 × 10 are vacuumized in furnace-3Pa；Then, helium injection gas to furnace pressure is
50-80kPa；It is warming up to 1300-1450 DEG C of fusing, is cast in water cooled copper mould after stirring, refining stand-by；
（3）Obtained alloy cast ingot is crushed, vacuum is fitted into and gets rid of in the quartz ampoule in machine, quartz ampoule bottom end nozzle diameter is
0.5-0.8mm gets rid of after the cavity with machine vacuumizes vacuum, protective gas is filled with into cavity；It connects vacuum and gets rid of band electromechanical source,
The alloy in fused quartz pipe is heated, meanwhile, control quartz ampoule bottom end nozzle to copper roller surface distance is 1-5mm, adjusts vacuum
Band machine copper roller revolving speed is got rid of, makes copper roller revolving speed 55-65m/s, mother alloy melt is ejected on the copper roller of rotation, permanent magnetism material is obtained
Expect strip；Strip is placed in vacuum tube furnace and is heat-treated, heat treatment condition is：In 350 DEG C of -400 DEG C of temperature ranges
Heat preservation 15-20 hours is cast using copper mold after then re-melting and permanent-magnet material matrix is made；
(4) permanent-magnet material matrix is pre-processed：To matrix shaping, blasting treatment removes the attachment of matrix surface, and adopts
Coarse surface is cleaned with high pressure dry gas；
Permanent-magnet material matrix after pretreatment is subjected to the pre-heat treatment, preheating temperature 120-145 under vacuum conditions
DEG C, time 12-15min；
Permanent-magnet material matrix surface after preheat prepares one layer 15-25 μm of Ti-Al alloy-layer transition using plasma spraying
Layer；
In the Al that Ti-Al alloy-layer transition layer surface uses plasma spraying to prepare one layer 50-75 μm2O3- NiO composite ceramics
Layer, obtains product.
Preferably, permanent-magnet material matrix surface after preheat prepares one layer of Ti-Al alloy-layer mistake using plasma spraying
The Plasma Spray Parameters for crossing layer are：Spray voltage is 25-30V, and spraying current 300-350A, primary air amount is 1500-
2000L/h, powder feeding rate 150-180L/h, spray distance 50-75mm.
Preferably, one layer of Al is prepared using plasma spraying in Ti-Al alloy-layer transition layer surface2O3- NiO composite ceramics
Layer Plasma Spray Parameters be：Spray voltage is 40-45V, and spraying current 400-450A, primary air amount is 2000-
2400L/h, powder feeding rate 220-250L/h, spray distance 50-75mm.
Permanent magnet prepared by the present invention has following advantages：
（1）Permanent-magnet material made from this method has excellent, stable permanent magnetism performance, and can pass through simple and easy preparation
Method obtains；
（2）The present invention can guarantee magnet matrix and Al2O3Being connected firmly between-NiO composite ceramic coat, Al2O3- NiO is multiple
It closes ceramic coating to be less prone to bubble and fall, while Al is prepared using plasma spraying technology2O3- NiO composite ceramic coat from
And the protection of magnet surface high quality may be implemented.
Specific embodiment
Embodiment one
The Components Chemical formula of the present embodiment permanent-magnet material matrix is Mn57Bi42Co1。
Each element, which is weighed, according to mentioned component chemical formula carries out ingredient；Ingredient is placed in smelting furnace, is evacuated in furnace
Reach 5 × 10 less-3Pa；Then, helium injection gas to furnace pressure is 50kPa；1300 DEG C of fusings are warming up to, are cast after stirring, refining
It is stand-by into water cooled copper mould.
Obtained alloy cast ingot is crushed, vacuum is fitted into and gets rid of in the quartz ampoule in machine, quartz ampoule bottom end nozzle diameter is
0.5mm gets rid of after the cavity with machine vacuumizes vacuum, protective gas is filled with into cavity；It connects vacuum and gets rid of band electromechanical source, heating
Alloy in fused quartz pipe, meanwhile, control quartz ampoule bottom end nozzle to copper roller surface distance is 1mm, and adjustment vacuum gets rid of band machine
Copper roller revolving speed makes copper roller revolving speed 55m/s, mother alloy melt is ejected on the copper roller of rotation, permanent-magnet material strip is obtained；
Strip is placed in vacuum tube furnace and is heat-treated, heat treatment condition is：It is small in 350 DEG C of temperature range inside holdings 15
When, it is cast after then re-melting using copper mold and permanent-magnet material matrix is made.
Permanent-magnet material matrix is pre-processed：To matrix shaping, blasting treatment removes the attachment of matrix surface, and adopts
Coarse surface is cleaned with high pressure dry gas；Will by pretreatment after permanent-magnet material matrix under vacuum conditions into
Row the pre-heat treatment, preheating temperature are 120 DEG C, time 12min；Permanent-magnet material matrix surface after preheat uses plasma spray
Apply the Ti-Al alloy-layer transition zone of one layer 15 μm of preparation；Permanent-magnet material matrix surface after preheat is coated using plasma spray
It is for the Plasma Spray Parameters of one layer of Ti-Al alloy-layer transition zone：Spray voltage is 25-30V, spraying current 300A, master
Throughput is 1500L/h, powder feeding rate 150L/h, spray distance 50mm.
In the Al that Ti-Al alloy-layer transition layer surface uses plasma spraying to prepare one layer 50 μm2O3- NiO composite ceramics
Layer, obtains product.One layer of Al is prepared using plasma spraying in Ti-Al alloy-layer transition layer surface2O3- NiO composite ceramic layer
Plasma Spray Parameters are：Spray voltage is 40V, and spraying current 400A, primary air amount is 2000L/h, and powder feeding rate is
220L/h, spray distance 50mm.
Embodiment two
The Components Chemical formula of the present embodiment permanent-magnet material matrix is Mn52Bi45Co3。
Each element, which is weighed, according to mentioned component chemical formula carries out ingredient；Ingredient is placed in smelting furnace, is evacuated in furnace
Reach 5 × 10 less-3Pa；Then, helium injection gas to furnace pressure is 80kPa；1450 DEG C of fusings are warming up to, are cast after stirring, refining
It is stand-by into water cooled copper mould.
Obtained alloy cast ingot is crushed, vacuum is fitted into and gets rid of in the quartz ampoule in machine, quartz ampoule bottom end nozzle diameter is
0.8mm gets rid of after the cavity with machine vacuumizes vacuum, protective gas is filled with into cavity；It connects vacuum and gets rid of band electromechanical source, heating
Alloy in fused quartz pipe, meanwhile, control quartz ampoule bottom end nozzle to copper roller surface distance is 1-5mm, and adjustment vacuum gets rid of band
Machine copper roller revolving speed makes copper roller revolving speed 65m/s, mother alloy melt is ejected on the copper roller of rotation, permanent-magnet material strip is obtained；
Strip is placed in vacuum tube furnace and is heat-treated, heat treatment condition is：It is small in 400 DEG C of temperature range inside holdings 20
When, it is cast after then re-melting using copper mold and permanent-magnet material matrix is made.
Permanent-magnet material matrix is pre-processed：To matrix shaping, blasting treatment removes the attachment of matrix surface, and adopts
Coarse surface is cleaned with high pressure dry gas；Will by pretreatment after permanent-magnet material matrix under vacuum conditions into
Row the pre-heat treatment, preheating temperature are 145 DEG C, time 15min.
Permanent-magnet material matrix surface after preheat prepares one layer 25 μm of Ti-Al alloy-layer transition using plasma spraying
Layer；Permanent-magnet material matrix surface after preheat prepares the plasma of one layer of Ti-Al alloy-layer transition zone using plasma spraying
Spray parameters are：Spray voltage is 30V, and spraying current 350A, primary air amount is 2000L/h, powder feeding rate 180L/h, spray
Applying distance is 75mm.
In the Al that Ti-Al alloy-layer transition layer surface uses plasma spraying to prepare one layer 75 μm2O3- NiO composite ceramics
Layer, obtains product.One layer of Al is prepared using plasma spraying in Ti-Al alloy-layer transition layer surface2O3- NiO composite ceramic layer
Plasma Spray Parameters are：Spray voltage is 45V, and spraying current 450A, primary air amount is 2400L/h, and powder feeding rate is
250L/h, spray distance 75mm.
Claims (3)
1. a kind of preparation method of the Mn-Bi permanent magnet with ceramic protection layer, the Components Chemical formula of the permanent-magnet material matrix are
Mn100-x-yBixCoy, wherein x=42-45, y=1-3；
This method comprises the following steps：
（1）Each element, which is weighed, according to mentioned component chemical formula carries out ingredient；
（2）Ingredient is placed in smelting furnace, at least up to 5 × 10 are vacuumized in furnace-3Pa；Then, helium injection gas to furnace pressure is
50-80kPa；It is warming up to 1300-1450 DEG C of fusing, is cast in water cooled copper mould after stirring, refining stand-by；
（3）Obtained alloy cast ingot is crushed, vacuum is fitted into and gets rid of in the quartz ampoule in machine, quartz ampoule bottom end nozzle diameter is
0.5-0.8mm gets rid of after the cavity with machine vacuumizes vacuum, protective gas is filled with into cavity；It connects vacuum and gets rid of band electromechanical source,
The alloy in fused quartz pipe is heated, meanwhile, control quartz ampoule bottom end nozzle to copper roller surface distance is 1-5mm, adjusts vacuum
Band machine copper roller revolving speed is got rid of, makes copper roller revolving speed 55-65m/s, mother alloy melt is ejected on the copper roller of rotation, permanent magnetism material is obtained
Expect strip；Strip is placed in vacuum tube furnace and is heat-treated, heat treatment condition is：In 350 DEG C of -400 DEG C of temperature ranges
Heat preservation 15-20 hours is cast using copper mold after then re-melting and permanent-magnet material matrix is made；
(4) permanent-magnet material matrix is pre-processed：To matrix shaping, blasting treatment removes the attachment of matrix surface, and adopts
Coarse surface is cleaned with high pressure dry gas；
Permanent-magnet material matrix after pretreatment is subjected to the pre-heat treatment, preheating temperature 120-145 under vacuum conditions
DEG C, time 12-15min；
Permanent-magnet material matrix surface after preheat prepares one layer 15-25 μm of Ti-Al alloy-layer transition using plasma spraying
Layer；
In the Al that Ti-Al alloy-layer transition layer surface uses plasma spraying to prepare one layer 50-75 μm2O3- NiO composite ceramic layer,
Obtain product.
2. the method as described in claim 1, which is characterized in that permanent-magnet material matrix surface after preheat uses plasma spray
Apply preparation one layer of Ti-Al alloy-layer transition zone Plasma Spray Parameters be：Spray voltage is 25-30V, spraying current 300-
350A, primary air amount are 1500-2000L/h, powder feeding rate 150-180L/h, spray distance 50-75mm.
3. method according to claim 1 or 2, which is characterized in that use plasma spray in Ti-Al alloy-layer transition layer surface
Apply one layer of Al of preparation2O3The Plasma Spray Parameters of-NiO composite ceramic layer are：Spray voltage is 40-45V, and spraying current is
400-450A, primary air amount are 2000-2400L/h, powder feeding rate 220-250L/h, spray distance 50-75mm.
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| CN201810704772.1A CN108878091A (en) | 2018-06-30 | 2018-06-30 | A kind of preparation method of the Mn-Bi permanent magnet with ceramic protection layer |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109326436A (en) * | 2018-12-18 | 2019-02-12 | 王顺良 | A kind of method of two-phase manganese bismuth permanent-magnet material |
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| CN102909381A (en) * | 2012-10-17 | 2013-02-06 | 北京工业大学 | Method for preparing high coercive force manganese-bismuth magnetic powder by doping cobalt nano-particles |
| CN107254656A (en) * | 2017-08-17 | 2017-10-17 | 桂林电子科技大学 | Neodymium-iron-boron permanent magnetic material surface plasma sprayed ceramic layer and preparation method thereof |
| CN107799291A (en) * | 2017-10-22 | 2018-03-13 | 苏州南尔材料科技有限公司 | A kind of preparation method of the manganese bismuth permanent-magnet material with electrodeposited coating |
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2018
- 2018-06-30 CN CN201810704772.1A patent/CN108878091A/en active Pending
Patent Citations (3)
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| CN102909381A (en) * | 2012-10-17 | 2013-02-06 | 北京工业大学 | Method for preparing high coercive force manganese-bismuth magnetic powder by doping cobalt nano-particles |
| CN107254656A (en) * | 2017-08-17 | 2017-10-17 | 桂林电子科技大学 | Neodymium-iron-boron permanent magnetic material surface plasma sprayed ceramic layer and preparation method thereof |
| CN107799291A (en) * | 2017-10-22 | 2018-03-13 | 苏州南尔材料科技有限公司 | A kind of preparation method of the manganese bismuth permanent-magnet material with electrodeposited coating |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109326436A (en) * | 2018-12-18 | 2019-02-12 | 王顺良 | A kind of method of two-phase manganese bismuth permanent-magnet material |
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Application publication date: 20181123 |