CN102134691B - Preparation method of cobalt-based amorphous giant magneto-impedance ribbon - Google Patents
Preparation method of cobalt-based amorphous giant magneto-impedance ribbon Download PDFInfo
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- CN102134691B CN102134691B CN 201010619558 CN201010619558A CN102134691B CN 102134691 B CN102134691 B CN 102134691B CN 201010619558 CN201010619558 CN 201010619558 CN 201010619558 A CN201010619558 A CN 201010619558A CN 102134691 B CN102134691 B CN 102134691B
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Abstract
The invention discloses a cobalt-based amorphous giant magneto-impedance ribbon which is characterized in that the ribbon is made from a cobalt-based amorphous material as raw materials and obtained by taking the steps of orderly smelting, rapid quenching and current heating rapid annealing heat treatment, wherein a direct-current magnetic field is applied during the heat treatment, the expression of the components of the cobalt-based amorphous material is Co(alpha)Fe(beta)V(gamma)Si(delta)B(epsilon), beta is equal to 0-5, gamma is equal to 0-3, epsilon is equal to 12-20, delta is equal to 5-10, both beta and gamma are not equal to 0, and alpha plus beta plus gamma plus delta plus epsilon is equal to 100. The invention also discloses a preparation method of the giant magneto-impedance ribbon. Compared with the prior art, the cobalt-based amorphous giant magneto-impedance ribbon has the advantages that the cobalt-based alloy with excellent soft magnetic property and mechanical property is used as mother alloy and current heating rapid annealing treatment under magnetic field condition is carried out so that the processing cost is saved, the production efficiency is improved and the obtained material has higher giant magneto-impedance change rate and magnetic field sensitivity while having excellent soft magnetic property and flexibility.
Description
Technical field
The present invention relates to a kind of cobalt base amorphous giant magnetic impedance strip, the invention still further relates to the preparation method of this giant magnetic impedance strip, belong to giant magnetic impedance material technology field.
Background technology
The Maoli Jianianxiongs of Japan Nagoya university in 1992 etc. are at first at amorphous Co
70.5Fe
4.5Si
15B
10Find giant magnetoresistance effect in the silk, and caused countries in the world scientists' great attention.The giant magnetoresistance effect material can be used as magnetic sensing and head technology core component, has wide application prospect in fields such as industrial robot, robotization, magnetic detector, data storage.
Widespread use along with iron-based/nano crystal soft magnetic material; A lot of scholars have carried out the research work of iron-based/nanocrystalline giant magnetic impedance material; Like the patent No. is the Chinese invention patent " a kind of is base and doped particle thin-belt magnetic resistance material and preparation method thereof with CoCu " (Granted publication number be CN1053759C) of ZL94100108.3; And for example the patent No. is the Chinese invention patent " giant magnetoresistance anti-effect non-crystalline thin-band material and preparation method thereof " (Granted publication number for CN1059934C) of ZL98110465.7, can also be with reference to CN1062611C.
But above-mentioned open source literature is handled this type material require subsequent annealing, and there is the easily broken phenomenon of embrittlement in material after the crystallization, and the impedance rate of change of material is not very high.Because of thin-belt giant magnetic impedance material has good uniformity, preparation, advantage such as easy to use have development prospect preferably.So also have some scholars that giant magnetoresistance films is studied, thin-film material has promoter action for the microminiaturization of device, but the preparation technology of film is complicated, and homogeneity of ingredients control is difficult, is difficult for promoting.
Summary of the invention
Technical problem to be solved by this invention is that a kind of cobalt base amorphous giant magnetic impedance strip that need not can have through the anneal operation of long period higher giant magnetoresistance effect is provided to the above-mentioned state of the art.
Another technical problem to be solved by this invention provides the cobalt base amorphous giant magnetic impedance strip that has better flowing property in a kind of spray process.
Another technical problem to be solved by this invention provides a kind of need not can have the preparation method of the cobalt base amorphous giant magnetic impedance strip of higher giant magnetoresistance effect through the anneal operation of long period.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: a kind of cobalt base amorphous giant magnetic impedance strip; It is characterized in that this strip is a raw material with cobalt base amorphous material; Obtain through melting, fast quenching, current flow heats short annealing thermal treatment successively; Wherein, the aforesaid heat treated direct magnetic field that applies simultaneously, aforesaid cobalt base amorphous material component expression formula is Co
αFe
βV
γSi
δB
ε, and satisfy: β=0～5, γ=0～3, ε=12～20, δ=5～10, β and γ are all non-vanishing, alpha+beta+γ+δ+ε=100.
As preferably, described cobalt base amorphous material component expression formula is Co
66Fe
4V
2Si
8B
20Or Co
64Fe
3V
3Si
10B
20
A kind of preparation method of cobalt base amorphous giant magnetic impedance strip is characterized in that comprising the steps:
1. batching with cobalt, iron, vanadium, silicon metal, ferro-boron and boron powder, is pressed atomic molar per-cent batching;
2. melting once is put into the high frequency vacuum induction melting furnace with confected materials and is being carried out melting once, and furnace cooling obtains mother alloy;
3. secondary smelting places high frequency furnace or medium-frequency induction furnace to carry out secondary smelting melted mother alloy, obtains amorphous thin ribbon;
4. thermal treatment; The amorphous thin ribbon two ends are sandwiched in the galvanic current annealing device, and banded zone places applying dc magnetic field, magnetic field size 40～80Oe; Under the air atmosphere condition, carry out the current flow heats anneal; Size of current 400mA～800mA, be 30～240s conduction time, promptly obtains cobalt base amorphous giant magnetic impedance strip.
Further, condition is for vacuumizing earlier, when vacuum tightness reaches 0.1Pa when above during the melting once of step described in 2.; Charge into argon gas at the high frequency vacuum induction melting furnace; Air pressure is controlled at 0.5～1.5 normal atmosphere, and 1200～2000 ℃ of smelting temperatures, smelting time are 10～30 minutes.
Further, during the 3. described secondary smelting of step mother alloy is put into silica tube, place high frequency furnace or medium-frequency induction furnace to carry out secondary smelting silica tube again, described silica tube bottom has the rectangle aperture.Can also adopt other vessel such as crucible except silica tube.Condition is for when the mother alloy temperature reaches 1250～1400 ℃ during the 3. described secondary smelting of step; Charge into 99.99% argon gas, and protection furnace pressure 1～1.5 normal atmosphere, protection roller mouth spacing 0.3～0.5mm; The fused alloy is sprayed onto on the water-cooled copper roller of rotation; Speed of cooling is 25～50m/s, and it is wide to process 5～20mm, the amorphous thin ribbon of 20～40 μ m thickness.
Compared with prior art, the invention has the advantages that: adopting the excellent cobalt base alloy of good soft magnetic performance and mechanical property is mother alloy, and having good mobility can; Be easy to spray, handle, saved processing cost through the current flow heats short annealing under the magnetic field condition; And improved production efficiency; The material that obtains has excellent soft magnetic performance and flexible while, has higher giant magnetic impedance velocity of variation and magnetic field sensitivity, can be widely used in the magneto-dependent sensor technical field.
Description of drawings
Fig. 1 is that the impedance rate of change of amorphous alloy ribbon among the embodiment 1 is measured graphic representation.
Fig. 2 is that the impedance rate of change of amorphous alloy ribbon among the embodiment 2 is measured graphic representation.
Fig. 3 is that the impedance rate of change of amorphous alloy ribbon in the Comparative Examples 1 is measured graphic representation.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is described in further detail.
Embodiment 1, and the material composition of this instance consists of Co
66Fe
4V
2Si
8B
20, form batching, material purity>=99.9% according to chemical element; Confected materials is put into vacuum induction melting furnace, vacuumize, when vacuum tightness reaches 0.01Pa; Charge into purity and be 99.99% argon gas, air pressure is controlled at 1.2 normal atmosphere, about 1300 ℃ of smelting temperatures; Time is 25 minutes, and furnace cooling obtains mother alloy.
Melted mother alloy is put into the silica tube of bottom opening, place medium-frequency induction furnace to carry out secondary smelting silica tube, when alloy temperature reaches 1320 ℃; Charge into 99.99% argon gas, and keep furnace pressure 1.2 normal atmosphere, protection roller mouth spacing 0.3～0.5mm; The fused alloy is sprayed onto on the water-cooled copper roller of rotation; Speed of cooling is 36m/s, and it is wide to process 9mm, the amorphous thin ribbon of 32 μ m thickness.
The amorphous ribbon two ends that obtain are sandwiched the current annealing device; Put into applying dc magnetic field to the strip portion of current annealing device then, externally-applied magnetic field is provided by Helmholtz coil, and the direct magnetic field size is 50Oe; Be 90s conduction time; Current density 600mA utilizes the accurate electric impedance analyzer of HP4294A that its impedance is measured with the variation of foreign field, and externally-applied magnetic field is provided by Helmholtz coil.The measurement curve is as shown in Figure 1, the maximum resistance variation rate of this amorphous alloy ribbon (Δ Z/Z)
Max=378%.
Melted mother alloy is put into the silica tube of bottom opening, place medium-frequency induction furnace to carry out secondary smelting silica tube, when alloy temperature reaches 1350 ℃; Charge into 99.99% argon gas, and keep furnace pressure 1.4 normal atmosphere, protection roller mouth spacing 0.3～0.5mm; The fused alloy is sprayed onto on the water-cooled copper roller of rotation; Speed of cooling is 40m/s, and it is wide to process 7mm, the amorphous thin ribbon of 28 μ m thickness.
The amorphous ribbon two ends that obtain are sandwiched the current annealing device, put into applying dc magnetic field to the strip portion of current annealing device then, externally-applied magnetic field is provided by Helmholtz coil; The direct magnetic field size is 60Oe; Under open air atmosphere condition, carry out the current flow heats anneal, be 100s conduction time, current density 500mA; Utilize the accurate electric impedance analyzer of HP4294A that its impedance is measured with the variation of foreign field, externally-applied magnetic field by.The measurement curve is as shown in Figure 2, the maximum resistance variation rate of this amorphous alloy ribbon (Δ Z/Z)
Max=407%.
Comparative Examples 1, the component that 1 spray of instance is obtained is Co
66Fe
4V
2Si
8B
20Amorphous thin ribbon, put into heat treatment furnace, under open air atmosphere condition, carry out isothermal annealing thermal treatment, thermal treatment temp is 300 ℃, 50 minutes treatment times, furnace cooling then.Utilize the accurate electric impedance analyzer of HP4294A that its impedance is measured with the variation of foreign field, externally-applied magnetic field is provided by Helmholtz coil.The measurement curve is as shown in Figure 3, the maximum resistance variation rate of this amorphous alloy ribbon (Δ Z/Z)
Max=342%.
From Comparative Examples 1, can find out to have the same effect of conventional isothermal annealing treatment process through the amorphous thin ribbon that applies current annealing under the applying dc magnetic field condition, and increased the giant magnetic impedance velocity of variation of material.
Claims (3)
1. the preparation method of a cobalt base amorphous giant magnetic impedance strip; It is characterized in that this strip is a raw material with cobalt base amorphous material; Obtain through melting, fast quenching, current flow heats short annealing thermal treatment successively; Wherein, the aforesaid heat treated direct magnetic field that applies simultaneously, aforesaid cobalt base amorphous material component expression formula is Co
αFe
βV
γSi
δB
ε, and satisfy: β=0～5, γ=0～3, ε=12～20, δ=5～10, β and γ are all non-vanishing, and alpha+beta+γ+δ+ε=100 comprise the steps:
1. batching with cobalt, iron, vanadium, silicon metal, ferro-boron and boron powder, is pressed atomic molar per-cent batching;
2. melting once is put into the high frequency vacuum induction melting furnace with confected materials and is being carried out melting once, and furnace cooling obtains mother alloy;
3. secondary smelting places high frequency furnace or medium-frequency induction furnace to carry out secondary smelting melted mother alloy, obtains amorphous thin ribbon;
4. thermal treatment; The amorphous thin ribbon two ends are sandwiched in the galvanic current annealing device, and banded zone places applying dc magnetic field, magnetic field size 40～80Oe; Under the air atmosphere condition, carry out the current flow heats anneal; Size of current 400mA～800mA, be 30～240s conduction time, promptly obtains cobalt base amorphous giant magnetic impedance strip;
Condition is for vacuumizing earlier during the melting once of step described in 2.; When vacuum tightness reaches 0.1Pa when above, charge into argon gas at the high frequency vacuum induction melting furnace, air pressure is controlled at 0.5～1.5 normal atmosphere; 1200～2000 ℃ of smelting temperatures, smelting time are 10～30 minutes;
Condition is for when the mother alloy temperature reaches 1250～1400 ℃ during the 3. described secondary smelting of step; Charge into 99.99% argon gas, and protection furnace pressure 1～1.5 normal atmosphere, protection roller mouth spacing 0.3～0.5mm; The fused alloy is sprayed onto on the water-cooled copper roller of rotation; Speed of cooling is 25～50m/s, and it is wide to process 5～20mm, the amorphous thin ribbon of 20～40 μ m thickness.
2. preparation method according to claim 1 is characterized in that described cobalt base amorphous material component expression formula is Co
66Fe
4V
2Si
8B
20Or Co
64Fe
3V
3Si
10B
20
3. preparation method according to claim 1; When it is characterized in that the 3. described secondary smelting of step mother alloy is put into silica tube; Place high frequency furnace or medium-frequency induction furnace to carry out secondary smelting silica tube again, described silica tube bottom has the rectangle aperture.
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| CN103824649B (en) * | 2014-01-25 | 2016-11-09 | 陕西师范大学 | A kind of method utilizing Electromagnetic Heating to optimize transparent conductive oxide film quality |
| CN104032243B (en) * | 2014-06-05 | 2016-04-20 | 同济大学 | A kind of containing cobalt base amorphous giant magnetic impedance alloy thin band of Cr and preparation method thereof |
| CN104109822B (en) * | 2014-06-05 | 2017-01-04 | 同济大学 | A kind of containing Ni cobalt base amorphous giant magnetic impedance alloy thin band and preparation method thereof |
| CN104882239B (en) * | 2015-06-03 | 2017-12-05 | 山东大学 | One kind makes Fe78Si9B13The method that amorphous saturation magnetization improves and coercivity reduces |
| CN110565032A (en) * | 2019-09-17 | 2019-12-13 | 哈尔滨工业大学 | Amorphous fiber with giant magneto-impedance effect and preparation method and application thereof |
| CN113088637B (en) * | 2021-03-26 | 2022-08-02 | 深圳技术大学 | Deep pulse current annealing, signal conditioning and collecting method and device for permalloy |
| CN117626151A (en) * | 2023-12-14 | 2024-03-01 | 东莞市昱懋纳米科技有限公司 | Amorphous micrometer wire with high saturation magnetic induction intensity and high magnetic conductivity and heat treatment method |
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| CN101805876A (en) * | 2009-12-09 | 2010-08-18 | 青岛云路新能源科技有限公司 | Non-crystaline amorphous metal strip with high-saturation magnetic induction strength |
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Inventor after: Ji Song Inventor after: Zhang Yansong Inventor after: Ding Ang Inventor after: Qian Kunming Inventor after: Li Mingli Inventor before: Ji Song Inventor before: Zhang Yansong Inventor before: Ding Ang Inventor before: Qian Kunming Inventor before: Li Mingli |