CN101701327B - Iron-based bulk amorphous soft magnetic alloy and preparation method thereof - Google Patents
Iron-based bulk amorphous soft magnetic alloy and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an iron-based bulk amorphous soft magnetic alloy and a preparation method thereof; the molecular formula of the amorphous alloy is (Fe 0.5Co0.5) 70.7-xB20Si5Nb4.3Tbx; wherein the numeric range of x is x larger than or equal to 0 and less than or equal to 2.5; the amorphous alloy is obtained by adding a rare earth element Tb into FeCo BSiNb system. Compared with the prior art, the iron-based bulk amorphous soft magnetic alloy prepared by industrial material has bigger amorphous formation capability and excellent soft magnetic performance; the diameter of the prepared amorphous bar material is 2mm-3mm, the saturation magnetization strength is 0.69 T-0.92 T, and the coercive force is 2.1A/m-3.8 A/m, which are relatively row compared with other doped rare-earth element systems. The preparation method is simple and has lower cost. The iron-based bulk amorphous soft magnetic alloy can be used as a core of a magnetic sensor and is applied to fields such as information, communication and the like.
Description
Technical field
The present invention relates to the amorphous alloy field, the industrial feedstock production of particularly a kind of usefulness have FeCoBSiNbTb Al-Cu-Zn block amorphous alloy material of excellent soft magnet performance and preparation method thereof.
Background technology
Amorphous alloy also is called as glassy alloy; Normally under extreme harsh conditions, be prepared from; With the melt metal alloy with the cooling of cooling rate faster; In fast cold process, suppressed the formation of nucleus and grown up, be the unordered amorphous alloy of long-range on a kind of structure thereby directly solidify to form.1938, the Kramer reported first successfully prepared noncrystalline membrane (list of references 1:J.Karmer, Z.Phys. with the method for hydatogenesis; 106 (1937) 675); The method of employing electro-deposition such as Brenner has soon been prepared Ni-P, the Co-P thin film of amorphous alloy, and be used for protecting metallic surface (list of references 2:A.Brenner D.E.Couch and E.Killiams as face coat; J Res.Natn.Bur.Stand., 29 (1950) 1049).But non-crystaline amorphous metal truly is to the sixties in 20th century.Nineteen sixty, Duwez group of California Inst Tech USA has invented that to adopt lance technology to come the rapid quenching technology of chilling metal liquid to prepare AuSi be amorphous ribbon, the non-crystaline amorphous metal of the reported first in the world of called optical imaging that Here it is.(W.Klement，R.H.Wilens，and?Duwez，Nature.，181(1960)869-870)。But the preparation of traditional non-crystaline amorphous metal needs 10
5-10
6High critical cooling rate (the R of k/s
c), so mostly non-crystaline amorphous metal is low dimension shapes such as film, band, filament or powder, this has also limited the range of application of amorphous in actual engineering widely.
For the restriction of the shape and size that overcome amorphous alloy material, people were making unremitting effort for the preparation bulk amorphous alloys in the last few years.As through transforming technology of preparing and optimizing alloying component, break through the restriction of high cooling condition with this.Usually we are defined as the non-crystaline amorphous metal of mm size large block amorphous.1974, the Pd-Cu-Si alloy that contains precious metal element Pd was with 10
3The cooldown rate of K/s is prepared to amorphous bar (document 3, H.S.Chen, the Acta Metall. that diameter is 1mm; 1974, Vol.22, pp1505-1508.); Since then; The large block amorphous beginning occurs, and the application prospect of amorphous alloy material has been expanded in its appearance, and becomes a hot issue in amorphous field.Up to 1989, the Inoue etc. of Japan has found not contain noble metal first and can prepare millimetre-sized MgCuY through the copper mold casting was non-crystaline amorphous metal formation system (document 4, A.Inoue with LaAlNi; T.Zhang and T.Masumoto; Mater.Trans., JIM, 30 (1989) 965-972).After this, under low cooldown rate, can form large block amorphous alloy system and be developed in succession, comprise alloy systems such as Mg-, Ln-, Zr-, Cu-, Co-, Ni-, Nd-, Fe-base.But owing to all comprise a large amount of precious metals or rare metal in most noncrystal substrates, the expensive prices of raw and semifnished materials make non-crystaline amorphous metal be difficult to obtain broad practice.Wherein Fe-based amorphous alloy is compared with other bulk amorphous alloys system, and the prices of raw and semifnished materials reduce greatly.
As everyone knows, transducer is the basis of various instrument and meters and automation equipment, and especially current is that sensor technology is more being born the important task of the information of obtaining in the information-intensive society that indicates with the electronic computer.Not hard to imagine; If lose the support of sensor technology; Any advanced person's automation equipment all will become " castles in the air ", and difficulty is had place to show one's prowess, so the state-of-art of transducer has been represented the industrialized level and the whole scientific and technological level of a country to a certain extent.Wherein magnetic sensor is the important branch of transducer, and is increasingly extensive in the application of every field such as national economy every profession and trade, guidance navigation, defence and military, safety, environmental protection and geophysical observatory.The key element of magnetic sensor is a core body; Because amorphous alloy has excellent soft magnet performance; Thereby adopt non-crystalline material to have highly sensitive as the transducer of core body; Frequency response is good, characteristics such as low in energy consumption and DC measurement good stability, and this has promoted the research of people to Fe base block amorphous alloy with unique soft magnet performance to a great extent.It is soft magnetic amorphous strip that the development of Fe base soft magnetic amorphous alloy is successfully developed FePC since U.S. professor Duwez in 1967, and from then on many scientists have paid a large amount of effort in the process of synthesizing the novel Fe base noncrystal alloy with excellent soft magnet performance.U.S. Allied Signal companies in 1979 develop the planar flows Cast Strip technology in non-crystaline amorphous metal broadband; And in the Fe base system row amorphous alloy strips (document 5 of nineteen eighty-two release called after Metglass; Hsiao A; Turqut Z.Crystallization and nanocrystallization kinetics ofFe-based amorphous alloys.Mater Res Soc Symp Proc, 1999,577:551-556.).The people such as Yashiawa of FDAC metal company in 1988 develop FeCuNbSiB nano-crystal soft magnetic alloy with low cost through the crystallization processing on the non-crystaline amorphous metal basis.Along with the continuous progress of science, people deepen continuously to the understanding of Fe base amorphous alloy, and existing a large amount of non-crystaline amorphous metal system is developed.Wherein comparatively be typically nineteen ninety-five, begin one's study Fe base massive non-crystalline material and of A.Inoue at Fe
72Al
5Ga
2P
11C
6B
4And Fe
73Al
5Ga
2P
11C
5B
4Successfully synthetic bulk Fe base noncrystal alloy (document 6, A.Inoue, G.S.Gook in the alloy; Mater.Trans.JIM 36 (1995) 1180-1183.) and 2004, B.L.Shen, A.Inoue and C.T.Chang exploitation have the superhigh intensity and a better (Fe of soft magnet performance; Co)-B-Si-Nb (document 6; B.L.Shen, A.Inoue and C.T.Shen, Appl.Phys.Lett.85 (2004); 4911-4913.) Fe-based amorphous alloy has excellent soft magnet performance, has high saturation and magnetic intensity and low-coercivity.
Summary of the invention
First technical problem to be solved by this invention is to provide a kind of cost low, easy preparation to the above-mentioned state of the art, has the iron-based bulk amorphous soft magnetic alloy material of good amorphous formation ability, thermal stability and excellent soft magnet performance simultaneously.
Second technical problem to be solved by this invention provides low, the easy preparation of a kind of cost, has the preparation method of the iron-based bulk amorphous soft magnetic alloy of good amorphous formation ability, thermal stability and excellent soft magnet performance simultaneously.
The technical scheme that the present invention is taked for above-mentioned first technical problem of solution is: a kind of iron-based bulk amorphous soft magnetic alloy is characterized in that the molecule skeleton symbol of this alloy is (Fe
0.5Co
0.5)
70.7-xB
20Si
5Nb
4.3Tb
x, wherein the span of x is 0≤x≤2.5.
Described iron-based bulk amorphous soft magnetic alloy obtains through in FeCoBSiNb system, adding rare earth element tb.
In non-crystaline amorphous metal, add proper amount of rare-earth element T b, the content of Tb is controlled within 2.5% (the atomic molar percentage), and the amorphous formation ability of alloy is improved.The effect of Tb in alloy is many-sided, and according to the Inoue theory analysis, rare earth Tb role in system can be thought: the difference of the atomic size that the one side rare earth causes and the more negative heat of mixing play bigger effect in amorphous formation ability.Tb has bigger atomic size 0.178nm; And the negative heat of mixing of it and little atom B, Si is all very big, and (Tb-B is-36KJ/mol; Tb-Si is-57KJ/mol); The interpolation of rare earth has caused variation continuous on the atomic size, has produced the new atom pair with big negative heat of mixing simultaneously, must cause the stacking provisions of system tightr.On the other hand, from the thermodynamics viewpoint, alloy middle rare earth Tb has very strong adsorptivity to oxygen, thereby has suppressed the adverse effect of oxygen in fusion and casting process, has suppressed heterogeneous forming core, can improve amorphous formation ability.On Shen Baolong researcher has given to the world the result of one's studies the basis (document 6, B.L.Shen, A.Inoue and C.T.Shen, Appl.Phys.Lett.85 (2004) 4911-4913.) adds that previous experiments gropes, and obtains alloy system (Fe
0.5Co
0.5)
70.7-xB
20Si
5Nb
4.3Tb
xSo this iron-base block amorphous alloy is characterised in that this molecule skeleton symbol is (Fe
0.5Co
0.5)
70.7-xB
20Si
5Nb
4.3Tb
x, and the span of x is 0≤x≤2.5.
The present invention for above-mentioned second technical scheme that technical problem adopted of solution is: a kind of preparation method of iron-base large-block amorphous alloy is characterized in that comprising following step:
1) batching; According to the atomic molar ratio Fe in the component, Co, B, Si, Nb, Tb are prepared burden; Fe: Co: B: Si: Nb: Tb=(34.1～35.35) wherein: (34.1～35.35): 20: 5: 4.3: (0～2.5); Earlier convert alloy atom percentage into mass percent, distinguish the good Fe of weighing, Co, Tb, Si, Nb, FeB in proportion, what pay special attention to is that B is the form adding with industrial FeB alloy;
2) preparation alloy pig, in being full of the arc furnace of argon gas, with each the component batching in the step 1), melting obtains mother alloy ingot after the cooling;
3) casting alloy bar uses the permanent mold casting method, with step 2) the mother alloy ingot refuse that makes, through copper mold casting preparation amorphous bar, perhaps use single roller to get rid of the band method and make continuous amorphous ribbon;
The molecule skeleton symbol of described a kind of iron-base large-block amorphous alloy is (Fe
0.5Co
0.5)
70.7-xB
20Si
5Nb
4.3Tb
x, wherein the span of x is 0≤x≤2.5;
In the batching, the purity of Fe, Co, Tb raw material all is not higher than 99.0wt%.
As improvement; Use the electric arc melting melt back three to four times before the used Co batching in the step 1); The rare earth Tb of as easy as rolling off a log oxidation is then with the grinder buffing surface or with three to four times polishings again of electric arc melting melt back, to reduce the impurity in the raw material or to remove oxide layer;
As improvement, described non-crystaline amorphous metal diameter of rod is 2mm-3mm.
As improvement, will test coercitive amorphous ribbon annealing, annealing process is annealing temperature T
g-30K～T
gStress annealing 250-350S under the-70K.
Compared with prior art, iron-base large-block amorphous alloy provided by the invention is compared with existing non-crystaline amorphous metal, and its advantage is:
(1) has wide supercooling liquid phase region, its Δ T
x(Δ T
x=T
g-T
x, T
gBe glass transformation temperature, T
xBe crystallization temperature) between 58K-84K, and the increase gradually along with increasing of Tb content;
(2) have high reduction glass transformation temperature, its T
g/ T
1(T
gBe glass transformation temperature, T
1Be liquidus temperature) between 0.597-0.614;
(3) have stronger amorphous formation ability, will use the alloy pig casting non-crystal bar of industrial preparation of raw material with copper mold casting method, its diameter is at 2-3mm;
(4) has higher saturation induction density, its saturation magnetization M
sBe 0.69T-0.92T;
(5) has low-coercivity, its H
cBetween 2.1-3.8A/m;
Its raw material of the preparation method of a kind of iron-base large-block amorphous alloy provided by the invention adopts industrial raw material, and the preparation method is simple, and cost is lower.
Description of drawings
Fig. 1 is that the diameter of embodiment 3 preparations is the XRD figure of the large block amorphous sample of 3mm;
Fig. 2 is the photo in kind of the iron-base large-block amorphous sample of embodiment 3 preparations;
Fig. 3 is poor formula scanning calorimetric (DSC) curve chart of the iron-base large-block amorphous sample of embodiment 1-6 preparation, and its rate of heat addition is 0.67K/s, mainly tests its Curie temperature T
c, glass transition temperature T
gAnd crystallization temperature T
x
Fig. 4 is poor formula scanning calorimetric (DSC) curve chart of the iron-base large-block amorphous sample of embodiment 1-6 preparation, and the heating rate of heating-up section is 0.67K/s, and the cooling curve rate of temperature fall is 0.067K/s, mainly tests its fusion temperature T
mAnd liquidus temperature T
1
Fig. 5 is the B-H magnetic hysteresis loop figure of the iron-base large-block amorphous sample of embodiment 1-6 preparation.
Embodiment
Below in conjunction with examples of implementation the present invention is further specified.
Embodiment 3
Preparation (Fe
0.5Co
0.5)
69.7B
20Si
5Nb
4.3Tb
1.0Bulk metallic glass.
With raw material Fe, Co, FeB; Si; Nb, Tb is Fe: Co: B: Si: Nb: Tb=34.85 by atomic percent: 34.85: 20: 5: 4.3: 1 batchings, the purity of Fe, Co, Tb all is not higher than 99.0wt% and B and adds with the form of industrial FeB alloy in the raw material; The arc-melting furnace of the material for preparing being put into argon atmospher mixes and melting 4-5 time, obtains (Fe after the cooling
0.5Co
0.5)
69.7B
20Si
5Nb
4.3Tb
1.0Mother alloy ingot, and spindle is broken into fritter; Use vacuum copper mold casting method then, with this fritter ingot casting refuse, the foundry alloy melt is pressed among the copper mold, can obtain composition is (Fe
0.5Co
0.5)
69.7B
20Si
5Nb
4.3Tb
1.0, diameter is the bulk amorphous alloys of 3mm.
Can prove that from X-ray diffraction shown in Figure 1 (XRD) diameter is 3mm (Fe
0.5Co
0.5)
69.7B
20Si
5Nb
4.3Tb
1.0Alloy is an amorphous alloy completely.Fig. 2 is a series of amorphous bars of this composition preparation photo in kind, and wherein full-size is 3mm.Comprised among Fig. 3 and Fig. 4 and be (Fe
0.5Co
0.5)
69.7B
20Si
5Nb
4.3Tb
1.0Heat analysis (DSC) figure of bulk amorphous alloys, as can be seen from the figure: its Curie temperature (T
c), glass transition temperature (T
g), crystallization begins temperature (T
x), the width Delta T of mistake cold-zone liquid phase
xAnd liquidus temperature (T
1) be respectively 599K, 844K, 909K, 65K and 1374K.In addition, this alloy also has higher reduction glass temperature (T
Rg), its value is 0.614.T
RgValue can be used for judging the glass forming ability of non-crystaline amorphous metal usually.Therefore (Fe
0.5Co
0.5)
69.7B
20Si
5Nb
4.3Tb
1.0Bulk amorphous alloys has stronger amorphous formation ability.Its room temperature magnetic hysteresis loop is as shown in Figure 5, and the result shows, (Fe
0.5Co
0.5)
69.7B
20Si
5Nb
4.3Tb
1.0The saturation magnetization of bulk amorphous alloys is 0.88T, has also listed the coercive force of this composition among Fig. 5, and coercive force is 2.5A/m.
Embodiment 1,2, and 4,5,6
The iron-base large-block amorphous alloy for preparing various proportionings.
Prepare a series of iron-base large-block amorphous alloys of various proportionings by the method for embodiment 1, it is formed and thermal physical property parameter is listed in the table 1.
Annotate: 1) the symbol implication is following in the table:
Cut off diameter size under Φ---this experiment condition; T
c---Curie temperature; T
g---glass transformation temperature; Δ T
x---the supercooling liquid phase region width; T
1---liquidus temperature; T
Rg---the reduction glass temperature; M
s---saturation magnetization; H
c---coercive force.
2)T
rg＝T
g/T
1；
3) in the table during each composition sample in measurement the used rate of heat addition be 40K/min.
The composition of the iron-base large-block amorphous alloy of table 1. various proportionings of the present invention, thermal property and magnetic performance parameter
| Embodiment | Alloying component | Φ (mm) | T c(K) | T g(K) | T x(K) | ΔT x(K) | T 1(K) | T g/T 1 | M s(T) | H c (A/m) |
| 1 | (Fe 0.5Co 0.5) 70.7B 20Si 5Nb 4.3Tb | 2 | 625 | 842 | 900 | 58 | 1410 | 0.597 | 0.92 | 2.1 |
| 2 | (Fe 0.5Co 0.5) 70.2B 20Si 5Nb 4.3Tb 0.5 | 2.5 | 613 | 842 | 901 | 59 | 1386 | 0.608 | 0.91 | 2.3 |
| 3 | (Fe 0.5Co 0.5) 69.7B 20Si 5Nb 4.3Tb 1.0 | 3 | 599 | 844 | 909 | 65 | 1374 | 0.614 | 0.88 | 2.5 |
| 4 | (Fe 0.5Co 0.5) 69.2B 20Si 5Nb 4.3Tb 1.5 | 2.5 | 599 | 846 | 912 | 66 | 1380 | 0.613 | 0.84 | 3.2 |
| 5 | (Fe 0.5Co 0.5) 68.7B 20Si 5Nb 4.3Tb 2.0 | 2 | 579 | 852 | 928 | 76 | 1414 | 0.603 | 0.84 | 3.8 |
| 6 | (Fe 0.5Co 0.5) 68.2B 20Si 5Nb 4.3Tb 2.5 | 2 | 523 | 863 | 947 | 84 | 1431 | 0.603 | 0.69 | 3.8 |
Iron-base large-block amorphous alloy provided by the invention has stronger amorphous formation ability and excellent soft magnet performance, can be applied to the magnetic device in fields such as information, communication.
Claims (1)
1. an iron-based bulk amorphous soft magnetic alloy is characterized in that the molecular formula of this alloy is (Fe
0.5Co
0.5)
70.7-xB
20Si
5Nb
4.3Tb
x, wherein the span of x is 0＜x≤2.5;
Its preparation process is:
1) batching; According to the atomic molar ratio Fe in the component, Co, B, Si, Nb, Tb are prepared burden; Fe: Co: B: Si: Nb: Tb=(34.1～35.35) wherein: (34.1～35.35): 20: 5: 4.3: (0～2.5); Wherein B is the form adding with industrial FeB alloy, and Fe, Co, Tb purity all are no more than 99.0%;
2) the preparation master alloy ingot places arc furnace with the above-mentioned raw material for preparing, and melt back is four to five times under argon shield, obtains mother alloy ingot after the cooling;
3) casting alloy bar uses the permanent mold casting method, with step 2) the mother alloy ingot refuse that makes, adopt copper mold casting method, make (Fe
0.5Co
0.5)
70.7-xB
20Si
5Nb
4.3Tb
xThe Al-Cu-Zn block amorphous alloy bar perhaps gets rid of the band method with single roller and prepares continuous amorphous ribbon;
Wherein, will use the electric arc melting melt back three to four times before the raw material Co batching, and rare earth Tb to use grinder buffing surperficial or with emery wheel superficial layer is polished for three to four times with the electric arc melting melt back again;
The diameter that makes described non-crystaline amorphous metal bar is 2mm-3mm.
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| CN101928896B (en) * | 2010-08-19 | 2012-05-30 | 中国科学院宁波材料技术与工程研究所 | Large amorphous forming ability iron-based block amorphous magnetic alloy material and preparation method thereof |
| CN102565109B (en) * | 2012-01-06 | 2015-08-19 | 青岛云路新能源科技有限公司 | Phase Analysis |
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| CN103290342B (en) * | 2013-06-19 | 2015-09-02 | 天津非晶科技有限公司 | Fe base noncrystal alloy and preparation method thereof |
| CN103882348B (en) * | 2013-06-21 | 2015-09-30 | 洛阳威尔若普检测技术有限公司 | Galvanomagnetic effect sensor high magnetic permeability amorphous soft magnetic ribbon material and method |
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