CN109754976A - A kind of iron base amorphous magnetically-soft alloy and application - Google Patents
A kind of iron base amorphous magnetically-soft alloy and application Download PDFInfo
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Abstract
The present invention relates to a kind of iron base amorphous magnetically-soft alloy and application, the alloy expression formula of the iron base amorphous magnetically-soft alloy is FeaSibBcCudCe, a, b, c, d and e respectively indicate the atomic percent of each component in alloy expression formula, and meet the following conditions: it be 8~11, c be 9~13, d be 0 ~ 1.5, e is 0~1.5, a+b+c+d+e=100 that a, which is 76~81, b,;The iron base amorphous magnetically-soft alloy is applied to transformer, saturable reactor or filter inductor;The iron base amorphous magnetically-soft alloy simple, low production cost with excellent synthesis soft magnet performance and its good moldability, preparation process.
Description
Technical field
The invention belongs to amorphous alloy technical fields, and in particular to a kind of iron base amorphous magnetically-soft alloy and application.
Background technique
Non-crystalline material has excellent soft magnet performance, such as higher saturation magnetic flux density and magnetic conductivity, lower to rectify
Stupid power and loss etc..The 1K101 amorphous ribbon for having realized large-scale productionization at present is typical amorphous alloy, is had excellent
Soft magnet performance, but magnetic saturation intensityB sOnly 1.56T, and the magnetic saturation intensity of silicon steel is up to 2T, therefore compared with traditional silicon steel,
The performance of current Fe-based amorphous material in some aspects is still clearly present larger gap.Numerous studies person attempts non-by reducing
The methods of ferromagnetic element is added soft magnetisms such as the saturation magnetic flux densities that improves amorphous alloy in ferromagnetic element content
Can, but after iron content reaches certain value in non-crystalline material, amorphous formation ability will decline to a great extent, and it is non-not can guarantee its
Brilliant Forming ability, and be unable to ensure the grain size formed after crystallization in nanoscale and then improve its soft magnet performance;In addition, cobalt is first
The addition of element also substantially increases cost other than increasing the coercivity after Fe-based amorphous anneal of material.
Fe is disclosed in the patent that Authorization Notice No. is CN102509603B75Si3B14.5Cr4Hf3.5Alloy, after annealing
Saturation magnetic flux density be 1.48T, coercivity 1.3A/m, but the alloy contains Hf element, increases production cost, and
Saturation magnetic flux density is significantly lower than 1K101.
A kind of nanometer crystal alloy FeSiBPCuC is disclosed in the patent of Patent No. CN106756643A, because it contains
Have Volatile Elements P, the easy scaling loss in fusion process and cause composition tolerances, and nanometer crystal alloy annealing temperature is high, prepares work
Skill is more cumbersome than amorphous alloy.
A kind of FeBC alloy is disclosed in the patent of Patent No. US4226619, the magnetic saturation induction after annealing is strong
Degree has reached 1.7T, but its coercivity is excessive, and alloy strip steel rolled stock has biggish brittleness, is unfavorable for realizing heavy industrialization
Production.
In addition, Metglass2605 Fe67Co18B14Si1Alloy has the saturation magnetic flux density of 1.75T, but it contains
There is cobalt element, substantially increase production cost, is unfavorable for amorphous alloy large-scale production and application.
Currently, the novel Fe-based amorphous soft magnetism that there is excellent comprehensive magnetic energy and can be realized large-scale production is developed to close
Gold not only has directive significance to industrial production, and can promote the industrial technology revolution of a new round to a certain extent.It is close several
Year with amorphous soft magnetic material development, amorphous soft magnetic material is widely used in the components such as mobile phone, and Mobile phone
Publication, will also promote research of more researchers to amorphous soft-magnetic alloy.In conclusion amorphous soft-magnetic alloy is in industry and life
It is all with a wide range of applications in work.Therefore, developing the more excellent novel amorphous soft-magnetic alloy of comprehensive performance has weight
The meaning wanted.
Summary of the invention
The problems such as poor the invention solves traditional iron base amorphous magnetically-soft alloy comprehensive performance, to solve the above-mentioned problems,
The present invention provides a kind of iron base amorphous magnetically-soft alloy, it has excellent synthesis soft magnet performance and its good moldability, preparation process
Simply, low production cost.
The object of the present invention is achieved in the following manner:
A kind of iron base amorphous magnetically-soft alloy, its alloy expression formula are FeaSibBcCudCe, a, b, c, d and e in alloy expression formula
Respectively indicate the atom percentage content of each component, and meet the following conditions: it be 8~11, c is that 9~13, d is that a, which is 76~81, b,
0 ~ 1.5, e are 0~1.5, a+b+c+d+e=100.
Iron base amorphous magnetically-soft alloy as described above, it be 9~10, c is 9~12, d that a, which is 77~80, b, in alloy expression formula
It is 0~1.4 for 0 ~ 1.4, e.
Iron base amorphous magnetically-soft alloy as described above, it be 9~10, c is 10~11, d that a, which is 78~79, b, in alloy expression formula
It is 0~1.3 for 0 ~ 1.3, e.
As example:
A is 79, b 9.522, c 11.178, d 0.3, e 0 in alloy expression formula.
A is 79, b 9.43, c 11.07, d 0.5, e 0 in alloy expression formula.
A is 78.7, b 9.2, c 10.8, d 1, e 0.3 in alloy expression formula.
A is 78, b 9.2, c 10.8, d 1, e 1 in alloy expression formula.
The application of iron base amorphous magnetically-soft alloy as described above, is applied to transformer, saturable reactor, filter inductor
Equal fields.
Si and B belong to metalloid element, are known as biggish Atomic radiuses difference, in iron base amorphous magnetically-soft alloy, B with Fe member
Noncrystal substrate can be made to stablize, crystal grain is prevented to grow up, improve amorphous formation ability;Si can be such that magnetostriction coefficient reduces, curie point
It increases, improves thermal stability.
Since Cu separates Fe-based amorphous be easy to happen mutually with the presence of the positive enthalpy of mixing of Fe, copper clusters provide forming core for α-Fe
Particle can be such that two crystallization peaks of Fe-based amorphous alloy separate, ensure that the safety of its annealing process.
The present invention utilizes Cu member by adding micro Cu element and C element on the basis of traditional Fe-based amorphous 1K101
Element provides nucleation mass point for α-Fe to promote Fe-based amorphous heterogeneous forming core to improve its soft magnet performance, while micro C element can
Guarantee the amorphous formation ability of alloy system, and Cu element and C element are relatively broad in industrial application, low in cost.
In conjunction with above-mentioned, present invention significant advantage compared with existing similar technique is embodied in:
1. being free of in present component containing to the advantageous Cu element of iron base amorphous magnetically-soft alloy comprehensive performance and C element is improved
The ferromagnetic element for having the prices such as Co, Ni more expensive, and in preparation process of the present invention can applicable industry raw material, without using expensive
High pure raw material reduces the production cost of iron base amorphous magnetically-soft alloy;
2. iron base amorphous magnetically-soft alloy of the present invention has good amorphous formation ability, alloy strip steel rolled stock molding is easy, and prepares work
Skill is simple, is advantageously implemented large-scale industrial production.
It is to a certain extent industrial productivity 3. iron base amorphous magnetically-soft alloy of the present invention has excellent comprehensive performance
The more excellent amorphous band of energy provides directive significance.
In conclusion iron base amorphous magnetically-soft alloy of the present invention has excellent comprehensive performance, with high saturation magnetic strength
Answer intensityB s, high and stable Effective permeabilityμ e, low coercivityH cWith good amorphous formation ability, alloy strip steel rolled stock molding
Property is good, it is easy to accomplish large-scale industrial production.
Detailed description of the invention
Fig. 1 is the XRD diagram of iron base amorphous magnetically-soft alloy in Examples 1 to 8 and comparative example 1;Abscissa is scan angle in figure
Degree, ordinate is intensity;
Fig. 2 is the DSC figure of iron base amorphous magnetically-soft alloy in Examples 1 to 8 and comparative example 1;Abscissa is temperature, ordinate in figure
For thermal discharge;
Fig. 3 is the partial enlarged view of the VSM in section Example and comparative example 1 before iron base amorphous magnetically-soft alloy annealing;It is horizontal in figure
Coordinate is magnetic field strength, and ordinate is saturation magnetic flux density;
Fig. 4 is the saturation magnetic flux density variation diagram in Examples 1 to 8 and comparative example 1 before iron base amorphous magnetically-soft alloy annealing;Figure
Middle abscissa is ingredient symbol, and ordinate is saturation magnetic flux density;
Fig. 5 be in section Example and comparative example 1 after iron base amorphous magnetically-soft alloy stress relief annealing under different impressed frequencies
Magnetic conductivity figure;Abscissa is frequency in figure, and ordinate is Effective permeability;
Fig. 6 is the magnetic conductivity variation diagram in Examples 1 to 8 and comparative example 1 after iron base amorphous magnetically-soft alloy stress relief annealing;In figure
Abscissa is ingredient symbol, and ordinate is Effective permeability;
Fig. 7 is the coercivity variation diagram in Examples 1 to 8 and comparative example 1 after iron base amorphous magnetically-soft alloy stress relief annealing;In figure
Abscissa is ingredient symbol, and ordinate is coercivity;
Fig. 8 is the VSM comparison diagram of iron base amorphous magnetically-soft alloy annealing front and back in embodiment 7 and example 8;Abscissa is magnetic field in figure
Intensity, ordinate are saturation magnetic flux density;
Fig. 9 is the XRD diagram of iron base amorphous magnetically-soft alloy in comparative example 2;Abscissa is scanning angle in figure, and ordinate is intensity;
Figure 10 is the DSC figure of iron base amorphous magnetically-soft alloy in comparative example 2;Abscissa is temperature in figure, and ordinate is thermal discharge;
Figure 11 is the VSM figure in comparative example 2 after iron base amorphous magnetically-soft alloy annealing;Abscissa is magnetic field strength, ordinate in figure
For saturation magnetic flux density.
Specific embodiment
The present invention is described further combined with specific embodiments below, but protection scope of the present invention is not limited to
This.
Embodiment 1
A kind of iron base amorphous magnetically-soft alloy, alloy expression formula are Fe79Si9.522B11.178Cu0.3, it is denoted as H-1;As more detailed
Example, its preparation method include the following steps:
(1) ingredient: choose content be 99.9wt% Fe, content be 99.99wt% Si, B content be 17.40wt% FeB and contain
Amount is the Cu of 99.99wt%, carries out ingredient according to above-mentioned alloy expression formula;Before weighing raw material, pass through sand paper or grinding wheel
Machine polishing raw material, remove the oxide layer on surface, Fe, Cu raw material are put into the beaker for filling dehydrated alcohol after polishing
In, and ultrasonic cleaning 240S is used, further remove the impurity such as oxide debris, greasy dirt of material surface, then using blowing
Blower is dried;
(2) melting: will weigh and the raw material handled well is put into silica crucible, in order to reduce the burning of fusion process chinese raw materials
Damage, density is big and low-melting alloying component is placed on the upper surface of metalloid and volatile metal, the original placed in silica crucible
Material sequence is followed successively by Cu, Fe, Si and FeB from top to bottom;The silica crucible for filling raw material is put into vacuum induction melting furnace cavity
Induction coil in, close fire door, vacuumized first using mechanical pump, when vacuum degree reaches 6.0 × 10-1After Pa, machine is closed
Tool pumps and opens diffusion pump up to vacuum degree to 6.0 × 10-3Pa is then charged with the argon gas that the purity of 0.05 MPa is 99.999%
As protective gas;Opening induction heating power and adjusting electric current is that 2A carries out preheating material, is added rapidly to electric current after 1 min
8A carries out melting, and electric current is down to 4A after alloy melts completely, carries out more uniform melting, cooling after melting to expand
Pump is dissipated, power supply is closed;
(3) prepare amorphous thin ribbon: the master alloy that melting is finished is crushed frustillatum, and 7 g master alloys of clamping are put into bottom and are provided with
In the quartz ampoule of 0.5 mm circular hole;Quartz ampoule is put into vacuum to get rid of in the induction coil with machine, adjustment quartz ampoule height is up to it
At 1 mm right above copper wheel;It is vacuumized first using mechanical pump, when vacuum degree reaches 6.0 × 10-1After Pa, opens and expand
Pump is dissipated until vacuum is extracted into 6.0 × 10-3Pa closes diffusion pump, is then charged with the argon gas that 0.05MPa purity is 99.999%,
Quartz ampoule inside and outside differential pressure is 0.05MPa at this time, and unlatching gets rid of the copper wheel for being connected with cooling circulating water in carrying device cavity, sets copper wheel
Linear velocity is 40 m/s;Induction heating power and setting electric current value are opened, current value starts to be set as 3A, it is set as 12A after 5S,
When master alloy color is changed into brilliant white by kermesinus in observation quartz ampoule, determine that the master alloy in quartz ampoule is completely molten at this time
Change, the master alloy being completely melt is ejected into the high-speed rotating copper wheel for being connected with cooling circulating water using quartz ampoule inside and outside differential pressure
On, to prepare amorphous thin ribbon;Since the thermal expansion coefficient difference of quartz ampoule and master alloy is larger, induced current starts to set
It is smaller, avoid master alloy and quartz ampoule from damaging quartz ampoule due to adding thermogenetic deflection to have big difference, when master alloy occurs
When color change will melt, high current to 12A accelerates the burn-off rate of master alloy, avoids heating time too long iron-based soft
The Partial Elements of magnetic master alloy cause the amorphous ribbon performance prepared bad with quartzy tube reaction;In addition, small in quartz ampoule
Blocky iron-based soft magnetic master alloy avoids excessive, otherwise quartz ampoule is easy to cause to rupture during heating;Liquid after alloy melting
Injecting time avoid it is too long because this to will lead to overheat or burning loss of alloy serious and composition tolerances occur.
Embodiment 2
A kind of iron base amorphous magnetically-soft alloy, alloy expression formula are Fe79Si9.43B11.07Cu0.5, it is denoted as H-2;As showing in more detail
Example, its preparation method include the following steps:
(1) ingredient: choose content be 99.9wt% Fe, content be 99.99wt% Si, B content be 17.40wt% FeB and contain
Amount is the Cu of 99.99wt%, carries out ingredient according to above-mentioned alloy expression formula;Before weighing raw material, pass through sand paper or grinding wheel
Machine polishing raw material, remove the oxide layer on surface, Fe, Cu raw material are put into the beaker for filling dehydrated alcohol after polishing
In, and ultrasonic cleaning 240S is used, further remove the impurity such as oxide debris, greasy dirt of material surface, then using blowing
Blower is dried;
(2) melting: will weigh and the raw material handled well is put into silica crucible, in order to reduce the burning of fusion process chinese raw materials
Damage, density is big and low-melting alloying component is placed on the upper surface of metalloid and volatile metal, the original placed in silica crucible
Material sequence is followed successively by Cu, Fe, Si and FeB from top to bottom;The silica crucible for filling raw material is put into vacuum induction melting furnace cavity
Induction coil in, close fire door, vacuumized first using mechanical pump, when vacuum degree reaches 5.0 × 10-1After Pa, machine is closed
Tool pumps and opens diffusion pump up to vacuum degree to 6.0 × 10-3Pa is then charged with the argon gas that the purity of 0.05 MPa is 99.999%
As protective gas;Opening induction heating power and adjusting electric current is that 2A carries out preheating material, is added rapidly to electric current after 1 min
8A carries out melting, and electric current is down to 4A after alloy melts completely, carries out more uniform melting, cooling after melting to expand
Pump is dissipated, power supply is closed;
(3) prepare amorphous thin ribbon: the master alloy that melting is finished is crushed frustillatum, and 7 g master alloys of clamping are put into bottom and are provided with
In the quartz ampoule of 0.5 mm circular hole;Quartz ampoule is put into vacuum to get rid of in the induction coil with machine, adjustment quartz ampoule height is up to it
At 1 mm right above copper wheel;It is vacuumized first using mechanical pump, when vacuum degree reaches 5.0 × 10-1After Pa, opens and expand
Pump is dissipated until vacuum is extracted into 6.0 × 10-3Pa closes diffusion pump, is then charged with the argon gas that 0.05MPa purity is 99.999%,
Quartz ampoule inside and outside differential pressure is 0.05MPa at this time, and unlatching gets rid of the copper wheel for being connected with cooling circulating water in carrying device cavity, sets copper wheel
Linear velocity is 40 m/s;Induction heating power and setting electric current value are opened, current value starts to be set as 3A, it is set as 12A after 5S,
When master alloy color is changed into brilliant white by kermesinus in observation quartz ampoule, determine that the master alloy in quartz ampoule is completely molten at this time
Change, the master alloy being completely melt is ejected into the high-speed rotating copper wheel for being connected with cooling circulating water using quartz ampoule inside and outside differential pressure
On, to prepare amorphous thin ribbon;Since the thermal expansion coefficient difference of quartz ampoule and master alloy is larger, induced current starts to set
It is smaller, avoid master alloy and quartz ampoule from damaging quartz ampoule due to adding thermogenetic deflection to have big difference, when master alloy occurs
When color change will melt, high current to 12A accelerates the burn-off rate of master alloy, avoids heating time too long iron-based soft
The Partial Elements of magnetic master alloy cause the amorphous ribbon performance prepared bad with quartzy tube reaction;In addition, small in quartz ampoule
Blocky iron-based soft magnetic master alloy avoids excessive, otherwise quartz ampoule is easy to cause to rupture during heating;Liquid after alloy melting
Injecting time avoid it is too long because this to will lead to overheat or burning loss of alloy serious and composition tolerances occur.
Embodiment 3
A kind of iron base amorphous magnetically-soft alloy, alloy expression formula are Fe79Si9.34B10.96Cu0.7, it is denoted as H-3;As showing in more detail
Example, its preparation method include the following steps:
(1) ingredient: choose content be 99.9wt% Fe, content be 99.99wt% Si, B content be 17.40wt% FeB and contain
Amount is the Cu of 99.99wt%, carries out ingredient according to above-mentioned alloy expression formula;Before weighing raw material, pass through sand paper or grinding wheel
Machine polishing raw material, remove the oxide layer on surface, Fe, Cu raw material are put into the beaker for filling dehydrated alcohol after polishing
In, and ultrasonic cleaning 240S is used, further remove the impurity such as oxide debris, greasy dirt of material surface, then using blowing
Blower is dried;
(2) melting: will weigh and the raw material handled well is put into silica crucible, in order to reduce the burning of fusion process chinese raw materials
Damage, density is big and low-melting alloying component is placed on the upper surface of metalloid and volatile metal, the original placed in silica crucible
Material sequence is followed successively by Cu, Fe, Si and FeB from top to bottom;The silica crucible for filling raw material is put into vacuum induction melting furnace cavity
Induction coil in, close fire door, vacuumized first using mechanical pump, when vacuum degree reaches 4.0 × 10-1After Pa, machine is closed
Tool pumps and opens diffusion pump up to vacuum degree to 6.0 × 10-3Pa is then charged with the argon gas that the purity of 0.05 MPa is 99.999%
As protective gas;Opening induction heating power and adjusting electric current is that 2A carries out preheating material, is added rapidly to electric current after 1 min
8A carries out melting, and electric current is down to 4A after alloy melts completely, carries out more uniform melting, cooling after melting to expand
Pump is dissipated, power supply is closed;
(3) prepare amorphous thin ribbon: the master alloy that melting is finished is crushed frustillatum, and 7 g master alloys of clamping are put into bottom and are provided with
In the quartz ampoule of 0.5 mm circular hole;Quartz ampoule is put into vacuum to get rid of in the induction coil with machine, adjustment quartz ampoule height is up to it
At 1 mm right above copper wheel;It is vacuumized first using mechanical pump, when vacuum degree reaches 6.0 × 10-1After Pa, opens and expand
Pump is dissipated until vacuum is extracted into 6.0 × 10-3Pa closes diffusion pump, is then charged with the argon gas that 0.05MPa purity is 99.999%,
Quartz ampoule inside and outside differential pressure is 0.05MPa at this time, and unlatching gets rid of the copper wheel for being connected with cooling circulating water in carrying device cavity, sets copper wheel
Linear velocity is 40 m/s;Induction heating power and setting electric current value are opened, current value starts to be set as 3A, it is set as 12A after 5S,
When master alloy color is changed into brilliant white by kermesinus in observation quartz ampoule, determine that the master alloy in quartz ampoule is completely molten at this time
Change, the master alloy being completely melt is ejected into the high-speed rotating copper wheel for being connected with cooling circulating water using quartz ampoule inside and outside differential pressure
On, to prepare amorphous thin ribbon;Since the thermal expansion coefficient difference of quartz ampoule and master alloy is larger, induced current starts to set
It is smaller, avoid master alloy and quartz ampoule from damaging quartz ampoule due to adding thermogenetic deflection to have big difference, when master alloy occurs
When color change will melt, high current to 12A accelerates the burn-off rate of master alloy, avoids heating time too long iron-based soft
The Partial Elements of magnetic master alloy cause the amorphous ribbon performance prepared bad with quartzy tube reaction;In addition, small in quartz ampoule
Blocky iron-based soft magnetic master alloy avoids excessive, otherwise quartz ampoule is easy to cause to rupture during heating;Liquid after alloy melting
Injecting time avoid it is too long because this to will lead to overheat or burning loss of alloy serious and composition tolerances occur.
Embodiment 4
A kind of iron base amorphous magnetically-soft alloy, alloy expression formula are Fe79Si9.2B10.8Cu1, it is denoted as H-4;As more detailed example,
Its preparation method includes the following steps:
(1) ingredient: choose content be 99.9wt% Fe, content be 99.99wt% Si, B content be 17.40wt% FeB and contain
Amount is the Cu of 99.99wt%, carries out ingredient according to above-mentioned alloy expression formula;Before weighing raw material, pass through sand paper or grinding wheel
Machine polishing raw material, remove the oxide layer on surface, Fe, Cu raw material are put into the beaker for filling dehydrated alcohol after polishing
In, and ultrasonic cleaning 240S is used, further remove the impurity such as oxide debris, greasy dirt of material surface, then using blowing
Blower is dried;
(2) melting: will weigh and the raw material handled well is put into silica crucible, in order to reduce the burning of fusion process chinese raw materials
Damage, density is big and low-melting alloying component is placed on the upper surface of metalloid and volatile metal, the original placed in silica crucible
Material sequence is followed successively by Cu, Fe, Si and FeB from top to bottom;The silica crucible for filling raw material is put into vacuum induction melting furnace cavity
Induction coil in, close fire door, vacuumized first using mechanical pump, when vacuum degree reaches 3.0 × 10-1After Pa, machine is closed
Tool pumps and opens diffusion pump up to vacuum degree to 6.0 × 10-3Pa is then charged with the argon gas that the purity of 0.05 MPa is 99.999%
As protective gas;Opening induction heating power and adjusting electric current is that 2A carries out preheating material, is added rapidly to electric current after 1 min
8A carries out melting, and electric current is down to 4A after alloy melts completely, carries out more uniform melting, cooling after melting to expand
Pump is dissipated, power supply is closed;
(3) prepare amorphous thin ribbon: the master alloy that melting is finished is crushed frustillatum, and 7 g master alloys of clamping are put into bottom and are provided with
In the quartz ampoule of 0.5 mm circular hole;Quartz ampoule is put into vacuum to get rid of in the induction coil with machine, adjustment quartz ampoule height is up to it
At 1 mm right above copper wheel;It is vacuumized first using mechanical pump, when vacuum degree reaches 3.0 × 10-1After Pa, diffusion is opened
Pump is until vacuum is extracted into 6.0 × 10-3Pa closes diffusion pump, is then charged with the argon gas that 0.05MPa purity is 99.999%, this
When quartz ampoule inside and outside differential pressure be 0.05MPa, unlatching get rid of the copper wheel that cooling circulating water is connected in carrying device cavity, set the line of copper wheel
Speed is 40 m/s;Induction heating power and setting electric current value are opened, current value starts to be set as 3A, and 12A is set as after 5S, sees
When examining that master alloy color is changed into brilliant white by kermesinus in quartz ampoule, determine that the master alloy in quartz ampoule is completely melt at this time,
The master alloy being completely melt is ejected on the high-speed rotating copper wheel for being connected with cooling circulating water using quartz ampoule inside and outside differential pressure, from
And prepare amorphous thin ribbon;Since the thermal expansion coefficient difference of quartz ampoule and master alloy is larger, induced current start setting it is smaller,
It avoids master alloy and quartz ampoule from damaging quartz ampoule due to adding thermogenetic deflection to have big difference, becomes when color occurs for master alloy
When change will melt, high current to 12A accelerates the burn-off rate of master alloy, and heating time too long iron-based soft magnetic mother is avoided to close
The Partial Elements of gold cause the amorphous ribbon performance prepared bad with quartzy tube reaction;In addition, the small blocky iron in quartz ampoule
Base soft magnetism master alloy avoids excessive, otherwise quartz ampoule is easy to cause to rupture during heating;The injection of liquid after alloy melting
Time avoid it is too long because this to will lead to overheat or burning loss of alloy serious and composition tolerances occur.
Embodiment 5
A kind of iron base amorphous magnetically-soft alloy, alloy expression formula are Fe78.9Si9.2B10.8Cu1C0.1, it is denoted as H-5;As more detailed
Example, its preparation method include the following steps:
(1) ingredient: choose content be 99.9wt% Fe, content be 99.99wt% Si, B content be 17.40wt% FeB, C contain
The FeC that amount the is 3.5 wt% and Cu that content is 99.99wt%, carries out ingredient according to above-mentioned alloy expression formula;Weighing raw material
Before, by sand paper or abrasive machine polishing raw material, the oxide layer on surface is removed, puts Fe, Cu raw material after polishing
Enter to fill in the beaker of dehydrated alcohol, and use ultrasonic cleaning 240S, further removes oxide debris, the oil of material surface
The impurity such as dirt, are then dried using hair dryer;
(2) melting: will weigh and the raw material handled well is put into silica crucible, in order to reduce the burning of fusion process chinese raw materials
Damage, density is big and low-melting alloying component is placed on the upper surface of metalloid and volatile metal, the original placed in silica crucible
Material sequence is followed successively by Cu, Fe, Si, FeB and FeC from top to bottom;The silica crucible for filling raw material is put into vacuum induction melting furnace
In the induction coil of cavity, fire door is closed, is vacuumized first using mechanical pump, when vacuum degree reaches 6.0 × 10-1After Pa, close
It closes mechanical pump and opens diffusion pump up to vacuum degree to 6.0 × 10-3Pa, the purity for being then charged with 0.05 MPa is 99.999%
Argon gas is as protective gas;Opening induction heating power and adjusting electric current is that 2A carries out preheating material, electric current is rapid after 1 min
It is added to 8A and carries out melting, electric current is down to 4A after alloy melts completely, carries out more uniform melting, it is cold after melting
But diffusion pump closes power supply;
(3) prepare amorphous thin ribbon: the master alloy that melting is finished is crushed frustillatum, and 7 g master alloys of clamping are put into bottom and are provided with
In the quartz ampoule of 0.5 mm circular hole;Quartz ampoule is put into vacuum to get rid of in the induction coil with machine, adjustment quartz ampoule height is up to it
At 1 mm right above copper wheel;It is vacuumized first using mechanical pump, when vacuum degree reaches 6.0 × 10-1After Pa, diffusion is opened
Pump is until vacuum is extracted into 6.0 × 10-3Pa closes diffusion pump, is then charged with the argon gas that 0.05MPa purity is 99.999%, this
When quartz ampoule inside and outside differential pressure be 0.05MPa, unlatching get rid of the copper wheel that cooling circulating water is connected in carrying device cavity, set the line of copper wheel
Speed is 40 m/s;Induction heating power and setting electric current value are opened, current value starts to be set as 3A, and 12A is set as after 5S, sees
When examining that master alloy color is changed into brilliant white by kermesinus in quartz ampoule, determine that the master alloy in quartz ampoule is completely melt at this time,
The master alloy being completely melt is ejected on the high-speed rotating copper wheel for being connected with cooling circulating water using quartz ampoule inside and outside differential pressure, from
And prepare amorphous thin ribbon;Since the thermal expansion coefficient difference of quartz ampoule and master alloy is larger, induced current start setting it is smaller,
It avoids master alloy and quartz ampoule from damaging quartz ampoule due to adding thermogenetic deflection to have big difference, becomes when color occurs for master alloy
When change will melt, high current to 12A accelerates the burn-off rate of master alloy, and heating time too long iron-based soft magnetic mother is avoided to close
The Partial Elements of gold cause the amorphous ribbon performance prepared bad with quartzy tube reaction;In addition, the small blocky iron in quartz ampoule
Base soft magnetism master alloy avoids excessive, otherwise quartz ampoule is easy to cause to rupture during heating;The injection of liquid after alloy melting
Time avoid it is too long because this to will lead to overheat or burning loss of alloy serious and composition tolerances occur.
Embodiment 6
A kind of iron base amorphous magnetically-soft alloy, alloy expression formula are Fe78.7Si9.2B10.8Cu1C0.3, it is denoted as H-6;As more detailed
Example, its preparation method include the following steps:
(1) ingredient: choose content be 99.9wt% Fe, content be 99.99wt% Si, B content be 17.40wt% FeB, C contain
The FeC that amount the is 3.5 wt% and Cu that content is 99.99wt%, carries out ingredient according to above-mentioned alloy expression formula;Weighing raw material
Before, by sand paper or abrasive machine polishing raw material, the oxide layer on surface is removed, puts Fe, Cu raw material after polishing
Enter to fill in the beaker of dehydrated alcohol, and use ultrasonic cleaning 240S, further removes oxide debris, the oil of material surface
The impurity such as dirt, are then dried using hair dryer;
(2) melting: will weigh and the raw material handled well is put into silica crucible, in order to reduce the burning of fusion process chinese raw materials
Damage, density is big and low-melting alloying component is placed on the upper surface of metalloid and volatile metal, the original placed in silica crucible
Material sequence is followed successively by Cu, Fe, Si, FeB and FeC from top to bottom;The silica crucible for filling raw material is put into vacuum induction melting furnace
In the induction coil of cavity, fire door is closed, is vacuumized first using mechanical pump, when vacuum degree reaches 5.0 × 10-1After Pa, close
It closes mechanical pump and opens diffusion pump up to vacuum degree to 6.0 × 10-3Pa, the purity for being then charged with 0.05 MPa is 99.999%
Argon gas is as protective gas;Opening induction heating power and adjusting electric current is that 2A carries out preheating material, electric current is rapid after 1 min
It is added to 8A and carries out melting, electric current is down to 4A after alloy melts completely, carries out more uniform melting, it is cold after melting
But diffusion pump closes power supply;
(3) prepare amorphous thin ribbon: the master alloy that melting is finished is crushed frustillatum, and 7 g master alloys of clamping are put into bottom and are provided with
In the quartz ampoule of 0.5 mm circular hole;Quartz ampoule is put into vacuum to get rid of in the induction coil with machine, adjustment quartz ampoule height is up to it
At 1 mm right above copper wheel;It is vacuumized first using mechanical pump, when vacuum degree reaches 5.0 × 10-1After Pa, diffusion is opened
Pump is until vacuum is extracted into 6.0 × 10-3Pa closes diffusion pump, is then charged with the argon gas that 0.05MPa purity is 99.999%, this
When quartz ampoule inside and outside differential pressure be 0.05MPa, unlatching get rid of the copper wheel that cooling circulating water is connected in carrying device cavity, set the line of copper wheel
Speed is 40 m/s;Induction heating power and setting electric current value are opened, current value starts to be set as 3A, and 12A is set as after 5S, sees
When examining that master alloy color is changed into brilliant white by kermesinus in quartz ampoule, determine that the master alloy in quartz ampoule is completely melt at this time,
The master alloy being completely melt is ejected on the high-speed rotating copper wheel for being connected with cooling circulating water using quartz ampoule inside and outside differential pressure, from
And prepare amorphous thin ribbon;Since the thermal expansion coefficient difference of quartz ampoule and master alloy is larger, induced current start setting it is smaller,
It avoids master alloy and quartz ampoule from damaging quartz ampoule due to adding thermogenetic deflection to have big difference, becomes when color occurs for master alloy
When change will melt, high current to 12A accelerates the burn-off rate of master alloy, and heating time too long iron-based soft magnetic mother is avoided to close
The Partial Elements of gold cause the amorphous ribbon performance prepared bad with quartzy tube reaction;In addition, the small blocky iron in quartz ampoule
Base soft magnetism master alloy avoids excessive, otherwise quartz ampoule is easy to cause to rupture during heating;The injection of liquid after alloy melting
Time avoid it is too long because this to will lead to overheat or burning loss of alloy serious and composition tolerances occur.
Embodiment 7
A kind of iron base amorphous magnetically-soft alloy, alloy expression formula are Fe78.3Si9.2B10.8Cu1C0.7, it is denoted as H-7;As more detailed
Example, its preparation method include the following steps:
(1) ingredient: choose content be 99.9wt% Fe, content be 99.99wt% Si, B content be 17.40wt% FeB, C contain
The FeC that amount the is 3.5 wt% and Cu that content is 99.99wt%, carries out ingredient according to above-mentioned alloy expression formula;Weighing raw material
Before, by sand paper or abrasive machine polishing raw material, the oxide layer on surface is removed, puts Fe, Cu raw material after polishing
Enter to fill in the beaker of dehydrated alcohol, and use ultrasonic cleaning 240S, further removes oxide debris, the oil of material surface
The impurity such as dirt, are then dried using hair dryer;
(2) melting: will weigh and the raw material handled well is put into silica crucible, in order to reduce the burning of fusion process chinese raw materials
Damage, density is big and low-melting alloying component is placed on the upper surface of metalloid and volatile metal, the original placed in silica crucible
Material sequence is followed successively by Cu, Fe, Si, FeB and FeC from top to bottom;The silica crucible for filling raw material is put into vacuum induction melting furnace
In the induction coil of cavity, fire door is closed, is vacuumized first using mechanical pump, when vacuum degree reaches 4.0 × 10-1After Pa, close
It closes mechanical pump and opens diffusion pump up to vacuum degree to 6.0 × 10-3Pa, the purity for being then charged with 0.05 MPa is 99.999%
Argon gas is as protective gas;Opening induction heating power and adjusting electric current is that 2A carries out preheating material, electric current is rapid after 1 min
It is added to 8A and carries out melting, electric current is down to 4A after alloy melts completely, carries out more uniform melting, it is cold after melting
But diffusion pump closes power supply;
(3) prepare amorphous thin ribbon: the master alloy that melting is finished is crushed frustillatum, and 7 g master alloys of clamping are put into bottom and are provided with
In the quartz ampoule of 0.5 mm circular hole;Quartz ampoule is put into vacuum to get rid of in the induction coil with machine, adjustment quartz ampoule height is up to it
At 1 mm right above copper wheel;It is vacuumized first using mechanical pump, when vacuum degree reaches 4.0 × 10-1After Pa, diffusion is opened
Pump is until vacuum is extracted into 6.0 × 10-3Pa closes diffusion pump, is then charged with the argon gas that 0.05MPa purity is 99.999%, this
When quartz ampoule inside and outside differential pressure be 0.05MPa, unlatching get rid of the copper wheel that cooling circulating water is connected in carrying device cavity, set the line of copper wheel
Speed is 40 m/s;Induction heating power and setting electric current value are opened, current value starts to be set as 3A, and 12A is set as after 5S, sees
When examining that master alloy color is changed into brilliant white by kermesinus in quartz ampoule, determine that the master alloy in quartz ampoule is completely melt at this time,
The master alloy being completely melt is ejected on the high-speed rotating copper wheel for being connected with cooling circulating water using quartz ampoule inside and outside differential pressure, from
And prepare amorphous thin ribbon;Since the thermal expansion coefficient difference of quartz ampoule and master alloy is larger, induced current start setting it is smaller,
It avoids master alloy and quartz ampoule from damaging quartz ampoule due to adding thermogenetic deflection to have big difference, becomes when color occurs for master alloy
When change will melt, high current to 12A accelerates the burn-off rate of master alloy, and heating time too long iron-based soft magnetic mother is avoided to close
The Partial Elements of gold cause the amorphous ribbon performance prepared bad with quartzy tube reaction;In addition, the small blocky iron in quartz ampoule
Base soft magnetism master alloy avoids excessive, otherwise quartz ampoule is easy to cause to rupture during heating;The injection of liquid after alloy melting
Time avoid it is too long because this to will lead to overheat or burning loss of alloy serious and composition tolerances occur.
Embodiment 8
A kind of iron base amorphous magnetically-soft alloy, alloy expression formula are Fe78Si9.2B10.8Cu1C1, it is denoted as H-8;As showing in more detail
Example, its preparation method include the following steps:
(1) ingredient: choose content be 99.9wt% Fe, content be 99.99wt% Si, B content be 17.40wt% FeB, C contain
The FeC that amount the is 3.5 wt% and Cu that content is 99.99wt%, carries out ingredient according to above-mentioned alloy expression formula;Weighing raw material
Before, by sand paper or abrasive machine polishing raw material, the oxide layer on surface is removed, puts Fe, Cu raw material after polishing
Enter to fill in the beaker of dehydrated alcohol, and use ultrasonic cleaning 240S, further removes oxide debris, the oil of material surface
The impurity such as dirt, are then dried using hair dryer;
(2) melting: will weigh and the raw material handled well is put into silica crucible, in order to reduce the burning of fusion process chinese raw materials
Damage, density is big and low-melting alloying component is placed on the upper surface of metalloid and volatile metal, the original placed in silica crucible
Material sequence is followed successively by Cu, Fe, Si, FeB and FeC from top to bottom;The silica crucible for filling raw material is put into vacuum induction melting furnace
In the induction coil of cavity, fire door is closed, is vacuumized first using mechanical pump, when vacuum degree reaches 3.0 × 10-1After Pa, close
It closes mechanical pump and opens diffusion pump up to vacuum degree to 6.0 × 10-3Pa, the purity for being then charged with 0.05 MPa is 99.999%
Argon gas is as protective gas;Opening induction heating power and adjusting electric current is that 2A carries out preheating material, electric current is rapid after 1 min
It is added to 8A and carries out melting, electric current is down to 4A after alloy melts completely, carries out more uniform melting, it is cold after melting
But diffusion pump closes power supply;
(3) prepare amorphous thin ribbon: the master alloy that melting is finished is crushed frustillatum, and 7 g master alloys of clamping are put into bottom and are provided with
In the quartz ampoule of 0.5 mm circular hole;Quartz ampoule is put into vacuum to get rid of in the induction coil with machine, adjustment quartz ampoule height is up to it
At 1 mm right above copper wheel;It is vacuumized first using mechanical pump, when vacuum degree reaches 3.0 × 10-1After Pa, diffusion is opened
Pump is until vacuum is extracted into 6.0 × 10-3Pa closes diffusion pump, is then charged with the argon gas that 0.05MPa purity is 99.999%, this
When quartz ampoule inside and outside differential pressure be 0.05MPa, unlatching get rid of the copper wheel that cooling circulating water is connected in carrying device cavity, set the line of copper wheel
Speed is 40 m/s;Induction heating power and setting electric current value are opened, current value starts to be set as 3A, and 12A is set as after 5S, sees
When examining that master alloy color is changed into brilliant white by kermesinus in quartz ampoule, determine that the master alloy in quartz ampoule is completely melt at this time,
The master alloy being completely melt is ejected on the high-speed rotating copper wheel for being connected with cooling circulating water using quartz ampoule inside and outside differential pressure, from
And prepare amorphous thin ribbon;Since the thermal expansion coefficient difference of quartz ampoule and master alloy is larger, induced current start setting it is smaller,
It avoids master alloy and quartz ampoule from damaging quartz ampoule due to adding thermogenetic deflection to have big difference, becomes when color occurs for master alloy
When change will melt, high current to 12A accelerates the burn-off rate of master alloy, and heating time too long iron-based soft magnetic mother is avoided to close
The Partial Elements of gold cause the amorphous ribbon performance prepared bad with quartzy tube reaction;In addition, the small blocky iron in quartz ampoule
Base soft magnetism master alloy avoids excessive, otherwise quartz ampoule is easy to cause to rupture during heating;The injection of liquid after alloy melting
Time avoid it is too long because this to will lead to overheat or burning loss of alloy serious and composition tolerances occur.
Comparative example 1
A kind of iron base amorphous magnetically-soft alloy, alloy expression formula are Fe78.5Si9.2B10.8Cu1C0.5, it is denoted as D.As showing in more detail
Example, its preparation method include the following steps:
(1) ingredient: choose content be 99.9wt% Fe, content be 99.99wt% Si, B content be 17.40wt% FeB, C contain
The FeC that amount the is 3.5 wt% and Cu that content is 99.99wt%, carries out ingredient according to above-mentioned alloy expression formula;Weighing raw material
Before, by sand paper or abrasive machine polishing raw material, the oxide layer on surface is removed, puts Fe, Cu raw material after polishing
Enter to fill in the beaker of dehydrated alcohol, and use ultrasonic cleaning 240S, further removes oxide debris, the oil of material surface
The impurity such as dirt, are then dried using hair dryer;
(2) melting: will weigh and the raw material handled well is put into silica crucible, in order to reduce the burning of fusion process chinese raw materials
Damage, density is big and low-melting alloying component is placed on the upper surface of metalloid and volatile metal, the original placed in silica crucible
Material sequence is followed successively by Cu, Fe, Si, FeB and FeC from top to bottom;The silica crucible for filling raw material is put into vacuum induction melting furnace
In the induction coil of cavity, fire door is closed, is vacuumized first using mechanical pump, when vacuum degree reaches 6.0 × 10-1After Pa, close
It closes mechanical pump and opens diffusion pump up to vacuum degree to 6.0 × 10-3Pa, the purity for being then charged with 0.05 MPa is 99.999%
Argon gas is as protective gas;Opening induction heating power and adjusting electric current is that 2A carries out preheating material, electric current is rapid after 1 min
It is added to 8A and carries out melting, electric current is down to 4A after alloy melts completely, carries out more uniform melting, it is cold after melting
But diffusion pump closes power supply;
(3) prepare amorphous thin ribbon: the master alloy that melting is finished is crushed frustillatum, and 7 g master alloys of clamping are put into bottom and are provided with
In the quartz ampoule of 0.5 mm circular hole;Quartz ampoule is put into vacuum to get rid of in the induction coil with machine, adjustment quartz ampoule height is up to it
At 1 mm right above copper wheel;It is vacuumized first using mechanical pump, when vacuum degree reaches 6.0 × 10-1After Pa, opens and expand
Pump is dissipated until vacuum is extracted into 6.0 × 10-3Pa closes diffusion pump, is then charged with the argon gas that 0.05MPa purity is 99.999%,
Quartz ampoule inside and outside differential pressure is 0.05MPa at this time, and unlatching gets rid of the copper wheel for being connected with cooling circulating water in carrying device cavity, sets copper wheel
Linear velocity is 40 m/s;Induction heating power and setting electric current value are opened, current value starts to be set as 3A, it is set as 12A after 5S,
When master alloy color is changed into brilliant white by kermesinus in observation quartz ampoule, determine that the master alloy in quartz ampoule is completely molten at this time
Change, the master alloy being completely melt is ejected into the high-speed rotating copper wheel for being connected with cooling circulating water using quartz ampoule inside and outside differential pressure
On, to prepare amorphous thin ribbon;Since the thermal expansion coefficient difference of quartz ampoule and master alloy is larger, induced current starts to set
It is smaller, avoid master alloy and quartz ampoule from damaging quartz ampoule due to adding thermogenetic deflection to have big difference, when master alloy occurs
When color change will melt, high current to 12A accelerates the burn-off rate of master alloy, avoids heating time too long iron-based soft
The Partial Elements of magnetic master alloy cause the amorphous ribbon performance prepared bad with quartzy tube reaction;In addition, small in quartz ampoule
Blocky iron-based soft magnetic master alloy avoids excessive, otherwise quartz ampoule is easy to cause to rupture during heating;Liquid after alloy melting
Injecting time avoid it is too long because this to will lead to overheat or burning loss of alloy serious and composition tolerances occur.
The Properties Testing of iron base amorphous magnetically-soft alloy band in Examples 1 to 8 and comparative example 1:
Iron-base soft magnetic alloy strip in above-described embodiment 1~8 and comparative example is respectively adhered on after alcohol washes and drying
Glass slide on, be put into instrument model be Ultima IV XRD equipment in tested.Using Cu palladium and K ɑ ray, model is scanned
Enclosing is 20 ° to 90 °, and scanning speed is 4 °/min.Using the exotherm of differential scanning calorimetry (DSC) measurement sample, made
Instrument model is NETZSCH STA, and heating rate is 20 K/min.By testing to obtain iron base amorphous magnetically-soft alloy above
XRD and DSC curve, XRD curve as shown in Figure 1, its DSC curve as shown in Fig. 2, XRD in above-described embodiment as seen from Figure 1
Only it is 45 ° or so in the angle of diffraction in map and a roomy diffraction maximum occurs, illustrates that iron base amorphous magnetically-soft alloy is amorphous
State, this shows that the iron base amorphous magnetically-soft alloy has good amorphous formation ability.As shown in Figure 2, alloy is brilliant in embodiment
Changing temperature is 420~470 DEG C, and alloy crystallization temperature is higher in embodiment, and it is good to show that iron base amorphous magnetically-soft alloy of the present invention has
Good thermal stability.
The iron base amorphous magnetically-soft alloy band prepared in Examples 1 to 8 and comparative example 1 is fitted into quartz ampoule, is carried out
It vacuumizes, when vacuum degree is 2.0 × 10-3 When Pa, it is put into batch-type furnace and carries out stress relief annealing process, annealing temperature
100 DEG C before one crystallization peak temperature, 10 min of soaking time.After the completion of annealing, the vibration sample of model 7410 is used
The saturation induction density of iron base amorphous magnetically-soft alloy band after product magnetometer (VSM) measurement annealing, before in addition needing test to anneal
Iron base amorphous magnetically-soft alloy band saturation induction density to make comparisons.Fig. 3 is iron-based in section Example and comparative example 1
VSM enlarged drawing before amorphous soft-magnetic alloy annealing, as seen from Figure 3, the saturation magnetic before iron base amorphous magnetically-soft alloy annealing in figure
Saturation magnetic flux density is not much different after induction is annealed with 1K101, and the 1K101 saturation magnetic flux density after annealing is
1.56T.Fig. 4 is the magnetic saturation variation diagram in Examples 1 to 8 and comparative example 1 before iron base amorphous magnetically-soft alloy annealing, by Fig. 4
As it can be seen that a certain amount of copper and carbon can be improved its magnetic saturation, but it will lead to the deterioration of soft magnet performance when copper and higher carbon content.
Use Effective permeability of the impedance analyzer test annealed sample of model 4294A under different impressed frequenciesμ e, Fig. 5 is real
Apply Effective permeability figure of the iron base amorphous magnetically-soft alloy under different impressed frequencies in example and comparative example 1, as seen from Figure 5, this hair
Bright iron base amorphous magnetically-soft alloy shows preferable stability when frequency is 1k -10k Hz, and its Effective permeability is obviously high
In the Effective permeability of comparative example.Fig. 6 is the magnetic conductivity variation of iron base amorphous magnetically-soft alloy in section Example and comparative example 1
Figure, as seen from Figure 6, although as the increase of copper content, reduced trend is presented in magnetic conductivity, but is added in the present invention suitable
Carbon improves the magnetic conductivity of alloy, when in addition C content is 0.3 in the embodiment of the present invention, magnetic conductivity highest.Use model
The coercivity of annealed sample is measured for the DC hysteresis loops measuring instrument of BHS-40H c, Fig. 7 is the iron in embodiment and comparative example 1
The coercivity variation diagram of base amorphous soft-magnetic alloy, as seen from Figure 7, iron base amorphous magnetically-soft alloy coercivity is minimum in above-described embodiment
Only 5.7Am-1, coercivity is lower, and hysteresis loop is longer and narrower, and the area surrounded is smaller, and magnetic hystersis loss is smaller.Fig. 8 is real
The magnetically saturated comparison diagram in iron base amorphous magnetically-soft alloy annealing front and back in example 7 and embodiment 8 is applied, although knowing that part is iron-based in conjunction with Fig. 3
Magnetic saturation is lower before amorphous soft-magnetic alloy is annealed, and saturation magnetic flux density differs after magnetic saturation is annealed with industrial 1 K 101
Less, but their saturation magnetic flux density is substantially better than 1K101 amorphous ribbon after annealing.Due to iron-based non-in the present invention
Brilliant magnetically soft alloy contains Cu element, and Cu element provides nucleation mass point for α-Fe in annealing process, therefore can in annealing process
To improve its saturation magnetic flux density.
The comprehensive performance of iron base amorphous magnetically-soft alloy is as shown in table 1 below in Examples 1 to 8 and comparative example 1, is known by table 1, to the greatest extent
The coercivity of iron base amorphous magnetically-soft alloy is lower in pipe comparative example 1, but its magnetic conductivity is significantly lower than iron-based non-in embodiment
Brilliant magnetically soft alloy.Fe in embodiment 379Si9.34B10.96Cu0.7The magnetic conductivity of alloy is apparently higher than the magnetic conductance of alloy in comparative example
Rate, and coercivity is lower.Fe in embodiment 678.7Si9.2B10.8Cu1C0.3The magnetic conductivity of alloy is higher, and comprehensive magnetic can be excellent
It is different.
The comprehensive performance table of the iron base amorphous magnetically-soft alloy of the permanent magnetic conductivity of table 1
Comparative example 2
A kind of iron base amorphous magnetically-soft alloy, alloy expression formula are Fe87.5Si1.78B9..24P0.95Cu0.53, it is denoted as d.As more detailed
Example, its preparation method includes the following steps:
(1) ingredient: choose content be 99.9wt% Fe, content be 99.99wt% Si, B content be 17.40wt% FeB, C contain
Amount is the FeP of the Cu and 24.98wt% of FeC, 99.99wt% of 3.5 wt%, carries out ingredient according to above-mentioned alloy expression formula;Claiming
Before taking raw material, by sand paper or abrasive machine polishing raw material, the oxide layer on surface is removed, by Fe, Cu after polishing
Raw material are put into the beaker for filling dehydrated alcohol, and use ultrasonic cleaning 240S, further remove the oxidation of material surface
The impurity such as object clast, greasy dirt, are then dried using hair dryer;
(2) melting: will weigh and the raw material handled well is put into silica crucible, in order to reduce the burning of fusion process chinese raw materials
Damage, density is big and low-melting alloying component is placed on the upper surface of metalloid and volatile metal, the original placed in silica crucible
Material sequence is followed successively by Cu, Fe, Si, FeB, FeC and FeP from top to bottom;The silica crucible for filling raw material is put into vacuum induction to melt
In the induction coil of furnace cavity, fire door is closed, is vacuumized first using mechanical pump, when vacuum degree reaches 6.0 × 10-1Pa it
Afterwards, it closes mechanical pump and opens diffusion pump up to vacuum degree to 6.0 × 10-3Pa, the purity for being then charged with 0.05 MPa are
99.999% argon gas is as protective gas;Opening induction heating power and adjusting electric current is that 2A carries out preheating material, will after 45S
Electric current is added rapidly to 8A and carries out melting, and electric current is down to 4A after alloy melts completely, carries out more uniform melting, melting
After cooling diffusion pump, close power supply;
(3) prepare amorphous thin ribbon: the master alloy that melting is finished is crushed frustillatum, and 7 g master alloys of clamping are put into bottom and are provided with
In the quartz ampoule of 0.5 mm circular hole;Quartz ampoule is put into vacuum to get rid of in the induction coil with machine, adjustment quartz ampoule height is up to it
At 1 mm right above copper wheel;It is vacuumized first using mechanical pump, when vacuum degree reaches 6.0 × 10-1After Pa, opens and expand
Pump is dissipated until vacuum is extracted into 6.0 × 10-3Pa closes diffusion pump, is then charged with the argon gas that 0.05MPa purity is 99.999%,
Quartz ampoule inside and outside differential pressure is 0.05MPa at this time, and unlatching gets rid of the copper wheel for being connected with cooling circulating water in carrying device cavity, sets copper wheel
Linear velocity is 40 m/s;Induction heating power and setting electric current value are opened, current value starts to be set as 3A, it is set as 12A after 5S,
When master alloy color is changed into brilliant white by kermesinus in observation quartz ampoule, determine that the master alloy in quartz ampoule is completely molten at this time
Change, the master alloy being completely melt is ejected into the high-speed rotating copper wheel for being connected with cooling circulating water using quartz ampoule inside and outside differential pressure
On, to prepare amorphous thin ribbon;Since the thermal expansion coefficient difference of quartz ampoule and master alloy is larger, induced current starts to set
It is smaller, avoid master alloy and quartz ampoule from damaging quartz ampoule due to adding thermogenetic deflection to have big difference, when master alloy occurs
When color change will melt, high current to 12A accelerates the burn-off rate of master alloy, avoids heating time too long iron-based soft
The Partial Elements of magnetic master alloy cause the amorphous ribbon performance prepared bad with quartzy tube reaction;In addition, small in quartz ampoule
Blocky iron-based soft magnetic master alloy avoids excessive, otherwise quartz ampoule is easy to cause to rupture during heating;Liquid after alloy melting
Injecting time avoid it is too long because this to will lead to overheat or burning loss of alloy serious and composition tolerances occur.
Also according to above-mentioned test method, iron base amorphous magnetically-soft alloy Fe in comparative example 287.5Si1.78B9..24P0.95Cu0.53
XRD curve as shown in figure 9, its DSC curve is as shown in Figure 10, iron base amorphous magnetically-soft alloy in comparative example 2 as seen from Figure 9
Only it is 45 ° or so in the angle of diffraction in XRD spectrum and a roomy diffraction maximum occurs, illustrates that the iron base amorphous magnetically-soft alloy is
Amorphous state.As shown in Figure 10, alloy crystallization temperature is 400 DEG C or so in comparative example 2, and alloy crystallization temperature is in embodiment
420~470 DEG C, iron base amorphous magnetically-soft alloy alloy crystallization temperature is higher in embodiment, shows that the Fe-based amorphous soft magnetism of the present invention closes
Fitting has good thermal stability.
Figure 11 is the VSM figure after the iron base amorphous magnetically-soft alloy annealing in comparative example 2, and magnetic saturation is about 1.6T, is lower than
1.64 T of magnetic saturation of iron base amorphous magnetically-soft alloy in the embodiment of the present invention 7.In addition to this, Volatile Elements P is contained in alloy,
It is be easy to cause fusion process ingredient scaling loss, when iron content is higher than 83 at%, the amorphous formation ability decline of alloy, with comparison
Example is compared, and the amorphous formation ability of iron base amorphous magnetically-soft alloy of the present invention is strong, and tapability is excellent.
In conclusion iron base amorphous magnetically-soft alloy saturation induction density with higher of the present inventionB s, it is higher effectively
Magnetic conductivityμ eWith lower coercivityH c.Iron base amorphous magnetically-soft alloy of the present invention its synthesis soft magnet performance after annealing is obviously excellent
In the iron-based amorphous ribbon of 1K101 series of current industrial production, and high-cost ferromagnetic element is not contained, without using
High pure raw material, lower production costs, AMORPHOUS ALLOY RIBBONS good moldability, preparation process is simple, is very beneficial for industrialized production
With application.
What has been described above is only a preferred embodiment of the present invention, it is noted that for those skilled in the art,
Without depart from that overall concept of the invention, several changes and improvements can also be made, these also should be considered as of the invention
Protection scope.
Claims (8)
1. a kind of iron base amorphous magnetically-soft alloy, which is characterized in that its alloy expression formula is FeaSibBcCudCe, alloy expression formula
Middle a, b, c, d and e respectively indicate the atom percentage content of each component, and meet the following conditions: a is that 76~81, b is 8~11,
It is 0 ~ 1.5, e is 0~1.5, a+b+c+d+e=100 that c, which is 9~13, d,.
2. iron base amorphous magnetically-soft alloy according to claim 1, which is characterized in that in the alloy expression formula a be 77~
80, b be 9~10, c be 9~12, d be 0 ~ 1.4, e be 0~1.4.
3. iron base amorphous magnetically-soft alloy according to claim 1, which is characterized in that in the alloy expression formula a be 78~
79, b be 9~10, c be 10~11, d be 0 ~ 1.3, e be 0~1.3.
4. iron base amorphous magnetically-soft alloy according to claim 1, which is characterized in that a is 79, b in the alloy expression formula
For 9.522, c 11.178, d 0.3, e 0.
5. iron base amorphous magnetically-soft alloy according to claim 1, which is characterized in that a is 79, b in the alloy expression formula
For 9.43, c 11.07, d 0.5, e 0.
6. iron base amorphous magnetically-soft alloy according to claim 1, which is characterized in that a is 78.7 in the alloy expression formula,
B is 9.2, c 10.8, d 1, e 0.3.
7. iron base amorphous magnetically-soft alloy according to claim 1, which is characterized in that a is 78, b in the alloy expression formula
For 9.2, c 10.8, d 1, e 1.
8. iron base amorphous magnetically-soft alloy according to claim 1 is applied to transformer, saturable reactor or filter inductor.
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Application publication date: 20190514 |