CN102094156A - Method for preparing iron-based nanocrystalline material by mid-low-frequency magnetic pulse - Google Patents
Method for preparing iron-based nanocrystalline material by mid-low-frequency magnetic pulse Download PDFInfo
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- CN102094156A CN102094156A CN 201110037735 CN201110037735A CN102094156A CN 102094156 A CN102094156 A CN 102094156A CN 201110037735 CN201110037735 CN 201110037735 CN 201110037735 A CN201110037735 A CN 201110037735A CN 102094156 A CN102094156 A CN 102094156A
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Abstract
The invention relates to the technical field of the preparation of soft magnetic materials, in particular to a method for preparing an iron-based nanocrystalline material by a mid-low-frequency magnetic pulse. The method comprises the following steps: at a vacuum degree below 5*10<-3>Pa, smelting alloy materials into a mother alloy molten mass in a vacuum high-frequency furnace or arc furnace; then, at a vacuum degree of 2*10<-3>Pa, injecting the mother alloy molten mass into a vacuum single-roller molten mass rapid-cooling device under the protection of an argon gas atmosphere, and preparing the mother alloy into an amorphous thin strip, wherein the linear surface velocity of a cooling roller is 45-49m/s, the distance between a quartz nozzle and a copper roller is 0.5mm, the superheating temperature of the molten mass at the outlet of the nozzle is 50K; and finally, carrying out magnetic pulse treatment on the amorphous thin strip in a multi-function process control pulse magnetic field generator to obtain the amorphous nanocrystalline material, wherein the field intensity Hp of the magnetic pulse is 100-400Oe, the frequency f is 20-2000Hz, and the operation time tp is 5-10 minutes.
Description
Technical field
The present invention relates to the soft magnetic materials preparing technical field, be specifically related to a kind of method for preparing the iron based nano crystal material by the medium and low frequency magnetic-pulse.
Background technology
The iron based nano crystal material is the biphase alloy that is distributed in the residue noncrystal substrate after nano-crystallization is handled by the Fe-based amorphous nanocrystalline disperse that obtains.It has soft magnetic performance preferably, and promptly coercive force is low, saturation magnetization is high, and is more extensive in the application in fields such as power transformer, switch power supply, fast-response probe.Nanoalloy-HITPERM of forming of FeCoHfBCu amorphous nano crystallization particularly, its high temperature magnetic induction density is big, coercive force is low, and working temperature can reach more than 500 ℃, is the preferred material of the electronic space shuttle magnet of the s-generation.
At present both at home and abroad the preparation iron based nano crystal material that generally adopts is annealing treatment logos, promptly amorphous is carried out 〉=vacuum annealing of 1h the preparation Nanoalloy under ℃ condition of temperature 〉=500.This technique process complexity, long reaction time, and cause the annealing embrittlement of iron based nano crystal material easily.
Summary of the invention
The objective of the invention is the deficiency that exists at prior art, provide a kind of and prepare the method for iron based nano crystal material, prepare the iron based nano crystal material of more excellent performance by the medium and low frequency magnetic-pulse.
The technical scheme that realizes the object of the invention is to carry out as follows:
(1) in vacuum tightness less than 5 * 10
-3Under the Pa, alloy raw material is smelted into the mother alloy melt in vacuum high frequency furnace or electric arc furnace;
(2) be 2 * 10 in vacuum tightness
-3Pa, argon gas atmosphere protection is injected the single roller melt supercooled of vacuum equipment with the mother alloy melt mother alloy is made amorphous thin ribbon down, cooling roller linear resonance surface velocity 45～49m/s, quartz nozzle and copper roller apart from 0.5mm, jet exit melt overheat degree 50K;
(3) in multiprogrammability pulsed magnetic field generator, amorphous thin ribbon is carried out magnetic-pulse and handle magnetic-pulse field intensity H
p=100～400Oe, frequency f=20～2000Hz, action time, tp=5min～10min obtained the amorphous nano-crystalline material.
Compared with prior art, characteristics of the present invention and beneficial effect thereof are:
1 by adjusting field intensity, frequency and controlling the crystallization amount action time, realizes that the crystallization amount is controlled;
2 traditional crystallization method temperature rises reach more than 500 ℃, cause the annealing embrittlement of non-crystaline amorphous metal easily.Δ T of the present invention≤20 ℃ avoids the embrittlement of annealing;
The maximum crystallization region size of 3 tradition annealing crystallization methods reaches micron order, causes alloy embrittlement.Maximum crystallization region size of the present invention is tens nanometer scale only, has avoided alloy embrittlement;
The coercive force H of the Nanoalloy-HITPERM of 4 present method preparation
c≤ 50A/m, saturation magnetization 150emu/g～175emu/g.
Description of drawings:Fig. 1 is a multiprogrammability pulsed magnetic field generator structural representation of the present invention;
Fig. 2 is multiprogrammability pulsed magnetic field generator electronic control principle figure of the present invention.
Embodiment
Below in conjunction with embodiment the present invention is elaborated, but protection scope of the present invention is not limited only to following embodiment:
The used material FeSiB of the present invention is provided by Beijing Iron and Steel Research Geueral Inst; Fe (Co) HfBCu amorphous spray carrying equipment is the single roller melt supercooled of the German Hechigen Edmund B ü hler of a company vacuum equipment, medium and low frequency pulsed magnetic field treatment unit is a multiprogrammability pulsed magnetic field generator, as Fig. 1, shown in Figure 2, wherein treater is the solenoid coil of hollow, internal diameter is 100mm, and the magnetic-pulse of non-crystalline material is handled and carried out in the cavity of treater; Adopt Mossbauer spectrometer to measure finished product crystallization amount, nanocrystalline distribution and size are observed by the transmission electron microscope high resolution picture.
Embodiment 1: non-crystalline material
(Fe 1-x Co x ) 86 Hf 7 B 6 Cu 1 Magnetic-pulse is handled
:
(1) in vacuum tightness less than 5 * 10
-3Under the Pa, Fe, Si, B, Co, Hf and Cu are smelted into (Fe
1-xCo
x)
86Hf
7B
6Cu
1(x=0.4) mother alloy melt;
(2) be 2 * 10 in vacuum tightness
-3Pa is under the argon gas atmosphere protection, with (Fe
1-xCo
x)
86Hf
7B
6Cu
1(x=0.4) the mother alloy melt injects the single roller melt supercooled of vacuum equipment mother alloy is made amorphous thin ribbon, cooling roller linear resonance surface velocity 45～49m/s, quartz nozzle and copper roller apart from 0.5mm, jet exit melt overheat degree 50K;
(3) in multiprogrammability pulsed magnetic field generator, amorphous thin ribbon is carried out magnetic-pulse and handles, the magnetic-pulse frequency be 1000Hz, field intensity 200Oe, action time 600s;
Amorphous sample is handled back crystallization volume fraction at magnetic-pulse and is reached 17.6%, and the corresponding hyperfine magnetic field of crystallization is 324.99kOe; Maximum crystallization region size is in 5～10 nanometer scale.
Embodiment 2: non-crystalline material Fe
78Si
9B
13Magnetic-pulse is handled
: under the identical situation of other conditions and embodiment 1,When magnetic-pulse frequency 20Hz, field intensity 200Oe, action time during 120s, the crystallization volume fraction of amorphous is 2.1%;
When magnetic-pulse frequency 20Hz, field intensity 400Oe, action time during 120s, the crystallization volume fraction of amorphous is 5.0%;
When magnetic-pulse frequency 40Hz, field intensity 200Oe, action time during 120s, the crystallization volume fraction of amorphous is 7.8%.
Embodiment 3: non-crystalline material Fe
73.5Cu
1Nb
3Si
13.5B
9Magnetic-pulse handle: this amorphous is carried out the low frequency magnetic-pulse handles, when field intensity is that 296Oe, frequency are that 30Hz, action time are 300,600, during 900sec., amorphous Fe
73.5Cu
1Nb
3Si
13.5B
9Nano-crystallization takes place, and the crystallization volume fraction is respectively: 2.3,2.6,3.4;
When field intensity is that 379Oe, frequency are 20,30,40Hz, action time are 240sec., amorphous Fe
73.5Cu
1Nb
3Si
13.5B
9Nano-crystallization takes place, and the crystallization volume fraction is respectively: 3.1,3.3,5.5.
Claims (4)
1. one kind prepares the method for iron based nano crystal material by the medium and low frequency magnetic-pulse, it is characterized in that carrying out as follows:
(1) the amorphous master alloy raw material is smelted into the mother alloy melt;
(2) the mother alloy melt is made amorphous thin ribbon;
(3) in multiprogrammability pulsed magnetic field generator, amorphous thin ribbon is carried out magnetic-pulse and handle magnetic-pulse field intensity H
p=100～400Oe, frequency f=20～200Hz, action time, tp=5min～30min obtained the amorphous nano-crystalline material;
(4) under 550 ℃ of temperature condition,, obtain the finished product to amorphous nano-crystalline anneal of material 1 hour.
2. according to claim 1ly a kind ofly prepare the method for iron based nano crystal material by the medium and low frequency magnetic-pulse, the mother alloy that it is characterized in that being smelted into melt is Fe
78Si
9B
13Or Fe
73.5Cu
1Nb
3Si
13.5B
9Or (Fe
1-xCo
x)
86Hf
7B
6Cu
1
3. according to claim 1ly a kind ofly prepare the method for iron based nano crystal material by the medium and low frequency magnetic-pulse, the vacuum tightness when it is characterized in that the melting in the step (1) is less than 5 * 10
-3Pa carries out in the vacuum high frequency furnace.
4. according to claim 1ly a kind ofly prepare the method for iron based nano crystal material, it is characterized in that in the step (2) the mother alloy melt being made amorphous thin ribbon is that making vacuum tightness is 2 * 10 under argon gas atmosphere is protected by the medium and low frequency magnetic-pulse
-4Pa makes amorphous thin ribbon with the mother alloy melt in the single roller melt supercooled of vacuum equipment, spray line speed 39m/s, quartz nozzle and copper roller apart from 0.5mm, jet exit melt overheat degree 50～100K.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103741008A (en) * | 2013-12-27 | 2014-04-23 | 青岛云路新能源科技有限公司 | Preparation method of iron-based nano-crystal alloy |
| CN105586554A (en) * | 2014-10-21 | 2016-05-18 | 中国科学院金属研究所 | Nanocrystalline copper material and application thereof |
| CN107653426A (en) * | 2017-09-12 | 2018-02-02 | 西北工业大学 | Ti is improved using magnetic field48Zr20Nb12Cu5Be15The method of mechanical property |
| CN112008053A (en) * | 2020-08-27 | 2020-12-01 | 燕山大学 | Preparation device of alloy and current application method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0294605A (en) * | 1988-09-30 | 1990-04-05 | Hitachi Metals Ltd | Excitation circuit including magnetic pulse compression circuit |
| US5364477A (en) * | 1989-07-14 | 1994-11-15 | Alliedsignal Inc. | Iron rich metallic glasses having high saturation induction and superior soft ferromagnetic properties at high magnetization rates |
| CN1721567A (en) * | 2004-07-05 | 2006-01-18 | 日立金属株式会社 | Fe-based amorphous alloy ribbon and magnetic core formed thereby |
-
2011
- 2011-02-14 CN CN 201110037735 patent/CN102094156A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0294605A (en) * | 1988-09-30 | 1990-04-05 | Hitachi Metals Ltd | Excitation circuit including magnetic pulse compression circuit |
| US5364477A (en) * | 1989-07-14 | 1994-11-15 | Alliedsignal Inc. | Iron rich metallic glasses having high saturation induction and superior soft ferromagnetic properties at high magnetization rates |
| CN1721567A (en) * | 2004-07-05 | 2006-01-18 | 日立金属株式会社 | Fe-based amorphous alloy ribbon and magnetic core formed thereby |
Non-Patent Citations (1)
| Title |
|---|
| 《东北大学学报》 20031031 张艳辉，晁月盛 Fe78Si9B13非晶合金纳米晶化的低频脉冲磁场处理方法 第1018-1020页 第24卷, 第10期 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103741008A (en) * | 2013-12-27 | 2014-04-23 | 青岛云路新能源科技有限公司 | Preparation method of iron-based nano-crystal alloy |
| CN103741008B (en) * | 2013-12-27 | 2016-05-11 | 青岛云路先进材料技术有限公司 | A kind of preparation method of iron-base nanometer crystal alloy |
| CN105586554A (en) * | 2014-10-21 | 2016-05-18 | 中国科学院金属研究所 | Nanocrystalline copper material and application thereof |
| CN107653426A (en) * | 2017-09-12 | 2018-02-02 | 西北工业大学 | Ti is improved using magnetic field48Zr20Nb12Cu5Be15The method of mechanical property |
| CN112008053A (en) * | 2020-08-27 | 2020-12-01 | 燕山大学 | Preparation device of alloy and current application method |
| CN112008053B (en) * | 2020-08-27 | 2021-09-17 | 燕山大学 | Preparation device of alloy and current application method |
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Application publication date: 20110615 |