CN108396263A - A kind of iron base amorphous magnetically-soft alloy and its preparation method and application with high saturated magnetic induction - Google Patents
A kind of iron base amorphous magnetically-soft alloy and its preparation method and application with high saturated magnetic induction Download PDFInfo
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- CN108396263A CN108396263A CN201810122242.6A CN201810122242A CN108396263A CN 108396263 A CN108396263 A CN 108396263A CN 201810122242 A CN201810122242 A CN 201810122242A CN 108396263 A CN108396263 A CN 108396263A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/02—Amorphous alloys with iron as the major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/003—Making ferrous alloys making amorphous alloys
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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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Abstract
The invention discloses a kind of iron base amorphous magnetically-soft alloy and its preparation method and application with high saturated magnetic induction.The expression formula of the alloy is FeaSibBcGad, a, b, c and d indicate the atom percentage content of each corresponding component respectively in the expression formula, and it be 7.2~8.6, c be 10.5~12.5, d is 1~4, a+b+c+d=100 that wherein a, which is 78, b,.The alloy adds certain Ga elements that can improve non-crystaline amorphous metal magnetic saturation intensity in Fe Si B systems non-crystaline amorphous metal, makes it have high saturation induction density, low coercivity, high magnetic conductivity, and preparation process condition is loose, good moldability.
Description
Technical field
The invention belongs to non-crystaline amorphous metal technical fields, and in particular to a kind of iron-based with high saturated magnetic induction is non-
Brilliant magnetically soft alloy and its preparation method and application.
Background technology
After Fe-based amorphous-crystalline state nanometer soft magnetic materials comes out, due to the special atomic structure (long-range of amorphous alloy
Unordered, shortrange order) many performances for being better than crystalline material are made it have, such as high saturated magnetic induction, high magnetic permeability, low
Coercivity, low core loss, low excitation current and good stability, and moulding process is simple, does not have to special processing work
Skill, be widely used in distribution transformer, intermediate frequency power supply transformer, filter reactor, saturable reactor, motor stator and
In the power electronic devices such as Magnetic Sensor, Just because of this, the development of Fe-based amorphous-crystalline state nanometer soft magnetic materials also promotes
Development of the whole world transformer towards green environmental protection and energy saving direction.
Although Fe-based amorphous soft magnetic materials has many excellent physical and chemical properties, but with it is widely used at present
Silicon steel sheet is compared to there are still following shortcomings：(1) compared with silicon steel sheet (2.03T) there is very big difference in saturation induction density
Away from if the trade mark of the Fe-based amorphous alloy in current industrialized production is mainly Metglas2605SA1, ingredient Fe80Si9B11
(at%), BSOnly 1.56T (referring to Chinese patent CN101840764A), limits the amorphous transformer of industrialized production
To small quantization, lightweight, the development of energy-saving；(2) magnetic conductivity is not high, and magnetic conductivity with working frequency increase exponentially
Decline, high frequency stability is poor, causes the electronic device under high-frequency work that cannot be widely applied, and high initial permeability can
To effectively reduce soft magnetic materials additional exciting current and exciting power in use, to reduce materials'use
Loss in the process；Based on this, the researcher of various countries improves the soft magnetism of FeSiB systems amorphous alloy strips by various methods
Performance and corrosion resisting property, such as the various alloying elements of Co, Ni, Mo, Cr, Cu, Mo are added into FeSiB, wherein having plenty of individually
Addition has plenty of joint addition.Iron base amorphous magnetically-soft alloy used in transformer core can be summarized as following several at present
Class：1. FeSiB systems (referring to Chinese patent CN101840764A)；2. FeSiBAl systems are (referring to Chinese patent CN103915231A
And CN101206943A)；3. FeSiBC systems (referring to Chinese patent CN1721563A and CN101840764A)；；④
FeSiPCAl systems (referring to Chinese patent CN101589169A) 5. FeSiBPC systems (referring to Japan Patent JP57185957A)；⑥
FeSiBCrM systems (referring to Chinese patent CN102509603A) etc..
Alloy system is 1.：Saturation induction density only has 1.56T, limits transformer and develops to lightweight, energy-saving.
Alloy system is 2.：Chinese patent literature CN103915231A is certain by being added in Fe-Si-B based amorphous alloys
It measures Al and forms FeaSibBcAldIt is amorphous-nano-crystalline state magnetically soft alloy, wherein a is 78~86at%, and b is 2~9at%, c
For 9~14at%, d is 1~5at%, the alloy after stress relief annealing, saturation induction density up to 1.62~
1.778T.It is Fe that a kind of expression formula is described in Chinese patent literature CN101206943AaBbSicAldCeAlloy system, according to
Atomic percentage, wherein a be 77~83at%, b be 7~13at%, c be 1~4at%, d be 3~6at%, e be 4~
7at%, saturation induction density can reach 1.380~1.760T；However the addition of C (3555 DEG C of fusing point) element is molten
It is difficult to alloying during refining, considerably increases melting cost.
Alloy system is 3.：It is Fe that Chinese patent CN1721563A, which discloses a kind of expression formula,aSibBcCdAlloy system, wherein a
It is≤12at% for 76~83.5at%, b, c is 8-~18at%, and d is 0.01~3at%.Its saturation induction density exists
1.55~1.69T, but C is to blow CO and CO by being relied in molten bath bottom2What the form of gas was added, then utilize oxygen
Change reduction reaction and displaces a certain amount of C.Its production technology is excessively complicated, and C content is difficult to control, for industrial production
Technological parameter controllability is relatively low.
Alloy system is 4.：Chinese patent CN101589169 describes a kind of Fe containing 78~86at%, 6~20at%'s
One or two kinds of elements in Si, Al of the C of P, 2~10at%, 0.1~5at%.Its P content is higher, in fusion process
It volatilizees more serious, it is larger so as to cause ultimate constituent deviation, and strip face quality is relatively low, it is difficult to reach industrialized production
Requirement to zone face quality.
Alloy system is 5.：Japan Patent JP57185957A describes the alloy that a kind of expression formula is FeSiBPC, but its B
Constituent content ＜ 5at%, can make the amorphous formation ability of alloy and thermal stability be greatly lowered；And C element is in melting
It is difficult to alloying in the process, best C content is also difficult to control in industrial production.
Alloy system is 6.：Chinese patent CN102509603A describes a kind of FexSiyBzCraMbAlloy system wherein 74≤x≤
80at%, 1.5≤y≤4at%, 12≤z≤18at%, 2≤a≤6at%, 2≤b≤7at%；M is W, Nb, Mo, Ta or Hf
In one or more kinds of combinations；Dystectic element M is added to improve high-temperature stability with crossing, but M is nearly all
It is noble metal, and saturation induction density (BS) also there was only 1.45~1.65T, with the FeSiB alloy system phases of industrialized production
Than no advantage.
In addition, also (bibliography such as northeastern Japan university Akihiro professors Makino： JOURNAL OF
APPLIED PHYSICS 109,07A302 (2011)) research and development Fe85Si2B8P4Cu1Serial NANOMET alloys, most
Big advantage is saturation induction density (B after nano-crystallization annealingS) it may be up to 1.9T, however its as cast condition band magnetic saturation intensity
Only 1.2T or so.In addition, NANOMET alloy preparation technologies and its complexity：Non-crystaline amorphous metal is first prepared, then using complexity
And harsh subsequent annealing process (it is required that the rate of heat addition reaches 400 DEG C/min).This is in the industrial production prior art
It is extremely difficult to its requirement, it can not industrial applications.
Invention content
To solve the above problems, the present invention provides a kind of iron base amorphous magnetically-soft alloy with high saturated magnetic induction
And its preparation method and application, while improving its saturation induction density, coercivity does not increase the alloy, and magnetic conductivity is not
It reduces.
The purpose of the present invention is what is realized in the following manner：
A kind of iron base amorphous magnetically-soft alloy with high saturated magnetic induction, the expression formula of the alloy are
FeaSibBcGad, a, b, c and d indicate that the atom percentage content of each corresponding component, wherein a are 78 respectively in the expression formula,
It is 10.5~12.5, d is 1~4, a+b+c+d=100 that b, which is 7.2~8.6, c,.
The a is 78, b 8.59, c 12.41, d 1.
The a is 78, b 8.18, c 11.82, d 2..
The a is 78, b 7.77, c 11.23, d 3.
The a is 78, b 7.36, c 10.64, d 4.
A kind of preparation method of the iron base amorphous magnetically-soft alloy with high saturated magnetic induction, includes the following steps：
1) dispensing：Use the Si that purity is 99.999wt% for the Fe of 99.9wt%, purity, B content 19.62wt%
FeB, purity be 99.99wt% Ga, according to above-mentioned alloy expression formula atomic percentage content carry out dispensing；
2) master alloy melting：Proportioned raw material is positioned in non-consumable arc furnace, suction to 4-5 ×
10-3Pa is filled with the argon gas protective gas that purity is 99.99%；15~25A of electric current is adjusted, is refined raw material by electric arc melting
At master alloy ingot, by master alloy ingot melt back 5-7 times, ensure that the uniformity of master alloy ingredient is closed to get Fe-based amorphous soft magnetism
Gold；
3) preparation of band：Under the conditions of Discontinuous manufacture, by female conjunction under being protected in high vacuum conditions with argon gas
Ingot refuse is injected on high-speed rotating copper wheel, is prepared into iron-based amorphous thin ribbon, and copper wheel linear resonance surface velocity is 20~
30m/s。
In step (3) by melted master alloy take 6-8g be put into bottom be provided with a diameter of 0.6mm in circular hole and hole~
In the quartz ampoule of 0.9mm, in the induction coil being then placed in vacuum induction founding chamber and be fixed on 0.3 above copper wheel~
At 0.6mm height, 5.0~6.0 × 10 are evacuated to mechanical pump and diffusion pump successively-3
It is filled with the argon gas that purity is 99.99% after Pa as protective gas, is then turned on the copper wheel for being connected with cooling water and sense
Heating power supply is answered, then melts by the way of high-frequency induction heating under the protection of argon gas the master alloy in quartz ampoule equal
It is even, then it is ejected on high-speed rotating copper wheel in the case where quartz ampoule inside and outside differential pressure is 0.05MP a uniform master alloy is melted,
Prepare band.
A kind of iron core of the iron base amorphous magnetically-soft alloy for transformer with high saturated magnetic induction, the iron core
It is made of the iron base amorphous magnetically-soft alloy with high saturated magnetic induction.
Fe atom percentage contents are constant in 78 (at%) in alloy of the present invention, ensure that saturation induction density will not
It reduces.
Appropriate be added with of Si is conducive to Fe-based amorphous formation, meanwhile, it can hinder electronics in iron-based non-crystalline alloy
Movement, improves the resistivity of alloy, plays the role of reducing eddy-current loss.
B is known as larger atomic radius difference with Fe members, and meeting in three empirical laws that name on well proposes long has greatly
The requirement of atomic radius is conducive to the decrystallized of ferrous alloy.B content can significantly improve alloy more than 9 (at%)
Amorphous formation ability and stability；When its content is less than 5 (at%), the thermal stability of amorphous soft magnetic material is deteriorated, but works as B
When content is higher than 18 (at%), being further added by for content is substantially decrystallized to alloy without too big contribution, in addition B element
Also it is improved the effect of magnetic saturation intensity.
The addition of Ga elements increases this alloy constituent element type, is conducive to the supercooling liquid phase region and the amorphous phase that expand alloy
Formation；In metal-metalloid alloy system, nonmetallic sp electronics is fewer, and saturation induction density is bigger.
Compared with the existing technology, the present invention has the following advantages：
1. keeping Fe constituent contents constant in present component, integrally replace metalloid element to improve it by Ga
Whole saturation induction density reduces its volume so as to improve the magnetic flux density of amorphous power transformer, saves transformation
Device production cost.
2. alloying component constituent element of the present invention is simple, there are Si, B metalloid element, and content proportioning is reasonable, ingredient is unique,
Be conducive to improve and form amorphous formation ability, mouldability, and obtains excellent soft magnet performance；
3. alloy strip of the present invention has the excellent synthesis such as high magnetic saturation intensity, low coercivity, high magnetic conductivity
Magnetic property；
4. the excellent soft magnet performance of amorphous alloy component of the present invention need to only do stress relief annealing process and can be obtained, without
Complicated harsh annealing process processing, flow are short.
5. alloying component of the present invention adds to reduce the content of Si and B by Ga elements, Δ Tx gradually increases to 90 DEG C,
The precipitation for being conducive to α-Fe soft magnetic phases is obtained nanocrystalline by appropriate subsequent annealing technique.
Description of the drawings
Fig. 1 is the XRD curve graphs of 1-4 iron-based non-crystalline magnetically soft alloy of embodiment, and abscissa is 2 θ of angle of diffraction, indulges and sits
It is designated as intensity；
Fig. 2 is the DSC curve figure of 1-4 iron-based non-crystalline magnetically soft alloy of embodiment, and abscissa is temperature, and ordinate is heat
Amount；
Fig. 3 is the VSM curve graphs of 1-4 iron-based non-crystalline magnetically soft alloy of embodiment, and abscissa is applied field strengths, is indulged
Coordinate is magnetic induction intensity；
Fig. 4 is the VSM curve partial enlarged views of 1-4 iron-based non-crystalline magnetically soft alloy of embodiment, and abscissa is additional magnetic
Field intensity, ordinate are magnetic induction intensity；
Fig. 5 is the permeability curcve figure of 1-4 iron-based non-crystalline magnetically soft alloy of embodiment, and abscissa is frequency, ordinate
For magnetic conductivity；
Fig. 6 is the coercivity curve graph of 1-4 iron-based non-crystalline magnetically soft alloy of embodiment, and abscissa is that externally-applied magnetic field is strong
Degree, ordinate is magnetic induction intensity.
Specific implementation mode
Embodiment 1：
A kind of iron base amorphous magnetically-soft alloy Fe with high saturated magnetic induction78Si8.59B12.41Ga1, it is denoted as Y1,
Preparation method includes the following steps：
1) dispensing：Use the Si that purity is 99.999wt% for the Fe of 99.9wt%, purity, B content 19.62wt%
FeB, purity be 99.99wt% Ga, according to above-mentioned alloy expression formula atomic percentage content carry out dispensing；
2) master alloy melting：Proportioned raw material is positioned in non-consumable arc furnace, suction to 4 × 10- 3Pa is filled with the argon gas protective gas that purity is 99.99%；Electric current 15A is adjusted, raw material is refined by electric arc melting and is closed at mother
Master alloy ingot melt back 6 times is ensured the uniformity of master alloy ingredient to get iron base amorphous magnetically-soft alloy by ingot；
3) preparation of band：Under the conditions of Discontinuous manufacture, by female conjunction under being protected in high vacuum conditions with argon gas
Ingot refuse is injected on high-speed rotating copper wheel, is prepared into iron-based amorphous thin ribbon, and copper wheel linear resonance surface velocity is 30m/
s。
6g is taken to be put into the stone that bottom is provided with circular hole and a diameter of 0.7 mm in hole melted master alloy in step (3)
Ying Guanzhong in the induction coil being then placed in vacuum induction founding chamber and is fixed on above copper wheel at 0.3mm height, according to
It is secondary to be evacuated to 5.3 × 10 with mechanical pump and diffusion pump-3The argon gas that purity is 99.99% is filled with after Pa as protective gas, so
The copper wheel and induction heating power for being connected with cooling water are opened afterwards, and the side of high-frequency induction heating is then used under the protection of argon gas
It is uniform that formula makes the master alloy in quartz ampoule melt, then in the case where quartz ampoule inside and outside differential pressure is 0.05MP a the uniform female conjunction of melting
Gold is ejected on high-speed rotating copper wheel, prepares band.
As depicted in figs. 1 and 2, by the iron base amorphous magnetically-soft alloy strip Y1 of gained, X-ray diffractometer (X-ray is utilized
Diffraction, XRD；UItima IV diffractometer, Japan；Cu-K α) detection sample structure.Using differential
Scanning calorimetry (NETZSCH STA type Differential scanning calorimetry, DSC) is with the liter of 20K/min
Warm rate carrys out the glass transformation temperature Tg and initial crystallization temperature T of the iron base amorphous magnetically-soft alloy of determination samplex.It can obtain
State the XRD and DSC curve of Fe-based alloy ribbon.It will be seen from figure 1 that alloy strip is non crystalline structure.Figure it is seen that
The crystallization of this non-crystaline amorphous metal is completed in two steps.
As shown in figures 3 to 6, the iron base amorphous magnetically-soft alloy strip Y1 of gained is made annealing treatment, Y1 is packed into stone
Ying Guanli is vacuumized, when vacuum degree is 2.0 × 10-3When MPa, tube sealing processing is carried out, is then gone in batch-type furnace
Stress annealing, annealing temperature are 4 21 DEG C (Tx-100 DEG C), soaking time 10min.Then vibrating specimen magnetometer is used
(vibra ting sample magnetometer, VSM；7410, Lake Shore, the U.S.) measure annealed sample saturation
Magnetic induction density BS；The coercivity of annealed sample is measured with DC hysteresis loops measuring instrument (BHS-40, Rike n, Japan)；With
Impedance analyzer (4294A, Agilent, the U.S.) measures stress relief annealing sample under the extrinsic motivated magnetic field of different frequency
Magnetic conductivity.
Embodiment 2：
A kind of iron base amorphous magnetically-soft alloy Fe with high saturated magnetic induction78Si8.18B11.82Ga2, it is denoted as Y2,
Preparation method includes the following steps：
1) dispensing：Use the Si that purity is 99.999wt% for the Fe of 99.9wt%, purity, B content 19.62wt%
FeB, purity be 99.99wt% Ga, according to above-mentioned alloy expression formula atomic percentage content carry out dispensing；
2) master alloy melting：Proportioned raw material is positioned in non-consumable arc furnace, suction to 5 × 10- 3Pa is filled with the argon gas protective gas that purity is 99.99%；Electric current 17A is adjusted, raw material is refined by electric arc melting and is closed at mother
Master alloy ingot melt back 5 times is ensured the uniformity of master alloy ingredient to get iron base amorphous magnetically-soft alloy by ingot；
3) preparation of band：Under the conditions of Discontinuous manufacture, by female conjunction under being protected in high vacuum conditions with argon gas
Ingot refuse is injected on high-speed rotating copper wheel, is prepared into iron-based amorphous thin ribbon, and copper wheel linear resonance surface velocity is 20m/
s。
Melted master alloy is taken that 8g is put into that bottom is provided with circular hole and hole in step (3) a diameter of 0.6
In the quartz ampoule of mm, in the induction coil being then placed in vacuum induction founding chamber and it is fixed on above copper wheel
At 0.6mm height, 5.8 × 10 are evacuated to mechanical pump and diffusion pump successively-3The argon gas that purity is 99.99% is filled with after Pa
As protective gas, it is then turned on the copper wheel and induction heating power for being connected with cooling water, then using height under the protection of argon gas
It is uniform that the mode of frequency sensing heating makes the master alloy in quartz ampoule melt, then in the case where quartz ampoule inside and outside differential pressure is 0.05MP a
It is ejected on high-speed rotating copper wheel uniform master alloy is melted, prepares band.
As depicted in figs. 1 and 2, by the iron base amorphous magnetically-soft alloy strip Y2 of gained, X-ray diffractometer (X-ray is utilized
Diffraction, XRD；UItima IV diffractometer, Japan；Cu-K α) detection sample structure.Using differential
Scanning calorimetry (NETZSCH STA type Differential scanning calorimetry, DSC) is with the liter of 20K/min
Warm rate carrys out the glass transformation temperature Tg and initial crystallization temperature T of the iron base amorphous magnetically-soft alloy of determination samplex.It can obtain
State the XRD and DSC curve of Fe-based alloy ribbon.It will be seen from figure 1 that alloy strip is non crystalline structure.Figure it is seen that
The crystallization of this non-crystaline amorphous metal is completed in two steps.
As shown in figures 3 to 6, the iron base amorphous magnetically-soft alloy strip Y2 of gained is made annealing treatment, Y1 is packed into stone
Ying Guanli is vacuumized, when vacuum degree is 2.0 × 10-3When MPa, tube sealing processing is carried out, is then gone in batch-type furnace
Stress annealing, annealing temperature are 4 03 DEG C (Tx-100 DEG C), soaking time 10min.Then vibrating specimen magnetometer is used
(vibra ting sample magnetometer, VSM；7410, Lake Shore, the U.S.) measure annealed sample saturation
Magnetic induction density BS；The coercivity of annealed sample is measured with DC hysteresis loops measuring instrument (BHS-40, Rike n, Japan)；With
Impedance analyzer (4294A, Agilent, the U.S.) measures stress relief annealing sample under the extrinsic motivated magnetic field of different frequency
Magnetic conductivity.
Embodiment 3
A kind of iron base amorphous magnetically-soft alloy Fe with high saturated magnetic induction78Si7.77B11.23Ga3, it is denoted as Y3,
Preparation method includes the following steps：
1) dispensing：Use the Si that purity is 99.999wt% for the Fe of 99.9wt%, purity, B content 19.62wt%
FeB, purity be 99.99wt% Ga, according to above-mentioned alloy expression formula atomic percentage content carry out dispensing；
2) master alloy melting：Proportioned raw material is positioned in non-consumable arc furnace, suction to 4.5 ×
10-3Pa is filled with the argon gas protective gas that purity is 99.99%；Electric current 25A is adjusted, is refined raw material at mother by electric arc melting
Master alloy ingot melt back 6 times is ensured the uniformity of master alloy ingredient to get iron base amorphous magnetically-soft alloy by alloy pig；
3) preparation of band：Under the conditions of Discontinuous manufacture, by female conjunction under being protected in high vacuum conditions with argon gas
Ingot refuse is injected on high-speed rotating copper wheel, is prepared into iron-based amorphous thin ribbon, and copper wheel linear resonance surface velocity is 23m/
s。
7g is taken to be put into the stone that bottom is provided with circular hole and a diameter of 0.9 mm in hole melted master alloy in step (3)
Ying Guanzhong in the induction coil being then placed in vacuum induction founding chamber and is fixed on above copper wheel at 0.5mm height, according to
It is secondary to be evacuated to 5 × 10 with mechanical pump and diffusion pump-3The argon gas that purity is 99.99% is filled with after Pa as protective gas, then
The copper wheel and induction heating power for being connected with cooling water are opened, then under the protection of argon gas by the way of high-frequency induction heating
The master alloy in quartz ampoule is set to melt uniform, then in the case where quartz ampoule inside and outside differential pressure is 0.05MP a the uniform master alloy of melting
It is ejected on high-speed rotating copper wheel, prepares band.
As depicted in figs. 1 and 2, by the iron base amorphous magnetically-soft alloy strip Y3 of gained, X-ray diffractometer (X-ray is utilized
Diffraction, XRD；UItima IV diffractometer, Japan；Cu-K α) detection sample structure.Using differential
Scanning calorimetry (NETZSCH STA type Differential scanning calorimetry, DSC) is with the liter of 20K/min
Warm rate carrys out the glass transformation temperature T of the iron base amorphous magnetically-soft alloy of determination samplegWith initial crystallization temperature Tx.It can obtain
State the XRD and DSC curve of Fe-based alloy ribbon.It will be seen from figure 1 that alloy strip is non crystalline structure.Figure it is seen that
The crystallization of this non-crystaline amorphous metal is completed in two steps.
As shown in figures 3 to 6, the iron base amorphous magnetically-soft alloy strip Y2 of gained is made annealing treatment, Y1 is packed into stone
Ying Guanli is vacuumized, when vacuum degree is 2.0 × 10-3When MPa, tube sealing processing is carried out, is then gone in batch-type furnace
Stress annealing, annealing temperature are 3 80 DEG C (Tx-100 DEG C), soaking time 10min.Then vibrating specimen magnetometer is used
(vibra ting sample magnetometer, VSM；7410, Lake Shore, the U.S.) measure annealed sample saturation
Magnetic induction density BS；The coercivity of annealed sample is measured with DC hysteresis loops measuring instrument (BHS-40, Rike n, Japan)；With
Impedance analyzer (4294A, Agilent, the U.S.) measures stress relief annealing sample under the extrinsic motivated magnetic field of different frequency
Magnetic conductivity.
Embodiment 4
A kind of iron base amorphous magnetically-soft alloy Fe with high saturated magnetic induction78Si7.36B10.64Ga4, it is denoted as Y4,
Preparation method includes the following steps：
1) dispensing：Use the Si that purity is 99.999wt% for the Fe of 99.9wt%, purity, B content 19.62wt%
FeB, purity be 99.99wt% Ga, according to above-mentioned alloy expression formula atomic percentage content carry out dispensing；
2) master alloy melting：Proportioned raw material is positioned in non-consumable arc furnace, suction to 4.3 ×
10-3Pa is filled with the argon gas protective gas that purity is 99.99%；Electric current 20A is adjusted, is refined raw material at mother by electric arc melting
Master alloy ingot melt back 7 times is ensured the uniformity of master alloy ingredient to get iron base amorphous magnetically-soft alloy by alloy pig；
3) preparation of band：Under the conditions of Discontinuous manufacture, by female conjunction under being protected in high vacuum conditions with argon gas
Ingot refuse is injected on high-speed rotating copper wheel, is prepared into iron-based amorphous thin ribbon, and copper wheel linear resonance surface velocity is 28m/
s。
6g is taken to be put into the stone that bottom is provided with circular hole and a diameter of 0.8 mm in hole melted master alloy in step (3)
Ying Guanzhong in the induction coil being then placed in vacuum induction founding chamber and is fixed on above copper wheel at 0.4mm height, according to
It is secondary to be evacuated to 6 × 10 with mechanical pump and diffusion pump-3The argon gas that purity is 99.99% is filled with after Pa as protective gas, then
The copper wheel and induction heating power for being connected with cooling water are opened, then under the protection of argon gas by the way of high-frequency induction heating
The master alloy in quartz ampoule is set to melt uniform, then in the case where quartz ampoule inside and outside differential pressure is 0.05MP a the uniform master alloy of melting
It is ejected on high-speed rotating copper wheel, prepares band.
As depicted in figs. 1 and 2, by the iron base amorphous magnetically-soft alloy strip Y1-Y4 of gained, X-ray diffractometer (X- is utilized
Ray diffraction, XRD；UItima IV diffractometer, Japan；Cu-K α) detection sample structure.Using
Differential scanning calorimetry (NETZSCH STA type Differential scanning calorimetry, DSC) is with 20K/min
Heating rate come determination sample iron base amorphous magnetically-soft alloy glass transformation temperature Tg and initial crystallization temperature Tx.It can obtain
To the XRD and DSC curve of above-mentioned Fe-based alloy ribbon.It will be seen from figure 1 that alloy strip is non crystalline structure.It can be with from Fig. 2
Find out, the crystallization of this non-crystaline amorphous metal is completed in two steps.
As shown in figures 3 to 6, the iron base amorphous magnetically-soft alloy strip of gained is packed into quartz ampoule, is vacuumized, when
Vacuum degree is 2.0 × 10-3When MPa, tube sealing processing is carried out, stress relief annealing is then carried out in batch-type furnace, annealing temperature is
367 DEG C (Tx-100 DEG C), soaking time 10min.Then vibrating specimen magnetometer (vibrating sample are used
Magnetomet er, VSM；7410, Lake Shore, the U.S.) measure annealed sample saturation induction density BS；Use direct current
Hysteresisgraph (BHS-40, Riken, Japan) measures the coercivity of annealed sample；With impedance analyzer (4294A,
Agilent, the U.S.) measure magnetic conductivity of the stress relief annealing sample under the extrinsic motivated magnetic field of different frequency.
What has been described above is only a preferred embodiment of the present invention, it is noted that those skilled in the art is come
It says, under the premise of not departing from general idea of the present invention, several changes and improvements can also be made, these should also be considered as this hair
Bright protection domain.
Claims (8)
1. a kind of iron base amorphous magnetically-soft alloy with high saturated magnetic induction, it is characterised in that：The expression formula of the alloy
For FeaSibBcGad, a, b, c and d indicate that the atom percentage content of each corresponding component, wherein a are respectively in the expression formula
78, b be 7.2~8.6, c be 10.5~12.5, d be 1~4, a+b+c+d=100.
2. the iron base amorphous magnetically-soft alloy according to claim 1 with high saturated magnetic induction, it is characterised in that：Institute
It is 78, b 8.59, c 12.41, d 1 to state a.
3. the iron base amorphous magnetically-soft alloy according to claim 1 with high saturated magnetic induction, it is characterised in that：Institute
It is 78, b 8.18, c 11.82, d 2 to state a..
4. the iron base amorphous magnetically-soft alloy according to claim 1 with high saturated magnetic induction, it is characterised in that：Institute
It is 78, b 7.77, c 11.23, d 3 to state a.
5. the iron base amorphous magnetically-soft alloy according to claim 1 with high saturated magnetic induction, it is characterised in that：Institute
It is 78, b 7.36, c 10.64, d 4 to state a.
6. the preparation method of the iron base amorphous magnetically-soft alloy according to claim 1 with high saturated magnetic induction,
It is characterized in that including the following steps：
1) dispensing：Use FeB that Si, B content that purity is 99.999wt% for the Fe of 99.9wt%, purity are 19.62wt%,
Purity is the Ga of 99.99wt%, and dispensing is carried out according to above-mentioned alloy expression formula atomic percentage content；
2) master alloy melting：Proportioned raw material is positioned in non-consumable arc furnace, suction to 4-5 × 10-3Pa,
It is filled with the argon gas protective gas that purity is 99.99%；15~25A of electric current is adjusted, raw material is refined by electric arc melting and is closed at mother
Master alloy ingot melt back 5-7 times is ensured the uniformity of master alloy ingredient to get iron base amorphous magnetically-soft alloy by ingot；
3) preparation of band：Under the conditions of Discontinuous manufacture, by the master alloy ingot under being protected in high vacuum conditions with argon gas
Refuse is injected on high-speed rotating copper wheel, is prepared into iron-based amorphous thin ribbon, and copper wheel linear resonance surface velocity is 20~30m/s.
7. the preparation method of the iron base amorphous magnetically-soft alloy according to claim 6 with high saturated magnetic induction,
It is characterized in that：In step (3) by melted master alloy take 6-8g be put into bottom be provided with a diameter of 0.6mm in circular hole and hole~
In the quartz ampoule of 0.9mm, in the induction coil being then placed in vacuum induction founding chamber and be fixed on 0.3 above copper wheel~
At 0.6mm height, 5.0~6.0 × 10 are evacuated to mechanical pump and diffusion pump successively-3It is 99.99% that purity is filled with after Pa
Argon gas is then turned on the copper wheel and induction heating power for being connected with cooling water as protective gas, using height under the protection of argon gas
It is uniform that the mode of frequency sensing heating makes the master alloy in quartz ampoule melt, then the handle in the case where quartz ampoule inside and outside differential pressure is 0.05MPa
It melts uniform master alloy to be ejected on high-speed rotating copper wheel, prepares band.
8. a kind of iron core of the iron base amorphous magnetically-soft alloy for transformer with high saturated magnetic induction, it is characterised in that：
The iron core is made of the iron base amorphous magnetically-soft alloy described in claim 1 with high saturated magnetic induction.
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