CN101620905A - Orientation metal soft magnetic alloy material and preparation method thereof - Google Patents

Orientation metal soft magnetic alloy material and preparation method thereof Download PDF

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CN101620905A
CN101620905A CN200810122839A CN200810122839A CN101620905A CN 101620905 A CN101620905 A CN 101620905A CN 200810122839 A CN200810122839 A CN 200810122839A CN 200810122839 A CN200810122839 A CN 200810122839A CN 101620905 A CN101620905 A CN 101620905A
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orientation
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陈�光
张中武
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Nanjing University of Science and Technology
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Abstract

The invention discloses an orientation metal soft magnetic alloy material and a preparation method thereof. The metal soft magnetic alloy material is obtained through ingot casting, forging cogging, rolling and directional annealing. In a directional annealing process, the metal soft magnetic alloy material regionally heated; meanwhile, a region adjacent to the region for heating the material is cooled by use of cooling fluid so as to allow a temperature gradient distribution to be produced in a temperature field in the material; meanwhile, the material is moved relative to a thermal region at a constant speed so as to form directional annealing; the material is subjected to directional recrystallization and crystal grains grow up directionally by utilizing directional annealing; and the orientation metal soft magnetic alloy material with columnar crystal microstructure and obvious crystallographic texture is obtained. The preparation method improves the soft magnetic properties of the orientation metal soft magnetic alloy material by controlling the crystallographic orientation/texture thereof. The method provided for controlling crystallographic orientation and then improving the soft magnetic properties of the material can be widely applicable to the metal soft magnetic alloy materials having requirements for orientation.

Description

Orientation metal soft magnetic alloy material and preparation method thereof
Technical field
The invention belongs to and have the metal soft magnetic alloy material technology, particularly a kind of orientation metal soft magnetic alloy material and preparation method thereof that orientation requires.
Background technology
Soft magnetic material is the indispensable important materials of electric power, electronics and war industry.Especially in power industry, from the generation of electric energy, be transferred to the process of utilization, soft magnetic material plays important power conversion effect.Metal soft magnetic material is meant that with iron, cobalt, three kinds of main ferromagnetic elements of nickel be main component, or their single metal, or the suitable component of the two and even three among them cooperates, or add one or more other elements on this basis again, be formed by combining as molybdenum, silicon, aluminium, vanadium.The metal soft magnetic alloy material of ferro-silicium (silicon steel sheet) amount of being to use maximum wherein.Magnetic flux density and high magnetic permeability high under low remanent magnetism, coercive force and iron loss and the high-intensity magnetic field are the very important technical indicators of soft magnetic material.
Because there is magnetocrystalline anisotropy in metal soft magnetic alloy material, promptly the magnetic monocrystal material exists easy magnetization and hard direction, therefore, has the potentiality of improving magnetic property from crystallography.This potentiality are paid attention to by people for a long time always.For example advancing by leaps and bounds greatly several times of silicon steel performance all is to prepare as Goss texture, cubic texture and high oriented material by technological invention.This advances by leaps and bounds greatly several times and all obtains from orientation control.Metal soft magnetic alloy material has critical role in fields such as power conversion and information processings, and the exploitation of technology of preparing has important engineering meaning and commercial value.Therefore, all very active always to the research-and-development activity of such alloy in the world.But, the orientation control technology complexity of metal soft magnetic alloy material, therefore in succession the various control metal soft magnetic alloy materials of exploitation especially the method for silicon steel crystalline orientation all obtained patent protection.The method of general control silicon steel orientation is to utilize controlled rolling technology and annealing process to realize.As the United States Patent (USP) (patent No.: 4371405) provide finishing temperature by the control hot rolling between 700 ℃ to 1000 ℃, can omit the intermediate annealing after the hot rolling.General MnS in the process of preparation orientation silicon steel, grain growth inhibitors such as AlN have important function in the material secondary recrystallization process.Therefore in traditional preparation orientation silicon steel process, solid solution and the depositing technology of controlling these grain growth inhibitors are the hot issues of research.For example, the United States Patent (USP) (patent No.: 3151005) provided the form and the distribution that utilize control carbide and precipitated phase and improved the content of siliceous 3.25% silicon steel plate Goss texture and then improve magnetic property.United States Patent (USP) (the patent No.: 4319936) also provide a kind of method that in 3.25% silicon steel, prepares Goss texture.This method is improved crystallography texture and magnetic property according to Al in the material and N content by the temperature of controlling initial annealing temperature and initial quenching.Because above-mentioned factor makes the complicated process of preparation of orientation silicon steel, simultaneously, the adding of the inhibitor of growing up also is unfavorable for the performance of the magnetic property of silicon steel own.
Will experience cold-rolled process in the preparation process of orientation silicon steel, the Si content of an orientation silicon steel is generally all about 3.25%.Because silicon content reaches more than 4%,, can not utilize traditional cold-rolling process preparation because processing characteristics sharply descends.Yet along with the increase of silicone content, the resistivity of silicon steel increases, and eddy current loss reduces, thereby shows good magnetic under upper frequency.When silicone content reached 6.5% left and right sides, magnetostriction coefficient leveled off to zero, and magnetic permeability is increased to maximum, and iron loss drops to minimum.Because the variation of electronic device, especially in the application in high frequency field, improving silicone content is the effective way that further improves the silicon steel magnetic property, has been subjected to paying close attention to widely.Because siliceous silicon steel more than 4% can not utilize traditional cold-rolling process preparation.At present, study in succession with methods such as CVD siliconising method, rapid solidification method, powder metallurgic method, special rolled method, powder coatings and prepare this high silicon plate or strip various countries.Japan Patent (the patent No.: S56-3625) developed and utilize single Kun or the direct casting of two Kun for example.Japan Patent (the patent No.: S62-103321) developed the warm-rolling method.Japan Patent (the patent No.: H5-171281) developed the ply rolling method, be about to high silicon plate holder and in the middle of low silicon plate, be rolled.The patent No. be Wo 2004/044252 A1 Patent exploitation utilize the technology of the high silicon steel of coating preparation orientation, this technology at first adopts traditional hot rolling to add the silicon steel material that cold-rolling practice prepares 3.3%Si, before last secondary recrystallization annealing, be coated with Fe-Si base agglomerated powder and use MgO then, under the condition of high annealing, realize siliconising and orientation control as annealing separation agent (annealing separator) at material surface.At present, these methods all do not have to realize commercially producing because of its complex process.3423253) etc. the Japan Patent (patent No.: S62-227-078) and the United States Patent (USP) (patent No.: developed SiCl4 siliconising method, the 3% non-orientation silicon steel surface siliconising that is chemical vapor deposition (CVD) method after cold rolling, and prepare the high silicon steel of siliceous 6.5wt% by the homogenizing annealing means.Although this method has realized commercially producing.Yet, compare with 3% common silicon steel, owing to adopted CVD technology to make its cost improve 5 times.In addition, these methods all are only to utilize the raising silicone content to improve magnetic property, and are difficult to realize that the texture by controlling high silicon steel further improves its magnetic property.At present, under the situation that does not adopt CVD technology, can't realize commercially producing of high silicon steel.People such as Zhang Zhongwu once attempted the microstructure of pure iron material is controlled (Acta Mater., 2007,55:5988, Mater.Sci.Eng., A434 (2006) 58, Mater.Sci.Eng., A435-436 (2006) 573, Mater.Sci.and Eng., A422 (2006) 241).At present, although in pure iron, can prepare the column crystal microstructure, can't effectively control its orientation.Simultaneously, because the soft magnet performance of orientation magnetically soft alloy material has strict demand to the orientation of material, its technology controlling and process mechanism and parameter are different from above-mentioned simple metal material fully.The existence that is orientated alloying element in the magnetically soft alloy material has simultaneously seriously hindered the control to its microstructure and orientation.Therefore will improve the performance of metal soft magnetic alloy material, especially reaching in the high silicon steel 4% or more further at silicone content, its magnetic property of raising must find the effective way that can directly control this material grains form and crystallography texture.
Summary of the invention
The object of the present invention is to provide a kind ofly to have the orientation that obvious crystallography is selected the superior, and make metal soft magnetic alloy material that its soft magnet performance is greatly improved and preparation method thereof.
The technical solution that realizes the object of the invention is: a kind of orientation metal soft magnetic alloy material, at metal soft magnetic alloy material through ingot casting, hammer cogging, utilize orientation anneal after rolling and obtain, in the orientation anneal process, metal soft magnetic alloy material is carried out the zone heating, adjacent area in this material heating utilizes cooling fluid to cool off the temperature gradient distribution of temperature field generation that makes in the material to reach simultaneously, material is moved with constant speed relative to the hot-zone and form orientation anneal, utilize orientation anneal make material generation orientation again crystallization and crystal grain orienting grow up, obtain having the column crystal microstructure and the obvious orientation metal soft magnetic alloy material of crystallography texture at last.
A kind of method for preparing orientation metal soft magnetic alloy material, at metal soft magnetic alloy material through ingot casting, hammer cogging, carry out orientation anneal after rolling, in the orientation anneal process, metal soft magnetic alloy material is carried out the zone heating, adjacent area in this material heating utilizes cooling fluid to cool off the temperature gradient distribution of temperature field generation that makes in the material to reach simultaneously, material is moved with constant speed relative to the hot-zone and form orientation anneal, utilize orientation anneal make material generation orientation again crystallization and crystal grain orienting grow up, obtain having the column crystal microstructure and the obvious orientation metal soft magnetic alloy material of crystallography texture at last.
The present invention compared with prior art, its remarkable advantage: (1) by control orientation metal soft magnetic alloy material crystalline orientation/texture improve its soft magnet performance.Control is to utilize crystal grain selectivity in the directed recrystallization process to grow up and the competition migration mechanism of crystal boundary is controlled the grow up orientation of crystal grain of orientation to the crystalline orientation of metal soft magnetic alloy material, thus the crystallography texture and the soft magnet performance of control material.Therefore, the secondary recrystallization process that in the preparation process of metal soft magnetic alloy material, does not need the grain inhibitor control material.Simultaneously, do not need to carry out cold rolling to material.Must utilize the cold rolling technical barrier of realizing crystalline orientation control thereby broken through to orientation metal soft magnetic alloy material, for the orientation control that solves the difficult metal soft magnetic alloy material that is out of shape provides new method.(2) the control crystalline orientation that provides and and then the method that improves its soft magnet performance can be widely applicable for the metal soft magnetic alloy material that will have orientation requirement.Especially for high silicon steel material, because its huge potential value on commercial Application obtains extensive studies always.But because its fragility problem never is resolved, present high silicon steel technology of preparing also rests at first carries out cold rollingly to low-silicon steel, and then it is carried out methods such as CVD siliconising or coating prepare.Therefore, prior art also can't directly be orientated control to it, makes its soft magnet performance to bring into play.The present invention has broken through this technical bottleneck, material is carried out under the cold rolling condition not needing, thereby directly utilize the selectivity of the directed control of crystallization technique again crystal grain to grow up and the competition migration of crystal boundary realizes the control of the crystalline orientation of material is improved its soft magnet performance.(3) on the basis of traditional ingot casting, cogging, utilize orientation anneal to realize at material, so this method is simple, is applicable to industrial-scale production.
Below in conjunction with accompanying drawing the present invention is described in further detail.
Description of drawings
Fig. 1 is that the preparation method of orientation metal soft magnetic alloy material of the present invention uses the orientation anneal schematic representation of apparatus.
Fig. 2 is the high silicon steel material ingot casting of the present invention through again it being carried out 850 ℃ of micro-structure diagrams behind the isothermal annealing 30min after hammer cogging and the hot rolling.
Fig. 3 is the microstructure and the crystalline orientation distribution map of the high silicon steel material of embodiment 1 preparation, and as seen from the figure, the crystal boundary between column crystal is made of the coincidence dot matrix crystal boundary of low-angle boundary and low ∑ value.
Fig. 4 is that high silicon steel material is the different withdrawing rate orientations typical microstructure figure after the crystallization again under 1200 ℃ the condition in the hot-zone temperature.
Fig. 5 be different hot-zones temperature with different withdrawing rate conditions under the draw ratio curve chart of the high silicon steel material crystal grain for preparing.
Fig. 6 is the crystalline orientation distribution function figure of high silicon steel material, (a) for utilizing Comparative Examples 1 method to prepare the orientation density of high silicon steel material, be to utilize the orientation density that embodiment 1 method is prepared high silicon steel material (b) for the orientation density (c) of utilizing Comparative Examples 2 methods to prepare high silicon steel material.
Fig. 7 is the soft magnet performance curve chart of high silicon steel material, i.e. the coercive force of different directions in the sample.
Embodiment
Orientation metal soft magnetic alloy material of the present invention is through ingot casting at metal soft magnetic alloy material, hammer cogging, carry out orientation anneal after rolling, in the orientation anneal process, metal soft magnetic alloy material is carried out the zone heating, adjacent area in this material heating utilizes cooling fluid to cool off the temperature gradient distribution of temperature field generation that makes in the material to reach simultaneously, material is moved with constant speed relative to the hot-zone and form orientation anneal, crystallization and crystal grain orienting are grown up again to utilize orientation anneal to make material generation orientation, obtain orientation metal soft magnetic alloy material at last, this metal soft magnetic alloy material has the directed microstructure of column crystal, column crystal has preferred orientation, is the low energy crystal boundary between column crystal.Utilize the competition of the selective growth of crystal grain and crystal boundary to move to control the orientation orientation of crystal grain of growing up again in crystallization and the crystal grain orienting growth process in orientation, thereby realize also and then improve the soft magnet performance of metal soft magnetic alloy material the control of material crystals texture.
The temperature of the zone heating in the above-mentioned orientation anneal is between 600 ℃-1500 ℃, and the hot-zone width of zone heating is between 5mm-50mm.The translational speed of the relative hot-zone of metal soft magnetic alloy material is between 0.5 μ m/s-100 μ m/s.Temperature gradient distribution is between 5 ℃/mm-100 ℃/mm.
Wherein, metal soft magnetic alloy material is that the suitable component with the two and even three in iron, cobalt, three kinds of ferromagnetic elements of nickel cooperates, or the molybdenum, silicon, aluminium or the vanadium that add one or more on the basis of iron, cobalt, three kinds of ferromagnetic elements of nickel again combine.And siliceous percentage by weight is 3.5%~7.5% high silicon steel material is most important a kind of in the metal soft magnetic alloy material.For high silicon steel material, the temperature of zone heating is between 1100 ℃-1200 ℃, and the hot-zone width of zone heating is between 5mm-10mm; The translational speed of hot-zone is between 0.6 μ m/s-8 μ m/s relatively.
The present invention is the magnetocrystalline anisotropy that exists according to metal soft magnetic alloy material, and promptly the magnetic monocrystal material exists the characteristic of easy magnetization and hard direction to improve its soft magnet performance by the control to material crystals texture.The control of crystallography texture is to utilize in the annealing process that the directional profile of hot-fluid realizes directed recrystallization process in the material.Simultaneously the selectivity of crystal grain in the directed recrystallization process is grown up and crystal boundary competition migration is controlled.The realization that the selectivity of directed crystallization again and crystal grain is grown up is by to the hot-zone temperature of material in the orientation anneal process, and the Temperature Distribution in the sample and the movement rate of sample are controlled and realized.Based on this, the present invention control orientation metal soft magnetic alloy material orientation and and then the control that improves its soft magnet performance be that material utilizes after traditional smelting, cogging in the annealing process that the directional profile of hot-fluid realizes in the control material, promptly realize by orientation anneal.Therefore, thus control orientation anneal technology realizes that it is key of the present invention that the selectivity of directed crystallization again and crystal grain is grown up.
Orientation anneal of the present invention is to finish in vacuum oriented annealing furnace.Orientation anneal must satisfy following several process conditions simultaneously: the orientation anneal stove must have the thermal source of a stable and controllable.Simultaneously, the temperature of thermal source and hot-zone width must can free adjustment, promptly can form narrower hot-zone, thereby realize regional annealing.Must be able to guarantee in the annealing process of area of the sample, in sample, to form bigger temperature gradient distribution.Therefore must in the orientation anneal stove, be equipped with corresponding coolant, thereby in annealing process, can in sample, produce a bigger temperature gradient with the hot-zone acting in conjunction.In annealing process, sample must be able to move relative to the hot-zone, promptly guarantee a withdrawing rate, and this withdrawing rate is controlled.Thereby sample can be moved in certain temperature gradient and certain temperature conditions lower edge, hot-zone direction of heat flow, thereby realize continuous crystal boundary directional migration.
In conjunction with Fig. 1, realize that orientation anneal of the present invention mainly is made of following several parts:
A. thermal source 1, and the present invention utilizes high frequency induction power supply as thermal source, utilizes single-turn induction coil that metal soft magnetic alloy material is carried out the zone and adds the narrower hot-zone of thermosetting.
B. hygrosensor 8, and the present invention utilizes infrared temperature detector measurement temperature and realizes hot-zone temperature control by the control to high frequency induction power supply.
C. cooling fluid 3, and the present invention utilizes the Ga-In liquid alloy as cooling fluid, make metal soft magnetic alloy material can keep controlled in a big way temperature gradient in the orientation anneal process.Temperature gradient is adjusted with the distance of metal cools liquid level by adjusting induction coil, and metal cools liquid is cooled off by recirculated cooling water.
D. pull system 5, the present invention utilizes the power of servomotor as the pull system.Metal soft magnetic alloy material in annealing process under the drive of servomotor can more than, move down and finish orientation anneal.Rate travel and direction are controlled by servomotor.
E. recirculated cooling water outlet 4, and recirculated cooling water is used for the cool metal cooling fluid.Recirculated cooling water inlet 6 constitutes loop with recirculated cooling water outlet 4.
F. vacuum chamber 7, and orientation anneal is finished in vacuum chamber, and vacuum degree is greater than 10 -3Pa.
Further specify content of the present invention below by embodiment and Comparative Examples, with the draw ratio sign microstructure of crystal grain, the big more column crystal microstructure that shows of draw ratio is good more; With the soft magnet performance of coercive force characterizing metal magnetically soft alloy material, the coercive force bright soft magnet performance of novel more is good more.
Embodiment 1
(1) choices of raw materials
The high silicon steel material of the selected boracic Fe-6.5wt%Si of present case is the hot-roll annealing attitude.Material composition such as table 1.
The chemical composition (wt%) of the high silicon steel of table 1 boracic Fe-6.5wt%Si
Figure S2008101228397D00061
(2) orientation anneal pre-treatment
Material waters into ingot casting after proportionately dividing melting, and ingot casting is obtained slab at 1000 ℃ of left and right sides hammer coggings, then slab is carried out hot rolling at 1050 ℃-850 ℃ and obtains the thick sheet material of 1.5mm.To this hot rolled plate at 850 ℃ of isothermal annealing 30min.The microstructure of high silicon steel as shown in Figure 2 after the isothermal annealing.Axle such as the microstructure after isothermal annealing polycrystalline structure as seen from Figure 2, grain size is about 77 μ m.
(3) orientation anneal sample pretreatment
Before orientation anneal, at first material is carried out mechanical polishing.In order to remove the areal deformation layer, the sample after the polishing is etch 10min in 10% dilute sulfuric acid, cleans with acetone then.
(4) orientation anneal process
Concrete orientation anneal process is as follows:
The sample that preliminary treatment is good is installed on the pumping rod that connects servomotor in the orientation anneal stove.The upper end of sample is consistent with the induction coil upper end.
Induction coil thickness 10mm, induction coil is 13mm with metal cools liquid level distance.
Close the orientation anneal bell be evacuated to~10 -3Pa.
Start the induction power supply heating, setting the hot-zone temperature is 1150 ℃, after the hot-zone temperature reaches design temperature, starts servomotor, and sample is moved from bottom to top, and rate travel is 3 μ m/s
The sample of preparing has the column crystal microstructure, as shown in Figure 3.The orientation of crystal grain and the misorientation of crystal boundary have been marked among Fig. 3 simultaneously.Fig. 3 shows that high silicon steel material has obtained the column crystal microstructure under the process conditions of present embodiment.The average length of column crystal is about 1.2mm, and width is about 0.38mm.Crystal boundary between column crystal is made of the coincidence dot matrix crystal boundary of low-angle boundary and low ∑ value.
Embodiment 2
Adopt with embodiment 1 identical material composition and method and obtain to forge slab.On the forging slab, directly cut out the orientation anneal sample.By the 3rd method of embodiment 1 sample is carried out preliminary treatment then.Pretreated sample is carried out orientation anneal.The orientation anneal process is identical with the 4th of embodiment 1.The concrete technological parameter of orientation anneal is as follows;
Induction coil thickness 10mm, induction coil is 13mm with metal cools liquid level distance.Annealing furnace vacuum degree~10 -3Pa.The hot-zone temperature is 1100 ℃-1200 ℃, and withdrawing rate is 0.6 μ m/s-8 μ m/s.In above-mentioned processing range, all prepare the column crystal microstructure.Fig. 4 is the microstructure of high silicon steel after directed crystallization again under 1200 ℃ of different withdrawing rate conditions.Withdrawing rate is respectively (a) 0.6 μ m/s, (b) 0.8 μ m/s, (c) 1 μ m/s, (d) typical microstructure of 3 μ m/s (e), 8 μ m/s.Fig. 4 (a) shows that the length of column crystal is about 3.6mm, and width is about 1.1mm; Fig. 4 (b) shows that the length of column crystal is about 4.1mm, and width is about about 0.8mm; Fig. 4 (c) shows that column crystal length is that width is about 1.3mm about 10mm; Fig. 4 (d) shows that column crystal length is about 23mm, and width is about 2.3mm; Fig. 4 (e) shows that column crystal length is about 1.2mm, and width is about 0.44mm.Wherein, the draw ratio of different orientation anneal technologies acquisitions as shown in Figure 5.Fig. 5 shows in the process conditions scope of present embodiment all can obtain the column crystal microstructure, and promptly the draw ratio of column crystal is greater than 1.
Embodiment 3
The crystalline orientation of metal soft magnetic alloy material.Utilize X-ray diffraction to measure { 110}, { 200} and { three utmost point figure of 211}, and calculate the distribution of orientations that orientation distribution function comes analysis of material the metal soft magnetic alloy material of embodiment 1 preparation according to utmost point figure.What experiment recorded the results are shown in Figure 6.For comparative illustration, adopt identical experimental technique and condition to measure the orientation distribution function of through 850 ℃ isothermal annealing 30min after the material (Comparative Examples 1) identical with embodiment 1 metal soft magnetic alloy material composition, with the hot rolled plate identical with embodiment 1 metal soft magnetic alloy material composition and behind 850 ℃ of isothermal annealing 30min again through the orientation distribution function of the material (Comparative Examples 2) of 1150 ℃ of isothermal annealing 30min.The result of Comparative Examples 1 and Comparative Examples 2 sees Fig. 6 and Fig. 6 respectively.Fig. 6 is the crystalline orientation distribution function figure of high silicon steel material, (a) for utilizing Comparative Examples 1 method to prepare the orientation density of high silicon steel material, be to utilize the orientation density that embodiment 1 method is prepared high silicon steel material (b) for the orientation density (c) of utilizing Comparative Examples 2 methods to prepare high silicon steel material.As seen from Figure 6, the crystallography texture of Comparative Examples 1 and Comparative Examples 2 materials is not obvious; And embodiments of the invention 1 metal soft magnetic alloy material has tangible crystallography preferred orientation.Closely 111}<110〉and near 110}<111〉orientation density obviously strengthens.Show that the present invention improves the effect highly significant of metal soft magnetic alloy material crystalline orientation.
Embodiment 4
The soft magnet performance of metal soft magnetic alloy material.High silicon steel material to embodiment 1 preparation carries out the magnetic property sign, measures it along the coercive force that becomes different angles with the orientation anneal direction, to characterize the influence of crystalline orientation to soft magnet performance.The coercive force of the material of test as shown in Figure 7.For comparative illustration, the coercive force of material in Comparative Examples 1 and the Comparative Examples 2 is also characterized respectively, the results are shown in Figure 7.Fig. 7 is the soft magnet performance curve chart of high silicon steel material, i.e. the coercive force of different directions in the sample.As seen from Figure 7, because crystallography texture is not obvious, so material is at 0 ° in Comparative Examples 1 and Comparative Examples 2 materials, and 45 °, 60 °, the coercive force difference of 90 ° of directions is not obvious, and coercive force is higher simultaneously, and soft magnet performance is relatively poor; And the metal soft magnetic alloy material of embodiments of the invention 1 preparation is owing to have tangible crystallography preferred orientation, therefore along becoming the coercive force of different angles to have notable difference with the orientation anneal direction, coercive force minimum along 60 ℃ of directions, littler more than 5 times than the coercitive maximum of this material, the while also is far smaller than the coercivity value of the high silicon steel material of Comparative Examples 1 and Comparative Examples 2 preparations.Show that the present invention is significantly improved soft magnet performance owing to improving the metal soft magnetic alloy material crystalline orientation.
Comparative Examples 1
Adopt identical experimental technique and condition to measure through 850 ℃ isothermal annealing 30min after the orientation distribution function of material identical and the results are shown in Figure 6 (a) with embodiment 1 metal soft magnetic alloy material composition.
Comparative Examples 2
Get hot rolled plate and the material through 850 ℃ isothermal annealing 30min after identical with embodiment 1 metal soft magnetic alloy material composition.This material at 1150 ℃ of isothermal annealing 30min, and is measured its orientation distribution function.Measurement result is seen Fig. 6 (b).
At except that the metal soft magnetic alloy material of 6.5% high silicon steel material, with iron, cobalt, in three kinds of ferromagnetic elements of nickel the two and even three's suitable component cooperates, or at iron, cobalt, add one or more molybdenum on the basis of three kinds of ferromagnetic elements of nickel again, silicon, the metal soft magnetic alloy material that aluminium or vanadium combine, step according to the foregoing description 1 and embodiment 2 also can obtain having the directed microstructure of column crystal, column crystal has preferred orientation, be the low energy crystal boundary between column crystal, and the metal soft magnetic alloy material that its soft magnet performance is greatly improved.The temperature of the zone heating in their orientation anneal is between 600 ℃-1500 ℃, and the hot-zone width of zone heating is between 5mm-50mm; The translational speed of the relative hot-zone of metal soft magnetic alloy material is between 0.5 μ m/s-100 μ m/s; Temperature gradient distribution is between 5 ℃/mm-100 ℃/mm.

Claims (9)

1, a kind of orientation metal soft magnetic alloy material, it is characterized in that at metal soft magnetic alloy material through ingot casting, hammer cogging, utilize orientation anneal after rolling and obtain, in the orientation anneal process, metal soft magnetic alloy material is carried out the zone heating, adjacent area in this material heating utilizes cooling fluid to cool off the temperature gradient distribution of temperature field generation that makes in the material to reach simultaneously, material is moved with constant speed relative to the hot-zone and form orientation anneal, utilize orientation anneal make material generation orientation again crystallization and crystal grain orienting grow up, obtain having the column crystal microstructure and the obvious orientation metal soft magnetic alloy material of crystallography texture at last.
2, a kind of method for preparing orientation metal soft magnetic alloy material, it is characterized in that at metal soft magnetic alloy material through ingot casting, hammer cogging, carry out orientation anneal after rolling, in the orientation anneal process, metal soft magnetic alloy material is carried out the zone heating, adjacent area in this material heating utilizes cooling fluid to cool off the temperature gradient distribution of temperature field generation that makes in the material to reach simultaneously, material is moved with constant speed relative to the hot-zone and form orientation anneal, utilize orientation anneal make material generation orientation again crystallization and crystal grain orienting grow up, obtain having the column crystal microstructure and the obvious orientation metal soft magnetic alloy material of crystallography texture at last.
3, the preparation method of orientation metal soft magnetic alloy material according to claim 2, it is characterized in that metal soft magnetic alloy material is that suitable component with the two and even three in iron, cobalt, three kinds of ferromagnetic elements of nickel cooperates, or the molybdenum, silicon, aluminium or the vanadium that add one or more on the basis of iron, cobalt, three kinds of ferromagnetic elements of nickel again combine.
4, the preparation method of orientation metal soft magnetic alloy material according to claim 3 is characterized in that: metal soft magnetic alloy material is that siliceous percentage by weight is 3.5%~7.5% high silicon steel material.
5, the preparation method of orientation metal soft magnetic alloy material according to claim 2 is characterized in that: the temperature of the zone heating in the orientation anneal is between 600 ℃-1500 ℃, and the hot-zone width of zone heating is between 5mm-50mm.
6, the preparation method of orientation metal soft magnetic alloy material according to claim 2 is characterized in that: the translational speed of the relative hot-zone of metal soft magnetic alloy material is between 0.5 μ m/s-100 μ m/s.
7, according to the preparation method of claim 5 or 6 described orientation metal soft magnetic alloy materials, it is characterized in that: for high silicon steel material, the temperature of zone heating is between 1100 ℃-1200 ℃, and the hot-zone width of zone heating is between 5mm-10mm; The translational speed of hot-zone is between 0.6 μ m/s-8 μ m/s relatively.
8, the preparation method of orientation metal soft magnetic alloy material according to claim 2 is characterized in that: temperature gradient distribution is between 5 ℃/mm-100 ℃/mm.
9, the preparation method of orientation metal soft magnetic alloy material according to claim 2, it is characterized in that: utilize the competition of the selective growth of crystal grain and crystal boundary to move to control the orientation orientation of crystal grain of growing up again in crystallization and the crystal grain orienting growth process in orientation, thereby realize also and then improve the soft magnet performance of metal soft magnetic alloy material the control of material crystals texture.
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CN101831527A (en) * 2010-04-30 2010-09-15 衡阳市金则利特种合金有限公司 Production process for continuous casting anti-corrosion magnetically soft alloy bars with light sections
CN102031347A (en) * 2010-09-26 2011-04-27 北京鼎臣超导科技有限公司 Annealing device and annealing method for improving impedance effect of soft magnetic material
CN102423800A (en) * 2011-11-25 2012-04-25 上海工程技术大学 Crystal oriented growth control method of magnetic material in low-temperature gradient
CN103898300A (en) * 2014-04-04 2014-07-02 哈尔滨工程大学 Method for controlling feature distribution of crystal boundary of high silicon steel through orientation recrystallization
CN104240890A (en) * 2014-09-19 2014-12-24 广东省工业技术研究院(广州有色金属研究院) Fe-6.5% Si magnetic powder core
CN112048605A (en) * 2020-08-03 2020-12-08 西北工业大学 Directional annealing device and method for preparing metal columnar crystals
CN115233082A (en) * 2022-07-28 2022-10-25 东北大学 Method for preparing electrical steel thin strip with strong {100} surface texture through directional recrystallization

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101831527A (en) * 2010-04-30 2010-09-15 衡阳市金则利特种合金有限公司 Production process for continuous casting anti-corrosion magnetically soft alloy bars with light sections
CN102031347A (en) * 2010-09-26 2011-04-27 北京鼎臣超导科技有限公司 Annealing device and annealing method for improving impedance effect of soft magnetic material
CN102031347B (en) * 2010-09-26 2012-09-05 北京鼎臣超导科技有限公司 Annealing device and annealing method for improving impedance effect of soft magnetic material
CN102423800A (en) * 2011-11-25 2012-04-25 上海工程技术大学 Crystal oriented growth control method of magnetic material in low-temperature gradient
CN102423800B (en) * 2011-11-25 2014-11-05 上海工程技术大学 Crystal oriented growth control method of magnetic material in low-temperature gradient
CN103898300A (en) * 2014-04-04 2014-07-02 哈尔滨工程大学 Method for controlling feature distribution of crystal boundary of high silicon steel through orientation recrystallization
CN104240890A (en) * 2014-09-19 2014-12-24 广东省工业技术研究院(广州有色金属研究院) Fe-6.5% Si magnetic powder core
CN104240890B (en) * 2014-09-19 2017-08-04 广东省工业技术研究院(广州有色金属研究院) A kind of powder core
CN112048605A (en) * 2020-08-03 2020-12-08 西北工业大学 Directional annealing device and method for preparing metal columnar crystals
CN115233082A (en) * 2022-07-28 2022-10-25 东北大学 Method for preparing electrical steel thin strip with strong {100} surface texture through directional recrystallization
CN115233082B (en) * 2022-07-28 2023-02-24 东北大学 Method for preparing electrical steel thin strip with strong {100} surface texture through directional recrystallization

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