CN109599239A - It is a kind of perseverance magnetic conductivity iron base amorphous magnetically-soft alloy and application - Google Patents
It is a kind of perseverance magnetic conductivity iron base amorphous magnetically-soft alloy and application Download PDFInfo
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- CN109599239A CN109599239A CN201811512283.2A CN201811512283A CN109599239A CN 109599239 A CN109599239 A CN 109599239A CN 201811512283 A CN201811512283 A CN 201811512283A CN 109599239 A CN109599239 A CN 109599239A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/153—Amorphous metallic alloys, e.g. glassy metals
- H01F1/15308—Amorphous metallic alloys, e.g. glassy metals based on Fe/Ni
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
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- H01F1/15341—Preparation processes therefor
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Abstract
The present invention relates to a kind of iron base amorphous magnetically-soft alloy of permanent magnetic conductivity and application, the iron base amorphous magnetically-soft alloy alloy expression formula of the perseverance magnetic conductivity is FeaSibBcPdCueCof, a, b, c, d, e and f respectively indicate the atom percentage content of each corresponding component in alloy expression formula, and meet the following conditions: it be 2~6, c be 9~14, d be 0 ~ 2, e be 0~1.3, f is 0~5, a+b+c+d+e+f=100 that a, which is 78~86, b,；The iron base amorphous magnetically-soft alloy of the perseverance magnetic conductivity is applied to prepare distribution transformer, pulse transformer, magnetic amplifier, intermediate-frequency transformer or inverter iron core；Permanent magnetic conductivity iron base amorphous magnetically-soft alloy of the invention has high saturation induction density, high Effective permeability, low coercivity, low core loss, it has high frequency stability simultaneously, application of the amorphous soft-magnetic alloy under high frequency condition is widened, and good moldability, preparation process condition are loose, low production cost.
Description
Technical field
The invention belongs to amorphous alloy technical fields, and in particular to it is a kind of perseverance magnetic conductivity iron base amorphous magnetically-soft alloy and answer
With.
Background technique
Non-crystalline material has the distinguishing feature of green energy conservation, and lower, magnetic loss is lost with excellent soft magnet performance in it
The 1/5 ~ 1/3 of silicon steel is just corresponded to, but compared with traditional silicon steel, there are still deficiency, the magnetic saturation intensity of silicon steel is up to 2T, and allusion quotation
The amorphous alloy Fe of type78Si9B13Magnetic saturation intensity Bs be only 1.56T.Currently, many researchers attempt to improve Fe-based amorphous
The magnetic saturation intensity of magnetically soft alloy, high saturation magnetic flux density amorphous alloy component design are all based on greatly: (1) improving ferro element and contain
Amount reduces non-ferromagnetic amorphous into constituent content；(2) add cobalt element in right amount, using its between iron atom between strong friendship
It changes coupling and improves magnetic induction intensity；(3) large atomic radius for avoiding largely addition that amorphous formation ability can be improved is non magnetic
Otherwise metallic element will be substantially reduced the magnetic induction intensity of alloy, and greatly improve the cost of raw material of alloy.Wherein most typically
Example be Metglas2605Co alloy that saturation induction density is 1.8T, but include 18% Co atom, valence in the alloy
Lattice are expensive, may not apply to industrialization magnetic product.In addition, FeSiB amorphous alloy magnetic conductivity is more with frequency raising reduction, because
It is used below that this FeSiB amorphous alloy is more limited to 10kHz.
Fe is disclosed in the patent of authorization Publication No. CN104802042A53.83Co23.07Cu0.6Nb2.5Si11B9With
Fe67Co18Si11B4Amorphous alloy carries out surface physics polishing to the scope of freedom of amorphous soft magnetic ribbon, through physics polish with
Its initial permeability in 1kHz-1MHz frequency range of amorphous soft magnetic ribbon afterwards obviously increases substantially, but to amorphous
Alloy surface carries out physics polishing and increases process flow, and its magnetic conductivity is not sufficiently stable at high frequencies.
It is disclosed in the patent of authorization Publication No. CN104862619A a kind of with high initial magnetoconductivity and high-quality
The composite amorphous magnetically soft alloy of factor, ingredient Fe69.21Co7.69Cu0.6Nb2.5Si11B9-Ni71P29, need to prepare first non-
Then brilliant soft magnetic alloy sheet-band prepares chemical nickel phosphorus plating plating solution and prepares composite amorphous magnetically soft alloy using chemical deposition, can
The superior composite alloy of high frequency performance is obtained, because preparation process need to increase work to amorphous alloy chemical deposition nickel-plated phosphor
Skill complexity, and increased production cost, will also result in industrial pollution.
It is disclosed in the granted patent of Publication No. CN106834930A a kind of simultaneous with the high impurity of high magnetic flux density
The iron-base nanometer crystal alloy of capacitive, alloy expression formula are as follows: FeaSibBcPdCeCufMg, wherein M is the impurity or not in raw material
The trace additives of alloy property are substantially change, but strip surface could be inhibited with the oxygen content in atmosphere by adjusting system
It is more difficult to prepare amorphous ribbon for crystallization.
It is disclosed in the granted patent of Publication No. CN104021910A a kind of for high frequency condition and with high initial
The magnetically soft alloy of magnetic conductivity, is made of Fe, Co, Cu, Nb, Si and B, each component mass percent are as follows: Fe15.38%,
Cu0.6%, Nb2.5%, Si11%, B9%, surplus Co.Its high frequency performance is excellent, but Co too high levels, increases industry
Cost is not suitable for industrialized production.
It is Fe that a kind of alloy expression formula is disclosed in the granted patent of Publication No. CN101206943AaBbCcSidAle's
Alloy system, a, b, c, d and e respectively indicate the atom percentage content of each corresponding component in alloy expression formula, and wherein a is 77 ~ 83,
It is 3 ~ 6, d be 4 ~ 7, e is 1 ~ 4 that b, which is 7 ~ 13, c, and saturation induction density can achieve 1.380 ~ 1.760T, but its C content compared with
Height, and more a height of 3555 DEG C of the fusing point of C, cause plurality of raw materials to be difficult to complete alloying in fusion process, considerably increases molten
It is smelt this, and the control of its best C content is difficult to realize in the industrial production.
It is higher that Nippon Steel company discloses a kind of iron content in the granted patent of Publication No. CN1356403A
Fe-Si-B-C-P amorphous alloy, iron content is between 82 ~ 90%, and magnetic induction intensity reaches 1.75T, but it excessively pursues magnetic strength
Intensity is answered, the limitation of amorphous formation ability is ignored, design of alloy is unreasonable, and amorphous formation ability is limited, conventional fast quenching
Method cannot prepare complete amorphous sample.The said firm also discloses in the patent that grant number is CN101589169A a kind of low
Iron content Fe-Si-B-C-P amorphous alloy, the iron content of alloy is between 78 ~ 86%, however the P content of the alloy 6 ~ 20% is obvious
Reduce the magnetic induction intensity of alloy.In addition, excessively high P and C content greatly improves the melting difficulty and system band work of alloy
Skill requirement.
In addition, Japan Patent JP 2008248380 discloses a kind of FeSiBP alloy containing Al, core loss value is in 0.1W/
Kg hereinafter, but Al is oxidizable element, when content is high, be difficult to prepare under air.And its P content is excessively high, P content be 8 ~
20%.Studies have shown that such as Si, B, P, C and Ge in common metal element, low-alloyed saturation induction density drops in P element
Most it is preceding be it is obvious, the saturation induction density of alloy is lower when P content is excessively high.
Currently, AND ENERGY RESOURCES CONSUMPTION IN CHINA and environmental pollution is serious, and steel industry excess capacity, it is excellent that design obtains comprehensive performance
Different, low in cost, energy-saving and environment-friendly new iron-based amorphous soft-magnetic alloy has great importance.It is strong wherein to obtain saturation induction
Degree is higher, and preferably new iron-based amorphous soft-magnetic alloy is particularly important with high-frequency stabilization performance.
Summary of the invention
Poor, magnetic conductivity stability difference problem that the invention solves traditional iron base amorphous magnetically-soft alloy comprehensive performances is
It solves the above problems, the present invention provides a kind of iron base amorphous magnetically-soft alloy of permanent magnetic conductivity, it has high and stablizes effective
Magnetic conductivityμ e, low coercivityH c, high saturation induction densityB s, and its good moldability, preparation process condition are loose, production
It is low in cost.
The object of the present invention is achieved in the following manner:
A kind of iron base amorphous magnetically-soft alloy of perseverance magnetic conductivity, its alloy expression formula is FeaSibBcPdCueCof, alloy expression formula
Middle a, b, c, d, e and f respectively indicate the atom percentage content of each corresponding component, and meet the following conditions: a is that 78~86, b is
It is 0 ~ 2, e be 0~1.3, f is 0~5, a+b+c+d+e+f=100 that 2~6, c, which are 9~14, d,.
The iron base amorphous magnetically-soft alloy of perseverance magnetic conductivity as described above, it is 2~5, c that a, which is 79~85, b, in alloy expression formula
It is 0 ~ 1.5, e for 10~13, d be 0~1.2, f is 0~5.
The iron base amorphous magnetically-soft alloy of perseverance magnetic conductivity as described above, it is 2~3, c that a, which is 81~84, b, in alloy expression formula
It is 0 ~ 1.3, e for 11~13, d be 0~0.8, f is 0~4.
As example:
A is 83.50, b 2.35, c 12.20, d 1.25, e 0.7, f 0 in alloy expression formula.
A is 82.66, b 2.33, c 12.08, d 1.24, e 0.69, f 1 in alloy expression formula.
A is 81.83, b 2.30, c 11.96, d 1.22, e 0.69, f 2 in alloy expression formula.
A is 81.00, b 2.38, c 11.83, d 1.21, e 0.68, f 3 in alloy expression formula.
The application of the iron base amorphous magnetically-soft alloy of perseverance magnetic conductivity as described above, is applied to prepare distribution transformer, arteries and veins
Rush transformer, magnetic amplifier, intermediate-frequency transformer or inverter iron core.
The atom percentage content of Fe ensure that the amorphous formation of ferrous alloy in 78 ~ 85% ranges in alloy of the present invention
Ability and high saturation induction density Bs.
P element is greater than Si and B for effect of the FeSiBP alloy on amorphous phase is formed, but P content is excessively high, can reduce
The saturation induction density of alloy.The additive amount of P element is relatively reasonable in the perseverance magnetic conductivity Fe-based amorphous alloy, ensure that amorphous
The formation and high saturation induction density of alloy.
The appropriate formation added with conducive to Fe base amorphous that the preferred scope of Si is 2~6%, Si in alloy of the present invention, together
When, movement of the electronics in Fe base amorphous alloy can be hindered, the resistivity of alloy is improved, thus reduction eddy-current loss can be played
Effect.
B and Fe member are known as biggish atomic radius difference, also correspond to have large atomic radius difference on well in three principles
It is required that being conducive to the decrystallized of Fe based alloy.When B content is lower than 5%, the thermal stability of amorphous soft magnetic material is deteriorated, and content exists
9% or more, the amorphous formation ability and stability of alloy can be significantly improved, but when B content is higher than 18%, content is again
Increase is decrystallized on alloy almost without influence, therefore the preferred scope of B content is 9~14% in the present invention.
Cu element can promote forming core in alloy of the present invention, but its effect is with the difference of the microstructure in state band of quenching
And there is significant difference.In the present invention, design of alloy selects low content of Cu, guarantees the amorphous formation energy that alloy is not greatly reduced
Power.
Appropriate addition cobalt element, using its between iron atom between strongly exchange coupled effect improve magnetic induction intensity, this
The preferred scope of Co content is 0~5% in invention.
In conjunction with above-mentioned, present invention significant advantage compared with existing similar technique is embodied in:
1. containing to raising Fe base amorphous soft-magnetic alloy comprehensive performance advantageous element P, Cu and Co in present component.
2. alloying component of the present invention has (Fe, M)80(Si, B)20Composition characteristic is conducive to the formation of alloy amorphous state.
3. alloying component of the present invention, which can use industrial pure material, melts purification method acquisition amorphous state by glass bag
Alloy, substitution use high pure raw material, reduce production cost.
4. alloy strip of the present invention obtains stablizing promotion, magnetic conductance by the addition of micro Co, magnetic saturation and soft magnet performance
Rate is smaller with impressed frequency variation, other opposite amorphous alloy magnetic conductivities are constant, and micro Co addition can guarantee production cost
Magnetic property is greatly improved while not high.
5. Fe of the present invention81.83Si2.30B11.96P1.22Cu0.69Co2The higher reachable 1.70T of amorphous soft-magnetic alloy magnetic saturation intensity.
Iron base amorphous magnetically-soft alloy of the present invention has excellent comprehensive performance, has high saturation induction densityB s, it is high
And constant Effective permeabilityμ e, with high frequency stability, low coercivityH cWith good amorphous formation ability, be conducive to work
The production application of industry.
Detailed description of the invention
Fig. 1 is the XRD diagram of iron base amorphous magnetically-soft alloy in Examples 1 to 5；Abscissa is scanning angle, ordinate in figure
For intensity；
Fig. 2 is the DSC figure of iron base amorphous magnetically-soft alloy in Examples 1 to 5；Abscissa is temperature in figure, and ordinate is thermal discharge；
Fig. 3 is the VSM partial enlarged view of iron base amorphous magnetically-soft alloy in Examples 1 to 5；Abscissa is magnetic field strength in figure, is indulged
Coordinate is the intensity of magnetization；
Fig. 4 is the magnetic conductivity figure under different impressed frequencies of iron base amorphous magnetically-soft alloy in Examples 1 to 5；Abscissa in figure
For frequency, ordinate is Effective permeability；
Fig. 5 is the magnetic conductivity Local map under different impressed frequencies of iron base amorphous magnetically-soft alloy in Examples 1 to 5；It is horizontal in figure
Coordinate is frequency, and ordinate is Effective permeability；
Fig. 6 is that the coercive of iron base amorphous magnetically-soft alloy in Examples 1 to 5 is tried hard to；Abscissa is magnetic field strength in figure, and ordinate is
The intensity of magnetization；
Fig. 7 is the VSM figure of iron base amorphous magnetically-soft alloy in comparative example；Abscissa is magnetic field strength in figure, and ordinate is that magnetization is strong
Degree；
Fig. 8 is the magnetic conductivity figure under different impressed frequencies of iron base amorphous magnetically-soft alloy in comparative example；Abscissa is frequency in figure
Rate, ordinate are Effective permeability；
Fig. 9 is that the coercive of iron base amorphous magnetically-soft alloy in comparative example is tried hard to；Abscissa is magnetic field strength in figure, and ordinate is magnetization
Intensity.
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 of perseverance magnetic conductivity, alloy expression formula is Fe83.25Si2.37B12.23P1.45Cu0.7, it is denoted as X1；
As more detailed example, its preparation method includes the following steps:
(1) ingredient: choose purity be 99.9wt% Fe, purity be 99.99wt% Si, B content be 17.40wt% FeB, P contain
The Cu that amount is the FeP of 24.98 wt%, purity is 99.99wt% carries out ingredient according to above-mentioned alloy expression formula；Weighing raw material
Before, the sand paper such as oxidation film above raw material or abrasive machine polishing removal, after the raw material such as Fe, Cu be put into fill nothing
In the beaker of water-ethanol, ultrasonic cleaning 250S is carried out, is then completely dried with hair dryer；
(2) master alloy melting: by prepared master alloy raw material and B203Raw material is put into silica crucible, and density is big and fusing point is low
Alloying component be placed on above, silica crucible is put into the induction coil in vacuum induction founding cavity, seal vacuum induction
Smelting-casting equipment is simultaneously vacuumized with mechanical pump and diffusion pump, when vacuum degree reaches 3.0 × 10-3 The purity of 0.05 MPa is filled with after Pa
For 99.999% argon gas, as protective gas；Opening induction heating power and adjusting electric current is 8A, carries out the melting of master alloy, female
Heated current is reduced after alloy melting and reduces ingredient scaling loss, is carried out wrapping molten purified treatment, is closed power supply after melting；
(3) fast quenching is at band: the master alloy after melting being crushed frustillatum, clamping 6g master alloy is put into bottom and opens round-meshed stone
Ying Guanzhong, the diameter of circular hole are 0.6mm；Quartz ampoule is put into the induction coil of fast melt-quenching equipment cavity, quartz ampoule is in copper
Right above wheel at 1 mm height；Induction fast melt-quenching equipment cavity is evacuated to 6.0 × 10-3Pa vacuum degree is filled after backward cavity is interior
The argon gas that the purity of 0.05MPa is 99.999%, opens the copper wheel that cooling circulating water is connected in equipment cavity, and copper wheel linear velocity is
32m/s；Induction heating power and setting electric current value are opened, current value starts to be set as 3A, and 12A, observation quartz are set as after 5S
When master alloy color is changed into brilliant white by kermesinus in pipe, determine that the master alloy in quartz ampoule is completely melt, utilizes stone 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 by English pipe inside and outside differential pressure, to prepare
Amorphous thin ribbon out；Since the thermal expansion coefficient difference of quartz ampoule and master alloy is larger, induced current start setting it is smaller, avoid mother
Alloy and quartz ampoule damage quartz ampoule due to adding thermogenetic deflection to have big difference, when color change occurs for master alloy will
When fusing, high current to 12A accelerates the burn-off rate of master alloy, avoids the part member of heating time too long soft magnetism master alloy
Element causes the amorphous thin ribbon performance prepared bad with quartzy tube reaction.
Embodiment 2
A kind of iron base amorphous magnetically-soft alloy of perseverance magnetic conductivity, alloy expression formula is Fe83.50Si2.35B12.20P1.25Cu0.7, it is denoted as X2；
As more detailed example, its preparation method includes the following steps:
(1) ingredient: choose purity be 99.9wt% Fe, purity be 99.99wt% Si, B content be 17.40wt% FeB, P contain
The Cu that amount is the FeP of 24.98 wt%, purity is 99.99wt% carries out ingredient according to above-mentioned alloy expression formula；Weighing raw material
Before, the sand paper such as oxidation film above raw material or abrasive machine polishing removal, after the raw material such as Fe, Cu be put into fill nothing
In the beaker of water-ethanol, ultrasonic cleaning 250S is carried out, is then completely dried with hair dryer；
(2) master alloy melting: by prepared master alloy raw material and B203Raw material is put into silica crucible, and density is big and fusing point is low
Alloying component be placed on above, silica crucible is put into the induction coil in vacuum induction founding cavity, seal vacuum induction
Smelting-casting equipment is simultaneously vacuumized with mechanical pump and diffusion pump, when vacuum degree reaches 3.0 × 10-3 The purity of 0.05 MPa is filled with after Pa
For 99.999% argon gas, as protective gas；Opening induction heating power and adjusting electric current is 9A, carries out the melting of master alloy, female
Heated current is reduced after alloy melting and reduces ingredient scaling loss, is carried out wrapping molten purified treatment, is closed power supply after melting；
(3) fast quenching is at band: the master alloy after melting being crushed frustillatum, clamping 6g master alloy is put into bottom and opens round-meshed stone
Ying Guanzhong, the diameter of circular hole are 0.6mm；Quartz ampoule is put into the induction coil of fast melt-quenching equipment cavity, quartz ampoule is in copper
Right above wheel at 1 mm height；Induction fast melt-quenching equipment cavity is evacuated to 5.0 × 10-3Pa vacuum degree is filled after backward cavity is interior
The argon gas that the purity of 0.05MPa is 99.999%, opens the copper wheel that cooling circulating water is connected in equipment cavity, and copper wheel linear velocity is
32m/s；Induction heating power and setting electric current value are opened, current value starts to be set as 5A, and 13A, observation quartz are set as after 5S
When master alloy color is changed into brilliant white by kermesinus in pipe, determine that the master alloy in quartz ampoule is completely melt, utilizes stone 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 by English pipe inside and outside differential pressure, to prepare
Amorphous thin ribbon out；Since the thermal expansion coefficient difference of quartz ampoule and master alloy is larger, induced current start setting it is smaller, avoid mother
Alloy and quartz ampoule damage quartz ampoule due to adding thermogenetic deflection to have big difference, when color change occurs for master alloy will
When fusing, high current to 13A accelerates the burn-off rate of master alloy, avoids the part member of heating time too long soft magnetism master alloy
Element causes the amorphous thin ribbon performance prepared bad with quartzy tube reaction.
Embodiment 3
A kind of iron base amorphous magnetically-soft alloy of perseverance magnetic conductivity, alloy expression formula is Fe82.66Si2.33B12.08P1.24Cu0.69Co1, note
Make X3；As more detailed example, its preparation method includes the following steps:
(1) ingredient: choose purity be 99.9wt% Fe, purity be 99.99wt% Si, B content be 17.40wt% FeB, P contain
The Co that amount is the FeP of 24.98 wt%, purity is 99.99wt% Cu, purity are 99.99wt%, according to above-mentioned alloy expression formula into
Row ingredient；Before weighing raw material, the sand paper such as oxidation film above raw material or abrasive machine polishing removal, after by Fe,
The raw material such as Cu, Co are put into the beaker for filling dehydrated alcohol, carry out ultrasonic cleaning 250S, then with hair dryer that it is complete
It is dry；
(2) master alloy melting: by prepared master alloy raw material and B203Raw material is put into silica crucible, and density is big and fusing point is low
Alloying component be placed on above, silica crucible is put into the induction coil in vacuum induction founding cavity, seal vacuum induction
Smelting-casting equipment is simultaneously vacuumized with mechanical pump and diffusion pump, when vacuum degree reaches 3.0 × 10-3 The purity of 0.05 MPa is filled with after Pa
For 99.999% argon gas, as protective gas；Opening induction heating power and adjusting electric current is 8A, carries out the melting of master alloy, female
Heated current is reduced after alloy melting and reduces ingredient scaling loss, is carried out wrapping molten purified treatment, is closed power supply after melting；
(3) fast quenching is at band: the master alloy after melting being crushed frustillatum, clamping 7g master alloy is put into bottom and opens round-meshed stone
Ying Guanzhong, the diameter of circular hole are 0.6mm；Quartz ampoule is put into the induction coil of fast melt-quenching equipment cavity, quartz ampoule is in copper
Right above wheel at 1 mm height；Induction fast melt-quenching equipment cavity is evacuated to 6.0 × 10-3Pa vacuum degree is filled after backward cavity is interior
The argon gas that the purity of 0.05MPa is 99.999%, opens the copper wheel that cooling circulating water is connected in equipment cavity, and copper wheel linear velocity is
31m/s；Induction heating power and setting electric current value are opened, current value starts to be set as 5A, and 13A, observation quartz are set as after 5S
When master alloy color is changed into brilliant white by kermesinus in pipe, determine that the master alloy in quartz ampoule is completely melt, utilizes stone 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 by English pipe inside and outside differential pressure, to prepare
Amorphous thin ribbon out；Since the thermal expansion coefficient difference of quartz ampoule and master alloy is larger, induced current start setting it is smaller, avoid mother
Alloy and quartz ampoule damage quartz ampoule due to adding thermogenetic deflection to have big difference, when color change occurs for master alloy will
When fusing, high current to 13A accelerates the burn-off rate of master alloy, avoids the part member of heating time too long soft magnetism master alloy
Element causes the amorphous thin ribbon performance prepared bad with quartzy tube reaction.
Embodiment 4
A kind of iron base amorphous magnetically-soft alloy of perseverance magnetic conductivity, alloy expression formula is Fe81.83Si2.30B11.96P1.22Cu0.69Co2, note
Make X4；As more detailed example, its preparation method includes the following steps:
(1) ingredient: choose purity be 99.9wt% Fe, purity be 99.99wt% Si, B content be 17.40wt% FeB, P contain
The Co that amount is the FeP of 24.98 wt%, purity is 99.99wt% Cu, purity are 99.99wt%, according to above-mentioned alloy expression formula into
Row ingredient；Before weighing raw material, the sand paper such as oxidation film above raw material or abrasive machine polishing removal, after by Fe,
The raw material such as Cu, Co are put into the beaker for filling dehydrated alcohol, carry out ultrasonic cleaning 250S, then with hair dryer that it is complete
It is dry；
(2) master alloy melting: by prepared master alloy raw material and B203Raw material is put into silica crucible, and density is big and fusing point is low
Alloying component be placed on above, silica crucible is put into the induction coil in vacuum induction founding cavity, seal vacuum induction
Smelting-casting equipment is simultaneously vacuumized with mechanical pump and diffusion pump, when vacuum degree reaches 3.0 × 10-3 The purity of 0.05 MPa is filled with after Pa
For 99.999% argon gas, as protective gas；Opening induction heating power and adjusting electric current is 8A, carries out the melting of master alloy, female
Heated current is reduced after alloy melting and reduces ingredient scaling loss, is carried out wrapping molten purified treatment, is closed power supply after melting；
(3) fast quenching is at band: the master alloy after melting being crushed frustillatum, clamping 7g master alloy is put into bottom and opens round-meshed stone
Ying Guanzhong, the diameter of circular hole are 0.6mm；Quartz ampoule is put into the induction coil of fast melt-quenching equipment cavity, quartz ampoule is in copper
Right above wheel at 1 mm height；Induction fast melt-quenching equipment cavity is evacuated to 6.0 × 10-3Pa vacuum degree is filled after backward cavity is interior
The argon gas that the purity of 0.05MPa is 99.999%, opens the copper wheel that cooling circulating water is connected in equipment cavity, and copper wheel linear velocity is
32m/s；Induction heating power and setting electric current value are opened, current value starts to be set as 3A, and 11A, observation quartz are set as after 5S
When master alloy color is changed into brilliant white by kermesinus in pipe, determine that the master alloy in quartz ampoule is completely melt, utilizes stone 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 by English pipe inside and outside differential pressure, to prepare
Amorphous thin ribbon out；Since the thermal expansion coefficient difference of quartz ampoule and master alloy is larger, induced current start setting it is smaller, avoid mother
Alloy and quartz ampoule damage quartz ampoule due to adding thermogenetic deflection to have big difference, when color change occurs for master alloy will
When fusing, high current to 12A accelerates the burn-off rate of master alloy, avoids the part member of heating time too long soft magnetism master alloy
Element causes the amorphous thin ribbon performance prepared bad with quartzy tube reaction.
Embodiment 5
A kind of iron base amorphous magnetically-soft alloy of perseverance magnetic conductivity, alloy expression formula is Fe81.00Si2.38B11.83P1.21Cu0.68Co3, note
Make X5；As more detailed example, its preparation method includes the following steps:
(1) ingredient: choose purity be 99.9wt% Fe, purity be 99.99wt% Si, B content be 17.40wt% FeB, P contain
The Co that amount is the FeP of 24.98 wt%, purity is 99.99wt% Cu, purity are 99.99wt%, according to above-mentioned alloy expression formula into
Row ingredient；Before weighing raw material, the sand paper such as oxidation film above raw material or abrasive machine polishing removal, after by Fe,
The raw material such as Cu, Co are put into the beaker for filling dehydrated alcohol, carry out ultrasonic cleaning 240S, then with hair dryer that it is complete
It is dry；
(2) master alloy melting: by prepared master alloy raw material and B203Raw material is put into silica crucible, and density is big and fusing point is low
Alloying component be placed on above, silica crucible is put into the induction coil in vacuum induction founding cavity, seal vacuum induction
Smelting-casting equipment is simultaneously vacuumized with mechanical pump and diffusion pump, when vacuum degree reaches 3.0 × 10-3 The purity of 0.05 MPa is filled with after Pa
For 99.999% argon gas, as protective gas；Opening induction heating power and adjusting electric current is 8A, carries out the melting of master alloy, female
Heated current is reduced after alloy melting and reduces ingredient scaling loss, carries out wrapping molten purified treatment, melting terminates to close power supply；
(3) fast quenching is at band: the master alloy after melting being crushed frustillatum, clamping 6g master alloy is put into bottom and opens round-meshed stone
Ying Guanzhong, the diameter of circular hole are 0.6mm；Quartz ampoule is put into the induction coil of fast melt-quenching equipment cavity, quartz ampoule is in copper
Right above wheel at 1 mm height；Induction fast melt-quenching equipment cavity is evacuated to 5.0 × 10-3Pa vacuum degree is filled after backward cavity is interior
The argon gas that the purity of 0.05MPa is 99.999%, opens the copper wheel that cooling circulating water is connected in equipment cavity, and copper wheel linear velocity is
32m/s；Induction heating power and setting electric current value are opened, current value starts to be set as 3A, and 12A, observation quartz are set as after 5S
When master alloy color is changed into brilliant white by kermesinus in pipe, determine that the master alloy in quartz ampoule is completely melt, utilizes stone 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 by English pipe inside and outside differential pressure, to prepare
Amorphous thin ribbon out；Since the thermal expansion coefficient difference of quartz ampoule and master alloy is larger, induced current start setting it is smaller, avoid mother
Alloy and quartz ampoule damage quartz ampoule due to adding thermogenetic deflection to have big difference, when color change occurs for master alloy will
When fusing, high current to 12A accelerates the burn-off rate of master alloy, avoids the part member of heating time too long soft magnetism master alloy
Element causes the amorphous thin ribbon performance prepared bad with quartzy tube reaction.
The Properties Testing of the iron base amorphous magnetically-soft alloy strip of permanent magnetic conductivity:
Iron-base soft magnetic alloy strip in above-described embodiment 1~5 is respectively adhered on smooth, free of contamination glass slide, is put into
It is tested in XRD test equipment.It is Ultima IV that XRD, which tests used instrument model, using Cu palladium and K ɑ ray, scanning
Range is 30 ° to 80 °, and scanning speed is 8 °/min.The initial crystallization temperature of sample is measured using differential scanning calorimetry (DSC)
Tx, used device model are NETZSCH STA, and heating rate is 20 DEG C/min.The above test can obtain permanent magnetic conductivity
The XRD and DSC curve of iron base amorphous magnetically-soft alloy, XRD curve are shown in that Fig. 1, DSC curve are shown in Fig. 2, as seen from Figure 1 above-mentioned reality
Applying ferrous alloy in example is amorphous state, this shows that the iron base amorphous magnetically-soft alloy of the perseverance magnetic conductivity has good amorphous formation
Ability and mobility.As shown in Figure 2, crystallization temperature is higher up to 418 DEG C, which has good thermostabilization
Property.
The iron-based non-crystalline magnetically soft alloy prepared in Examples 1 to 5 is fitted into quartz ampoule, and is vacuumized, to true
Reciprocal of duty cycle is 2.0 × 10-3Tube sealing processing is carried out when Pa, after carry out stress relief annealing in batch-type furnace, annealing temperature is lower than crystallization
100 DEG C of temperature, soaking time 10min.The vibrating specimen magnetometer (VSM) of model 7410 is used to survey after the completion of stress relief annealing
Determine the saturation induction density Bs of annealed sample.Fig. 3 is the VSM partial enlargement of iron base amorphous magnetically-soft alloy in Examples 1 to 5
Figure, as seen from Figure 3, the saturation induction density Bs of iron base amorphous magnetically-soft alloy is 1.62~1.7T, magnetic in Examples 1 to 5
Saturation is substantially better than 1K101 amorphous ribbon, and umber of turn is reduced in the higher operating point that iron core can be improved of magnetic saturation, and copper is used in saving
Or with aluminum amount, reduces small product size, reduces cost.Existed with the impedance analyzer measurement stress relief annealing sample of model 4294A
Effective permeability μ e, Fig. 4 under the extrinsic motivated magnetic field of different frequency are iron base amorphous magnetically-soft alloy in Examples 1 to 5 not
With the magnetic conductivity figure under impressed frequency, Fig. 5 is magnetic conductance of the iron base amorphous magnetically-soft alloy under 1 ~ 20kHz frequency in Examples 1 to 5
Rate figure, by Fig. 4 and Fig. 5 as it can be seen that the peak of iron base amorphous magnetically-soft alloy magnetic conductivity is up to 8500.16 in above-described embodiment, magnetic
Conductance is very high, and alloy its magnetic conductivity for furthermore adding Co element is kept constant under 1 ~ 101kHz frequency, and it is in high-frequency
Under still have good magnetic property.The high frequency that the addition of Co element of the present invention improves iron base amorphous magnetically-soft alloy magnetic conductivity is steady
It is qualitative.Using the coercivity H of the DC hysteresis loops measuring instrument measurement annealed sample of model BHS-40, Fig. 6 is embodiment 1
The coercive of iron base amorphous magnetically-soft alloy is tried hard in~5, and as seen from Figure 6, new iron-based amorphous soft-magnetic alloy is rectified in above-described embodiment
Minimum stupid power is only 1.708Am-1, coercivity is lower, and coercivity is lower, and hysteresis loop is longer and narrower, and the area surrounded is got over
Small, magnetic hystersis loss is smaller.
The comprehensive performance of iron base amorphous magnetically-soft alloy is as shown in table 1 below in Examples 1 to 5.
The comprehensive performance table of the iron base amorphous magnetically-soft alloy of the permanent magnetic conductivity of table 1
In conclusion the iron base amorphous magnetically-soft alloy of the perseverance magnetic conductivity has high saturation induction density Bs, high effective magnetic
Conductance μ e, high frequency stability, low coercivity H, low core loss and good lamination coefficient etc. integrate soft magnet performance
It is substantially better than the iron-based amorphous ribbon of 1K101 series of current industrial production, and cost is relatively low, preparation process is simple.
Comparative example
A kind of iron base amorphous magnetically-soft alloy, alloy expression formula are Fe83.08Si2.34B12.14P1.24Cu0.70Nb0.5, it is denoted as D-1.As
More detailed example, its preparation method include the following steps:
(1) ingredient: choose purity be 99.9wt% Fe, purity be 99.99wt% Si, B content be 17.40wt% FeB, P contain
The Nb that amount is the FeP of 24.98 wt%, purity is 99.99wt% Cu, purity are 99.99wt%, according to above-mentioned alloy expression formula into
Row ingredient；Before weighing raw material, the sand paper such as oxidation film above raw material or abrasive machine polishing removal, after by Fe,
The raw material such as Cu, Nb are put into the beaker for filling dehydrated alcohol, carry out ultrasonic cleaning 240S, then with hair dryer that it is complete
It is dry；
(2) master alloy melting: by prepared master alloy raw material and B203Raw material is put into silica crucible, and density is big and fusing point is low
Alloying component be placed on above, silica crucible is put into the induction coil in vacuum induction founding cavity, seal vacuum induction
Smelting-casting equipment is simultaneously vacuumized with mechanical pump and diffusion pump, when vacuum degree reaches 3.0 × 10-3 The purity of 0.05 MPa is filled with after Pa
For 99.999% argon gas, as protective gas；Opening induction heating power and adjusting electric current is 8A, carries out the melting of master alloy, female
Heated current is reduced after alloy melting and reduces ingredient scaling loss, carries out wrapping molten purified treatment, melting terminates to close power supply；
(3) fast quenching is at band: the master alloy after melting being crushed frustillatum, clamping 6g master alloy is put into bottom and opens round-meshed stone
Ying Guanzhong, the diameter of circular hole are 0.6mm；Quartz ampoule is put into the induction coil of fast melt-quenching equipment cavity, quartz ampoule is in copper
Right above wheel at 1 mm height；Induction fast melt-quenching equipment cavity is evacuated to 5.0 × 10-3Pa vacuum degree is filled after backward cavity is interior
The argon gas that the purity of 0.05MPa is 99.999%, opens the copper wheel that cooling circulating water is connected in equipment cavity, and copper wheel linear velocity is
32m/s；Induction heating power and setting electric current value are opened, current value starts to be set as 3A, and 12A, observation quartz are set as after 5S
When master alloy color is changed into brilliant white by kermesinus in pipe, determine that the master alloy in quartz ampoule is completely melt, utilizes stone 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 by English pipe inside and outside differential pressure, to prepare
Amorphous thin ribbon out；Since the thermal expansion coefficient difference of quartz ampoule and master alloy is larger, induced current start setting it is smaller, avoid mother
Alloy and quartz ampoule damage quartz ampoule due to adding thermogenetic deflection to have big difference, when color change occurs for master alloy will
When fusing, high current to 12A accelerates the burn-off rate of master alloy, avoids the part member of heating time too long soft magnetism master alloy
Element causes the amorphous thin ribbon performance prepared bad with quartzy tube reaction.
Fe in comparative example83.08Si2.34B12.14P1.24Cu0.70Nb0.5The performance test of iron base amorphous magnetically-soft alloy strip with point
Analysis:
The iron-based non-crystalline magnetically soft alloy prepared in comparative example is fitted into quartz ampoule, and is vacuumized, is 2.0 to vacuum degree
×10-3Tube sealing processing is carried out when Pa, after carry out stress relief annealing in batch-type furnace, annealing temperature be lower than 100 DEG C of crystallization temperature,
Crystallization temperature is 432 DEG C, soaking time 10min.The vibrating specimen magnetometer of model 7410 is used after the completion of stress relief annealing
(VSM) the saturation induction density Bs of annealed sample is measured.Fig. 7 is the VSM figure of iron base amorphous magnetically-soft alloy in comparative example, by scheming
7 as it can be seen that the saturation induction density Bs of iron base amorphous magnetically-soft alloy is 1.58T in comparative example, and magnetic saturation is significantly lower than implementation
Iron base amorphous magnetically-soft alloy band in example.Fig. 8 is magnetic conductance of the iron base amorphous magnetically-soft alloy under different impressed frequencies in comparative example
Rate figure will be as seen from Figure 8 6332.60 in the magnetic conductivity that the magnetic conductivity of 1kHz is 8770.55,10kHz, magnetic conductivity with
Frequency, which increases, to be significantly reduced, and does not have high frequency stability.Fig. 9 is that the coercive of iron base amorphous magnetically-soft alloy in comparative example is tried hard to,
As seen from Figure 9, the more a height of 3.432Am of the coercivity of iron base amorphous magnetically-soft alloy-1, magnetic hystersis loss is larger.
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 of perseverance magnetic conductivity, which is characterized in that its alloy expression formula is
FeaSibBcPdCueCof, a, b, c, d, e and f respectively indicate the atom percentage content of each corresponding component in alloy expression formula, and
Meet the following conditions: a be 78~86, b be 2~6, c be 9~14, d be 0 ~ 2, e be 0~1.3, f be 0~5, a+b+c+d+e+f=
100。
2. the iron base amorphous magnetically-soft alloy of perseverance magnetic conductivity according to claim 1, which is characterized in that the alloy expression formula
It is 2~5, c be 10~13, d be 0 ~ 1.5, e be 0~1.2, f is 0~5 that middle a, which is 79~85, b,.
3. the iron base amorphous magnetically-soft alloy of perseverance magnetic conductivity according to claim 1, which is characterized in that the alloy expression formula
It is 2~3, c be 11~13, d be 0 ~ 1.3, e be 0~0.8, f is 0~4 that middle a, which is 81~84, b,.
4. the iron base amorphous magnetically-soft alloy of perseverance magnetic conductivity according to claim 1, which is characterized in that the alloy expression formula
Middle a is 83.50, b 2.35, c 12.20, d 1.25, e 0.7, f 0.
5. the iron base amorphous magnetically-soft alloy of perseverance magnetic conductivity according to claim 1, which is characterized in that the alloy expression formula
Middle a is 82.66, b 2.33, c 12.08, d 1.24, e 0.69, f 1.
6. the iron base amorphous magnetically-soft alloy of perseverance magnetic conductivity according to claim 1, which is characterized in that the alloy expression formula
Middle a is 81.83, b 2.30, c 11.96, d 1.22, e 0.69, f 2.
7. the iron base amorphous magnetically-soft alloy of perseverance magnetic conductivity according to claim 1, which is characterized in that the alloy expression formula
Middle a is 81.00, b 2.38, c 11.83, d 1.21, e 0.68, f 3.
8. the iron base amorphous magnetically-soft alloy of perseverance magnetic conductivity according to claim 1 is applied to prepare distribution transformer, pulse
Transformer, magnetic amplifier, intermediate-frequency transformer or inverter iron core.
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