CN109402339A - A kind of pulse square wave current annealing method for modulating amorphous alloy wire performance - Google Patents
A kind of pulse square wave current annealing method for modulating amorphous alloy wire performance Download PDFInfo
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- CN109402339A CN109402339A CN201811249151.5A CN201811249151A CN109402339A CN 109402339 A CN109402339 A CN 109402339A CN 201811249151 A CN201811249151 A CN 201811249151A CN 109402339 A CN109402339 A CN 109402339A
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/26—Methods of annealing
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/04—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering with simultaneous application of supersonic waves, magnetic or electric fields
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/34—Methods of heating
- C21D1/40—Direct resistance heating
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/52—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length
- C21D9/525—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for wires; for strips ; for rods of unlimited length for wire, for rods
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Abstract
The present invention discloses a kind of pulse square wave current annealing method for modulating amorphous alloy wire performance, it is to fix at amorphous alloy wire both ends with special fixture, external dedicated annealing power source, power supply, which is controlled, by special-purpose software exports adjustable pulse square wave current, the electric current generates instantaneous Joule heat and circumferential magnetizing field, make the magnetic hysteresis coefficient of dilatation of amorphous wire closer to zero, effectively improve circumferential magnetic anisotropy and circumferential magnetic conductivity, improve GMI performance, with biggish impedance rate of change and higher magnetic field sensitivity, high sensitivity can be prepared using the amorphous wire after annealing, high-resolution and high-precision GMI sensor, the technological operation is easy, low energy consumption, it is high-efficient, and do not easily cause amorphous alloy wire hot-spot crystallization and surface oxidation etc., it can be widely used in magnetic-sensitive material heat treatment and magneto-dependent sensor technical field.
Description
Technical field
The present invention relates to a kind of pulse square wave current annealing methods for modulating amorphous alloy wire performance, belong to magnetic-sensitive material heat
Processing and magneto-dependent sensor technical field.
Background technique
With the faint variation of external magnetic field, huge variation occurs for the AC impedance of sensitive material, and this phenomenon is claimed
For giant magnetic impedance (Giant Magneto Impedance, GMI) effect.Magneto-dependent sensor based on effect preparation is referred to as
GMI sensor.
In order to obtain the GMI sensor of highly sensitive, resolution ratio and service precision, it is desirable that sensitive material has excellent
GMI performance namely biggish impedance rate of change and higher magnetic field sensitivity.In existing sensitive material, cobalt base amorphous conjunction
Spun gold is one of optimal sensitive material, and has been used in the manufacture of business GMI sensor.Currently, business preparation amorphous alloy
The main method of silk is water spinning and Taylor's method, and the amorphous alloy wire of water spinning preparation is relatively large in diameter, it is also necessary at subsequent drawing
Reason；The rapid cooling process of similar technique makes the presence of very big residual stress inside amorphous alloy wire, and internal structure is uneven, respectively to
The opposite sex is unevenly distributed, and seriously restricts its GMI and soft magnet performance, is not able to satisfy high-precision magneto-dependent sensor to sensitive material
Practical application request, need to be made annealing treatment through modulation appropriate eliminate internal stress, adjustment structure Relaxation and improve circumferential magnetic respectively to
Anisotropic and circumferential magnetic conductivity, and then improve GMI performance.
Currently, common modulator approach has isothermal annealing, stress annealing, current annealing etc..Isothermal annealing can be released effectively
The residual stress of amorphous wire promotes structure Relaxation, but this method power consumption is big, low efficiency, and is unfavorable for amorphous alloy wire circumferential direction
The formation of magnetic domain.Stress annealing changes magnetoelastic energy by tensile stress or torque, and induction magnetic domain changes, and improves the ring of amorphous wire
To anisotropy and circumferential magnetic conductivity, but requirement of this method to the stability of equipment, service life and fixture is relatively high.
Current annealing not only discharges the residualinternal stress of amorphous wire, causes random atomic migration by Joule heat and circumferential magnetizing field
Effect adjusts micro-structure relaxation and expands atomic rule arrangement microcell and the orderly oriented region of atomic magnetic moment, and magnetic hysteresis coefficient of dilatation becomes
It obtains closer to zero, magnetoelastic energy is relatively low, and under the action of toroidal magnetic field, and axial magnetic domain volume reduces, circumferential magnetic
Farmland volume expands, and effectively improves circumferential magnetic anisotropy and circumferential magnetic conductivity, therefore, current annealing is relatively good modulation methods
Method.But when electric current of annealing is Constant Direct Current, particularly significant, the thermogenetic temperature of electric current joule of current density size change
When suitable, toroidal magnetic field is not big enough, and current density is excessive, and amorphous wire is easy to happen hot-spot crystallization and surface oxidation.When
When electric current of annealing is simple alternating current, crosses thermal crystallisation phenomenon and weaken, but the effective acting time of toroidal magnetic field is still shorter, GMI
Performance need to be improved；When power frequency is not high enough, due to curent change caused by temperature fluctuation it is larger, be unfavorable for obtain performance
The treatment effect of stable homogeneous；Therefore it provides a kind of pulse square wave current annealing method for modulating amorphous alloy wire performance, generates
Instantaneous Joule heat and toroidal magnetic field extends toroidal magnetic field effective acting time, sufficiently discharges the residualinternal stress of amorphous wire, adjusts
Whole micro-structure relaxation simultaneously expands atomic rule arrangement microcell and the orderly oriented region of atomic magnetic moment, makes to generate in amorphous wire good
Circumferential anisotropy, while amorphous alloy wire hot-spot crystallization and surface oxidation are avoided, the preparation to high-performance GMI sensor
It has a very important significance.
Summary of the invention
The present invention provides one kind to make amorphous alloy wire have biggish impedance rate of change and higher magnetic field sensitivity
Modulate the pulse square wave current annealing method of amorphous alloy wire performance.
A kind of pulse square wave current annealing method of modulation amorphous alloy wire performance of the invention is to carry out according to the following steps
:
1) amorphous alloy wire both ends are fixed using special fixture, special fixture connects dedicated annealing power source；
2) by special-purpose software Interface Control, dedicated annealing power source exports adjustable pulse square wave current, and pulse square wave electric current passes through
Special fixture flows through amorphous alloy wire, generates instantaneous Joule heat and toroidal magnetic field, using control variate method, adjusts pulse square wave electricity
The parameters of stream, respectively make annealing treatment amorphous alloy wire under different current annealing parameters and to complete annealing parameter excellent
Change, the parameters range of pulse square wave electric current is as follows:
Pulse square wave current amplitude: 50mA~150mA
Pulse square wave current duty cycle: 20%-100%
Pulse square wave power frequency: 5-50KHz
Annealing time can freely be set
3) test obtains influence of the different current annealing parameters to amorphous alloy wire maximum resistance variation rate and magnetic field sensitivity
Rule comprehensively considers two performance indicators, can determine the current annealing parameter of best performance, while can also answer according to specific
With require select specific currents annealing parameter.
The present invention anneals to amorphous alloy wire using pulse square wave electric current, and pulse square wave electric current generates instantaneous Joule heat
And toroidal magnetic field, toroidal magnetic field effective acting time is longer, can sufficiently discharge residualinternal stress, and random atomic migration is caused to be imitated
It answers, adjusting micro-structure relaxation and expanding atomic rule arrangement microcell and the orderly oriented region of atomic magnetic moment, magnetic hysteresis coefficient of dilatation becomes
Closer to zero, magnetoelastic energy is relatively low, and under the action of toroidal magnetic field, axial magnetic domain volume reduces, circumferential magnetic domain volume
Expand, effectively improves circumferential magnetic anisotropy and circumferential magnetic conductivity, and then improve GMI performance, make amorphous wire that there is biggish resistance
Resistance rate and higher magnetic field sensitivity, this method is easy to operate, low energy consumption, high-efficient, and does not easily cause amorphous alloy wire
Hot-spot crystallization and surface oxidation.
Detailed description of the invention
Fig. 1 is the SEM photograph on amorphous alloy wire surface in the embodiment of the present invention after Mechanical Method removal glass bag coating.
Fig. 2 is pulse square wave current signal schematic diagram in the embodiment of the present invention.
Fig. 3 is the relationship of maximum resistance variation rate and pulse square wave current amplitude in the embodiment of the present invention.
Fig. 4 is the relationship of magnetic field sensitivity and pulse square wave current amplitude in the embodiment of the present invention.
Fig. 5 is the relationship of maximum resistance variation rate and pulse square wave current duty cycle in the embodiment of the present invention.
Fig. 6 is the relationship of magnetic field sensitivity and pulse square wave current duty cycle in the embodiment of the present invention.
Fig. 7 is the relationship of maximum resistance variation rate and annealing time in the embodiment of the present invention.
Fig. 8 is the relationship of magnetic field sensitivity and annealing time in the embodiment of the present invention.
Fig. 9 is the relationship of maximum resistance variation rate and pulse square wave power frequency in the embodiment of the present invention.
Figure 10 is the relationship of magnetic field sensitivity and pulse square wave power frequency in the embodiment of the present invention.
Fig. 3 " blank " into Figure 10 indicates the case where without the processing of pulse square wave current annealing, to compare.Maximum impedance
Change rate is (Z/Z)max=(Zm-Z0)/Z0× 100%, Z in formulamFor impedance maximum value, Z0When for additional axial magnetic field being zero
Impedance.Magnetic field sensitivity η=(Z/Z)max /Hk, H in formulakFor the corresponding additional axial magnetic field of impedance maximum value.
Specific embodiment
The present invention is described in further detail below with reference to embodiment attached drawing.
Embodiment
A kind of pulse square wave current annealing method of the modulation amorphous alloy wire performance of the present embodiment be according to the following steps into
Capable:
1, glass fluxing technique cobalt base amorphous alloy wire is prepared using Taylor's method, glass bag coating is removed using Mechanical Method.Such as Fig. 1 institute
Show, the smooth surface of amorphous alloy wire, clean and tidy after removing glass bag coating using Mechanical Method, the diameter of amorphous alloy wire is
31.6μm。
2, the amorphous alloy wire for preparing step 1 is cut into the segment of 16cm long, its both ends is fixed with steel tack fixture,
The external dedicated annealing power source of steel tack fixture.
3, in setting procedure 2 dedicated annealing power source parameter, pulse square wave current duty cycle is 60%, and annealing time is
300s, frequency 5KHz change pulse square wave current amplitude, from 100mA~150mA, stepping 10mA, in different pulse square waves
Under current amplitude, current annealing processing is carried out to amorphous alloy wire respectively, Fig. 2 is pulse square wave when current amplitude is equal to 100mA
The schematic diagram of current signal.The amorphous alloy wire that processing obtains is cut into the segment of 1cm long, is surveyed using Network Analyzer E5071C
Its impedance is tried with the situation of change of additional axial magnetic field, can be obtained different pulse square wave current amplitude annealing to amorphous alloy wire
The affecting laws of maximum resistance variation rate and magnetic field sensitivity.As shown in figure 3, when test frequency is 70MHz, with pulse
The increase of square wave current amplitude, maximum resistance variation take the lead in increasing after reducing, when pulse square wave current amplitude is 150mA, most
It is 173.9% that big impedance rate of change, which obtains maximum value,.As shown in figure 4, when test frequency is 70MHz, with pulse square wave electric current
The increase of amplitude, magnetic field sensitivity dullness increase, and when pulse square wave current amplitude is 150mA, magnetic field sensitivity obtains maximum
Value is 253.0%/Oe.Therefore, when pulse square wave current duty cycle be 60%, annealing time 300s, frequency be 5K when, the cobalt-based
The optimal annealing current amplitude of amorphous alloy wire is 150mA.
4, in setting procedure 2 dedicated annealing power source parameter, pulse square wave current amplitude is 150mA, and annealing time is
300s, frequency 5KHz change pulse square wave current duty cycle, from 40%~65%, under different pulse square wave current duty cycles,
Current annealing processing is carried out to amorphous alloy wire respectively.The amorphous alloy wire that processing obtains is cut into the segment of 1cm long, uses net
Network analyzer E5071C tests its impedance with the situation of change of additional axial magnetic field, can be obtained different pulse square wave electric current duties
Compare the affecting laws of amorphous alloy wire maximum resistance variation rate and magnetic field sensitivity.As shown in figure 5, when test frequency is
When 70MHz, with the increase of pulse square wave current duty cycle, maximum resistance variation rate first increases and then decreases, when pulse square wave electricity
When stream duty ratio is 60%, it is 173.9% that maximum resistance variation rate, which obtains maximum value,.As shown in fig. 6, when test frequency is 70MHz
When, with the increase of pulse square wave current duty cycle, magnetic field sensitivity first increases and then decreases, when pulse square wave current duty cycle is
When 60%, it is 253.0%/Oe that magnetic field sensitivity, which obtains maximum value,.Therefore, when pulse square wave current amplitude is 150mA, annealing time
For 300s, when frequency is 5KHz, the optimal annealing current duty cycle of the cobalt base amorphous alloy wire is 60%.
5, in setting procedure 2 dedicated annealing power source parameter, pulse square wave current amplitude be 150mA, duty ratio 60%,
Frequency is 5KHz, changes annealing time, from 300s~900s, under different annealing times, carries out electricity to amorphous alloy wire respectively
Stream annealing.The amorphous alloy wire that processing obtains is cut into the segment of 1cm long, tests its resistance using Network Analyzer E5071C
The anti-situation of change with additional axial magnetic field, can be obtained different annealing times to amorphous alloy wire maximum resistance variation rate and
The affecting laws of magnetic field sensitivity.As shown in fig. 7, when test frequency is 70MHz, with the increase of annealing time, maximum resistance
Resistance rate first increases and then decreases, when annealing time is 480s, it is 329.5% that maximum resistance variation rate, which obtains maximum value,.Such as figure
Shown in 8, when test frequency is 70MHz, with the increase of annealing time, magnetic field sensitivity first increases and then decreases, when annealing
Between be 480s when, magnetic field sensitivity obtain maximum value be 370.1%/Oe.Therefore, when pulse square wave current amplitude be 150mA, account for
Sky is than being 60%, and when frequency is 5KHz, the optimal annealing time of the cobalt base amorphous alloy wire is 480s.
6, in setting procedure 2 dedicated annealing power source parameter, pulse square wave current amplitude be 150mA, duty ratio 60%,
Annealing time is 480s, changes pulse square wave power frequency, from 5KHz~25KHz, stepping 5KHz, in different pulse square wave electricity
It flows under frequency, current annealing processing is carried out to amorphous alloy wire respectively.The amorphous alloy wire that processing obtains is cut into the small of 1cm long
Section tests its impedance with the situation of change of additional axial magnetic field using Network Analyzer E5071C, can be obtained different annealing electricity
Frequency is flowed to the affecting laws of amorphous alloy wire maximum resistance variation rate and magnetic field sensitivity.As shown in figure 9, working as test frequency
When for 70MHz, with the increase of pulse square wave power frequency, maximum resistance variation rate first increases and then decreases, when pulse square wave electricity
When stream frequency is 10KHz, it is 375.3% that maximum resistance variation rate, which obtains maximum value,.As shown in Figure 10, when test frequency is 70MHz
When, with the increase of pulse square wave power frequency, magnetic field sensitivity dullness reduces, when pulse square wave power frequency is 5KHz,
It is 370.1%/Oe that magnetic field sensitivity, which obtains maximum value,.Comprehensively consider, when pulse square wave current amplitude is 150mA, annealing time is
480s, when duty ratio is 60%, the optimal annealing power frequency of the cobalt base amorphous alloy wire is 5KHz.
To sum up, the optimal annealing parameter of the cobalt amorphous alloy wire are as follows: pulse square wave current amplitude is 150mA, annealing time
For 480s, duty ratio 60%, frequency 5KHz.
The above is only better embodiment of the invention, is not construed as limitation of the scope of the invention, Er Qieben
It invents advocated scope of the claims to be not limited thereto, all personages for being familiar with this field skill, according to presently disclosed
Technology contents, can think easily and equivalence changes, should all fall within the scope of protection of the present invention.
Claims (3)
1. a kind of pulse square wave current annealing method for modulating amorphous alloy wire performance, using special fixture by amorphous alloy wire two
End is fixed, and special fixture connects dedicated annealing power source.
2. dedicated annealing power source exports adjustable pulse square wave current by special-purpose software Interface Control, pulse square wave electric current passes through
Special fixture flows through amorphous alloy wire, generates Joule heat and sufficiently large circumferential magnetizing field, optimizes pulse square wave by adjusting
The parameters of electric current can either make amorphous alloy wire reach suitable annealing temperature by Joule heat, can also be by instantaneous
Square wave current generates sufficiently large circumferential magnetizing field, increases amorphous alloy wire circumferential direction magnetic domain volume, reaches circumferential magnetized
Purpose.
3. by pulse square wave current annealing mode can regulate and control the interior state of amorphous alloy wire, microstructure and its respectively to
Opposite sex distribution etc., to realize the modulation treatment of amorphous alloy wire performance, the parameters range of pulse square wave electric current is as follows:
Pulse square wave current amplitude: 50mA~150mA
Pulse square wave current duty cycle: 20%-100%
Pulse square wave power frequency: 5-50KHz
Annealing time can freely be set
After the optimization of each parameter, the purpose that the giant magnetic impedance performance of amorphous alloy wire increases substantially can achieve.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112307779A (en) * | 2020-11-06 | 2021-02-02 | 北京航空航天大学 | Method for optimizing ultra-high-precision GMI superconducting composite magnetometer |
| CN113088637A (en) * | 2021-03-26 | 2021-07-09 | 深圳技术大学 | Deep pulse current annealing, signal conditioning and collecting method and device for permalloy |
| CN114015957A (en) * | 2021-11-03 | 2022-02-08 | 松山湖材料实验室 | Filamentous coiled material, nanocrystalline metal wire and manufacturing method and equipment thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112307779A (en) * | 2020-11-06 | 2021-02-02 | 北京航空航天大学 | Method for optimizing ultra-high-precision GMI superconducting composite magnetometer |
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| CN114015957A (en) * | 2021-11-03 | 2022-02-08 | 松山湖材料实验室 | Filamentous coiled material, nanocrystalline metal wire and manufacturing method and equipment thereof |
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