CN101928896A - Large-amorphous forming capacity iron-based block amorphous magnetic alloy material and preparation method thereof - Google Patents
Large-amorphous forming capacity iron-based block amorphous magnetic alloy material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a large-amorphous forming capacity iron-based block amorphous magnetic alloy material and a preparation method thereof. The molecular formula of the large-amorphous forming capacity iron-based block amorphous magnetic alloy material is (Fe0.75-aMaB0.25-bSib) 1-cNbc, wherein M is one or more elements of Dy, Tb, Sm, Er, Ga and Y, a, b and c are atom percentages, a is not less than 0.005 and not greater than 0.1, b is not less than 0.03 and not greater than 0.07, and c is not less than 0.02 and not greater than 0.06. Compared with the prior art, the alloy material in the invention has the advantages of large amorphous forming capacity, favorable magnetostrictive coefficient and excellent soft magnetic performance, the reduced glass transition temperature of the alloy material reaches 0.5-0.7, the magnetostrictive coefficient reaches -50*10<-6> to 200*10<-6>, the alloy material can be prepared into amorphous bars with the diameters of 0.5mm-6mm due to the large amorphous forming capacity, thereby the alloy material can be widely applied in the fields of transformers, magnetic sensors and the like.
Description
Technical field
The present invention relates to the amorphous alloy technical field, relate in particular to large-amorphous forming capacity iron-based block amorphous magnetic alloy material and preparation method.
Background technology
People such as nineteen sixty Duwez adopt the melt rapid cooling method to prepare first amorphous alloy---the Au-Si amorphous alloy.Amorphous alloy does not possess the long-range atomic ordered, compare with traditional crystal alloy material, show the performance of many excellences, as the mechanical property of excellence, extremely strong erosion resistance and distinctive photoelectric characteristic etc., this makes amorphous alloy show application prospects, has become one of focus of type material research.
Fe-based amorphous magneticalloy because of its atom irregular alignment, aperiodicity, do not have the existence of crystal particle crystal boundary, thereby demonstrate good soft magnetic property, since 1967 come out, promptly received great concern.Thereafter, U.S. Allied-Signal company is successfully with the industrialization of iron-based non-crystalline magneticalloy, releasing trade mark is the series product of METGLAS, because of its high saturation and magnetic intensity that has more than the 1.5T is widely used in making power transmission and transformation transformer fe core material.
In addition, aspect sensor technology, magneticsensor is as wherein important branch, obtained increasingly extensive application in the every field of national economy.The key element of magneticsensor is a core body, because amorphous magnetic alloy has excellent soft magnetic performance, thereby adopts amorphous magnetic alloy material to have highly sensitive, characteristics such as frequency response good, low in energy consumption and direct current measurement good stability as the transmitter of core body.Wherein, big magnetostriction amorphous magnetic alloy transmitter can also be measured the instantaneous strain of the object of surveying except above advantage, so be widely used in the observing and controlling of aspects such as measuring micrometric displacement and liquid level.Traditional FeBSi is a non-crystaline amorphous metal because the restriction of amorphous formation ability, can only make the silk material that thickness is about 100 μ m less than band or the diameter of 30 μ m, and can not get block materials, so limited its use range.If improve the amorphous formation ability of Fe-based amorphous magneticalloy, then can make iron-based block amorphous magnetic alloy, thereby increase the volume occupation rate of iron level, this not only can reduce the production process of iron core, can also reduce the volume of iron core, thereby enlarge its use range.Therefore, since block amorphous alloy comes out, how to have improved the amorphous formation ability of Fe-based amorphous magneticalloy, be made into iron-based block amorphous magnetic alloy is an important research project always.
In order to break through the restriction of amorphous formation ability, people such as Shen Baolong have carried out the block work of Fe-based amorphous magneticalloy in aboveground research department, successfully synthesize FeCoBSiNb system first in the world, FeNiBSiNb, FeMoPCBSi are iron-based block amorphous magnetic alloy.These novel Fe-based amorphous magneticalloys are except having large-amorphous forming capacity, can directly cast to such an extent that maximum diameter (Φ) is outside the bar-shaped non-crystaline amorphous metal of 5mm, excellent mechanics and soft magnetic property have also been shown, the high strength (σ) that for example has 3300～4100MPa, the high Young's modulus of 155～210GPa (E); 0.8 the low-coercivity (H of～1.53T than high saturation and magnetic intensity (Is), 1.2～2.7A/m
c) etc., its Japanese Patent No. is opened 2005-256038 and Te Kai 2008-024985 for the spy.But, the magnetostriction coefficient (λ of these a series of Fe-based amorphous alloys
s) smaller, can only reach 9 * 10
-6～25 * 10
-6In addition, as far back as 1999, the people such as Wei Zhang in the work of aboveground research department developed Fe equally
80-x-yCo
xLn
yB
20(Ln=Nd, Sm, Tb or Dy) serial non-crystaline amorphous metal, this series Fe-based amorphous alloy have above 40 * 10
-6The high-magnetostriction performance, maximum magnetostriction coefficient can reach 58 * 10
-6, but amorphous formation ability that should the series Fe-based amorphous alloy is not strong, can not make the block amorphous alloy material.
Therefore, the synthetic iron-based block amorphous magnetic alloy material that has large-amorphous forming capacity and high-magnetostriction performance concurrently will be filled up domestic and international blank in this research field, further enlarges the use range of Fe-based amorphous magneticalloy simultaneously.
Summary of the invention
The purpose of this invention is to provide large-amorphous forming capacity iron-based block amorphous magnetic alloy material and preparation method, this amorphous magnetic alloy material has large-amorphous forming capacity and high-magnetostriction performance concurrently, and has excellent mechanical property and soft magnetic property.
The present invention realizes that the technical scheme that above-mentioned purpose adopts is: the large-amorphous forming capacity iron-based block amorphous magnetic alloy material, comprise Fe, Si, B and four kinds of principal elements of Nb and M element, the M element is one or more in Dy, Tb, Sm, Er, Ga, the Y element, and its molecular formula is (Fe
0.75-aM
aB
0.25-bSi
b)
1-cNb
c, a, b, c are the per-cent of atom in the formula, and 0.005≤a≤0.1,0.03≤b≤0.07,0.02≤c≤0.06.
Large-amorphous forming capacity iron-based block amorphous magnetic alloy preparation methods of the present invention comprises the steps:
Step 1: with purity is that pure Fe, M, B, Si, Nb element more than 99% is according to molecular formula (Fe
0.75-aM
aB
0.25-bSi
b)
1-cNb
cIn the atomic percent preparation raw material, wherein the M element is one or more in Dy, Tb, Sm, Er, Ga, the Y element, a, b, c are atomic percent, and 0.005≤a≤0.1,0.03≤b≤0.07,0.02≤c≤0.06;
Step 2: the raw material that step 1 preparation is obtained is placed in the arc-melting furnace, is evacuated to 0.5 * 10
-5～5 * 10
-5Pa, charging into argon gas to air pressure then is that 200～1000mbar carries out melting, continues melting 3～10 minutes after the fusing again, be cooled to solidify after rapidly with its upset, melt back 3～5 times obtains the uniform alloy pig of composition;
Step 3: the alloy pig that step 2 obtains is removed surface impurity, place the alcohol ultrasonic cleaning then, be broken into fritter afterwards;
Step 4: pack into the quartz glass tube of opening of the fritter alloy that step 3 is obtained is placed in the ruhmkorff coil of casting equipment, is evacuated to 0.5 * 10
-3～5 * 10
-3Charge into an amount of argon gas behind the Pa and carry out melting, utilize pressure difference that fused alloy hydraulic pressure is gone in the copper mold then, obtain the non-product magnetic alloy material of block.
Among the above-mentioned preparation method: the vacuum tightness of step 2 is preferably 10
-5Pa, the air pressure that charges into behind the argon gas is preferably 600mbar; Vacuum tightness after vacuumizing in the step 4 is preferably 10
-3Pa; Diameter 0.5mm～the 6mm of copper mold in the step 4, the block amorphous magnetic alloy material that obtains is the club shaped structure that diameter is 0.5mm～6mm.
Determine the amorphous structure of alloy material of the present invention with X-ray diffraction method (XRD).The XRD figure of amorphous alloy has the diffraction peak of the disperse of a broadening completely, and corresponding on the alloy diffracting spectrum of typical crystalline structure be sharp-pointed Bragg diffraction peak.
Measure the thermodynamical coordinate of amorphous magnetic alloy material of the present invention with dsc.Heating rate heating amorphous magnetic alloy material of the present invention with 40K/min makes its fusing, record glass transformation temperature (T
g), initial crystallization temperature (T
x), fusing point T
mAnd liquidus temperature (T
l), obtain the supercooling liquid phase region width Delta T
x(Δ T
x=T
x-T
g), reduction glass transformation temperature T
Rg(T
Rg=T
g/ T
l), with reduction glass transformation temperature T
RgEstimate the amorphous formation ability of amorphous magnetic alloy material of the present invention, use the supercooling liquid phase region width Delta T
xEstimate the glass forming ability of amorphous magnetic alloy material of the present invention.
Detect the magnetic performance of amorphous magnetic alloy material of the present invention with the magnetics testing tool, comprise magnetic permeability with the electric impedance analyzer specimen, with the coercive force of B-H instrument specimen, with the saturation induction density of vibrating sample magnetometer specimen, and with the magnetostriction coefficient of magnetostriction measurement instrument measure sample.
Compared with prior art, the advantage of large-amorphous forming capacity iron-based block amorphous magnetic alloy material of the present invention is: have big amorphous formation ability, high magnetostriction coefficient and excellent soft magnetic performance, its reduction glass transformation temperature reaches 0.5～0.7, the supercooling liquid phase region width is 40K～120K, and magnetostriction coefficient reaches-50 * 10
-6～200 * 10
-6, can make diameter is the amorphous bar of 0.5mm～6mm, thereby can be widely used in the fields such as transformer and magneticsensor.
Description of drawings
Fig. 1 is the sample photo of the amorphous magnetic alloy rod of embodiment 1;
Fig. 2 is the XRD figure of the amorphous magnetic alloy rod of embodiment 1;
Fig. 3 is the DSC heating curve of the amorphous magnetic alloy rod of embodiment 1;
Fig. 4 is the DSC temperature lowering curve of the amorphous magnetic alloy rod of embodiment 1;
Fig. 5 is the magnetostriction figure of the amorphous magnetic alloy rod of embodiment 1;
Fig. 6 is the XRD figure of the amorphous magnetic alloy rod of embodiment 2;
Fig. 7 is the DSC heating curve of the amorphous magnetic alloy rod of embodiment 2;
Fig. 8 is the DSC temperature lowering curve of the amorphous magnetic alloy rod of embodiment 2;
Fig. 9 is the magnetostriction figure of the amorphous magnetic alloy rod of embodiment 2.
Embodiment
Below in conjunction with drawings and Examples the present invention is described in further detail.
Embodiment 1:
The preparation diameter is the (Fe of 4mm
0.71Dy
0.04B
0.2Si
0.05)
0.96Nb
0.04The block amorphous magnetic alloy rod.
Concrete preparation method is as follows:
Step 1: with purity is that pure Fe, Si, B, Nb, Dy element more than 99% is according to molecular formula (Fe
0.71Dy
0.04B
0.2Si
0.05)
0.96Nb
0.04In the atomic percent preparation raw material;
Step 2: the raw material that step 1 preparation is obtained is placed in the water jacketed copper crucible of arc-melting furnace, at first is evacuated to 10
-5Pa, charging into argon gas to air pressure then is that 600mbar carries out melting, continues melting 5 minutes after the fusing again, allow then alloy with copper crucible be cooled to solidify after, rapidly with its upset, melt back 3～5 times obtains the uniform alloy pig of composition;
Step 3: the alloy pig that step 2 is obtained grinds off surface impurity with emery wheel, places the alcohol ultrasonic cleaning then, is broken into fritter at last;
Step 4: the fritter alloy that step 3 is obtained is packed in the quartz glass tube of lower ending opening, places the ruhmkorff coil of casting equipment then, is evacuated to 10
-3Charge into an amount of argon gas behind the pa, utilize pressure difference that fused alloy hydraulic pressure is gone in the common copper mold of 4mm, obtain the block amorphous magnetic alloy rod.
Figure 1 shows that the outside drawing of the amorphous magnetic alloy rod that method for preparing obtains, as can be seen from the figure this amorphous magnetic alloy is the bar-shaped block structure that diameter is 4mm.
Confirm the structure of this block amorphous magnetic alloy rod with X-ray diffraction method, Figure 2 shows that the XRD diffractogram of above-mentioned block amorphous magnetic alloy rod, show the diffraction peak of disperse among the figure, illustrate that this alloy bar is an amorphous structure with a broadening.
Measure the thermodynamical coordinate of this bulk amorphous alloy rod with dsc.From DSC heating curve shown in Figure 3 and DSC temperature lowering curve shown in Figure 4 its glass transformation temperature (T as can be seen
g) be 872K, liquidus temperature (T
l) be 1398K, initial crystallization temperature (T
x) be 974K, obtain reduction glass transformation temperature T
RgBe 0.624, the supercooling liquid phase region width Delta T
xBe 102.
Detect the magnetic performance of this block amorphous magnetic alloy rod with the magnetics testing tool, obtain magnetostriction figure shown in Figure 5, as can be seen magnetostriction coefficient (λ
s) up to 65.3 * 10
-6In addition, saturation induction density (I
s) be 0.75T, coercive force (H
c) be 4.3A/m
-1, magnetic permeability (μ
e) be 7172.
Embodiment 2:
The preparation diameter is the (Fe of 3.5mm
0.7Tb
0.05B
0.2Si
0.05)
0.96Nb
0.04The block amorphous magnetic alloy rod.
Concrete preparation method is as follows:
Step 1: with purity is that pure Fe, Si, B, Nb, Tb element more than 99% is according to molecular formula (Fe
0.7Tb
0.05B
0.2Si
0.05)
0.96Nb
0.04In the atomic percent preparation raw material;
Step 2: the raw material that step 1 preparation is obtained is placed in the water jacketed copper crucible of arc-melting furnace, at first is evacuated to 1.5 * 10
-5Pa, charging into argon gas to air pressure then is that 500mbar carries out melting, continues melting 6 minutes after the fusing again, allow then alloy with copper crucible be cooled to solidify after, rapidly with its upset, melt back 3～5 times obtains the uniform alloy pig of composition;
Step 3: the alloy pig that step 2 is obtained grinds off surface impurity with emery wheel, places the alcohol ultrasonic cleaning then, is broken into fritter at last;
Step 4: the fritter alloy that step 3 is obtained is packed in the quartz glass tube of lower ending opening, places the ruhmkorff coil of casting equipment then, is evacuated to 2 * 10
-3Charge into an amount of argon gas behind the pa, utilize pressure difference that fused alloy hydraulic pressure is gone in the common copper mold of 3.5mm, obtain the block amorphous magnetic alloy rod.
The outside drawing of above-mentioned amorphous magnetic alloy rod is similar shown in Figure 1, and being diameter is the bar-shaped block structure of 3.5mm.
Confirm the structure of this block amorphous magnetic alloy rod with X-ray diffraction method, Figure 6 shows that the XRD diffractogram of above-mentioned block amorphous magnetic alloy rod, show the diffraction peak of disperse among the figure, illustrate that this alloy bar is an amorphous structure with a broadening.
Measure the thermodynamical coordinate of this block amorphous magnetic alloy rod with dsc.From DSC heating curve shown in Figure 7 and DSC temperature lowering curve shown in Figure 8 its glass transformation temperature (T as can be seen
g) be 941K, liquidus temperature (T
l) be 1396K, initial crystallization temperature (T
x) be 995K, obtain reduction glass transformation temperature T
RgBe 0.674, the supercooling liquid phase region width Delta T
xBe 54.
Detect the magnetic performance of this block amorphous magnetic alloy rod with the magnetics testing tool, obtain magnetostriction figure shown in Figure 9, as can be seen magnetostriction coefficient (λ
s) be-30.6 * 10
-6In addition, saturation induction density (I
s) be 0.69T, coercive force (H
c) be 5A/m
-1, magnetic permeability (μ
e) be 5500.
Embodiment 3:
The preparation diameter is the (Fe of 1mm
0.74Dy
0.01B
0.2Si
0.05)
0.96Nb
0.04The block amorphous magnetic alloy rod.
Concrete preparation method is as follows:
Step 1: with purity is that pure Fe, Si, B, Nb, Dy element more than 99% is according to molecular formula (Fe
0.74Dy
0.01B
0.2Si
0.05)
0.96Nb
0.04In the atomic percent preparation raw material;
Step 2: the raw material of step 1 preparation is placed in the water jacketed copper crucible of arc-melting furnace, at first is evacuated to 2 * 10
-5Pa, charging into argon gas to air pressure then is that 700mbar carries out melting, continues melting 8 minutes after the fusing again, allow then alloy with copper crucible be cooled to solidify after, rapidly with its upset, melt back 3～5 times obtains the uniform alloy pig of composition;
Step 3: the alloy pig that step 2 is obtained grinds off surface impurity with emery wheel, places the alcohol ultrasonic cleaning then, is broken into fritter at last;
Step 4: the fritter alloy that step 3 is obtained is packed in the quartz glass tube of lower ending opening, places the ruhmkorff coil of casting equipment then, is evacuated to 1.5 * 10
-3Charge into an amount of argon gas behind the Pa, utilize pressure difference that fused alloy hydraulic pressure is gone in the common copper mold of 1mm, obtain the block amorphous magnetic alloy rod.
The outside drawing of above-mentioned amorphous alloy rod is similar shown in Figure 1, and being diameter is the bar-shaped block structure of 1mm.
Confirm the structure of this block amorphous magnetic alloy rod with X-ray diffraction method, the XRD diffractogram is similar shown in Figure 6, shows the diffraction peak of the disperse with a broadening among the figure, illustrates that this alloy bar is an amorphous structure.
Measure the thermodynamical coordinate of this block amorphous magnetic alloy rod with dsc.Can obtain its glass transformation temperature (T from DSC heating curve and DSC temperature lowering curve
g) be 833K, liquidus temperature (T
l) be 1461K, initial crystallization temperature (T
x) be 898K, obtain reduction glass transformation temperature T
RgBe 0.57, the supercooling liquid phase region width Delta T
xBe 65.
Detect the magnetic performance of this block amorphous magnetic alloy rod with the magnetics testing tool, obtain magnetostriction coefficient (λ
s) be 8.7 * 10
-6In addition, saturation induction density (I
s) be 1.12T, coercive force (H
c) be 3.8A/m
-1, magnetic permeability (μ
e) can reach 8606.
Embodiment 4:
The preparation diameter is the (Fe of 2mm
0.73Dy
0.02B
0.2Si
0.05)
0.96Nb
0.04The block amorphous magnetic alloy rod.
Concrete preparation method is as follows:
Step 1: with purity is that pure Fe, Si, B, Nb, Dy element more than 99% is according to molecular formula (Fe
0.73Dy
0.02B
0.2Si
0.05)
0.96Nb
0.04In the atomic percent preparation raw material;
Step 2: the raw material that step 1 preparation is obtained is placed in the water jacketed copper crucible of arc-melting furnace, at first is evacuated to 2.5 * 10
-5Pa, charging into argon gas to air pressure then is that 800mbar carries out melting, continues melting 3 minutes after the fusing again, allow then alloy with copper crucible be cooled to solidify after, rapidly with its upset, melt back 3～5 times obtains the uniform alloy pig of composition;
Step 3: the alloy pig that step 2 is obtained grinds off surface impurity with emery wheel, places the alcohol ultrasonic cleaning then, is broken into fritter at last;
Step 4: the fritter alloy that step 3 is obtained is packed in the quartz glass tube of lower ending opening, places the ruhmkorff coil of casting equipment then, is evacuated to 2 * 10
-3Charge into an amount of argon gas behind the pa, utilize pressure difference that fused alloy hydraulic pressure is gone in the common copper mold of 2mm, obtain the block amorphous magnetic alloy rod.
The outside drawing of above-mentioned amorphous magnetic alloy rod is similar shown in Figure 1, and being diameter is the bar-shaped block structure of 2mm.
Confirm the structure of this block amorphous magnetic alloy rod with X-ray diffraction method, the XRD diffractogram is similar shown in Figure 6, shows the diffraction peak of the disperse with a broadening among the figure, illustrates that this alloy bar is an amorphous structure.
Measure the thermodynamical coordinate of this bulk amorphous alloy rod with dsc.Can obtain its glass transformation temperature (T from DSC heating curve and DSC temperature lowering curve
g) be 851K, liquidus temperature (T
l) be 1441K, initial crystallization temperature (T
x) be 924K, obtain reduction glass transformation temperature T
RgBe 0.591, the supercooling liquid phase region width Delta T
xBe 73.
Detect the magnetic performance of this block amorphous magnetic alloy rod with the magnetics testing tool, obtain magnetostriction coefficient (λ
s) be 26.7 * 10
-6In addition, saturation induction density (I
s) be 0.99T, coercive force (H
c) be 3.7A/m
-1, magnetic permeability (μ
e) can reach 7388.
Embodiment 5:
The preparation diameter is the (Fe of 2.5mm
0.72Dy
0.03B
0.2Si
0.05)
0.96Nb
0.04The block amorphous magnetic alloy rod.
Concrete preparation method is as follows:
Step 1: with purity is that pure Fe, Si, B, Nb, Dy element more than 99% is according to molecular formula (Fe
0.72Dy
0.03B
0.2Si
0.05)
0.96Nb
0.04In the atomic percent preparation raw material;
Step 2: the raw material that step 1 preparation is obtained is placed in the water jacketed copper crucible of arc-melting furnace, at first is evacuated to 3 * 10
-5Pa, charging into argon gas to air pressure then is that 600mbar carries out melting, continues melting 10 minutes after the fusing again, allow then alloy with copper crucible be cooled to solidify after, rapidly with its upset, melt back 3～5 times obtains the uniform alloy pig of composition;
Step 3: the alloy pig that step 2 is obtained grinds off surface impurity with emery wheel, places the alcohol ultrasonic cleaning then, is broken into fritter at last;
Step 4: the fritter alloy that step 3 is obtained is packed in the quartz glass tube of lower ending opening, places the ruhmkorff coil of casting equipment then, is evacuated to 3 * 10
-3Charge into an amount of argon gas behind the Pa, utilize pressure difference that fused alloy hydraulic pressure is gone in the common copper mold of 2.5mm, obtain the block amorphous magnetic alloy rod.
The outside drawing of above-mentioned amorphous magnetic alloy rod is similar shown in Figure 1, and being diameter is the bar-shaped block structure of 2.5mm.
Confirm the structure of this block amorphous magnetic alloy rod with X-ray diffraction method, the XRD diffractogram is similar shown in Figure 6, shows the diffraction peak of the disperse with a broadening among the figure, illustrates that this alloy bar is an amorphous structure.
Measure the thermodynamical coordinate of this bulk amorphous alloy rod with dsc.Can obtain its glass transformation temperature (T from DSC heating curve and DSC temperature lowering curve
g) be 861K, liquidus temperature (T
l) be 1432K, initial crystallization temperature (T
x) be 946K, obtain reduction glass transformation temperature T
RgBe 0.605, the supercooling liquid phase region width Delta T
xBe 85.
Detect the magnetic performance of this block amorphous magnetic alloy rod with the magnetics testing tool, obtain magnetostriction coefficient (λ
s) be 64.5 * 10
-6In addition, saturation induction density (I
s) be 0.86T, coercive force (H
c) be 3.9A/m
-1, magnetic permeability (μ
e) can reach 7222.
Embodiment 6:
The preparation diameter is the (Fe of 3mm
0.7Dy
0.05B
0.2Si
0.05)
0.96Nb
0.04The block amorphous magnetic alloy rod.
Concrete preparation method is as follows:
Step 1: with purity is that pure Fe, Si, B, Nb, Dy element more than 99% is according to molecular formula (Fe
0.7Dy
0.05B
0.2Si
0.05)
0.96Nb
0.04In the atomic percent preparation raw material;
Step 2: the raw material that step 1 preparation is obtained is placed in the water jacketed copper crucible of arc-melting furnace, at first is evacuated to 5 * 10
-5Pa, charging into argon gas to air pressure then is that 1000mbar carries out melting, continues melting 5 minutes after the fusing again, allow then alloy with copper crucible be cooled to solidify after, rapidly with its upset, melt back 3～5 times obtains the uniform alloy pig of composition;
Step 3: the alloy pig that step 2 is obtained grinds off surface impurity with emery wheel, places the alcohol ultrasonic cleaning then, is broken into fritter at last;
Step 4: the fritter alloy that step 3 is obtained is packed in the quartz glass tube of lower ending opening, places the ruhmkorff coil of casting equipment then, is evacuated to 0.5 * 10
-3Charge into an amount of argon gas behind the pa, utilize pressure difference that fused alloy hydraulic pressure is gone in the common copper mold of 3mm, obtain the block amorphous magnetic alloy rod.
The outside drawing of above-mentioned amorphous magnetic alloy rod is similar shown in Figure 1, and being diameter is the bar-shaped block structure of 3mm.
Confirm the structure of this block amorphous magnetic alloy rod with X-ray diffraction method, the XRD diffractogram is similar shown in Figure 6, shows the diffraction peak of the disperse with a broadening among the figure, illustrates that this alloy bar is an amorphous structure.
Measure the thermodynamical coordinate of this bulk amorphous alloy rod with dsc.Can obtain its glass transformation temperature (T from DSC heating curve and DSC temperature lowering curve
g) be 938K, liquidus temperature (T
l) be 1405K, initial crystallization temperature (T
x) be 999K, obtain reduction glass transformation temperature T
RgBe 0.668, the supercooling liquid phase region width Delta T
xBe 61.
Detect the magnetic performance of this block amorphous magnetic alloy rod with the magnetics testing tool, obtain magnetostriction coefficient (λ
s) be 44.3 * 10
-6In addition, saturation induction density (I
s) be 0.65T, coercive force (H
c) be 5.3A/m
-1, magnetic permeability (μ
e) can reach 5427.
Embodiment 7:
The preparation diameter is the (Fe of 3mm
0.69Dy
0.06B
0.2Si
0.05)
0.96Nb
0.04The block amorphous magnetic alloy rod.
Concrete preparation method is as follows:
Step 1: with purity is that pure Fe, Si, B, Nb, Dy element more than 99% is according to molecular formula (Fe
0.69Dy
0.06B
0.2Si
0.05)
0.96Nb
0.04In the atomic percent preparation raw material;
Step 2: the raw material that step 1 preparation is obtained is placed in the water jacketed copper crucible of arc-melting furnace, at first is evacuated to 0.5 * 10
-5Pa, charging into argon gas to air pressure then is that 600mbar carries out melting, continues melting 5 minutes after the fusing again, allow then alloy with copper crucible be cooled to solidify after, rapidly with its upset, melt back 3～5 times obtains the uniform alloy pig of composition;
Step 3: the alloy pig that step 2 is obtained grinds off surface impurity with emery wheel, places the alcohol ultrasonic cleaning then, is broken into fritter at last;
Step 4: the fritter alloy that step 3 is obtained is packed in the quartz glass tube of lower ending opening, places the ruhmkorff coil of casting equipment then, is evacuated to 2.5 * 10
-3Charge into an amount of argon gas behind the pa, utilize pressure difference that fused alloy hydraulic pressure is gone in the common copper mold of 3mm, obtain the block amorphous magnetic alloy rod.
The outside drawing of above-mentioned amorphous magnetic alloy rod is similar shown in Figure 1, and being diameter is the bar-shaped block structure of 3mm.
Confirm the structure of this block amorphous magnetic alloy rod with X-ray diffraction method, the XRD diffractogram is similar shown in Figure 6, shows the diffraction peak of the disperse with a broadening among the figure, illustrates that this alloy bar is an amorphous structure.
Measure the thermodynamical coordinate of this bulk amorphous alloy rod with dsc.Can obtain its glass transformation temperature (T from DSC heating curve and DSC temperature lowering curve
g) be 948K, liquidus temperature (T
l) be 1419K, initial crystallization temperature (T
x) be 1013K, obtain reduction glass transformation temperature T
RgBe 0.668, the supercooling liquid phase region width Delta T
xBe 65.
Detect the magnetic performance of this block amorphous magnetic alloy rod with the magnetics testing tool, obtain magnetostriction coefficient (λ
s) be 15.6 * 10
-6In addition, saturation induction density (I
s) be 0.58T, coercive force (H
c) be 14.1A/m
-1, magnetic permeability (μ
e) can reach 3774.
Embodiment 8:
The preparation diameter is the (Fe of 2mm
0.68Dy
0.07B
0.2Si
0.05)
0.96Nb
0.04The block amorphous magnetic alloy rod.
Concrete preparation method is as follows:
Step 1: with purity is that pure Fe, Si, B, Nb, Dy element more than 99% is according to molecular formula (Fe
0.68Dy
0.07B
0.2Si
0.05)
0.96Nb
0.04In the atomic percent preparation raw material;
Step 2: the raw material that step 1 preparation is obtained is placed in the water jacketed copper crucible of arc-melting furnace, at first is evacuated to 2.5 * 10
-5Pa, charging into argon gas to air pressure then is that 700mbar carries out melting, continues melting 10 minutes after the fusing again, allow then alloy with copper crucible be cooled to solidify after, rapidly with its upset, melt back 3～5 times obtains the uniform alloy pig of composition;
Step 3: the alloy pig that step 2 is obtained grinds off surface impurity with emery wheel, places the alcohol ultrasonic cleaning then, is broken into fritter at last;
Step 4: the fritter alloy that step 3 is obtained is packed in the quartz glass tube of lower ending opening, places the ruhmkorff coil of casting equipment then, is evacuated to 3 * 10
-3Charge into an amount of argon gas behind the pa, utilize pressure difference that fused alloy hydraulic pressure is gone in the common copper mold of 2mm, obtain the block amorphous magnetic alloy rod.
The outside drawing of above-mentioned amorphous magnetic alloy rod is similar shown in Figure 1, and being diameter is the bar-shaped block structure of 2mm.
Confirm the structure of this block amorphous magnetic alloy rod with X-ray diffraction method, the XRD diffractogram is similar shown in Figure 6, shows the diffraction peak of the disperse with a broadening among the figure, illustrates that this alloy bar is an amorphous structure.
Measure the thermodynamical coordinate of this bulk amorphous alloy rod with dsc.Can obtain its glass transformation temperature (T from DSC heating curve and DSC temperature lowering curve
g) be 961K, liquidus temperature (T
l) be 1424K, initial crystallization temperature (T
x) be 1013K, obtain reduction glass transformation temperature T
RgBe 0.675, the supercooling liquid phase region width Delta T
xBe 52.
Detect the magnetic performance of this block amorphous magnetic alloy rod with the magnetics testing tool, obtain magnetostriction coefficient (λ
s) be-18.6 * 10
-6In addition, saturation induction density (I
s) be 0.51T, coercive force (H
c) be 36.3A/m
-1, magnetic permeability (μ
e) can reach 2326.
Shown in every performance of embodiment 1 to embodiment 8 obtained alloy sees the following form.
Claims (7)
1. large-amorphous forming capacity iron-based block amorphous magnetic alloy material is characterized in that: molecular formula is (Fe
0.75-aM
aB
0.25-bSi
b)
1-cNb
c, wherein the M element is one or more in Dy, Tb, Sm, Er, Ga, the Y element, a, b, c are atomic percent, and 0.005≤a≤0.1,0.03≤b≤0.07,0.02≤c≤0.06.
2. large-amorphous forming capacity iron-based block amorphous magnetic alloy material according to claim 1 is characterized in that: magnetostriction coefficient is-50 * 10
-6～200 * 10
-6, the reduction glass transition temp is 0.5～0.7.
3. large-amorphous forming capacity iron-based block amorphous magnetic alloy material according to claim 1 and 2 is characterized in that: the supercooling liquid phase region width is 40K～120K.
4. large-amorphous forming capacity iron-based block amorphous magnetic alloy material according to claim 1 and 2 is characterized in that: saturation induction density is 0.5T～1.4T.
5. large-amorphous forming capacity iron-based block amorphous magnetic alloy preparation methods as claimed in claim 1 is characterized in that: comprise the steps:
Step 1: with purity is that pure Fe, M, B, Si, Nb element more than 99% is according to molecular formula (Fe
0.75-aM
aB
0.25-bSi
b)
1-cNb
cIn the atomic percent preparation raw material, wherein the M element is one or more in Dy, Tb, Sm, Er, Ga, the Y element, a, b, c are atomic percent, and 0.005≤a≤0.1,0.03≤b≤0.07,0.02≤c≤0.06;
Step 2: the raw material that step 1 preparation is obtained is placed on and is evacuated to 0.5 * 10 in the arc-melting furnace
-5～5 * 10
-5Pa, charging into argon gas to air pressure then is that 200～1000mbar carries out melting, continues melting 3～10 minutes after the fusing again, be cooled to then solidify after, rapidly with its upset, melt back 3～5 times obtains the uniform alloy pig of composition;
Step 3: the alloy pig that step 2 obtains is removed surface impurity, place the alcohol ultrasonic cleaning then, be broken into fritter afterwards;
Step 4: pack into the quartz glass tube of opening of the fritter alloy that step 3 is obtained is placed in the ruhmkorff coil of casting equipment, is evacuated to 0.5 * 10
-3～5 * 10
-3Charge into an amount of argon gas behind the Pa and carry out melting, utilize pressure difference that fused alloy hydraulic pressure is gone in the copper mold then, obtain block amorphous magnetic alloy material.
6. large-amorphous forming capacity iron-based block amorphous magnetic alloy preparation methods according to claim 5 is characterized in that: charging into argon gas to air pressure in the described step 2 is 600mbar.
7. large-amorphous forming capacity iron-based block amorphous magnetic alloy preparation methods according to claim 5 is characterized in that: the block amorphous magnetic alloy material that obtains in the described step 4 is the club shaped structure that diameter is 0.5mm～6mm.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102268617A (en) * | 2011-08-19 | 2011-12-07 | 中国科学院宁波材料技术与工程研究所 | Fe-based bulk amorphous alloy with high glass forming ability and excellent magnetic property and preparation method thereof |
| CN102915820A (en) * | 2012-08-29 | 2013-02-06 | 中国科学院宁波材料技术与工程研究所 | Cobalt-base block amorphous soft magnetic alloy with high amorphous forming ability and preparation method thereof |
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| CN102268617A (en) * | 2011-08-19 | 2011-12-07 | 中国科学院宁波材料技术与工程研究所 | Fe-based bulk amorphous alloy with high glass forming ability and excellent magnetic property and preparation method thereof |
| CN102915820A (en) * | 2012-08-29 | 2013-02-06 | 中国科学院宁波材料技术与工程研究所 | Cobalt-base block amorphous soft magnetic alloy with high amorphous forming ability and preparation method thereof |
| CN103632836A (en) * | 2013-12-04 | 2014-03-12 | 中国矿业大学 | Preparation method for metallic glass magnetic core |
| CN103632836B (en) * | 2013-12-04 | 2015-11-04 | 中国矿业大学 | The preparation method of Metglas core |
| CN104198094A (en) * | 2014-08-29 | 2014-12-10 | 中国矿业大学 | Four-probe iron-based metal-glass magnetic-survey stressed magnetic-core sensor |
| CN104878326A (en) * | 2015-06-03 | 2015-09-02 | 上海理工大学 | Soft-magnet-based amorphous alloy product and preparation method thereof |
| CN108018504A (en) * | 2017-12-21 | 2018-05-11 | 青岛云路先进材料技术有限公司 | A kind of Fe-based amorphous alloy and preparation method thereof |
| CN108018504B (en) * | 2017-12-21 | 2020-05-08 | 青岛云路先进材料技术股份有限公司 | Iron-based amorphous alloy and preparation method thereof |
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