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CN102787281A - High-toughness iron-phosphorus based amorphous alloy thin strip and preparation method thereof - Google Patents

High-toughness iron-phosphorus based amorphous alloy thin strip and preparation method thereof Download PDF

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CN102787281A
CN102787281A CN2012102985494A CN201210298549A CN102787281A CN 102787281 A CN102787281 A CN 102787281A CN 2012102985494 A CN2012102985494 A CN 2012102985494A CN 201210298549 A CN201210298549 A CN 201210298549A CN 102787281 A CN102787281 A CN 102787281A
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alloy
base noncrystal
iron phosphorus
phosphorus base
iron
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CN102787281B (en
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周少雄
董帮少
李德红
陈文智
张淑兰
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Advanced Technology and Materials Co Ltd
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Abstract

The invention belongs to the field of magnetic functional materials and particularly relates to a high-toughness iron-phosphorus based amorphous alloy thin strip and a preparation method of the high-toughness iron-phosphorus based amorphous alloy thin strip. The iron-phosphorus based amorphous alloy has the chemical formula for FeaPbBcMd, wherein M is at least one of the Nb, V, Ta, and Ti. According to the atom percentage, b accounts for 2-20%, c accounts for 0.5-15% and d accounts for 0.5-5%, and the balance of a. The iron-phosphorus based amorphous alloy has the fracture strain epsilonf of above 0.02, the ductile-brittle transition temperature (TDB) of above 150 DEG C, the saturation magnetic induction intensity Bs of above 1.40T, the coercivity Hc of less than 3.0A/m and the loss P11/50 of less than 0.3W/kg. The iron-phosphorus based amorphous alloy also has the advantages of good ductility, excellent soft magnetic properties and good amorphous forming capacity, can be widely used for a variety of iron core materials and has important industrial application value.

Description

A kind of H.T. iron phosphorus base noncrystal alloy strip and preparation method thereof
Technical field
The present invention relates to the magnetic functional material field, particularly iron phosphorus base amorphous alloy strip of a kind of good-toughness and preparation method thereof can be widely used in various core materials.
Background technology
Non-crystaline amorphous metal has special magnetic property, erosion resistance and mechanical property, therefore has the important commercial using value.Yet, since non-crystaline amorphous metal fragility under certain condition, i.e. rapid reduction from ductility to brittle mechanical features, and its commercial applications is restricted.The performance of the above-mentioned fragility of non-crystaline amorphous metal under condition directly perceived is that the amorphous alloy that utilizes flash set technology to prepare can show the attitude fragility of quenching in some cases, causes difficulty for the following process of band.The attitude fragility of quenching of amorphous alloy has the reason of many aspects.At first, non-crystaline amorphous metal had both belonged to glass, belonged to metallic glass again, the natural fragility of this singularity decision amorphous alloy.Secondly, be the reason on the avoidable preparation technology.At last, alloying element, vitrifying constituent content and existence form etc. all influence the glass forming ability and the microtexture of band, thereby influence fragility.Therefore, the ideal alloy designs brings opportunity can for the fragility improvement of non-crystaline amorphous metal.
The Fe-based amorphous alloy Fe-P-C (1970s) the earliest that is born causes the non-crystaline amorphous metal embrittlement that makes owing to contain the alloy of P, big limitations its application as potential soft magnetic materials and structure.Other contain the P non-crystaline amorphous metal, for example FePB, FeCoP, FeSiP, the CoP of binary, FeP alloy etc. also is faced with same predicament.
People have attempted in the Fe-Si-B system, adding Sn, S improves crystallization and the thermally-stabilised problem of bringing because of technological factor, but being with of gained is frangible, and distribution of additives is inhomogeneous.Add P and C and can improve saturation induction density equally, but resulting also frangible, can't carry out following process and use.It is Fe that one Chinese patent application CN 1065295A discloses expression formula 79 ~ 80P 11 ~ 13C 6 ~ 8, Fe 77 ~ 81Si 1 ~ 3B 2 ~ 4P 1 ~ 11C 4 ~ 7, Fe 80 ~ 83Si 7 ~ 10P 8 ~ 10And the non-crystaline amorphous metal that contains the P element of combination, these cost of alloy are cheap, excellent performance, but, be faced with the problem of alloy embrittlement with above-mentioned similar.
U.S. Pat 5958153A has announced that a kind of P content is lower than 0.1%, thickness is (FeSiBC) in the expression formula of 40-90 μ m 100-xP xAlloy strip steel rolled stock, the P in the alloy mixes with approximate impurity form.
U.S. Pat 5626690 has been announced a kind of FeSiBP (C) alloy of the P of containing element, and alloy Fe content is all at 80 atom % and following, and Si content is higher than 10 atom %, and its P content is lower than 2 atom %.
This is most important reason wherein, possibly be the amorphous alloy that contains P, owing to gathering partially of P causes embrittlement.But the P element more promotes amorphous to form than Si element, be one of most important metalloid element during amorphous becomes, and the P element is with low cost, obtains easily.Therefore, the FeP base noncrystal alloy that contains P still has the important commercial exploitation and is worth.And suppress the gathering partially of P element, FeP base noncrystal alloy that development and Design goes out good-toughness, become one of major objective of material development personnel.
In sum, lacking toughness is good in the market FeP base noncrystal alloy and goods thereof, so this area still exists having the needs of fine magnetic property and flexible FeP base noncrystal alloy concurrently.
Summary of the invention
To the problems referred to above of the prior art, the purpose of this invention is to provide a kind of FeP base noncrystal alloy and preparation method thereof, it not only has good toughness, also possesses good plasticity, good magnetic property and good amorphous formation ability.
For realizing above-mentioned purpose, the invention provides following technical scheme:
A kind of H.T. iron phosphorus base noncrystal alloy strip, wherein, the chemical formula of said iron phosphorus base noncrystal alloy is Fe aP bB cM d, wherein M is Nb, V, and at least a among Ta and the Ti pressed atomic percent, and a is 100-b-c-d% in the formula, and b is 2-20%, and c is 0.5-15%, d is 0.5-5%.
The breaking strain ε of said iron phosphorus base noncrystal alloy strip fMore than 0.02, ductile-brittle transition temperature T DBMore than 150 ℃, saturation induction density Bs more than 1.40T, coercivity H below 3.0A/m, loss P 11/50Below 0.3W/kg.
The chemical formula of said iron phosphorus base noncrystal alloy is Fe aP bB cM d, wherein M is Nb, V, and at least a among Ta and the Ti pressed atomic percent, and a is 100-b-c-d% in the formula, and b is 8-15%, and c is 2-7%, d is 0.5-3%.
The breaking strain ε of said iron phosphorus base noncrystal alloy fMore than 0.025, ductile-brittle transition temperature T DBMore than 165 ℃, saturation induction density Bs more than 1.45T, coercivity H below 2.7A/m, loss P 11/50Below 0.28W/kg.
Fe is partly substituted by Co below the 50at% and/or Ni.
Fe can partly be substituted by at least a element among the Zr below the 5at%, Hf, W, Mo, Mn, Cr, Re, platinum family element, REE, Zn, In, As, Sb, Bi, Ca, Cu, S, Te, Be, Pb, the Mg.
P can partly be substituted by at least a element among the Si below the 5at%, N, Sn, Ge, Ga, Al, the C.
A kind of preparation method of H.T. iron phosphorus base noncrystal alloy strip, wherein, this method comprises the steps:
(1) chemical formula of this iron phosphorus base noncrystal alloy is Fe aP bB cM d, wherein M is Nb, V, and at least a among Ta and the Ti pressed atomic percent, and a is 100-b-c-d% in the formula, and b is 2-20%, and c is 0.5-15%, d is that the 0.5-5% batching is mother alloy;
(2) said mother alloy is heated to 1300 ℃, and with its fusing and be prepared into molten alloy;
(3) under atmosphere protection, said molten alloy is ejected into roller speed is rapid quench on the 28m/s copper roller, obtaining width is that 5 ± 0.1mm, thickness are the iron phosphorus base noncrystal alloy strip of 28 ± 1 μ m.
In step (1), be Fe according to the chemical formula of iron phosphorus base noncrystal alloy aP bB cM d, wherein M is Nb, V, and at least a among Ta and the Ti pressed atomic percent, and a is 100-b-c-d% in the formula, and b is 8-15%, and c is 2-7%, d is the 0.5-3% batching.
The alloy designs of FeP base noncrystal alloy of the present invention is according to as follows, and wherein the constituent content among the present invention is atomic percentage conc:
Fe is the important element of magneticsubstance.On the one hand, Fe content is 70% when following, and because of magneticflux-density is low and impracticable, on the other hand, Fe content surpasses at 85% o'clock, increases the Fe loss, and thermostability also worsens, so Fe content is limited in the scope of 70-85%.Preferably, the Fe content range is 75% to 83%.
P is the important element that promotes that amorphous forms, and its content will satisfy: 2%≤P≤20%, the scope that is more preferably are 8%≤P≤15%.In metalloid element, P is to maximum one of the saturation induction density contribution that reduces alloy, and the P too high levels can reduce the saturation induction density of alloy, and therefore, suitable P content is lower than 20%; And when P less than 2% the time, the promotion amorphous of P element forms, suppresses the effect of crystallization and can't bring into play.
B forms amorphous useful element, when B content less than 0.5% the time, the B constituent content is too low, then the thermostability of alloy is too poor, and is difficult for forming amorphous alloy; And when B content greater than 15% the time, then can reduce ferromagnetic element content in the alloy and reduce the saturation induction density of alloy.Therefore, B content of the present invention is in the scope of 0.5-15%.Preferably, B content is 2% to 7%.
The M element is the most important element that improves alloy toughness and add, and wherein M is Nb, V, Ta, at least a among the Ti.Contriver of the present invention is surprised to find that when in Fe-P-B ternary amorphous, adding an amount of M element, the toughness of alloy has greatly improved.Research thinks that this all has the intensive chemical interaction with Fe, P and B probably owing to the M element, and original P is gathered the size of particles reduction partially, thereby has reduced the destruction of P element.Thereby make the minimizing of FePBM non-crystaline amorphous metal of the present invention embrittlement, be suitable for industrial production and application.Because the M element is non-ferromagnetic elements, the M constituent content surpasses at 5% o'clock, can reduce saturation induction density; And the M constituent content is less than at 0.5% o'clock, is difficult to bring into play the M element and improves the effect of alloy flexible.Therefore, M of the present invention is Nb, V, and Ta, at least a among the Ti, and M content is in the scope of 0.5-5%.Preferably, M content is in the scope of 0.5-3%.
The preparation of iron phosphorus base noncrystal alloy of the present invention, similar with the amorphous band preparation method of routine.The mother alloy that is about to form composition of the present invention is heated to 1300 ℃, and with its fusing and be prepared into molten alloy.Under atmosphere protection, molten alloy is ejected into roller speed is rapid quench on the 28m/s copper roller, obtaining width is that 5 ± 0.1mm, thickness are the amorphous thin ribbon of 28 ± 1 μ m.Because toughness, fragility are the intrinsic properties of amorphous alloy, so tough-brittle transition can be ignored at this by the influence of thickness of strip.
Adopt following testing method to test the performance of iron phosphorus non-crystalline alloy of the present invention, specific as follows:
(1) adopts the quench breaking strain ε of attitude amorphous band of plate bending method measurement f
The amorphous alloy flexible characterizes has several different methods, wherein the most simply is the plate bending method, and this method is that the amorphous band of t places between two parallel plates with thickness, dwindles dull and stereotyped spacing, makes band crooked.If when distance between plates is d, strip breaks, then the toughness of band is represented with breaking strain:
ε f=t/(d-t) (1)
Work as ε f=1 o'clock, band showed as toughness fully, i.e. doubling is not ruptured for 180 °.Generally speaking 0<ε f≤1.
(2) ductile-brittle transition temperature T DB
Weighing the brittle another kind of domestic method of amorphous alloy is to confirm its toughness-brittle transition temperature, i.e. ductile-brittle transition temperature T DBIn the present invention, at first with the sample of heterogeneity at its crystallization temperature T xFollowing differing temps (for example 50-400 ℃, 10 ℃ of each temperature intervals) isothermal annealing 60 minutes at room temperature adopts the plate bending method to confirm T then DBValue.Ductile-brittle transition temperature is high more, shows that the toughness of this non-crystaline amorphous metal is good more, and fragility is poor more.The T of general Fe-based amorphous alloy DBValue is more than room temperature.
(3) soft magnetic performance
In order to measure soft magnetic performance of the present invention, it is that 20mm, internal diameter are the iron core of 16mm that above-mentioned amorphous band alloy of the present invention is wound into external diameter.Under argon shield, at the proper temperature that is lower than crystallization temperature 50K, isothermal annealing 60 minutes.The SY8232B-H tester is adopted in loss measurement, and test condition is magnetic strength 1.1T, and frequency is 50Hz, is designated as P 11/50The saturation induction density B of alloy sAdopting static magnetic energy measurement appearance, is that magnetic induction density under the 800A/m is as the saturation induction density B of alloy with magnetic field sThe coercive force H of alloy cAdopt B-H magnetic hysteresis loop tester to record.
Compared with prior art, beneficial effect of the present invention is:
Amorphous alloy material of the present invention has good toughness, good plasticity, the soft magnetic performance of excellence and good amorphous formation ability, can be widely used in various core materials; In addition, the preparation method of alloy material is simple, and therefore low production cost has important industrial application value.
Embodiment
Embodiment 1
At iron phosphorus base noncrystal alloy Fe of the present invention aP bB cM dComposition range in the preparation a different set of quad alloy sample; Wherein the composition of sample is as shown in table 1; Sample number into spectrum 1-21 is the embodiment prepared according to the present invention; Sample number into spectrum 22-31 is a Comparative Examples, is according to the prepared iron phosphorus base noncrystal alloy of the prior art of the method identical with present embodiment.
The mother alloy of forming shown in the table 1 is heated to 1300 ℃, and with its fusing and be prepared into molten alloy.Under atmosphere protection, molten alloy is ejected into roller speed is rapid quench on the 28m/s copper roller, obtaining width is that 5 ± 0.1mm, thickness are the amorphous thin ribbon of 28 ± 1 μ m.
According to testing method of the present invention, adopt the quench breaking strain ε of attitude amorphous band of flat band method measurement fAfter differing temps annealing, confirm the ductile-brittle transition temperature T of sample DBIt is that 20mm, internal diameter are the iron core of 16mm that the band alloy is wound into external diameter, and under argon shield, isothermal annealing is 60 minutes under 650K, measures its soft magnetic performance then, records the saturation induction density B of iron phosphorus base noncrystal alloy of the present invention respectively s, coercive force H cAnd loss P 11/50It is as shown in table 1 to test resulting result.
Can find out by table 1, according to iron phosphorus base noncrystal alloy Fe of the present invention aP bB cM dEmbodiment, i.e. sample 1-20, its saturation induction density B sAll more than 1.40T, coercive force H cAll below 3.0A/m, loss P 11/50All at 0.30W/kg and following, breaking strain ε fAll more than 0.02, ductile-brittle transition temperature T DBAll more than 150 ℃.The Fe-P-B ternary alloy of M element is not added in contrast, and promptly Comparative Examples 22-31 can find out, embodiments of the invention all obviously are superior to Comparative Examples of the prior art on toughness and soft magnetic performance.
The composition and the The performance test results of the iron phosphorus base noncrystal alloy of table 1 embodiment of the invention and Comparative Examples
Figure BDA00002036208200071
Annotate: subscript bal. represents surplus
Embodiment 2
According to the composition range of iron phosphorus base noncrystal alloy of the present invention, prepare a different set of quinary alloy sample, wherein the composition of sample is as shown in table 2, and sample number into spectrum 32-57 is another group embodiment prepared according to the present invention.
The mother alloy of forming shown in the table 2 is heated to 1300 ℃, and with its fusing and be prepared into molten alloy.Under atmosphere protection, molten alloy is ejected into roller speed is rapid quench on the 28m/s copper roller, obtaining width is that 5 ± 0.1mm, thickness are the amorphous thin ribbon of 28 ± 1 μ m.
According to testing method of the present invention, adopt the quench breaking strain ε of attitude amorphous band of flat band method measurement fAfter differing temps annealing, confirm the ductile-brittle transition temperature T of sample DBIt is that 20mm, internal diameter are the iron core of 16mm that the band alloy is wound into external diameter, and under argon shield, isothermal annealing is 60 minutes under 650K, measures its soft magnetic performance then, records the saturation induction density B of iron phosphorus base noncrystal alloy of the present invention respectively s, coercive force H cAnd loss P 11/50It is as shown in table 2 to test resulting result.
Can find out by table 2, according to iron phosphorus base noncrystal alloy Fe of the present invention aP bB cM dAnother group embodiment, i.e. sample 32-57, its saturation induction density Bs all more than 1.40T, coercivity H all below 3.0A/m, loss P 11/50All below 0.3W/kg, breaking strain ε fAll more than 0.20, ductile-brittle transition temperature T DBAll more than 150 ℃.The Fe-P-B ternary alloy of M element is not added in contrast, and promptly Comparative Examples 22-31 can find out, embodiments of the invention all obviously are superior to Comparative Examples of the prior art on toughness and soft magnetic performance.
The composition and the The performance test results of the iron phosphorus base noncrystal alloy of another group of table 2 the present invention embodiment
Figure BDA00002036208200091
Annotate: subscript bal. represents surplus

Claims (9)

1. H.T. iron phosphorus base noncrystal alloy strip, it is characterized in that: the chemical formula of said iron phosphorus base noncrystal alloy is Fe aP bB cM d, wherein M is Nb, V, and at least a among Ta and the Ti pressed atomic percent, and a is 100-b-c-d% in the formula, and b is 2-20%, and c is 0.5-15%, d is 0.5-5%.
2. iron phosphorus base noncrystal alloy strip according to claim 1 is characterized in that: the breaking strain ε of said iron phosphorus base noncrystal alloy strip fMore than 0.02, ductile-brittle transition temperature T DBMore than 150 ℃, saturation induction density Bs more than 1.40T, coercivity H below 3.0A/m, loss P 11/50Below 0.3W/kg.
3. iron phosphorus base noncrystal alloy strip according to claim 1, it is characterized in that: the chemical formula of said iron phosphorus base noncrystal alloy is Fe aP bB cM d, wherein M is Nb, V, and at least a among Ta and the Ti pressed atomic percent, and a is 100-b-c-d% in the formula, and b is 8-15%, and c is 2-7%, d is 0.5-3%.
4. iron phosphorus base noncrystal alloy strip according to claim 1 is characterized in that: the breaking strain ε of said iron phosphorus base noncrystal alloy fMore than 0.025, ductile-brittle transition temperature T DBMore than 165 ℃, saturation induction density Bs more than 1.45T, coercivity H below 2.7A/m, loss P 11/50Below 0.28W/kg.
5. according to claim 1 or 3 described iron phosphorus base noncrystal alloy strips, it is characterized in that: Fe is partly substituted by Co below the 50at% and/or Ni.
6. according to claim 1 or 3 described iron phosphorus base noncrystal alloy strips, it is characterized in that: Fe can partly be substituted by at least a element among the Zr below the 5at%, Hf, W, Mo, Mn, Cr, Re, platinum family element, REE, Zn, In, As, Sb, Bi, Ca, Cu, S, Te, Be, Pb, the Mg.
7. according to claim 1 or 3 described iron phosphorus base noncrystal alloy strips, it is characterized in that: P can partly be substituted by at least a element among the Si below the 5at%, N, Sn, Ge, Ga, Al, the C.
8. the preparation method of a H.T. iron phosphorus base noncrystal alloy strip as claimed in claim 1, it is characterized in that: this method comprises the steps:
(1) chemical formula of this iron phosphorus base noncrystal alloy is Fe aP bB cM d, wherein M is Nb, V, and at least a among Ta and the Ti pressed atomic percent, and a is 100-b-c-d% in the formula, and b is 2-20%, and c is 0.5-15%, d is that the 0.5-5% batching is mother alloy;
(2) said mother alloy is heated to 1300 ℃, and with its fusing and be prepared into molten alloy;
(3) under atmosphere protection, said molten alloy is ejected into roller speed is rapid quench on the 28m/s copper roller, obtaining width is that 5 ± 0.1mm, thickness are the iron phosphorus base noncrystal alloy strip of 28 ± 1 μ m.
9. preparation method according to claim 8 is characterized in that: in step (1), be Fe according to the chemical formula of iron phosphorus base noncrystal alloy aP bB cM d, wherein M is Nb, V, and at least a among Ta and the Ti pressed atomic percent, and a is 100-b-c-d% in the formula, and b is 8-15%, and c is 2-7%, d is the 0.5-3% batching.
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