CN107574367A - A kind of magnetic alloy and preparation method thereof - Google Patents
A kind of magnetic alloy and preparation method thereof Download PDFInfo
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- CN107574367A CN107574367A CN201710835466.7A CN201710835466A CN107574367A CN 107574367 A CN107574367 A CN 107574367A CN 201710835466 A CN201710835466 A CN 201710835466A CN 107574367 A CN107574367 A CN 107574367A
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Abstract
The present invention relates to a kind of magnetic alloy and preparation method thereof, raw magnetic alloy composition and weight percentage are：Ag0.03 0.05%, Sc0.8 1.4%, In0.2 0.7%, Al0.05 0.08%, Sn0.2 0.7%, Be0.09 0.15%, Pm0.05 0.12%, Au0.003 0.008%, Si1.6 1.9%, B2.1 2.9%, surplus is Fe, preparation method step includes dispensing, melting, system band, siliconising, heat treatment, the material has heat endurance good, and there is good magnetic property, preparation method technique is simple, and production cost is low, suitable for industrialized production.
Description
Technical field
The invention belongs to technical field of magnetic materials, and in particular to a kind of magnetic alloy and preparation method thereof.
Background technology
CN201310213199.1 discloses a kind of Mo-Zn-In systems Fe-based amorphous alloy strip, and it forms the original of each element
Sub- percentage is：Mo3-5、Zn8-10、In2-3、As0.5-0.8、Sb0.02-0.04、Bi0.9-1.2、Yb0.01-0.02、
Lu0.03-0.04, Fe surplus.The present invention prepare nanocrystalline strip to routine nanocrystalline strip preparation method it is similar, the application
Other compositions such as the dopant material based on Mo-Zn-In, addition Sb, Bi, Yb, optimize Technology for Heating Processing, hence it is evident that improve nanocrystalline
The stress distribution of alloy strip steel rolled stock so that nanometer crystal alloy material of the present invention has excellent toughness, good plasticity, excellent soft
Magnetic property and good nanocrystalline Forming ability, can be widely applied to various nano-crystalline thin ribbon annulus materials.But combination property
It is not high.
The content of the invention
In view of the shortcomings of the prior art, the present invention provides a kind of magnetic alloy and preparation method thereof, and the material has heat steady
It is qualitative good, and there is good magnetic property, preparation method technique is simple, and production cost is low, suitable for industrialized production.
The technical solution adopted by the present invention is：
A kind of magnetic alloy, its material composition and weight percentage are：Ag0.03-0.05%, Sc0.8-1.4%,
In0.2-0.7%, Al0.05-0.08%, Sn0.2-0.7%, Be0.09-0.15%, Pm0.05-0.12%, Au0.003-
0.008%th, Si1.6-1.9%, B2.1-2.9%, surplus Fe；The B is added in the form of ferro-boron intermediate alloy, in ferro-boron
Between in alloy B weight/mass percentage composition be 20-25%；
A kind of preparation method of magnetic alloy, step include：
A, by alloy raw material Ingredients Weight percentage composition be Ag0.03-0.05%, Sc0.8-1.4%, In0.2-0.7%,
Al0.05-0.08%, Sn0.2-0.7%, Be0.09-0.15%, Pm0.05-0.12%, Au0.003-0.008%, Si1.6-
1.9%th, B2.1-2.9%, surplus are that Fe carries out dispensing；The B is added in the form of ferro-boron intermediate alloy, ferro-boron intermediate alloy
Middle B weight/mass percentage composition is 20-25%.
B, raw material is put into melting in vaccum sensitive stove, smelting temperature is 1570~1600 DEG C, soaking time 6-
15min, foundry alloy is obtained after casting cooling；
C, vacuum rapid hardening is carried out after remelting being carried out in remelting tubular type crucible that foundry alloy is put into vacuum induction forming furnace
Get rid of band and alloy strip is made, remelting temperature is 1540~1560 DEG C；The remelting tubular type crucible bottom is provided with through hole, remelting tubular type earthenware
Crucible top connects nitrogen through valve, and the pressure of nitrogen is 1.4~1.6atm；The bottom of remelting tubular type crucible is placed in forming furnace runner
On wheel rim at 2~4mm, after foundry alloy melts, the valve on remelting tubular type crucible top is opened, melting foundry alloy is in nitrogen pressure
The forming furnace runner wheel rim of rotation is sprayed under power from the through hole of crucible bottom, forms continuous alloy strip；Remelting tubular type crucible
Internal diameter is 12~14mm, is highly 250~280mm, and the through-hole aperture of remelting tubular type crucible bottom is 1.3~1.5mm.Runner revolves
It is 24~26m/s to turn linear velocity；
D, fused salt is prepared：By FeCl2、MgCl2、KCl、NaCl、NaF、BeF2Material amount ratio be 0.1：0.1：1：3:1：
0.02-0.06 weighs each constituent element, and fused-salt medium is obtained after mixing, adds the powdery list for the 11%-15% for accounting for fused-salt medium quality
Crystal silicon, it is ground；
E, fused salt is put into salt bath furnace, is heated to 680-770 DEG C, constant temperature 20-30min, negative electrode is then done with silicon steel sheet
Immerse in liquid fused salt, alloy strip is immersed into logical direct current in liquid fused salt as anode carries out plating siliconising to alloy strip；It is described logical
Direct current is given electrically for pulse, average current density 65-75mA/cm2；The alloy Cast Strip is in fused salt with 0.11-
0.15m/min gait of march carries out uniform motion, and it is 25-30min to be kept for residence time of the alloy Cast Strip in fused salt；Institute
The percentage composition for stating silicon in silicon steel sheet is 4-6%；
F, the alloy strip after siliconising is placed in liquid nitrogen atmosphere and carries out low-temperature treatment, temperature is -150 DEG C~-165 DEG C, is protected
10~15min of temperature；It is then placed within room temperature condition and stands 1~1.5 hour；It is placed in again in resistance furnace and is heated to 220~240
DEG C, 1~3 hour is incubated, then cools to room temperature with the furnace, it is magnetic alloy that iron-based nano-crystalline thin ribbon material, which is made,.
In, Sn, Au and B collective effect can improve nanocrystalline Forming ability in magnetic alloy of the present invention.Si, Be and Pm can be with
Prevent crystal grain in heat treatment from growing up, refined crystal grain, so as to improve resistivity, reduced loss.Al and the second transition system
It Ag, can effectively suppress growing up for crystal grain, beneficial to the relatively fine uniform grain structure of acquisition, while the thermostabilization of magnet can be improved
Property.The Sc of First Transition system inhibits growing up for crystal grain intersection particle, has refined crystal grain, therefore may refrain from miscellaneous around them
The enhancing of end of a performance, and then improve magnetic property.
It is existing by the way of quick cooling, low-temperature deep Ageing Treatment and alloying combine in the preparation method of alloy
Effect reduces the phase size in alloy, ensures that chemical composition is uniformly distributed in material, ensure that the magnetic property of alloy, also by ladder
Internal stress caused by degree processing greatly reduces quick cooling, also ensure that the mechanical property of alloy.
Products obtained therefrom of the present invention has excellent soft magnet performance.Not having to heavy rare earth element in preparation, rare element dosage is few, its
Its cost of material is relatively low；Alloy in kind was prepared in addition, by quick cooling, ensure that the uniform of alloying component, tissue and performance
Property, it ensure that the quality of alloy.The alloy preparation technology is easy, and process is simple, and the alloy of production has good performance, very
It is easy to industrialized production.Material prepared by the present invention can apply to the magnetic device in the fields such as information, communication.
Embodiment
Embodiment 1
A kind of magnetic alloy, its material composition and weight percentage are：Ag0.03%, Sc 0.8%, In0.2%,
Al0.05%, Sn0.2%, Be0.09%, Pm0.05%, Au0.003%, Si1.6%, B2.1%, surplus Fe；The B with
The form of ferro-boron intermediate alloy (trade mark FeB23C0.05) adds, and B weight/mass percentage composition is 24% in ferro-boron intermediate alloy；
A kind of preparation method of magnetic alloy, step include：
A, by alloy raw material Ingredients Weight percentage composition be Ag0.03%, Sc 0.8%, In0.2%, Al0.05%,
Sn0.2%, Be0.09%, Pm0.05%, Au0.003%, Si1.6%, B2.1%, surplus are that Fe carries out dispensing；Ag in raw material,
Sc, In, Al, Sn, Be, Pm, Au, Si, Fe purity are all higher than 99.9%；The B is added in the form of ferro-boron intermediate alloy, boron
B weight/mass percentage composition is 24% in iron intermediate alloy.
B, raw material is put into melting in vaccum sensitive stove, smelting temperature is 1590 DEG C, is incubated 7min, is obtained after casting cooling
Foundry alloy；
C, vacuum rapid hardening is carried out after remelting being carried out in remelting tubular type crucible that foundry alloy is put into vacuum induction forming furnace
Get rid of band and alloy strip is made, remelting temperature is 1560 DEG C；The remelting tubular type crucible bottom is provided with through hole, remelting tubular type crucible top
Nitrogen is connected through valve, the pressure of nitrogen is 1.6atm；The bottom of remelting tubular type crucible is placed in 3mm on forming furnace runner wheel rim
Place, after foundry alloy melts, the valve on remelting tubular type crucible top is opened, melting foundry alloy is under nitrogen pressure from crucible bottom
Through hole in spray to the forming furnace runner wheel rim of rotation, form continuous alloy strip, the thickness of gained alloy strip is 250~260 μ
M, width are 3~5mm；Remelting tubular type crucible internal diameter is 13mm, is highly 260mm, the through-hole aperture of remelting tubular type crucible bottom
For 1.4mm.Runner linear velocity is 25m/s；
D, fused salt is prepared：By FeCl2、MgCl2、KCl、NaCl、NaF、BeF2Material amount ratio be 0.1：0.1：1：3:1：
0.03 weighs each constituent element, and fused-salt medium is obtained after mixing, adds the 12% powdery monocrystalline silicon for accounting for fused-salt medium quality, and grinding is mixed
It is even；FeCl2、MgCl2、KCl、NaCl、NaF、BeF2It is that analysis is pure, each constituent element is first dried into 8h at 200 DEG C before weighing；
E, fused salt is put into salt bath furnace, is heated to 770 DEG C, constant temperature 20min, is then done with the silicon steel sheet containing 4.5%Si
Negative electrode is immersed in liquid fused salt, and alloy strip is immersed into logical direct current in liquid fused salt as anode carries out plating siliconising to alloy strip；Institute
It is pulse to electrically to state logical direct current, average current density 70mA/cm2；The alloy Cast Strip is in fused salt with 0.13m/
Min gait of march carries out uniform motion, and it is 25min to be kept for residence time of the alloy Cast Strip in fused salt；
F, the alloy strip after siliconising is placed in liquid nitrogen atmosphere and carries out low-temperature treatment, temperature is -165 DEG C, is incubated 10min；
It is then placed within room temperature condition and stands 1.5 hours；It is placed in again in resistance furnace and is heated to 240 DEG C, 2 hours is incubated, then with stove
Room temperature is cooled to, it is magnetic alloy that iron-based nano-crystalline thin ribbon material, which is made,.
Embodiment 2
A kind of magnetic alloy, its material composition and weight percentage are：Ag0.05%, Sc 1.4%, In 0.7%, Al
0.08%th, Sn0.7%, Be0.15%, Pm0.12%, Au0.008%, Si1.9%, B2.9%, surplus Fe；The B is with boron
The form of iron intermediate alloy adds, and B weight/mass percentage composition is 24% in ferro-boron intermediate alloy；
A kind of preparation method of magnetic alloy, step include：
A, by alloy raw material Ingredients Weight percentage composition be Ag0.05%, Sc 1.4%, In 0.7%, Al 0.08%,
Sn0.7%, Be0.15%, Pm0.12%, Au0.008%, Si1.9%, B2.9%, surplus are that Fe carries out dispensing；Ag in raw material,
Sc, In, Al, Sn, Be, Pm, Au, Si, Fe purity are all higher than 99.9%；The B is added in the form of ferro-boron intermediate alloy, boron
B weight/mass percentage composition is 24% in iron intermediate alloy.
B, raw material being put into melting in vaccum sensitive stove, smelting temperature is 1580 DEG C, is incubated 12min, after casting cooling
To foundry alloy；
C, vacuum rapid hardening is carried out after remelting being carried out in remelting tubular type crucible that foundry alloy is put into vacuum induction forming furnace
Get rid of band and alloy strip is made, remelting temperature is 1550 DEG C；The remelting tubular type crucible bottom is provided with through hole, remelting tubular type crucible top
Nitrogen is connected through valve, the pressure of nitrogen is 1.4atm；The bottom of remelting tubular type crucible is placed in 3mm on forming furnace runner wheel rim
Place, after foundry alloy melts, the valve on remelting tubular type crucible top is opened, melting foundry alloy is under nitrogen pressure from crucible bottom
Through hole in spray to the forming furnace runner wheel rim of rotation, form continuous alloy strip, the thickness of gained alloy strip is 250~260 μ
M, width are 3~5mm；Remelting tubular type crucible internal diameter is 13mm, is highly 260mm, the through-hole aperture of remelting tubular type crucible bottom
For 1.4mm；Runner linear velocity is 26m/s；
D, fused salt is prepared：By FeCl2、MgCl2、KCl、NaCl、NaF、BeF2Material amount ratio be 0.1：0.1：1：3:1：
0.06 weighs each constituent element, and fused-salt medium is obtained after mixing, adds the 15% powdery monocrystalline silicon for accounting for fused-salt medium quality, and grinding is mixed
It is even；FeCl2、MgCl2、KCl、NaCl、NaF、BeF2It is that analysis is pure, each constituent element is first dried into 8h at 200 DEG C before weighing；
E, fused salt is put into salt bath furnace, is heated to 700 DEG C, constant temperature 20min, is then done with the silicon steel sheet containing 4.5%Si
Negative electrode is immersed in liquid fused salt, and alloy strip is immersed into logical direct current in liquid fused salt as anode carries out plating siliconising to alloy strip；Institute
It is pulse to electrically to state logical direct current, average current density 65mA/cm2；The alloy Cast Strip is in fused salt with 0.13m/
Min gait of march carries out uniform motion, and it is 30min to be kept for residence time of the alloy Cast Strip in fused salt；
F, the alloy strip after siliconising is placed in liquid nitrogen atmosphere and carries out low-temperature treatment, temperature is -155 DEG C, is incubated 15min；
It is then placed within room temperature condition and stands 1 hour；It is placed in again in resistance furnace and is heated to 220 DEG C, is incubated 3 hours, it is then cold with stove
But to room temperature, it is magnetic alloy that iron-based nano-crystalline thin ribbon material, which is made,.
Embodiment 3
A kind of magnetic alloy, its material composition and weight percentage are：Ag0.04%, Sc 1.2%, In0.5%, Al
0.06%th, Sn0.4%, Be0.13%, Pm0.08%, Au0.005%, Si1.7%, B2.5%, surplus Fe；The B is with boron
The form of iron intermediate alloy adds, and B weight/mass percentage composition is 24% in ferro-boron intermediate alloy；
A kind of preparation method of magnetic alloy, step include：
A, by alloy raw material Ingredients Weight percentage composition be Ag0.04%, Sc 1.2%, In0.5%, Al 0.06%,
Sn0.4%, Be0.13%, Pm0.08%, Au0.005%, Si1.7%, B2.5%, surplus are that Fe carries out dispensing；Ag in raw material,
Sc, In, Al, Sn, Be, Pm, Au, Si, Fe purity are all higher than 99.9%；The B is added in the form of ferro-boron intermediate alloy, boron
B weight/mass percentage composition is 24% in iron intermediate alloy.
B, raw material being put into melting in vaccum sensitive stove, smelting temperature is 1600 DEG C, is incubated 10min, after casting cooling
To foundry alloy；
C, vacuum rapid hardening is carried out after remelting being carried out in remelting tubular type crucible that foundry alloy is put into vacuum induction forming furnace
Get rid of band and alloy strip is made, remelting temperature is 1550 DEG C；The remelting tubular type crucible bottom is provided with through hole, remelting tubular type crucible top
Nitrogen is connected through valve, the pressure of nitrogen is 1.4atm；The bottom of remelting tubular type crucible is placed in 3mm on forming furnace runner wheel rim
Place, after foundry alloy melts, the valve on remelting tubular type crucible top is opened, melting foundry alloy is under nitrogen pressure from crucible bottom
Through hole in spray to the forming furnace runner wheel rim of rotation, form continuous alloy strip, the thickness of gained alloy strip is 250~260 μ
M, width are 3~5mm；Remelting tubular type crucible internal diameter is 13mm, is highly 260mm, the through-hole aperture of remelting tubular type crucible bottom
For 1.4mm；Runner linear velocity is 25m/s；
D, fused salt is prepared：By FeCl2、MgCl2、KCl、NaCl、NaF、BeF2Material amount ratio be 0.1：0.1：1：3:1：
0.05 weighs each constituent element, and fused-salt medium is obtained after mixing, adds the 14% powdery monocrystalline silicon for accounting for fused-salt medium quality, and grinding is mixed
It is even；FeCl2、MgCl2、KCl、NaCl、NaF、BeF2It is that analysis is pure, each constituent element is first dried into 8h at 200 DEG C before weighing；
E, fused salt is put into salt bath furnace, is heated to 730 DEG C, constant temperature 20min, is then done with the silicon steel sheet containing 4.5%Si
Negative electrode is immersed in liquid fused salt, and alloy strip is immersed into logical direct current in liquid fused salt as anode carries out plating siliconising to alloy strip；Institute
It is pulse to electrically to state logical direct current, average current density 75mA/cm2；The alloy Cast Strip is in fused salt with 0.15m/
Min gait of march carries out uniform motion, and it is 25min to be kept for residence time of the alloy Cast Strip in fused salt；
F, the alloy strip after siliconising is placed in liquid nitrogen atmosphere and carries out low-temperature treatment, temperature is -165 DEG C, is incubated 10min；
It is then placed within room temperature condition and stands 1 hour；It is placed in again in resistance furnace and is heated to 230 DEG C, is incubated 1 hour, it is then cold with stove
But to room temperature, it is magnetic alloy that iron-based nano-crystalline thin ribbon material, which is made,.
Permanent-magnet alloy performance prepared by embodiment 1-3 is as shown in table 1：
Table 1 implements permanent-magnet alloy performance prepared by embodiment 1-3
| Embodiment | 1 | 2 | 3 |
| Coercivity (A/m) | 2.5 | 2.35 | 2.45 |
| Saturation induction density (T) | 2.06 | 2.12 | 2.09 |
| P11/50 (W/kg) is lost | 0.18 | 0.15 | 0.16 |
Claims (4)
1. a kind of magnetic alloy, its material composition and weight percentage are：Ag0.03-0.05%, Sc0.8-1.4%,
In0.2-0.7%, Al0.05-0.08%, Sn0.2-0.7%, Be0.09-0.15%, Pm0.05-0.12%, Au0.003-
0.008%th, Si1.6-1.9%, B2.1-2.9%, surplus Fe.
2. magnetic alloy as claimed in claim 1, it is characterised in that：The B is added in the form of ferro-boron intermediate alloy, ferro-boron
B weight/mass percentage composition is 20-25% in intermediate alloy.
3. a kind of preparation method of magnetic alloy, step include：
A, by alloy raw material Ingredients Weight percentage composition be Ag0.03-0.05%, Sc0.8-1.4%, In0.2-0.7%,
Al0.05-0.08%, Sn0.2-0.7%, Be0.09-0.15%, Pm0.05-0.12%, Au0.003-0.008%, Si1.6-
1.9%th, B2.1-2.9%, surplus are that Fe carries out dispensing；The B is added in the form of ferro-boron intermediate alloy, ferro-boron intermediate alloy
Middle B weight/mass percentage composition is 20-25%.
B, raw material is put into melting in vaccum sensitive stove, smelting temperature is 1570~1600 DEG C, soaking time 6-15min, is poured
Foundry alloy is obtained after casting cooling；
C, it will carry out carrying out vacuum rapid hardening after remelting to get rid of band in remelting tubular type crucible that foundry alloy is put into vacuum induction forming furnace
Alloy strip is made, remelting temperature is 1540~1560 DEG C；
D, fused salt is prepared：By FeCl2、MgCl2、KCl、NaCl、NaF、BeF2Material amount ratio be 0.1：0.1：1：3:1：
0.02-0.06 weighs each constituent element, and fused-salt medium is obtained after mixing, adds the powdery list for the 11%-15% for accounting for fused-salt medium quality
Crystal silicon, it is ground；
E, fused salt is put into salt bath furnace, is heated to 680-770 DEG C, constant temperature 20-30min, negative electrode immersion is then done with silicon steel sheet
In liquid fused salt, alloy strip is immersed into logical direct current in liquid fused salt as anode plating siliconising is carried out to alloy strip；The logical direct current
Electricity is given electrically for pulse, average current density 65-75mA/cm2；The alloy Cast Strip is in fused salt with 0.11-0.15m/
Min gait of march carries out uniform motion, and it is 25-30min to be kept for residence time of the alloy Cast Strip in fused salt；
F, the alloy strip after siliconising is placed in liquid nitrogen atmosphere and carries out low-temperature treatment, temperature is -150 DEG C~-165 DEG C, insulation 10
~15min；It is then placed within room temperature condition and stands 1~1.5 hour；It is placed in again in resistance furnace and is heated to 220~240 DEG C, protects
Temperature 1~3 hour, then cools to room temperature with the furnace, and it is magnetic alloy that iron-based nano-crystalline thin ribbon material, which is made,.
4. preparation method as claimed in claim 3, it is characterised in that：The percentage of silicon contains in silicon steel sheet described in the step E
Measure as 4-6%.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60254709A (en) * | 1984-05-31 | 1985-12-16 | Daido Steel Co Ltd | Permanent magnet |
| CN101122022A (en) * | 2007-09-12 | 2008-02-13 | 河北理工大学 | Method for preparing Fe-6.5Wt%Si magnetically soft steel sheet |
| CN101432827A (en) * | 2006-04-28 | 2009-05-13 | 日立金属株式会社 | Magnetic core for current transformer, current transformer, and watt-hour meter |
| CN101650999A (en) * | 2009-08-13 | 2010-02-17 | 太原科技大学 | Fe-based amorphous or nanocrystalline soft magnetic alloy and preparation method thereof |
| CN103943297A (en) * | 2014-04-29 | 2014-07-23 | 王杨 | Method for preparing cobalt and nickel base soft magnetic material |
-
2017
- 2017-09-15 CN CN201710835466.7A patent/CN107574367A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60254709A (en) * | 1984-05-31 | 1985-12-16 | Daido Steel Co Ltd | Permanent magnet |
| CN101432827A (en) * | 2006-04-28 | 2009-05-13 | 日立金属株式会社 | Magnetic core for current transformer, current transformer, and watt-hour meter |
| CN101122022A (en) * | 2007-09-12 | 2008-02-13 | 河北理工大学 | Method for preparing Fe-6.5Wt%Si magnetically soft steel sheet |
| CN101650999A (en) * | 2009-08-13 | 2010-02-17 | 太原科技大学 | Fe-based amorphous or nanocrystalline soft magnetic alloy and preparation method thereof |
| CN103943297A (en) * | 2014-04-29 | 2014-07-23 | 王杨 | Method for preparing cobalt and nickel base soft magnetic material |
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Application publication date: 20180112 |