CN107680769A - A kind of preparation method of the soft magnetic bodies with ceramic coating - Google Patents
A kind of preparation method of the soft magnetic bodies with ceramic coating Download PDFInfo
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- CN107680769A CN107680769A CN201710967572.0A CN201710967572A CN107680769A CN 107680769 A CN107680769 A CN 107680769A CN 201710967572 A CN201710967572 A CN 201710967572A CN 107680769 A CN107680769 A CN 107680769A
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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
- H01F1/12—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 soft-magnetic materials
- H01F1/14—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 soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/14766—Fe-Si based alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/02—Amorphous alloys with iron as the major constituent
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- 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
- C23C24/00—Coating starting from inorganic powder
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
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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
- H01F41/0266—Moulding; Pressing
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Materials Engineering (AREA)
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- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Manufacturing & Machinery (AREA)
- Soft Magnetic Materials (AREA)
Abstract
The invention discloses the invention discloses a kind of preparation method of the soft magnetic bodies with ceramic coating, employ and improve Fe base amorphous soft-magnetic alloys combination property favourable multiple element Ni, Cr, Cu, Mg, P and C, the iron-based soft magnetic soft magnetic bodies matrix being prepared, the present invention is also surface-treated to soft magnetic bodies row, can make soft magnetic bodies for excellent corrosion resistance, ultralow the advantages that subtracting magnetic and shock resistance.
Description
Technical field
The present invention relates to magnetic material manufacturing field, and in particular to a kind of preparation side of the soft magnetic bodies with ceramic coating
Method.
Background technology
Current power electronic device develops to energy-saving, miniaturization and high precision int direction, and it is strong to possess high-saturation magnetic induction
Spending the soft magnetic materials of (BS), low-loss and high magnetic permeability (μ) turns into the important directions of field of magnetic material research and development.Amorphous,
Nano-crystal soft magnetic alloy due to above-mentioned soft magnetism feature, being increasingly becoming each relevant enterprise and research institution's exploitation in recent years
Focus.
Nano-crystal soft magnetic alloy is the Fe base amorphous alloys being prepared into by single roller melt-quenching method, thermally treated technique,
α-Fe the crystal grain that equally distributed 10nm or so is separated out from amorphous alloy is prepared.Due to the saturation induction of α-Fe phases
Intensity is up to 2.2T, so the precipitation of α-Fe crystal grain, can make the saturation induction density of obtained nanometer crystal alloy after heat treatment
Specific heat before processing is substantially improved, and coercivity is remarkably decreased, and comprehensive soft magnet performance is significantly improved.But amorphous state is closed
The shortcomings that obvious also be present in gold：Saturation induction density is not high, compared to the soft magnetic materials of other high saturated magnetic inductions,
The alloy material needs more volume under identical condition of work, and this greatly limits its application.
Because the property of magnetically soft alloy is active, thus the corrosion resisting property of whole magnetically soft alloy is become very poor, particularly exist
Easily corrosion in damp and hot environment, and caused by corrosion failure magnetic property decline or damage, had a strong impact on soft magnetism conjunction
The service life of gold, reduce the stability and reliability of product.The magnetic property of magnetically soft alloy has very big with its institutional framework
Relation.After magnetically soft alloy corrodes, huge change will occur for its magnetic property.Therefore, the Anticorrosion of magnetically soft alloy
Always magnetically soft alloy needs one of subject matter solved.
The content of the invention
The present invention provides a kind of preparation method of the soft magnetic bodies with ceramic coating, employs and improves the conjunction of Fe bases amorphous soft magnet
Golden combination property favourable multiple element Ni, Cr, Cu, Mg, P and C, the iron-based soft magnetic soft magnetic bodies matrix being prepared, the present invention
Also soft magnetic bodies row is surface-treated, can make that soft magnetic bodies possess excellent corrosion resistance, ultralow to subtract magnetic and shock resistance etc. excellent
Point.
To achieve these goals, above-mentioned purpose is realized, the invention provides a kind of soft magnetic bodies with ceramic coating
Preparation method, the iron-based soft magnetic soft magnetic bodies matrix host are made up of the alloy of following atom ratio：Fe100-a-b-c-d-e-f- gCaSibCucPdCreMgfNig, wherein a=0.05-0.1, b=0.5-1, c=9.5-10, d=0.01-0.03, e=3-3.5, f=12-
15, g=6-8；
This method comprises the following steps：
(1) weigh each element according to above-mentioned atom ratio and carry out dispensing；
(2) food ingredient is put into boron nitride crucible, allows density big as far as possible and low-melting steel alloy or alloying element are placed on
Above, it is then placed in the induction coil in vacuum induction founding cavity, is then vacuumized with mechanical pump and diffusion pump, work as vacuum
Degree reaches the argon gas for being filled with that 0.04MPa purity is 99.999% after 2.0 × 10-3 Pa, as protective gas.Then start to melt
Refine foundry alloy, melting it is complete once after, power off, after complete cooling, continue to heat melting, continuous four times of its process, finally
Master alloy ingot is prepared；
(3) mother alloy ingot is broken for fritter sample, non-crystaline amorphous metal is made using copper mold casting after re-melting；
(4) non-crystaline amorphous metal is subjected to Annealing Crystallization processing, is that the length of side is broken less than 5mm by the non-crystaline amorphous metal precrushing after annealing
Piece, then powder is further broken up into by ball mill, ball mill is respectively adopted and carries out Shape correction, removes sharp corners, then
Stress relief annealing process is carried out, the various powder after stress relief annealing process are sieved into 50-100 mesh powders through sieve respectively
It is standby；
（5）Above-mentioned powder is inserted in former mold cavity, carries out compressing, the briquetting pressure control 700- that floats
800Mpa, shaping compacting total time is 5-8s/pcs；Former is suppressed using 200t hydraulic presses, in compacting 8-
Repressurization, progress pressurize 3-5s, product are not stripped again after 10s, obtain blank；Under argon gas protection, less than crystallization temperature 30-
At a temperature of 40K, isothermal annealing 1-1.5h, soft magnetic bodies matrix is obtained；
（6）Weigh 15-25 mass parts isobutyl groups e pioic acid methyl ester, 25-35 mass parts acetone, 2-4 mass parts mercaptopropionic acid, 20-30
Mass parts methacrylate -1- methylsiloxanes propyl ester and 35-45 mass parts NiFe2O4Nanometer powder is added in reactor, in 70-
At a temperature of 75 DEG C after stirring reaction 1-2 h, 2-5 mass parts diethanol amine, the tertiary fourth fat of 10-15 mass parts peracetic acids are added
It is well mixed with 5-10 mass parts methyl iso-butyl ketone (MIBK)s, obtains mixed liquor；
（7）Above-mentioned mixed liquor is uniformly smeared on above-mentioned soft magnetism matrix, 1-2 μm of per pass dried film thickness, 15-18 roads is applied, is used after being painted with
1-2 h are warming up to 280-290 DEG C of constant temperature 1-2h, then dry 20-25min at 390-410 DEG C, obtain soft magnetic bodies.
Iron-based soft magnetic body prepared by the present invention possesses advantages below：
（1）Employ and improve Fe base amorphous soft-magnetic alloys combination property favourable multiple element Ni, Cr, Cu, Mg, P and C, prepare
Obtained iron-based soft magnetic soft magnetic bodies matrix；
（2）The present invention also to soft magnetic bodies row be surface-treated, can make soft magnetic bodies possess excellent corrosion resistance, it is ultralow subtract magnetic with
And the advantages that shock resistance.
Embodiment
Embodiment one
The iron-based soft magnetic soft magnetic bodies matrix host of the present embodiment is made up of the alloy of following atom ratio：
Fe68.94C0.05Si0.5Cu9.5P0.01Cr3Mg12Ni6。
Each element, which is weighed, according to above-mentioned atom ratio carries out dispensing；Food ingredient is put into boron nitride crucible, allowed as far as possible
Density is big and low-melting steel alloy or alloying element are placed on the induction coil above, being then placed in vacuum induction founding cavity
In, then vacuumized with mechanical pump and diffusion pump, the purity that 0.04MPa is filled with after vacuum reaches 2.0 × 10-3 Pa is
99.999% argon gas, as protective gas.Then start master alloy melting, melting it is complete once after, power off, treat completely cold
But after, continue to heat melting, continuous four times of its process, master alloy ingot is finally prepared.
Mother alloy ingot is broken for fritter sample, non-crystaline amorphous metal is made using copper mold casting after re-melting；Amorphous closes
Gold is ribbon, and strip width 1mm, thickness is 20 μm.
Non-crystaline amorphous metal is subjected to Annealing Crystallization processing, is that the length of side is broken less than 5mm by the non-crystaline amorphous metal precrushing after annealing
Piece, then powder is further broken up into by ball mill, ball mill is respectively adopted and carries out Shape correction, removes sharp corners, then
Stress relief annealing process is carried out, it is standby that the various powder after stress relief annealing process are sieved into through sieve to 50 mesh powders respectively
With；Annealing Crystallization processing procedure is：Non-crystaline amorphous metal is subjected to Crystallizing treatment in vacuum atmosphere with isothermal annealing, annealing temperature is
600 DEG C, annealing time is 1 minute, is then quenched to room temperature.
Above-mentioned powder is inserted in former mold cavity, carries out compressing, the briquetting pressure control 700Mpa that floats,
Shaping compacting total time is 5s/pcs；Former is suppressed using 200t hydraulic presses, the not repressurization after 8s is suppressed,
Pressurize 3s is carried out, product is stripped again, obtains blank, and under argon gas protection, at a temperature of less than crystallization temperature 30K, isothermal moves back
Fiery 1h, obtain soft magnetic bodies matrix.
Weigh 15 mass parts isobutyl group e pioic acid methyl esters, 25 mass parts acetone, 2 mass parts mercaptopropionic acids, 20 mass parts isobutyls
Olefin(e) acid -1- methylsiloxanes propyl ester and 35 mass parts NiFe2O4Nanometer powder is added in reactor, is stirred at a temperature of 70 DEG C anti-
After answering 1 h, 2 mass parts diethanol amine, the tertiary fourth fat of 10 mass parts peracetic acids and the mixing of 5 mass parts methyl iso-butyl ketone (MIBK)s are added
Uniformly, mixed liquor is obtained.
Above-mentioned mixed liquor is uniformly smeared on above-mentioned soft magnetism matrix, 1 μm of per pass dried film thickness, 18 are applied, with 1 h liters after being painted with
Then temperature dries 20min at 390 DEG C, obtains soft magnetic bodies to 280 DEG C of constant temperature 1h.
Embodiment two
The iron-based soft magnetic soft magnetic bodies matrix host of the present embodiment is made up of the alloy of following atom ratio：
Fe62.37C0.1Si1Cu10P0.03Cr3.5Mg15Ni8。
Each element, which is weighed, according to above-mentioned atom ratio carries out dispensing；Food ingredient is put into boron nitride crucible, allowed as far as possible
Density is big and low-melting steel alloy or alloying element are placed on the induction coil above, being then placed in vacuum induction founding cavity
In, then vacuumized with mechanical pump and diffusion pump, the purity that 0.04MPa is filled with after vacuum reaches 2.0 × 10-3 Pa is
99.999% argon gas, as protective gas.Then start master alloy melting, melting it is complete once after, power off, treat completely cold
But after, continue to heat melting, continuous four times of its process, master alloy ingot is finally prepared.
Mother alloy ingot is broken for fritter sample, non-crystaline amorphous metal is made using copper mold casting after re-melting；Amorphous closes
Gold is ribbon, and strip width 2mm, thickness is 25 μm.
Non-crystaline amorphous metal is subjected to Annealing Crystallization processing, is that the length of side is broken less than 5mm by the non-crystaline amorphous metal precrushing after annealing
Piece, then powder is further broken up into by ball mill, ball mill is respectively adopted and carries out Shape correction, removes sharp corners, then
Stress relief annealing process is carried out, it is standby that the various powder after stress relief annealing process are sieved into through sieve to 100 mesh powders respectively
With；Annealing Crystallization processing procedure is：Non-crystaline amorphous metal is subjected to Crystallizing treatment in vacuum atmosphere with isothermal annealing, annealing temperature is
650 DEG C, annealing time is 3 minutes, is then quenched to room temperature.
Above-mentioned powder is inserted in former mold cavity, carries out compressing, the briquetting pressure control 800Mpa that floats,
Shaping compacting total time is 8s/pcs；Former is suppressed using 200t hydraulic presses, is no longer added after 10s is suppressed
Pressure, pressurize 5s being carried out, product is stripped again, obtains blank, under argon gas protection, at a temperature of less than crystallization temperature 40K, isothermal
Anneal 1.5h, obtains soft magnetic bodies matrix.
Weigh 25 mass parts isobutyl group e pioic acid methyl esters, 35 mass parts acetone, 4 mass parts mercaptopropionic acids, 30 mass parts isobutyls
Olefin(e) acid -1- methylsiloxanes propyl ester and 45 mass parts NiFe2O4Nanometer powder is added in reactor, is stirred at a temperature of 75 DEG C anti-
After answering 2 h, add 5 mass parts diethanol amine, the tertiary fourth fat of 15 mass parts peracetic acids and 10 mass parts methyl iso-butyl ketone (MIBK)s and mix
Close uniformly, obtain mixed liquor.
Above-mentioned mixed liquor is uniformly smeared on above-mentioned soft magnetism matrix, 2 μm of per pass dried film thickness, 15 are applied, with 2 h liters after being painted with
Then temperature dries 25min at 410 DEG C, obtains soft magnetic bodies to 290 DEG C of constant temperature 2h.
Claims (1)
1. a kind of preparation method of the soft magnetic bodies with ceramic coating, the iron-based soft magnetic soft magnetic bodies matrix host are matched somebody with somebody by following atom
The alloy of ratio is made：Fe100-a-b-c-d-e-f-gCaSibCucPdCreMgfNig, wherein a=0.05-0.1, b=0.5-1, c=9.5-10,
D=0.01-0.03, e=3-3.5, f=12-15, g=6-8；
This method comprises the following steps：
(1) weigh each element according to above-mentioned atom ratio and carry out dispensing；
(2) food ingredient is put into boron nitride crucible, allows density big as far as possible and low-melting steel alloy or alloying element are placed on
Above, it is then placed in the induction coil in vacuum induction founding cavity, is then vacuumized with mechanical pump and diffusion pump, work as vacuum
Degree reaches the argon gas for being filled with that 0.04MPa purity is 99.999% after 2.0 × 10-3 Pa, as protective gas；
Then start master alloy melting, melting it is complete once after, power off, after complete cooling, continue to heat melting, its process
Continuous four times, master alloy ingot is finally prepared；
(3) mother alloy ingot is broken for fritter sample, non-crystaline amorphous metal is made using copper mold casting after re-melting；
(4) non-crystaline amorphous metal is subjected to Annealing Crystallization processing, is that the length of side is broken less than 5mm by the non-crystaline amorphous metal precrushing after annealing
Piece, then powder is further broken up into by ball mill, ball mill is respectively adopted and carries out Shape correction, removes sharp corners, then
Stress relief annealing process is carried out, the various powder after stress relief annealing process are sieved into 50-100 mesh powders through sieve respectively
It is standby；
（5）Above-mentioned powder is inserted in former mold cavity, carries out compressing, the briquetting pressure control 700- that floats
800Mpa, shaping compacting total time is 5-8s/pcs；Former is suppressed using 200t hydraulic presses, in compacting 8-
Repressurization, progress pressurize 3-5s, product are not stripped again after 10s, obtain blank；Under argon gas protection, less than crystallization temperature 30-
At a temperature of 40K, isothermal annealing 1-1.5h, soft magnetic bodies matrix is obtained；
（6）Weigh 15-25 mass parts isobutyl groups e pioic acid methyl ester, 25-35 mass parts acetone, 2-4 mass parts mercaptopropionic acid, 20-30
Mass parts methacrylate -1- methylsiloxanes propyl ester and 35-45 mass parts NiFe2O4Nanometer powder is added in reactor, in 70-
At a temperature of 75 DEG C after stirring reaction 1-2 h, 2-5 mass parts diethanol amine, the tertiary fourth fat of 10-15 mass parts peracetic acids are added
It is well mixed with 5-10 mass parts methyl iso-butyl ketone (MIBK)s, obtains mixed liquor；
（7）Above-mentioned mixed liquor is uniformly smeared on above-mentioned soft magnetism matrix, 1-2 μm of per pass dried film thickness, 15-18 roads is applied, is used after being painted with
1-2 h are warming up to 280-290 DEG C of constant temperature 1-2h, then dry 20-25min at 390-410 DEG C, obtain soft magnetic bodies.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108754324A (en) * | 2018-06-13 | 2018-11-06 | 苏州诺弘添恒材料科技有限公司 | A kind of preparation method of the iron-based soft magnetic body with nano coating |
| CN109300683A (en) * | 2018-12-17 | 2019-02-01 | 瞿凌飞 | A kind of preparation method of iron-based soft magnetic composite cores |
| CN109378206A (en) * | 2018-12-17 | 2019-02-22 | 瞿凌飞 | A kind of 3d printing preparation method of iron-based magnetic core |
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| JP2004297036A (en) * | 2002-12-04 | 2004-10-21 | Mitsubishi Materials Corp | Method of manufacturing iron soft magnetic powder coated with spinel ferrite film containing zinc and soft magnetic sintered composite material produced by this method |
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| CN108754324A (en) * | 2018-06-13 | 2018-11-06 | 苏州诺弘添恒材料科技有限公司 | A kind of preparation method of the iron-based soft magnetic body with nano coating |
| CN109300683A (en) * | 2018-12-17 | 2019-02-01 | 瞿凌飞 | A kind of preparation method of iron-based soft magnetic composite cores |
| CN109378206A (en) * | 2018-12-17 | 2019-02-22 | 瞿凌飞 | A kind of 3d printing preparation method of iron-based magnetic core |
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