CN1297994C - Method for preparing specific squareness ratio nanocrystalline soft magnetic material without magnetic field treatment - Google Patents
Method for preparing specific squareness ratio nanocrystalline soft magnetic material without magnetic field treatment Download PDFInfo
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- CN1297994C CN1297994C CNB2004100847245A CN200410084724A CN1297994C CN 1297994 C CN1297994 C CN 1297994C CN B2004100847245 A CNB2004100847245 A CN B2004100847245A CN 200410084724 A CN200410084724 A CN 200410084724A CN 1297994 C CN1297994 C CN 1297994C
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- squareness ratio
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Abstract
The present invention relates to a method for preparing a specific squareness ratio nano-crystal soft magnetic material without magnetic field processing, which comprises: the material compositions are prepared, and elements desired by alloy are calculated and designed according to the atomic ratio of Fe<76.5-x-y>CulNbxVySizB9 (x is greater than zero and smaller than five, y is greater than zero and smaller than seven, and z is greater than zero and smaller than twenty); the material compositions is made into mother alloy through a vacuum induction smelting furnace; a non-crystal alloy strip is prepared by using the single-roller rapid quenching method; the non-crystal strip is wound by a strip winding machine; nano-crystal alloy is prepared by using the non-crystal crystallizing technology. The present invention can be used for directly preparing middle-high squareness ratio and middle-low squareness ratio materials so as to omit the magnetic field loading equipment and reduce procedures and cost; compared with the magnetic field processing under the equal condition, the present invention is obviously lower in the loss characteristic and higher in the magnetic permeability.
Description
Technical field
The present invention relates to a kind of preparation method of nano crystal soft magnetic material, especially need not method magnetic field treated, that obtain the nano crystal soft magnetic material of special squareness ratio (Br/Bs).
Background technology
Nano crystal soft magnetic material is compared with traditional soft magnetic material has higher soft magnet performance, is widely used in the element manufacturing in electronics, the power industry, especially in order to satisfy the demand to special squareness ratio soft magnetic material.Obtaining the method for special squareness ratio material at present, generally is by magnetic-field heat treatment technology, promptly indulges the rectangle soft magnetic material that magnetic field obtains high squareness ratio by loading, and loads transverse magnetic field and obtains flat soft magnetic material, perhaps adopts the resultant field treatment process.Its fatal defective is: magnetic field treated equipment complexity, comprise field generator for magnetic, heater, atmosphere control etc., and technology is various, and cost increases, and is several times without magnetic field treated sample cost.
Summary of the invention
The objective of the invention is to overcome the defective of prior art and provide a kind of and save huge magnetic field loading equipemtn, reduce the method for need not magnetic field treated obtaining special squareness ratio nano crystal soft magnetic material that operation reduced cost, reduced the alloy material loss, enhances product performance.
Purpose of the present invention is achieved through the following technical solutions:
A kind of method of need not magnetic field treated obtaining special squareness ratio nano crystal soft magnetic material is characterized in that:
A, the allotment of raw material composition: adopt Armco iron Fe, cathode copper Cu, metal niobium Nb, vanadium metal V, silicon metal Si and ferro-boron B, each element is appraised and decided as follows by atomic ratio:
Fe
76.5-x-yCu
1Nb
xV
ySi
zB
9
0＜x in the formula＜5,0＜y＜7,0＜z＜20
B, the batching of above-mentioned element is placed in the vacuum induction melting furnace, be heated to 1300～1450 ℃ of smelting temperatures, under fully stirring, carry out vacuum melting and prepare foundry alloy;
C, use single-roller rapid quenching with quenching prepare the amorphous master alloy band, and the roller speed 25～40m/s of fast quenching machine, gained amorphous band thickness are 25～40 μ m;
D, use wrapping machine to carry out coiling by requirement on devices to the amorphous band of preparation;
E, prepare nanometer crystal alloy: the device of above-mentioned coiling is placed in the annealing furnace with amorphous crystallization technology, carrying out the amorphous subsequent annealing under the controlled atmosphere protection handles, require 520～600 ℃ of amorphous crystallization temperatures, temperature retention time 30～80 minutes, make nanometer crystal alloy;
Carry out performance test and structural analysis after f, the cooling.
Described controlled atmosphere protection is an insulation annealing under vacuum heat-preserving annealing or nitrogen, argon inert gas insulation annealing or the hydrogen reducing atmosphere.
The present invention compared with prior art, by composition allotment and technology optimization, directly the middle and high squareness ratio material of preparation and in, low squareness ratio material, saved the magnetic field loading equipemtn, reduce operation and reduced cost, under equal conditions obviously than using the low of magnetic field treated, magnetic permeability is than the height of magnetic field treated for its loss characteristic.
Embodiment
Specific embodiments of the present invention is: the method that need not magnetic field treated obtains special squareness ratio nano crystal soft magnetic material, its composition allotment comprises Armco iron Fe, cathode copper Cu, metal niobium Nb, vanadium metal V, silicon metal Si and ferro-boron B, and each element is appraised and decided as follows by atomic ratio:
Fe
76.5-x-yCu
1Nb
xV
ySi
zB
9
0＜x in the formula＜5,0＜y＜7,0＜z＜20
And must meet: (76.5-x-y)+1+x+y+z+9=100
Element Cu in the composition allotment is the core of non-Jingjingization, helps forming more fine grain.Nb has the effect that suppresses grain growth in the amorphous crystallization process, the adjustment of Si, B content can further improve and improve the comprehensive soft magnet performance of alloy, and the fragility of nano-crystal soft magnetic alloy new material is improved.
Employing partly substitutes the Nb element with Mo, V element; Under identical Si, B content, substitute 1.0at%Nb with 2.0at%V, the crystallite dimension D of the α-Fe of alloy inside (Si) is increase tendency, lattice parameter a
0Increase is that Si content reduces, and the fragility of its amorphous master alloy band is improved, and amorphous band is beneficial to the processing and fabricating of nano-crystal soft-magnetic device to tearing not brittle failure open.The effect of finding partly to substitute with V Nb simultaneously is better, and the loss of alloy (P) value descends, but magnetic permeability (μ) value also descends to some extent.Wherein substitute the best results of 1.0at%Nb with 2.0at%V, the loss of alloy (P) value significantly descends; Saturation induction density Bs slightly improves; Though magnetic permeability μ value has decline, but still has kept high value.
Si, B content adjust, under identical Si content (15at%), and the increase of B content (7,9at%), the crystallite dimension D of α-Fe (Si) increases, lattice parameter a
0Decline is that Si content increases, under identical B content (9.0at%), and the increase of Si content (13.5,15at%), the crystallite dimension D of α-Fe (Si) increases, lattice parameter a
0Decline is that Si content increases.The magnetic permeability of alloy can decrease, and loss also descends.Wherein with the best results of Si=15at%, B=9.0at%, loss P value significantly descends; Saturation induction density Bs and magnetic permeability μ value slightly descend.
With the alternative 1.0at%Nb of 2.0at%V and after adjusting Si, B content, the loss of alloy (P) value and magnetic permeability (μ) value all decrease.Wherein with Fe
71Cu
1Nb
2V
2Si
15B
9The loss of alloy reduces the most remarkable, and high squareness ratio (α) and higher magnetic permeability (μ) in having; Fe
73Cu
1Nb
2V
2Si
15B
7Alloy have low magnetic permeability (μ), high saturated magnetic induction (Bs) and in low squareness ratio (α).
The present invention is by composition allotment, technology optimization, directly prepare middle and high squareness ratio material and in, low squareness ratio material.Foundry alloy vacuum induction melting furnace melting, prepare amorphous alloy strips with single-roller rapid quenching with quenching again, wrapping machine carries out coiling, prepares nanometer crystal alloy with amorphous crystallization technology at last, to sample size is that the sample of φ 20 * 16 * 10 (mm) detects, and the result is as follows:
1, high magnetic permeability, low-loss, in high squareness ratio alloy property be:
Saturation induction density Bs=1.08T, static initial permeability μ
0=98.6mH/m, coercivity H=1.12A/m, loss P (0.5T, 20KHz)=14.78W/kg, P (0.3T, 100KHz)=73.81W/kg, α
e(1K)=77.4%.
2, low magnetic permeability, low-loss, in low squareness ratio alloy property be:
Saturation induction density Bs=1.25T, static initial permeability μ
0=28.0mH/m, coercivity H=6.79A/m, loss P (0.5T, 20KHz)=25.01W/kg, P (0.3T, 100KHz)=97.74W/kg, α
e(1K)=36.5%.
Embodiment sees table 1 for details:
Table 1, the present invention do not have the nano-crystal soft magnetic alloy performance table through magnetic-field heat treatment:
| Sequence number | Composition | T(℃) | μ e(1k，0.08A/m) (mH/m) | P 0.5T/20k (w/kg) | P 0.3T/100k (w/kg) | α (1KHz) |
| 1 | Fe 73.5Cu 1Nb 3Si 13.5B 9 | 580 | 124.37 | 20.082 | 118.9 | |
| 2 | Fe 71Cu 1Nb 2V 2Si 15B 9 | 580 | 96.73 | 14.784 | 73.812 | 0.774 |
| 3 | Fe 73Cu 1Nb 2V 2Si 15B 7 | 580 | 23.87 | 25.011 | 97.74 | 0.365 |
| 4 | Fe 70Cu 1Nb 2V 2Si 17B 8 | 520 | 62.81 | 19.604 | 83.344 | 0.595 |
| μ 0(0.08A/m) (mH/m) | μ m(mH/m) | B s(T) | B r(T) | α (static state) | H c(A/m) |
| 169.6 | 1.18 | 0.844 | 0.715 | 0.700 | |
| 98.6 | 482.7 | 1.08 | 0.729 | 0.675 | 1.12 |
| 28.0 | 47.8 | 1.25 | 0.511 | 0.409 | 6.79 |
| 67.0 | 203.7 | 1.05 | 0.572 | 0.545 | 1.970 |
The implication of table Chinese and English letter:
T-amorphous crystallization temperature
μ
E (1k, 0.08A/m)Dynamic magnetic conductance when-frequency is 1000Hz under 0.08A/m magnetic field
P
0.3T/100kLoss when-frequency is 100KHz under 0.3T magnetic field
α-squareness ratio Bs-saturation induction density Hc-coercive force
Claims (2)
1, a kind of method of need not magnetic field treated obtaining special squareness ratio nano crystal soft magnetic material is characterized in that:
A, the allotment of raw material composition: adopt Armco iron Fe, cathode copper Cu, metal niobium Nb, vanadium metal V, silicon metal Si and ferro-boron B, each element is appraised and decided as follows by atomic ratio:
Fe
76.5-x-yCu
1Nb
xV
ySi
zB
9
0＜x in the formula＜5,0＜y＜7,0＜z＜20
B, the batching of above-mentioned element is placed in the vacuum induction melting furnace, be heated to 1300～1450 ℃ of smelting temperatures, under fully stirring, carry out vacuum melting and prepare foundry alloy;
C, use single-roller rapid quenching with quenching prepare the amorphous master alloy band, and the roller speed 25～40m/s of fast quenching machine, gained amorphous band thickness are 25～40 μ m;
D, use wrapping machine to carry out coiling by requirement on devices to the amorphous band of preparation;
E, prepare nanometer crystal alloy: the device of above-mentioned coiling is placed in the annealing furnace with amorphous crystallization technology, carrying out the amorphous subsequent annealing under the controlled atmosphere protection handles, require 520～600 ℃ of amorphous crystallization temperatures, temperature retention time 30～80 minutes, make nanometer crystal alloy;
Carry out performance test and structural analysis after f, the cooling.
2, the method for need not magnetic field treated obtaining special squareness ratio nano crystal soft magnetic material according to claim 1 is characterized in that described controlled atmosphere protection is an insulation annealing under vacuum heat-preserving annealing or nitrogen, argon inert gas insulation annealing or the hydrogen reducing atmosphere.
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|---|---|---|---|
| CNB2004100847245A CN1297994C (en) | 2004-11-26 | 2004-11-26 | Method for preparing specific squareness ratio nanocrystalline soft magnetic material without magnetic field treatment |
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| CN1297994C true CN1297994C (en) | 2007-01-31 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100445410C (en) * | 2005-09-27 | 2008-12-24 | 同济大学 | Nano-crystal soft magnetic alloy material and its production |
| CN101445896B (en) * | 2008-12-29 | 2010-09-29 | 安泰科技股份有限公司 | Fast quenching amorphous alloy ribbon and preparation method thereof |
| CN101853723B (en) * | 2009-03-31 | 2012-11-21 | 比亚迪股份有限公司 | Composite magnetic material and preparation method thereof |
| CN101894649A (en) * | 2009-05-19 | 2010-11-24 | 南通海源机电设备有限公司 | New iron-based magnetically soft alloy with strong glass forming capability |
| CN102912257A (en) * | 2012-10-19 | 2013-02-06 | 张家港市清大星源微晶有限公司 | Microcrystalline material |
| CN103489555A (en) * | 2013-09-11 | 2014-01-01 | 南京航空航天大学 | Iron-based nano-crystalline soft magnetic alloy and method for manufacturing same |
| CN112342347B (en) * | 2020-10-21 | 2023-12-19 | 江苏大磁纳米材料有限公司 | Hydrogenation heat treatment process for amorphous nano alloy |
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| CN1092201A (en) * | 1994-01-29 | 1994-09-14 | 冶金工业部钢铁研究总院 | The manufacture method of iron-base quick-quenching soft magnetic alloy core |
| JPH0927412A (en) * | 1995-07-12 | 1997-01-28 | Hitachi Metals Ltd | Cut core and manufacture thereof |
| CN1185012A (en) * | 1996-12-11 | 1998-06-17 | 梅加日公司 | Process for mfg. magnetic component made of iron-based soft magnetic alloy having nanocrys talline structure |
| CN1289134A (en) * | 1999-09-16 | 2001-03-28 | 住友特殊金属株式会社 | Nanometer-grade composite magnet powder and mfg. method for magnet |
| CN1403615A (en) * | 2002-08-16 | 2003-03-19 | 安泰科技股份有限公司 | Iron-base bulk amorphous soft-magnetic alloy material |
| CN1440317A (en) * | 2000-10-06 | 2003-09-03 | 株式会社三德 | Process for producing, through strip casting, raw alloy for nanocomposite type permanent magnet |
| CN1475018A (en) * | 2000-09-15 | 2004-02-11 | ���ڻ� | Magnetic amplifier choke with magnetic core, use of magnetic amplifier choke and method for producing magnetic core for magnetic amplifier choke |
-
2004
- 2004-11-26 CN CNB2004100847245A patent/CN1297994C/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1092201A (en) * | 1994-01-29 | 1994-09-14 | 冶金工业部钢铁研究总院 | The manufacture method of iron-base quick-quenching soft magnetic alloy core |
| JPH0927412A (en) * | 1995-07-12 | 1997-01-28 | Hitachi Metals Ltd | Cut core and manufacture thereof |
| CN1185012A (en) * | 1996-12-11 | 1998-06-17 | 梅加日公司 | Process for mfg. magnetic component made of iron-based soft magnetic alloy having nanocrys talline structure |
| CN1289134A (en) * | 1999-09-16 | 2001-03-28 | 住友特殊金属株式会社 | Nanometer-grade composite magnet powder and mfg. method for magnet |
| CN1475018A (en) * | 2000-09-15 | 2004-02-11 | ���ڻ� | Magnetic amplifier choke with magnetic core, use of magnetic amplifier choke and method for producing magnetic core for magnetic amplifier choke |
| CN1440317A (en) * | 2000-10-06 | 2003-09-03 | 株式会社三德 | Process for producing, through strip casting, raw alloy for nanocomposite type permanent magnet |
| CN1403615A (en) * | 2002-08-16 | 2003-03-19 | 安泰科技股份有限公司 | Iron-base bulk amorphous soft-magnetic alloy material |
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