CN1403615A - Iron-base bulk amorphous soft-magnetic alloy material - Google Patents

Iron-base bulk amorphous soft-magnetic alloy material Download PDF

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CN1403615A
CN1403615A CN 02128857 CN02128857A CN1403615A CN 1403615 A CN1403615 A CN 1403615A CN 02128857 CN02128857 CN 02128857 CN 02128857 A CN02128857 A CN 02128857A CN 1403615 A CN1403615 A CN 1403615A
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alloy
amorphous
iron
alloy material
magnetic
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CN1173061C (en
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周少雄
金重勋
陈非非
卢志超
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Advanced Technology and Materials Co Ltd
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Central Iron and Steel Research Institute
Advanced Technology and Materials Co Ltd
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Abstract

The present invention relates to the production of functional material, and is the preparation of iron-base bulk amorphous soft-magnetic alloy material. The alloy material has the chemical components including: Fe 75-95 wt%, Sn 0.5-10 wt%, B 0.2-10 wt%, Al less than 6 wt%, V less than 10 wt%, Nb less than 10 wt%, Mo less than 10 wt%, P less than 15 wt%, C less than 5 wt%, Si less than 10 wt%, and Cr+Mn+Ta+Nd+Cu less than or equal to 10 wt%. Compared with available technology, the present invention has wider supercold liquid phase area and excellent soft magnetic performance.

Description

Iron-base bulk amorphous soft-magnetic alloy material
Technical field
The invention belongs to the manufacturing field of functional materials.Be applicable to that more preparation has the iron-base bulk amorphous soft-magnetic alloy material of good soft magnetic performance.
Background technology
Along with developing rapidly of electron trade, in each field every technical performance index of employed various electronic devices and components also in continuous raising, therefore adopt amorphous alloy as soft magnetic materials must use material, used widely already.As everyone knows, the preparation method of amorphous alloy material adopts single-roller method at present, the principle of work of single-roller method is to high speed copper roller rotating Quench face quick solidification forming with the direct spray of molten liquid steel, therefore this preparation method mass production amorphous alloy ribbon continuously, but industrialized mass production.This method has become one of most important method in order to the continuous production amorphous alloy ribbon in recent years.In 1988, the people such as Akihisa Inoue of Japan carried out research and development to the glass forming ability (GFA) of multicomponent amorphous alloys, and adopted methods such as shrend and die casting, successively found Mg-, Ln-, Zr-, Pd-Cu-, Pd-Fe-, several critical cooling rates such as Ti-(R c) low, have the alloy system of wide supercool liquid phase region (supercooled liquid region).But above block amorphous alloy does not all obtain ferromagnetic property.The supercool liquid phase region is an important indicator weighing alloy amorphous formation ability.Generally speaking, traditional non-crystaline amorphous metal does not have the supercool liquid phase region, and has wide supercool liquid phase region (Δ T x＞5OK) existence shows that then this alloy has bigger potential anti-crystallization ability, along with supercool liquid phase region (Δ T x) raising of width, this alloy forms the needed critical cooling rate (R of non-crystalline state c) just more little, therefore this alloy amorphous formation ability (GFA) is just big more.Because as glass transformation temperature (T g) and Tc (T x) between interval when big more, T gThe thermostability of above molten metal is high more, and alloy is difficult for crystallization more, and non-crystalline state is just stable more, also easy more formation bulk amorphous alloy.The size of supercool liquid phase region characterizes with following formula: supercool liquid phase region width (Δ T x)=Tc (T x)-glass transformation temperature (T g).Unit: K.The general differential scanning calorimetric analysis instrument that adopts is measured glass transformation temperature T gAnd Tc T x
In 7 years after nineteen ninety-five, people such as Akihisa Inoue utilize copper mold casting method, have obtained four class ferromegnetism block amorphous alloys, promptly (1) Fe-(Al, Ga)-(P, C, B) and Fe-Ga-(P, C, B),
(2)Fe-(Zr，Hf，Nb)-B，(3)Fe-(Cr，Mo)-B-C，(4)Fe-Co-Ln-B。Should
Class Fe base block amorphous alloy cording has supercool liquid phase region (the Δ T of broad x) and higher saturation induction
Intensity, and lower magnetic properties such as coercive force.See Table 1.
The base block amorphous non-retentive alloy performance of the part Fe of Akihisa Inoue in table 1 prior art
Alloy ???ΔT x(K) ????B s(T) ????B r/B s ????H c(A/m) ????μ o(1kHz)
????Fe 72Al 5Ga 2P 10C 6B 4S ????i 1 ????63 ????1.10 ????0.38- ????0.45 ????0.5- ????12.7 ????7000- ????12000
????Fe 72Al 5Ga 2P 11C 6B 4 ????61 ????1.07 About 0.40 ????5.1 ????9000
????Fe 74Al 4Ga 2P 12Si 4B 4 ????49 ????1.14 ????0.35 ????6.4 ????19000
????Fe 62Nb 8B 30 ????71 ????0.68 ????- ????2.6 ????19300
????Fe 56Co 7Ni 7Zr 10B 20 ????68 ????0.96 ????0.60 ????2.41 ????17700
????Co 40Fe 22Nb 8B 30 ????81 ????0.41 ????- ????2.0 ????29300
????Fe 62Co 9.5Gd 3.5B 25 ????63 ????1.41 ????- ????1.9 ????11000
But being material itself, the main drawback of this Fe base block amorphous alloy exists higher, square ratio of loss and magnetic permeability μ mCharacteristics such as all lower, metal Ga costs an arm and a leg still have certain distance with practicality.
Goal of the invention and content
The objective of the invention is to propose a kind of have wide supercool liquid phase region and all good iron-base bulk amorphous soft-magnetic alloy material of every soft magnetic performance technical indicator.
Iron-base bulk amorphous soft-magnetic alloy material proposed by the invention, it mainly is the material that is applicable to soft magnetic amorphous alloy, we consider is the magnetically soft alloy material of base in order to make material have the supercool liquid phase region of ideal soft magnetic property and broad with FeSnB so propose a kind of.The present invention is by to the reasonable adjustment of alloy ingredient, and by adding some other micro-metals, its purpose is to improve material behavior and every magnetic property of alloy of the present invention.Consider according to above-mentioned requirements and design, iron-base bulk amorphous soft-magnetic alloy material proposed by the invention, the concrete Chemical Composition that it is characterized in that forming this magnetically soft alloy material is (weight %): Fe.75-95%; Sn.0.5-10%; B.0.2-10%; Al.≤6%; V.≤10%; Nb.≤10%; Mo.≤10%; P.≤15%; C.≤5; Si.≤10; Any one or two kinds and two or more sum≤10% in Cr, Mn, W, Ta, Nd, the Cu element.By iron tin boryl bulk amorphous soft-magnetic alloy material proposed by the invention, to consider that promptly material has wide supercool liquid phase region, also to make material obtain good soft magnetic performance simultaneously.Therefore in the composition of material of the present invention, remain employing with the main composition element of iron as soft magnetic materials of the present invention, add as the important element that helps forming amorphous with boron, the interpolation of tin element is as the width that helps expanding the supercool liquid phase region, tin can also improve the operational characteristic of alloy material when casting simultaneously, and has advantages of cheap price.In iron-base bulk amorphous soft-magnetic alloy material of the present invention, be supercool liquid phase region width that further improves non-crystaline amorphous metal and the soft magnetic performance that improves alloy material, also added some other element, for example adding elements such as P, C, Si is to be beneficial to the metalloid element that forms non-crystalline material, adds V, Al, elements such as Nb, Mo for widening the supercool liquid phase region and forming the consideration of amorphous bulk.So Fe adds as main ferromagnetic element in the composition of amorphous bulk of the present invention, Sn is an alloy element, except that low price, mainly is the fusing point that is used to reduce alloy, can improve the technology of amorphous alloy material when casting significantly.B is a metalloid element, and except that can reducing the critical cooling rate that forms non-crystaline amorphous metal, its significant feature is the magnetic property that forms non-crystaline amorphous metal and improve non-crystaline amorphous metal, for example square ratio.Al is an alloy element, unite interpolation with Sn, can further expand supercool liquid phase region width, P, Si are metalloid elements, can reduce the critical cooling rate that forms non-crystaline amorphous metal, mainly also help the formation non-crystaline amorphous metal, C is a metalloid element, can improve the saturation induction density of non-crystaline amorphous metal, and help the formation of non-crystaline amorphous metal, V, Mo, Nb are alloy elements, except that further expanding supercool liquid phase region width, can also improve heat treatment of alloy stability.The material of iron tin boryl non-crystaline amorphous metal of the present invention can adopt single-roller method or copper mold casting method preparation.Adopting single-roller method is to get the mother alloy rod of set amount, puts into the nozzle bag of single roller spray band machine.Main processing parameter is regulated as follows: nozzle bag lower end nozzle mouth seam width is 0.2-0.6mm, and nitrogen or argon gas spraying pressure can be decided to be 0.01-0.5MPa, and nozzle to copper cooling roller spacing is 0.05-0.30mm, adjusts copper cooling roller wheel rim rotating speed to 15-40m/s.The amorphous ribbon width of preparation is 2-10mm, and thickness is 20-50 μ m.The equipment that is adopted is single roller spray band machine.Adopt " copper mold casting " preparation bulk amorphous alloy sample of the present invention, its principle is to utilize gaseous tension to promote metal liquid, copper mold is linked to each other with vacuum, and in furnace chamber, feed the argon gas malleation, after utilizing electric arc with alloy melting, draw back vacuum valve alloy is sucked (utilizing the furnace chamber gaseous tension to clamp-on) to copper mold, the bulk amorphous alloy sample among the present invention has employing " copper mold casting " to prepare.(and, before with molten alloy, can remove to melt a titanium piece to absorb oxygen in the furnace chamber with electric arc earlier in order to reduce the influence of oxygen content in the furnace chamber, melt sample again.) to adopt the diameter with wide supercool liquid phase region iron tin boron alloy made of the present invention be the bar of 1mm and 2mm, in order to obtain annular amorphous iron core sample, the copper mold groove directly can be designed to annular recesses, the sample that take out the casting back is annular block iron core.
Adopt the prepared sample of wide supercool liquid phase region iron tin boryl non-crystaline amorphous metal that has of the present invention, be: 1. differential scanning calorimetric analysis through different detection modes; Adopt the differential scanning calorimetric analysis instrument to measure the glass transformation temperature T of amorphous sample gAnd Tc T xAmorphous ribbon sample to be measured is inserted in the sample disc, get about 10 milligrams band each time.The temperature range of analyzing is 373 to 853K, and heating rate is controlled at 10-40K/min, and is protective atmosphere with the helium, and flow is 20-50cc/min.2.X x ray diffraction analysis x; Use the X-ray diffraction analysis instrument to identify the structure of alloy, with the continuous sweep of θ-2 θ wide-angle incident mode, sweep velocity is per minute 2 degree, is swept to 110 degree by 20 degree, and operating voltage is 30kV, and electric current is 20mA, and incident light source is the Co target.3. scanning electronic microscope; On example cross section, do X-Y grid scanning with electron beam, and on cathode tube, also scan, respectively organize on electron-beam position and the cathode tube each point on the sample and determined the pointwise corresponding relation, just form the image of sample in identical X-Y mode.4. coiling iron core; The amorphous ribbon of preparation is wound into internal diameter 23mm, the iron core of external diameter 25-31mm.5. iron core thermal treatment; Amorphous sample iron core to be measured is put into vacuum heat treatment furnace, and insulation was handled 5-300 minute according to measurement requirement under 320 ℃-565 ℃ temperature.6. static magnetic is measured; Adopt ballistic method to measure the static magnetic characteristic of heat-treatment amorphous sample iron core, come magnetic flux change in the test sample as integrator with ballistic galvanometer.7. DYNAMIC MAGNETIC is measured; At different AC magnetic field H mUnder measure the corresponding B of heat-treatment amorphous sample iron core mValue, the B that made this moment m-H mCurve is the dynamic magnetisation curve under the AC magnetic field.Adopt voltammetry to measure dynamic magnetisation curve.Utilize voltage meter to measure and the corresponding voltage U of B, measure and the corresponding electric current I of H, thereby determine B with current meter m(H m) magnetzation curve.Magnetizing field is: H m=1.414 IN 1/ l; In formula, N 1Be the magnetizing coil total number of turns, I is the magnetzation current virtual value that current meter measures, and l is the sample average length of magnetic path.Measure measurement coil N with the rectifier type voltage meter 2The mean value U of inductive emf Av, then can calculate: B m=U Av/ (4fN 2A s); In formula, f is the frequency of magnetzation current, A sSectional area for sample.
Adopt iron-base bulk amorphous soft-magnetic alloy material of the present invention compared with prior art, this iron-base bulk amorphous soft-magnetic alloy material has wide supercool liquid phase region and all good result of use of every soft magnetic performance technical indicator.According to above-mentioned to amorphous sample of the present invention measurement and the embodiment of the invention in table 3 result can find out, in iron tin boryl bulk amorphous soft-magnetic alloy of the present invention, most block amorphous alloy soft magnetic performance obviously is better than existing metallic substance, its characteristics have following some:
(1) iron-base bulk amorphous soft-magnetic alloy material of the present invention has wide supercool liquid phase region, as 1,2,3,9, No. 10 alloy;
(2) iron-base bulk amorphous soft-magnetic alloy material of the present invention has high B 10, as 1,4,5, No. 6 alloy;
(3) iron-base bulk amorphous soft-magnetic alloy material of the present invention has high square ratio, as No. 3 alloys;
(4) iron-base bulk amorphous soft-magnetic alloy material of the present invention has high μ m, as 1,5,7,8, No. 10 alloy;
(5) iron-base bulk amorphous soft-magnetic alloy material of the present invention has high Effective permeability μ e, as 7, No. 8 alloys;
(6) iron-base bulk amorphous soft-magnetic alloy material of the present invention has low H c, as 3,5,6,7,8, No. 10 alloys;
(7) iron-base bulk amorphous soft-magnetic alloy material of the present invention has low-loss P, as 3,5,7, No. 8 alloys.
Description of drawings
In the Figure of description of iron-base bulk amorphous soft-magnetic alloy material of the present invention, Fig. 1 is an alloy sequence number 3 of utilizing " suction casting method " preparation, 5, the outward appearance photo of 10 diameter 1mm and the block amorphous alloy pole of 2mm, Fig. 2 is the alloy sequence number 5 of diameter 2mm, the X-ray diffractogram of 10 block alloy pole cross sections, by this diffractogram as can be seen this alloy pole be non-crystalline state, Fig. 3 is the alloy sequence number 5 of diameter 2mm, the electron scanning micrograph of 10 block amorphous alloy pole cross sections, by this photo as can be seen this non-crystaline amorphous metal pole cross section do not have crystal grain and defective and exist, Fig. 4 is the differential scanning calorimetric curve of alloy sequence number 10 amorphous bands, the glass transformation temperature and the Tc of this non-crystaline amorphous metal are respectively 696.14K and 745.95K as can be known by this curve, so the supercool liquid phase region width of this non-crystaline amorphous metal is 49.81K, Fig. 5 is the alloy 5 that utilizes " suction casting method " preparation, ( 5 * 8 * 1mm), Fig. 6 are the alloys 6 that utilizes " suction casting method " preparation to 10 annular amorphous alloy iron cores, 10 annular amorphous alloy iron core ( 6 * 10 * 1mm).
Embodiment
Employing is in the composition scope of iron-base bulk amorphous soft-magnetic alloy material of the present invention, we have done 10 groups of tests (seeing Table 2) altogether, wherein sequence number 1,2,4,7,8,9 is the amorphous ribbon sample of thickness at 25-50 μ m, and sequence number 3,10 is the non-crystal bar sample of diameter phi 1mm.Sequence number 5,10 is the non-crystal bar sample of diameter phi 2mm, sequence number 5,10 is the amorphous annular sample of internal diameter 5 * external diameter 8 * high 1mm, sequence number 6,10 is the amorphous annular sample of internal diameter 6 * external diameter 10 * high 1mm, its use equipment is single roller spray band machine, preparation technology is the mother alloy rod of 50 gram amounts that sequence number 1,2,4,7,8,9 is respectively got, and puts into the nozzle bag of single roller spray band machine.Main processing parameter is regulated as follows: nozzle bag lower end nozzle mouth seam width is 0.5mm, and nitrogen or argon gas spraying pressure can be decided to be 0.2MPa, and nozzle to copper cooling roller spacing is 0.20mm, adjusts copper cooling roller wheel rim rotating speed to 30m/s.The amorphous ribbon width of preparation is 8mm, and thickness is 35 μ m.Adopt " suction casting method " preparation sequence number 5,6,10 to be prepared into the amorphous annular sample of internal diameter 5 * external diameter 8 * high 1mm and internal diameter 6 * external diameter 10 * high 1mm respectively, its technology is that feeding pressure is the argon gas malleation of 0.2Mpa in the furnace chamber of forvacuum, after utilizing electric arc with alloy melting, draw back vacuum valve, with copper mold cavity and vacuum (＜1.0 * 10 -2Pa) link to each other, utilize argon gas to promote metal liquid, alloy is sucked (utilizing the furnace chamber gaseous tension to clamp-on) to copper mold, the sample that take out the casting back is the annular block iron core of different set size.Following table 2 is the composition table (weight %) of the embodiment of the invention; Table 3 is every performance table of the embodiment of the invention; Table 4 is annular core (φ 5 * φ 8 * 1mm) soft magnetic performances of sequence number 6,10 among the embodiment.Table 2 embodiment of the invention composition table (weight %)
Sequence number ??Sn ??Al ??P ??Si ??B ??C ??Mo ????V ?Nb ??Cr ??Mn ??W ??Ta ??Nd ??Cu ??Fe
1 ??2.55 ??- ??- ??- ??5.11 ??- ??- ????- ?- ??- ??- ??- ??- ?- ??- Surplus
2 ??0.83 ??- ??6.92 ??2.09 ??0.81 ??- ??- ????- ?- ??- ??- ??- ??- ?- ??- Surplus
3 ??4.74 ??2.16 ??7.43 ??2.24 ??0.86 ??- ??- ????- ?- ??- ??- ??- ??- ?- ??- Surplus
4 ??4.98 ??2.27 ??1.95 ??1.77 ??2.27 ??2.65 ??- ????- ?- ??- ??- ??- ??- ?- ??- Surplus
5 ??3.80 ??2.18 ??3.78 ??3.79 ??1.46 ??1.24 ??- ????- ?- ??- ??- ??- ??- ?- ??- Surplus
6 ??4.90 ??2.23 ??2.56 ??2.32 ??2.68 ??- ??- ????- ?- ??- ??- ??- ??- ?3.17 ??- Surplus
7 ??4.62 ??2.10 ??6.03 ??2.19 ??0.84 ??- ??3.74 ????- ?- ??1.56 ??- ??- ??- ?- ??- Surplus
8 ??3.48 ??1.22 ??5.79 ??1.83 ??1.03 ??- ?- ??1.96 ?- ?- ??2.45 ??2.33 ??- ?- ??1.41 Surplus
9 ??3.68 ??4.35 ??5.65 ??1.95 ??0.92 ??- ?- ?- ?4.03 ?- ??- ?- ??1.02 ?- ??0.74 Surplus
10 ??4.58 ??2.05 ??4.87 ??2.35 ??1.14 ??0.47 ?2.42 ?- ?- ?- ??- ?- ??- ?- ???- Surplus
Every performance table of table 3 embodiment of the invention
The alloy sequence number ??Δ ??T x(K) ????B r(T) ??B 10(T) B r/B 10 ?μ m ??μ e(1kHz) ??H c(A/m) ??P 50Hz(W/kg)
????1 ??65 ????0.437 ??1.465 ?0.30 ?9.6×10 4 ???- ??6.2 ??-
????2 ??46.5 ????0.446 ??1.114 ?0.40 ?4.8×10 4 ???- ??7.687 ??0.249(0.9T)
????3 ??50.3 ????0.616 ??1.182 ?0.52 ?1.8×10 5 ???- ??3.449 ??0.161(1.1T)
????4 ??37.2 ????1.382 ??1.454 ?0.95 ?9000 ???- ??81.09 ??3.574(1.3T)
????5 ??31.7 ????0.761 ??1.305 ?0.56 ?1.9×10 5 ???- ??3.635 ??0.225(1.3T)
????6 ??21.0 ????1.123 ??1.357 ?0.83 ?- ???- ??4.526 ??-
????7 ??34.6 ????0.725 ??1.112 ?0.65 ?5.3×10 5 ??7.0×10 4 ??0.725 ??0.096(1.1T)
????8 ??40.9 ????0.736 ??1.227 ?0.60 ?1.6×10 5 ??6.6×10 4 ??1.870 ??0.153(1.2T)
????9 ??51.4 ????0.294 ??0.881 ?0.33 ?- ???- ??7.820 ??-
????10 ??49.8 ????0.74 ??1.175 ?0.63 ?2.3×10 5 ???- ??1.52 ??-
( 5 * 8 * 1mm) soft magnetic performances of the annular core of sequence number 10 among table 4 embodiment
Soft magnetic performance ??B 10(T) ??B 20(T) ??B 30(T) ??B r(T) ??H c(A/m)
The attitude of quenching ??0.658 ??0.896 ??1.005 ??- ??-
Annealing ??1.072 ??1.206 ??- ??0.012 ??4.82

Claims (2)

1. iron-base bulk amorphous soft-magnetic alloy material, the concrete Chemical Composition that it is characterized in that forming this iron-base bulk amorphous soft-magnetic alloy material is (weight %): Fe.75-95%; Sn.0.5-10%; B.0.2-10%; Al.≤6%; V.≤10%; Nb.≤10%; Mo.≤10%; P.≤15%; C.≤5; Si.≤10; In Cr, Mn, W, Ta, Nd, the Cu element any one≤10%.
2. according to the described alloy material of claim 1, it is characterized in that any two kinds and two or more sum≤10% in Cr, Mn, W, Ta, Nd, the Cu element in this composition.
CNB021288577A 2002-08-16 2002-08-16 Iron-base bulk amorphous soft-magnetic alloy material Expired - Fee Related CN1173061C (en)

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CN102787281A (en) * 2012-08-21 2012-11-21 安泰科技股份有限公司 High-toughness iron-phosphorus based amorphous alloy thin strip and preparation method thereof
CN102787281B (en) * 2012-08-21 2014-04-30 安泰科技股份有限公司 High-toughness iron-phosphorus based amorphous alloy thin strip and preparation method thereof
CN103451521A (en) * 2013-08-23 2013-12-18 苏州长盛机电有限公司 Tin-iron alloy material
CN103451521B (en) * 2013-08-23 2015-05-27 苏州长盛机电有限公司 Tin-iron alloy material
CN104801708A (en) * 2015-05-15 2015-07-29 福建农林大学 Full metal component iron-based amorphous alloy powder for powder metallurgy and preparation method thereof
CN111801437A (en) * 2018-02-21 2020-10-20 Tdk株式会社 Soft magnetic alloy and magnetic component
CN108796395A (en) * 2018-07-21 2018-11-13 芜湖君华材料有限公司 A kind of low iron loss amorphous alloy material processing technology
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CN112430791A (en) * 2019-08-26 2021-03-02 日立金属株式会社 Fe-based alloy composition, powder of Fe-based alloy composition, and magnetic core
CN114346243A (en) * 2021-12-27 2022-04-15 江西大有科技有限公司 Iron-based magnetic powder forming process and equipment

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