CN102732811A - High-saturated magnetization intensity Fe-based amorphous nanocrystalline soft magnetic alloy and its preparation method - Google Patents
High-saturated magnetization intensity Fe-based amorphous nanocrystalline soft magnetic alloy and its preparation method Download PDFInfo
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Abstract
The invention discloses a high-saturated magnetization intensity Fe-based amorphous nanocrystalline soft magnetic alloy and its preparation method. The alloy is prepared from the following components, by mole, 68-90% of Fe, 0-6% of X, 0-2% of Cu, 3-20% of Si, 4-20% of B and 0-10% of P, wherein the X comprises one or more of Al, Cr, Mn and Ti. The preparation method of the alloy comprises the technological steps of component designing and burdening, mother alloy melting, mother alloy fragmentation, band preparation through single-roller quenching, and band nanocrystallization processing. The preparation method of the invention can solve a problem of low saturated magnetic induction intensity of present Fe-based amorphous nanocrystalline soft magnetic alloys.
Description
Technical field
The present invention relates to a kind of iron-based amorphous and nanocrystalline soft magnetic alloy and preparation method thereof with high saturation and magnetic intensity.
Background technology
Fe-based amorphous have good comprehensive soft magnetic performance with nano-crystal soft magnetic alloy; Like characteristics such as the saturated magnetic strength value of height, high permeability, low-coercivity, low-loss, low magnetizing current and satisfactory stability property; Iron core, filter reactor, transductor, motor stator and the Magnetic Sensor etc. that can be used for substation transformer, intermediate frequency power supply X-former and switching mode power supply transformer are to use and study one of the widest amorphous nano peritectic alloy.Because the application of Fe-based amorphous nanocrystalline alloy has great economic implications and social benefit, recent decades, the research of relevant amorphous and nanometer crystal alloy was the research focus in material and the Condensed Matter Physics field all the time.The Fe-Cu-Nb-Si-B that the most noticeable research starts from people such as the Yoshizawa discovery of Hitachi Metals company in 1988 is an alloy.Because this series alloy has unique nanocrystalline structure and excellent soft magnetic performance, has caused researchist's extensive attention.Through the research of two more than ten years, present nano-crystal soft magnetic alloy mainly comprises three alloy systems, i.e. FeCuMSiB (M=Nb; Ta, W etc.) be Finemet alloy, FeMBCu (M=Zr, Hf; Nb etc.) be that Nanoperm alloy and FeCoMCuB (M=Zr, Hf, Nb etc.) are the Hitperm alloy.Wherein, Though Nanoperm and Hitperm alloy saturation magnetization are higher; But the soft magnetism over-all properties is not as good as the Finemet alloy; Also cause cost height and complicated process of preparation simultaneously, do not obtain real applying because contain a large amount of precious metal elements (like Zr, Nb, Co etc.) that are prone to oxidation.Comprehensively soft magnetic performance and lower cost are widely used the Finemet alloy at present in a lot of fields preferably owing to it.Yet its saturation induction density relatively low (the highest 1.4T that is merely is usually about 1.2T).This causes it to compare with the silicon steel of high saturated magnetic induction, needs bigger volume when under identical working conditions, using, and limits its application greatly.Be to adapt to the lightweight of device, the requirement of miniaturized development, increasing for the demand of the soft magnetic materials of novel high saturated magnetic induction, high magnetic permeability, low-loss, good high frequency performance.Along with the enforcement (requiring low-loss) of national energy-saving and emission-reduction policy, research and development have high saturated magnetic induction and low-loss new iron-based nano-crystal soft magnetic alloy simultaneously and become and become more and more important.For nano crystal soft magnetic material, improve the saturation induction density of alloy, need increase iron level as far as possible, and the nonferromagnetic metalloid element in the corresponding minimizing alloy.But the minimizing of these metalloid element content can cause the decline of the amorphous formation ability of nanometer crystal alloy presoma (amorphous), thereby brings difficulty for the preparation of amorphous band, and causes the deterioration of soft magnetic performance.Therefore, press for the exploitation new iron-based amorphous nano peritectic alloy that a kind of preparation technology is simple and soft magnetic performance is excellent, it has great importance for the development that promotes China's iron based amorphous nanocrystalline soft magnetic material and device related industries thereof.
Summary of the invention
The present invention seeks to: to the problems referred to above; The present invention provides a kind of high saturation magnetization intensity Fe-based amorphous and nanocrystalline soft magnetic alloy that has; Also disclose the preparation method of this alloy simultaneously, be intended to solve the lower problem of present iron-based amorphous and nanocrystalline soft magnetic alloy material saturation induction density
Technical scheme of the present invention is: described high saturation magnetization intensity Fe-based amorphous and nanocrystalline soft magnetic alloy, process by the composition of following corresponding molar percentage:
68 ~ 90% iron,
0 ~ 6% X, said X select one or more to aluminium, chromium, manganese, titanium, the vanadium,
0 ~ 2% copper,
3 ~ 20% silicon,
4 ~ 20% boron,
And 0 ~ 10% phosphorus.
That is to say that the composition of this high saturation magnetization intensity Fe-based amorphous and nanocrystalline soft magnetic alloy and the molar weight of each composition can be represented with following molecule skeleton symbol: Fe
aX
bCu
cSi
dB
eP
f, wherein, 68≤a≤90,0≤b≤6,0≤c≤2,3≤d≤20,4≤e≤20,0≤f≤10, and a+b+c+d+e+f=100, X is one or more among Al, Cr, Mn, Ti, the V.
The preparation method of above-mentioned this high saturation magnetization intensity Fe-based amorphous and nanocrystalline soft magnetic alloy may further comprise the steps:
1) according to following molar percentage proportioning raw material:
68 ~ 90% iron,
0 ~ 6% X, said X be in aluminium, chromium, manganese, titanium, the vanadium one or more (such as: X is chromium, manganese and titanium, and then chromium, manganese, titanium three's molar percentage sum is between 0 ~ 6%),
0 ~ 2% copper,
3 ~ 20% silicon,
4 ~ 20% boron,
And 0 ~ 10% phosphorus;
2) raw material that proportioning is good is packed in the crucible of vacuum induction furnace, and the method that under vacuum condition, adopts the Medium frequency induction melting is raw material melt back at least 3 times, and in fusion process, stirs and make each raw materials mix even, and pours into alloy pig;
3) alloy pig that melting is obtained is broken, and the block alloy of fragmentation is put into acetone soln successively with spirituous solution carries out ultrasonic cleaning, take out then dry naturally for use;
4) block alloy that cleans up is put into the silica tube of chilling system carrying equipment, used single roller to get rid of the band method and prepare amorphous alloy ribbon;
5) amorphous alloy ribbon that makes is put into heat treatment furnace, at pressure less than 10
-3Under the vacuum environment of Pa or under the environment of inert argon gas shield; (this temperature-rise period can be divided into for two steps to carry out: at first rise to a certain medium temperature with bigger temperature rise rate smaller or equal to the temperature rise rate of 25 ℃/min the heat treatment furnace temperature is increased to 360 ℃～480 ℃; And then rise to outlet temperature with less temperature rise rate; And guarantee big and less temperature rise rate all smaller or equal to 25 ℃/min); Behind insulation 0.5 ~ 2h, let amorphous alloy ribbon cool to room temperature with the furnace, obtain amorphous nano-crystalline two-phase compound iron-base soft magnetic alloy material.
As preferably, in said step 4), the width of said amorphous alloy ribbon is 2 ~ 50mm, and thickness is 20 ~ 30 um.
Advantage of the present invention is: the high saturation magnetization intensity Fe-based amorphous and nanocrystalline soft magnetic alloy of the present invention, its saturation magnetization is high.
Description of drawings
Below in conjunction with accompanying drawing and embodiment the present invention is further described:
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Embodiment 1:
1) composition design and batching:
According to following molar percentage proportioning raw material: 85% iron, 1% aluminium, 0.5% copper, 3.5% silicon, 6% boron and 4% phosphorus amount to 5kg;
2) mother alloy melting:
Confected materials is added in the crucible of vacuum medium frequency induction furnace, Medium frequency induction melting 4 times, and in fusion process, stir and make each raw materials mix even, and pour into alloy pig, obtain the uniform alloy pig of composition;
3) mother alloy is broken:
After the alloy pig Mechanical Crushing, the block alloy of fragmentation is put into acetone soln and spirituous solution carries out ultrasonic cleaning successively, take out the back and dry for use naturally;
4) single rod chilling system band:
The block alloy that cleans up is put into the silica tube of chilling system carrying equipment; Adopt induction heating method that it is melted; Utilize single roller chilling belt-rejecting technology, with the speed system band of 35m/s, making width is that 10mm, thickness are the amorphous alloy ribbon of 30um in air;
5) the band nano-crystallization is handled:
The amorphous alloy thin band is put into the tubular type vacuum heat treatment furnace, at pressure smaller or equal to 10
-3Under the vacuum environment of Pa; Heating rate with 15 ℃/min is warming up to 360 ℃; Be warming up to 400 ℃ with 5 ℃/min then, and insulation 0.5h, let amorphous alloy ribbon cool to room temperature with the furnace; Obtain amorphous nano-crystalline two-phase compound iron-base soft magnetic alloy material, the moity of this alloy material and the molar weight of each composition can be represented with following molecule skeleton symbol: Fe
85Al
1Cu
0.5Si
3.5B
6P
4
Performance Detection: the magneticmeasurement that passes through of the nanocrystalline strip after the thermal treatment (the promptly last amorphous nano-crystalline two-phase compound iron-base soft magnetic alloy material that obtains) obtains its saturation magnetization and is about 1.84T, and coercive force is about 19A/m, iron loss P1/50=0.46W/kg.
Embodiment 2:
1) according to following molar percentage proportioning raw material: 82% iron, 1% aluminium, 0.5% titanium, 0.5% copper, 0.5% silicon, 8% boron and 4% phosphorus, 5kg altogether;
2) confected materials is added in the crucible of vacuum medium frequency induction furnace, Medium frequency induction melting 4 times, and in fusion process, stir and make each raw materials mix even, and pour into alloy pig, obtain the uniform alloy pig of composition;
3) with after the alloy pig Mechanical Crushing, the block alloy of fragmentation is put into acetone soln and spirituous solution carries out ultrasonic cleaning successively, take out the back and dry for use naturally;
4) block alloy that cleans up is put into the silica tube of chilling system carrying equipment; Adopt induction heating method that it is melted; Utilize single roller chilling belt-rejecting technology, with the speed system band of 30m/s, making width is that 20mm, thickness are the amorphous alloy ribbon of 30um in air;
5) the amorphous alloy thin band is put into the tubular type vacuum heat treatment furnace, at pressure smaller or equal to 10
-3Under the vacuum environment of Pa; Heating rate with 20 ℃/min is warming up to 360 ℃; Be warming up to 480 ℃ with 5 ℃/min then, and insulation 0.5h, let amorphous alloy ribbon cool to room temperature with the furnace; Obtain amorphous nano-crystalline two-phase compound iron-base soft magnetic alloy material, the moity of this alloy material and the molar weight of each composition can be represented with following molecule skeleton symbol: Fe
82Al
1Ti
0.5Cu
0.5Si
4B
8P
4
The magneticmeasurement that passes through of the nanocrystalline strip after the thermal treatment obtains its saturation magnetization and is about 1.70T, and coercive force is about 10A/m, iron loss P1/50=0.34W/kg.
Embodiment 3:
1) according to following molar percentage proportioning raw material: 79% iron, 1.5% chromium, 1.5% manganese, 1.5% copper, 5% silicon, 7.5% boron and 4% phosphorus, 5kg altogether;
2) confected materials is added in the crucible of vacuum medium frequency induction furnace, Medium frequency induction melting 3 times, and in fusion process, stir and make each raw materials mix even, and pour into alloy pig, obtain the uniform alloy pig of composition;
3) with after the alloy pig Mechanical Crushing, the block alloy of fragmentation is put into acetone soln and spirituous solution carries out ultrasonic cleaning successively, take out the back and dry for use naturally;
4) block alloy that cleans up is put into the silica tube of chilling system carrying equipment; Adopt the method for induction heating that it is melted; Utilize single roller chilling belt-rejecting technology, with the speed system band of 35m/s, making width is that 25mm, thickness are the amorphous alloy ribbon of 30um in air;
5) the amorphous alloy thin band is put into the tubular type vacuum heat treatment furnace, at pressure smaller or equal to 10
-3Under the vacuum environment of Pa; Heating rate with 15 ℃/min is warming up to 360 ℃; Be warming up to 410 ℃ with 5 ℃/min then, and insulation 1h, let amorphous alloy ribbon cool to room temperature with the furnace; Obtain amorphous nano-crystalline two-phase compound iron-base soft magnetic alloy material, the moity of this alloy material and the molar weight of each composition can be represented with following molecule skeleton symbol: Fe
79Cr
1.5Mn
1.5Cu
1.5Si
5B
7.5P
4
The magneticmeasurement that passes through of the nanocrystalline strip after the thermal treatment (the promptly last amorphous nano-crystalline two-phase compound iron-base soft magnetic alloy material that obtains) obtains its saturation magnetization and is about 1.62T, and coercive force is about 7A/m, iron loss P1/50=0.22W/kg.
Embodiment 4:
1) according to following molar percentage proportioning raw material: 90% iron, 1% vanadium, 2% copper, 3% silicon, 4% boron amount to 5kg;
2) confected materials is added in the crucible of vacuum medium frequency induction furnace, Medium frequency induction melting 3 times, and in fusion process, stir and make each raw materials mix even, and pour into alloy pig, obtain the uniform alloy pig of composition;
3) with after the alloy pig Mechanical Crushing, the block alloy of fragmentation is put into acetone soln and spirituous solution carries out ultrasonic cleaning successively, take out the back and dry for use naturally;
4) block alloy that cleans up is put into the silica tube of chilling system carrying equipment; Adopt the method for induction heating that it is melted; Utilize single roller chilling belt-rejecting technology, with the speed system band of 35m/s, making width is that 2mm, thickness are the amorphous alloy ribbon of 21um in air;
5) the amorphous alloy thin band is put into the tubular type vacuum heat treatment furnace, at pressure smaller or equal to 10
-3Under the vacuum environment of Pa; Heating rate with 25 ℃/min is warming up to 360 ℃; Be warming up to 440 ℃ with 5 ℃/min then, and insulation 1h, let amorphous alloy ribbon cool to room temperature with the furnace; Obtain amorphous nano-crystalline two-phase compound iron-base soft magnetic alloy material, the moity of this alloy material and the molar weight of each composition can be represented with following molecule skeleton symbol: Fe
90V
1Cu
2Si
3B
4
The magneticmeasurement that passes through of the nanocrystalline strip after the thermal treatment obtains its saturation magnetization and is about 1.8T, and coercive force is about 15A/m, iron loss P1/50=0.42W/kg.
Embodiment 5:
1) according to following molar percentage proportioning raw material: 68% iron, 2% aluminium, 1% chromium, 1% manganese, 1% titanium, 1% vanadium, 1% copper, 20% silicon, 4% boron, 1% phosphorus amount to 5kg;
2) confected materials is added in the crucible of vacuum medium frequency induction furnace, Medium frequency induction melting 5 times, and in fusion process, stir and make each raw materials mix even, and pour into alloy pig, obtain the uniform alloy pig of composition;
3) with after the alloy pig Mechanical Crushing, the block alloy of fragmentation is put into acetone soln and spirituous solution carries out ultrasonic cleaning successively, take out the back and dry for use naturally;
4) block alloy that cleans up is put into the silica tube of chilling system carrying equipment; Adopt the method for induction heating that it is melted; Utilize single roller chilling belt-rejecting technology, with the speed system band of 35m/s, making width is that 50mm, thickness are the amorphous alloy ribbon of 30um in air;
5) the amorphous alloy thin band is put into the tubular type vacuum heat treatment furnace, at pressure smaller or equal to 10
-3Under the vacuum environment of Pa; Heating rate with 25 ℃/min is warming up to 360 ℃; Be warming up to 400 ℃ with 5 ℃/min then, and insulation 1h, let amorphous alloy ribbon cool to room temperature with the furnace; Obtain amorphous nano-crystalline two-phase compound iron-base soft magnetic alloy material, the moity of this alloy material and the molar weight of each composition can be represented with following molecule skeleton symbol: Fe
68Al
2Cr
1Mn
1Ti
1V
1Cu
1Si
20B
4P
1
Performance Detection: the magneticmeasurement that passes through of the nanocrystalline strip after the thermal treatment obtains its saturation magnetization and is about 1.6T, and coercive force is about 5A/m, iron loss P1/50=0.18W/kg.
Embodiment 6:
1) according to following molar percentage proportioning raw material: 68% iron, 3% silicon, 19% boron, 10% phosphorus amount to 5kg;
2) confected materials is added in the crucible of vacuum medium frequency induction furnace, Medium frequency induction melting 5 times, and in fusion process, stir and make each raw materials mix even, and pour into alloy pig, obtain the uniform alloy pig of composition;
3) with after the alloy pig Mechanical Crushing, the block alloy of fragmentation is put into acetone soln and spirituous solution carries out ultrasonic cleaning successively, take out the back and dry for use naturally;
4) block alloy that cleans up is put into the silica tube of chilling system carrying equipment; Adopt the method for induction heating that it is melted; Utilize single roller chilling belt-rejecting technology, with the speed system band of 35m/s, making width is that 2mm, thickness are the amorphous alloy ribbon of 20um in air;
5) the amorphous alloy thin band is put into heat treatment furnace; Under the environment of inert argon gas shield, be warming up to 340 ℃ with the heating rate of 25 ℃/min, be warming up to 360 ℃ with 5 ℃/min then; And insulation 2h; Let amorphous alloy ribbon cool to room temperature with the furnace, obtain amorphous nano-crystalline two-phase compound iron-base soft magnetic alloy material, the moity of this alloy material and the molar weight of each composition can be represented with following molecule skeleton symbol: Fe
68Si
3B
19P
10
The magneticmeasurement that passes through of the nanocrystalline strip after the thermal treatment obtains its saturation magnetization and is about 1.65T, and coercive force is about 16A/m, iron loss P1/50=0.36W/kg.
Embodiment 7:
1) according to following molar percentage proportioning raw material: 70% iron, 2% aluminium, 1% manganese, 7% silicon and 20% boron, 5kg altogether;
2) confected materials is added in the crucible of vacuum medium frequency induction furnace, Medium frequency induction melting 4 times, and in fusion process, stir and make each raw materials mix even, and pour into alloy pig, obtain the uniform alloy pig of composition;
3) with after the alloy pig Mechanical Crushing, the block alloy of fragmentation is put into acetone soln and spirituous solution carries out ultrasonic cleaning successively, take out the back and dry for use naturally;
4) block alloy that cleans up is put into the silica tube of chilling system carrying equipment; Adopt the method for induction heating that it is melted; Utilize single roller chilling belt-rejecting technology, with the speed system band of 35m/s, making width is that 10mm, thickness are the amorphous alloy ribbon of 20um in air;
5) the amorphous alloy thin band is put into the tubular type vacuum heat treatment furnace, at pressure smaller or equal to 10
-3Under the vacuum environment of Pa; Heating rate with 25 ℃/min is warming up to 360 ℃; Be warming up to 440 ℃ with 5 ℃/min then, and insulation 1.5h, let amorphous alloy ribbon cool to room temperature with the furnace; Obtain amorphous nano-crystalline two-phase compound iron-base soft magnetic alloy material, the moity of this alloy material and the molar weight of each composition can be represented with following molecule skeleton symbol: Fe
70Al
2Mn
1Si
7B
20
The magneticmeasurement that passes through of the nanocrystalline strip after the thermal treatment obtains its saturation magnetization and is about 1.56T, and coercive force is about 12A/m, iron loss P1/50=0.26W/kg.
Certainly, the foregoing description only is explanation technical conceive of the present invention and characteristics, and its purpose is to let people can understand content of the present invention and implements according to this, can not limit protection scope of the present invention with this.The all spirit of main technical schemes is done according to the present invention equivalent transformation or modification all should be encompassed within protection scope of the present invention.
Claims (3)
1. a high saturation magnetization intensity Fe-based amorphous and nanocrystalline soft magnetic alloy is characterized in that, it is processed by the composition of following corresponding molar percentage:
68 ~ 90% iron,
0 ~ 6% X, said X select one or more to aluminium, chromium, manganese, the titanium,
0 ~ 2% copper,
3 ~ 20% silicon,
4 ~ 20% boron,
And 0 ~ 10% phosphorus.
2. the preparation method of a high saturation magnetization intensity Fe-based amorphous and nanocrystalline soft magnetic alloy as claimed in claim 1 is characterized in that this method may further comprise the steps:
1) according to following molar percentage proportioning raw material:
68 ~ 90% iron,
0 ~ 6% X, said X are one or more in aluminium, chromium, manganese, titanium, the vanadium,
0 ~ 2% copper,
3 ~ 20% silicon,
4 ~ 20% boron,
And 0 ~ 10% phosphorus;
2) raw material that proportioning is good is packed in the crucible of vacuum induction furnace, and the method that under vacuum condition, adopts the Medium frequency induction melting is raw material melt back at least 3 times, and in fusion process, stirs and make each raw materials mix even, and pours into alloy pig;
3) alloy pig that melting is obtained is broken, and the block alloy of fragmentation is put into acetone soln successively with spirituous solution carries out ultrasonic cleaning, take out then dry naturally for use;
4) block alloy that cleans up is put into the silica tube of chilling system carrying equipment, used single roller to get rid of the band method and prepare amorphous alloy ribbon;
5) amorphous alloy ribbon that makes is put into heat treatment furnace, at pressure less than 10
-3Under the vacuum environment of Pa or under the environment of inert argon gas shield; Temperature rise rate with smaller or equal to 25 ℃/min is increased to 360 ℃～480 ℃ with the heat treatment furnace temperature; Behind insulation 0.5 ~ 2h; Let amorphous alloy ribbon cool to room temperature with the furnace, obtain amorphous nano-crystalline two-phase compound iron-base soft magnetic alloy material.
3. the preparation method of high saturation magnetization intensity Fe-based amorphous and nanocrystalline soft magnetic alloy according to claim 2, it is characterized in that: in said step 4), the width of said amorphous alloy ribbon is 2 ~ 50mm, and thickness is 20 ~ 30 um.
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