CN107299240B - A method of improving al-ti-b refiner structure property - Google Patents

A method of improving al-ti-b refiner structure property Download PDF

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CN107299240B
CN107299240B CN201710347819.9A CN201710347819A CN107299240B CN 107299240 B CN107299240 B CN 107299240B CN 201710347819 A CN201710347819 A CN 201710347819A CN 107299240 B CN107299240 B CN 107299240B
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stirring
refiner
tial
temperature
magnetic field
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CN107299240A (en
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屈福
高秋志
张明
王士祥
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Northeastern University Qinhuangdao Branch
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/06—Making non-ferrous alloys with the use of special agents for refining or deoxidising
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C22C1/026—Alloys based on aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C22C1/03—Making non-ferrous alloys by melting using master alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F3/00—Changing the physical structure of non-ferrous metals or alloys by special physical methods, e.g. treatment with neutrons
    • C22F3/02—Changing the physical structure of non-ferrous metals or alloys by special physical methods, e.g. treatment with neutrons by solidifying a melt controlled by supersonic waves or electric or magnetic fields

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Abstract

The invention discloses a kind of methods for improving al-ti-b refiner structure property, the following steps are included: taking Al-5Ti-1B intermediate alloy, graphite crucible is put into be placed in shaft furnace, it heats up after setting heating rate and set temperature, it keeps the temperature after reaching set temperature, then takes out graphite crucible, be put into low frequency magnetic field coil, electromagnetism, mechanical couplings stirring are carried out under heat-retaining condition, it is cooling by water cooled copper mould after stirring to obtain the final product.The present invention provides a kind of methods for improving al-ti-b refiner structure property, can be effectively improved the detailed performance of al-ti-b refiner.With the extension of mixing time and the raising of temperature, second phase particles TiAl3Size it is also smaller and smaller, become 50 μm or so from 200 μm or so, quantity also obviously becomes more, and distribution is also more uniform, no longer assembles agglomerating.And second phase particles TiB2Distribution it is also more uniform, occur without agglomerating phenomenon is assembled.Show good thinning effect.

Description

A method of improving al-ti-b refiner structure property
Technical field
The present invention relates to a kind of methods for improving al-ti-b refiner structure property, particularly belong to alloy refinement agent technology neck Domain.
Background technique
Aluminium and its alloy are as important raw material a kind of in modern industry, with density is small, specific strength is high, preferably leads The series of advantages such as electricity and thermal conductivity, stronger corrosion resistance, so largely being applied to aerospace, automobile manufacture, family A series of popular industries such as electric articles, mechanical building.People are more and more using aluminium and its alloy as the important raw material of industry To use.As aluminium alloy uses more and more extensive, all trades and professions naturally propose the service performance of aluminum alloy materials Going out harsher requirement, how to have made good use of corresponding reinforcement theory, the service performance enabled aluminum alloy to is further promoted, To meet the new demand of every field, always be materials science field important subject.
It is all had a problem that always in various intensifying methods, that is, often the intensity and plasticity of material is not It can be improved simultaneously.Both of which has a wherein Fang Bianqiang, and another party often dies down.Thus there are many raising metals The method of intensity, plasticity and toughness can be made, which to be reduced to one, in the degree obviously hindered industrial development.For at present only The method of refinement crystal grain can improve the intensity and toughness of material simultaneously.The method that aluminium grain is refined using fining agent is extensive It is considered most effective method.And al-ti-b refiner is as a kind of common fining agent that there is also deficiencies, such as aluminium titanium The metallurgical quality of boron fining agent itself is simultaneously bad, and some useless inclusion contents are high, aluminium and aluminium alloy easy to pollute；Aluminium titanium boron is thin TiB in agent2Particle size is larger and easily assembles agglomerating, thus brings many quality problems；The institutional framework of fining agent is to work The susceptibility of skill factor is high, even if its tissue morphology and thinning effect may also can be under the conditions of identical chemical component Difference, thinning effect are unstable etc..Therefore a kind of method for improving al-ti-b refiner structure property is studied, it is thin to improve aluminium titanium boron The thinning effect of agent, it appears particularly necessary.
Summary of the invention
To solve the deficiencies in the prior art, the purpose of the present invention is to provide a kind of improvement al-ti-b refiner structure properties Method, the detailed performance of al-ti-b refiner can be effectively improved.
In order to achieve the above objectives, the present invention adopts the following technical scheme that:
A method of improving al-ti-b refiner structure property, comprising the following steps: Al-5Ti-1B intermediate alloy is taken, It is put into graphite crucible to be placed in shaft furnace, heats up after heating rate and set temperature are set, keep the temperature one after reaching set temperature It fixes time, then takes out graphite crucible, be put into low frequency magnetic field coil, carry out electromagnetism under heat-retaining condition, mechanical couplings are stirred It mixes, it is cooling by water cooled copper mould after stirring to obtain the final product.Insulation can be applied in whipping process to graphite crucible convenient for prolonging Long soaking time.
In the aforementioned method for improving al-ti-b refiner structure property, heating rate is 10 DEG C/min~15 DEG C/min.
In the aforementioned method for improving al-ti-b refiner structure property, set temperature is 720 DEG C~820 DEG C.
In the aforementioned method for improving al-ti-b refiner structure property, reach set temperature heat preservation to protect at a set temperature Warm 10min~20min.
In the aforementioned method for improving al-ti-b refiner structure property, the magnetic field strength of low frequency magnetic field coil is 12000~ 15000AT；Mechanical stirring frequency is 2~3Hz in electromagnetism, mechanical couplings stirring.
In the aforementioned method for improving al-ti-b refiner structure property, mechanical stirring refers in electromagnetism, mechanical couplings stirring It is stirred with the ceramic stirring rod after preheating.
Further, in the aforementioned method for improving al-ti-b refiner structure property, ceramic stirring rod is at 600~700 DEG C 15~20min of lower preheating.
In the aforementioned method for improving al-ti-b refiner structure property, mixing time is 5~15min.
In order to ensure technical solution of the present invention is scientific, reasonable, effective, inventor has carried out a series of experiments verifying.
Studies have shown that the thinning effect of Al-5Ti-1B fining agent depends primarily on TiAl in its tissue3With TiB2Two kinds of work Shape, size, quantity and the distribution of property point.Wherein TiAl3Mutually mainly have there are three types of pattern, is blocky, rod-shaped respectively and flower Petaloid, and influence of these three appearances for thinning effect is also different, among these block-like TiAl3Phase thinning effect is most Good, because it is towards melt there are three crystal face, opposite his nucleation machine can be greatly increased with other patterns, thus he Thinning effect be best.And rod-shaped thinning effect be it is worst, its mode grown up is two-dimentional Zhi Jing, incubation period Long, solution rate is also very slow.Petal-like thinning effect is greater than rod-shaped and is less than bulk.TiAl simultaneously3The quantity of particle is got over Much better, it is also more more uniform better for being distributed, and size is the smaller the better.TiB2Generally in tiny graininess, the size of particle is thinner The small more uniform natural thinning effect of distribution is also better.So the means that predominantly detect for judging fining agent thinning effect are exactly aobvious Two kinds of active points TiAl in its tissue under micro mirror3With TiB2Shape, size, quantity and distribution.
1, the preparation of sample
1.1, material and equipment
Select domestic Al-5Ti-1B intermediate alloy as research object in the present invention, ingredient is as shown in table 1.
Table 1
1.2, the preparation of sample
Al-5Ti-1B intermediate alloy is taken, graphite crucible is put into and is placed in shaft furnace, setting heating rate (10~15 DEG C/ Min it) heats up with set temperature (720 DEG C, 740 DEG C, 760 DEG C, 780 DEG C, 800 DEG C, 820 DEG C), is kept the temperature after reaching set temperature afterwards (10~20min), then takes out graphite crucible, is put into low frequency magnetic field coil, and ceramic stirring rod is pre- at 600~700 DEG C After 15~20min of heat, electromagnetism, mechanical couplings stirring (5min, 10min, 15min) are carried out under heat-retaining condition, after stirring It is cooling by water cooled copper mould to obtain the final product.
2, test method
2.1, optical micro analysis: with the tissue topography for coming card optical microscopy DM-2500M observation sample and divided Analysis.
2.2, scanning electron microscope and energy spectrum analysis: by scanning electron microscopic observation sample topography, using electron probe energy disperse spectroscopy into Row point is swept and Surface scan, completes EDS test.
3, interpretation of result
3.1, optical micro analysis
Low power optical microscopy substantially observes the Al-5Ti-1B intermediate alloy original sample without the processing of high temperature coupled stir Tissue, is dispersed with a large amount of particles in aluminum substrate as shown in Figure 1, wherein there is biggish rod-shaped and blocky particle A uneven distribution In aluminum substrate, in addition there is the particle B of fine granularity Assembled distribution.
The discovery of Electronic Speculum test analysis, different disposal item are scanned by the fining agent handled different high temperature coupled stirs Any variation does not occur for the type of the Second Phase Particles under part in fining agent tissue, is all mainly TiAl3With TiB2Two kinds Phase, but it is different to be different the pattern of both phases under treatment conditions, size, quantity and distribution.
3.1.1 influence of the whipping temp to tissue
As shown in Fig. 2, TiAl in the tissue of untreated al-ti-b refiner3Size is very big, and full-size is even 200 μm or more are reached, most of size is all at 100 μm or so, and quantity is seldom, and distributed pole is uneven, poly- in lumps The trend of collection, pattern are mainly that elongated rod shape and lumps alternately exist, tiny TiB2Also there are aggregation situation, above several features All prove that the thinning effect of the fining agent is very unsatisfactory.
It is illustrated in figure 3 the sight of the metallographic structure of sample after identical coupled stir time (5min) different heating Temperature Treatment It examines and compares, the tissue topography of the second phase of the fining agent of discovery that can be apparent after the processing of high temperature coupled stir wants Better than the tissue topography of untreated fining agent, it is mainly reflected in Second Phase Particles TiAl3Size have and significantly reduce, Full-size also only has 100 μm or so, reduces 50% compared to original 200 μm.Further analysis is it can be found that at 760 DEG C Tissue topography with the al-ti-b refiner under 780 DEG C of processing is best, because of its Second Phase Particles TiAl3Scale topography Have and obviously changes.TiAl in (a) (b) (e) (f) four figure in al-ti-b refiner tissue3Size be mostly 100 μm, size is bigger, and distributing homogeneity is relatively poor, there is the case where assembling in lumps, and pattern is also mainly Elongated rod shape and lumps alternately exist, and there are also a small amount of petal-shapeds.And (c) TiAl in (d) two figure3Size averagely only have 50 μ M further improves its detailed performance compared to shortening 50% with 100 μm in (a) (b) (e) (f) four figure.And pattern Lumps all relatively good for thinning effect, quantity is also relatively more, and distribution is also more uniform, sends out without agglomerating phenomenon is assembled It is raw.These features all show that it possesses more excellent detailed performance, so most suitable in the case where coupled stir 5min Heating temperature section is 760 DEG C~780 DEG C.
The sight of the metallographic structure of sample after identical coupled stir time (10min) different heating Temperature Treatment as shown in Figure 4 It examines and compares, the tissue topography of the second phase of the fining agent of discovery that can be apparent after the processing of high temperature coupled stir wants Better than the tissue topography of untreated fining agent, it is mainly reflected in Second Phase Particles TiAl3Size have and significantly reduce, Full-size also only has 100 μm or so, reduces 50% compared to original 200 μm.Further analysis is it can be found that at 760 DEG C Tissue topography with the al-ti-b refiner under 780 DEG C of processing is best, because of its Second Phase Particles TiAl3Scale topography Have and obviously changes.TiAl in (a) (b) (e) (f) four figure in al-ti-b refiner tissue3Size be mostly 100 μm, size is bigger, and distribution is very uneven, there is the case where assembling in lumps, and pattern is also mainly elongated rod shape Alternately exist with lumps, there are also a small amount of petal-shapeds.And (c) TiAl in (d) two figure3Size averagely only have 50 μm, compare 50% is shortened with 100 μm in (a) (b) (e) (f) four figure, further improves its detailed performance.And pattern is also all thin Change the relatively good lumps of effect, quantity is also relatively more, and distribution is also more uniform, occurs without agglomerating phenomenon is assembled.This A little features all show that it possesses more excellent detailed performance, so most suitable heating in the case where coupled stir 10min Temperature range is also 760 DEG C~780 DEG C.
It is illustrated in figure 5 the metallographic structure of sample after identical coupled stir time (15min) different heating Temperature Treatment Observation and comparison, the tissue topography of the second phase of the fining agent of discovery that can be apparent after the processing of high temperature coupled stir It is better than the tissue topography of untreated fining agent, is mainly reflected in Second Phase Particles TiAl3Size have and significantly subtract Few, full-size also only has 100 μm or so, reduces 50% compared to original 200 μm, effect or apparent.Into one Step analysis it can be found that the tissue topography of al-ti-b refiner under handling at 760 DEG C and 780 DEG C is best because its second The scale topography of phase particle TiAl3, which has, obviously to be changed.The al-ti-b refiner tissue in (a) (b) (e) (f) four figure In the size of TiAl3 be mostly 100 μm, size is bigger, and is distributed very uneven, there is the case where assembling in lumps hair Raw, pattern is also mainly that elongated rod shape and lumps alternately exist, and there are also a small amount of petal-shapeds.And (c) TiAl in (d) two figure3's Size is average less than 50 μm, compared to shortening 50% with 100 μm in (a) (b) (e) (f) four figure, further improves its refinement Performance.And pattern is also all the relatively good lumps of thinning effect, quantity is also relatively more, and distribution is also more uniform, without Assemble agglomerating phenomenon to occur.These features all show that it possesses more excellent detailed performance, so in coupled stir 15min In the case where most suitable heating temperature section be also 760 DEG C~780 DEG C.
3.1.2 influence of the mixing time to tissue
As seen from Figure 6 when whipping temp is 760 DEG C, the tissue topography with the extension fining agent of mixing time is It becomes better and better, can be seen that TiAl in its second phase constitution from a figure3Pattern be substantially the relatively good agglomerate of thinning effect Shape or perhaps potato-like, and quantity is relatively more, and distribution is also relatively uniform, but still has fraction TiAl3Size It is bigger, illustrate that stirring is still not enough, is also to have part TiAl in b figure3Size it is bigger, and be distributed be not special Uniformly, hence it is evident that can see the TiAl in one piece of region3Seldom, illustrate that stirring is not especially sufficiently.TiAl in second phase constitution in c figure3 Pattern be extraordinary, be all the relatively good blocky potato-like in other words of thinning effect, size is all smaller, and quantity is non- Normal more distributions are also highly uniform, disperse.Thus as the tissue topography of the extension fining agent of mixing time is to become better and better 's.
As seen from Figure 7 when whipping temp is 780 DEG C, the tissue topography with the extension fining agent of mixing time is It becomes better and better, can be seen that TiAl in its second phase constitution from a figure3Pattern be substantially the relatively good agglomerate of thinning effect Shape or perhaps potato-like, and quantity is relatively more, and distribution is also relatively uniform, but still has fraction TiAl3Size It is bigger and get together, illustrate that stirring is still not enough, is also to have part TiAl in b figure3Size it is bigger, Er Qiefen Cloth is not especially uniformly, to illustrate that stirring is not especially sufficiently.TiAl in second phase constitution in c figure3Pattern be it is extraordinary, all It is the relatively good blocky potato-like in other words of thinning effect, size is all smaller, and the very more distributions of quantity are also very equal It is even, disperse.Thus as the tissue topography of the extension fining agent of mixing time becomes better and better.
3.2 sem analysis
Mainly there are α-Al, TiAl in al-ti-b refiner3、TiB2These three different phases.Respectively choose as former state, 720 DEG C, 780 DEG C and 820 DEG C of sample (do not stir as former state, remaining mixing time is 15min) is analyzed.
Electronic Speculum and EDAX results are scanned such as to the Al-5Ti-1B intermediate alloy handled without high temperature coupled stir Shown in Fig. 8.The percentage of biggish rod-shaped and blocky particle A the Al atom that is dispersed in aluminum substrate and Ti atom is close to 3 Than 1, therefore learn that it is TiAl3Phase, in Fig. 8 shown in (a).Its tissue is further amplified, can be sent out in conjunction with EDS spot scan Existing, in Fig. 8 shown in (d) and (e), wherein the percentage of the B atom of graininess Assembled distribution particle and Ti atom is close to 2 to 1, So learning that it is TiB2Phase, rest part are aluminum substrate.
Electronic Speculum is scanned to the Al-5Ti-1B intermediate alloy for being heated to 720 DEG C of stirring 15min high temperature coupled stir processing With EDAX results such as Fig. 9；It was found that the percentage of the Al atom for the biggish blocky particle being dispersed in aluminum substrate and Ti atom Than close to 3 to 1, so being TiAl3Phase, in Fig. 9 shown in (a).Its tissue is further amplified, it can be in conjunction with EDS spot scan It was found that wherein the percentage of the B atom of graininess Assembled distribution particle and Ti atom compares close to 2 as shown in (d) in Fig. 9 and (e) 1, so being TiB2Phase, rest part are similarly aluminum substrate.
Electronic Speculum is scanned to the Al-5Ti-1B intermediate alloy for being heated to 780 DEG C of stirring 15min high temperature coupled stir processing With EDAX results such as Figure 10；It was found that the hundred of the Al atom for the biggish lumps particle being dispersed in aluminum substrate and Ti atom Divide ratio close to 3 to 1, then learns its TiAl3Phase, in Figure 10 shown in (a).Its tissue is further amplified, is swept in conjunction with EDS point It retouches it can be found that as shown in (d) in Figure 10 and (e), wherein the percentage of the B atom of graininess Assembled distribution particle and Ti atom Close to 2 to 1, then learn it is TiB2Phase, rest part are similarly aluminum substrate.
Electronic Speculum is scanned to the Al-5Ti-1B intermediate alloy for being heated to 820 DEG C of stirring 15min high temperature coupled stir processing And energy spectrum analysis.As shown in figure 11, biggish rod-shaped and petal-shaped particle the Al atom and Ti atom being dispersed in aluminum substrate Percentage close to 3 to 1, learn it is TiAl3Phase, the wherein percentage of the B atom of graininess Assembled distribution particle and Ti atom Than learning it is TiB close to 2 to 12Phase, in Figure 11 shown in (a).Rest part is similarly aluminum substrate.
Pass through the spot scan and energy spectrum analysis to above several alloys, it is known that there are mainly two types of the in the al-ti-b refiner Two-phase particle, one is TiAl3Phase, size is bigger, and 50~150 μm are differed, predominantly lumps, it is rod-shaped with three kinds of petal-shaped Pattern, another kind are TiB2Phase, size is smaller, about 5 μm or so, is in granular form Assembled distribution.Surface scan point is carried out to sample Analysis, as a result as shown in figure 12.Complex chart 8~12 is it is found that in Al-5Ti-1B fining agent, and Ti element is mainly with TiAl3Xiang Yituan Blocky, elongated rod shape and petal-shaped is at random is distributed in matrix, and B element then Dispersed precipitate in matrix.
4, conclusion
(1) pass through the grinding to the tissue of Al-5Ti-1B fining agent to different mixings time (5min, 10min and 15min) Study carefully, finds with the extension of time, Al-5Ti-1B second phase particles TiAl3With TiB2Pattern, size, quantity and distribution have Obvious variation.With the extension of time, the thinning effect of Al-5Ti-1B fining agent is become better and better, by coming The analysis of card metallographic microscope and the discovery of its hoc scenario of scanning electron microscope analysis, second phase particles TiAl3With TiB2Pattern, big Small, quantity and distribution have obvious variation, and wherein the effect under 15min treatment conditions is best, because can be with Significantly observe its second phase particles TiAl3Pattern gradually from the poor petal-shaped of thinning effect and rod-shaped become agglomerate Shape, and its second phase particles TiAl3Size it is also smaller and smaller, become 50 μm or so from 200 μm or so, change very bright It is aobvious, and quantity also obviously becomes more, and distribution is also more uniform, no longer assembles agglomerating.And second phase particles TiB2Distribution It is more uniform, occur without agglomerating phenomenon is assembled, and size also reduces, therefore, with the extension of mixing time, The thinning effect of fining agent can improve.
(2) by the research to different whipping temps to the structure property of Al-5Ti-1B fining agent, as the result is shown with temperature The thinning effect of the raising Al-5Ti-1B fining agent of degree is first to rise to decline again, and it is best to reach effect at 760 DEG C~780 DEG C.It is logical It crosses and comes the analysis of card metallographic microscope and the discovery of its hoc scenario of scanning electron microscope analysis, second phase particles TiAl3With TiB2Shape Looks, size, quantity and distribution have obvious variation, wherein the effect under 760 DEG C~780 DEG C treatment conditions is best , because its second phase particles TiAl can be observed significantly3Pattern gradually by the poor petal-shaped of thinning effect and It is rod-shaped to become lumps, and its second phase particles TiAl3Size it is also smaller and smaller, become 50 μm or so from 200 μm or so, Change clearly, and quantity also obviously becomes more, distribution is also more uniform, no longer assembles agglomerating.And second phase particles TiB2Distribution it is also more uniform, occur without agglomerating phenomenon is assembled, and size also reduces, it is possible to regard to this Speculate, second phase particles TiAl3Forming the time should be stirred just at 760 DEG C~780 DEG C or so in that time Its second phase grain TiAl can be interrupted3, so that the size of its particle is become smaller, distribution is also more uniform, and pattern is more outstanding, natural number Amount is also just more.
The invention has the beneficial effects that: the present invention provides it is a kind of improve al-ti-b refiner structure property method, The original structure of al-ti-b refiner can be effectively improved.In the present invention by al-ti-b refiner in specific heating rate and It under specific temperature, is re-melted to obtain alloy liquid, shear at high temperature operation is implemented to alloy liquid, so as to improve aluminium titanium boron Fining agent structure property promotes the thinning effect of al-ti-b refiner.With the extension of mixing time and the raising of temperature, Secondary phase particle TiAl3Size it is also smaller and smaller, become 50 μm or so from 200 μm or so, variation clearly, and quantity Obvious to become more, distribution is also more uniform, no longer assembles agglomerating.And second phase particles TiB2Distribution it is also more uniform, without Assemble agglomerating phenomenon to occur, and size is also reducing.Show good thinning effect.
Detailed description of the invention
Fig. 1 is the metallographic microstructure figure of Al-5Ti-1B；
Fig. 2 is the metallic phase image figure of the sample without the processing of high temperature coupled stir；
Fig. 3 is coupled stir 5 minutes under different temperatures sample Metallographic Analysis figures；
Fig. 4 is different temperatures coupled stir 10 minutes sample Metallographic Analysis figures；
Fig. 5 is different temperatures coupled stir 15 minutes sample Metallographic Analysis figures；
Fig. 6 is the sample Metallographic Analysis figure of 760 DEG C of temperature coupled stir different times；
Fig. 7 is the sample Metallographic Analysis figure of 780 DEG C of coupled stir different times；
Fig. 8 is the scanning electron microscope tissue and energy spectrum analysis figure of Al-5Ti-1B；
Fig. 9 is the microstructure and EDS energy spectrum analysis figure of Al-5Ti-1B under the conditions of 720 DEG C of stirrings, 15min；
Figure 10 is the microstructure and EDS energy spectrum analysis figure of Al-5Ti-1B under the conditions of 780 DEG C of stirrings, 15min；
Figure 11 is the microstructure and EDS energy spectrum analysis figure of Al-5Ti-1B under the conditions of 820 DEG C of stirrings, 15min；
Figure 12 is Al-5Ti-1B Surface scan analysis chart；
The meaning of appended drawing reference in figure: Fig. 2: A~D: the sample without the processing of high temperature coupled stir；Fig. 3: (a) at 720 DEG C Reason, (b) 740 DEG C of processing, (c) 760 DEG C of processing, (d) 780 DEG C of processing, (e) 800 DEG C of processing, (f) 820 DEG C of processing；Fig. 4: (a) 720 DEG C of processing, (b) 740 DEG C of processing, (c) 760 DEG C of processing, (d) 780 DEG C of processing, (e) 800 DEG C of processing, (f) 820 DEG C of processing；Figure 5:(a) 720 DEG C of processing, (b) 740 DEG C of processing, (c) 760 DEG C of processing, (d) 780 DEG C of processing, (e) 800 DEG C of processing, (f) at 820 DEG C Reason；Fig. 6: (a) 5min is handled, and (b) 10min is handled, and (c) 15min is handled；Fig. 7: (a) 5min is handled, and (b) 10min is handled, (c) 15min processing.Fig. 8: (a) TiAl3Scanning electron microscope, (b) TiAl3Energy spectrum analysis, (c) α-Al energy spectrum analysis, (d) TiB2Scanning electricity Mirror, (e) TiB2Energy spectrum analysis；Fig. 9: (a) TiAl3Scanning electron microscope, (b) TiAl3Energy spectrum analysis, (c) α-Al energy spectrum analysis, (d) TiB2Scanning electron microscope, (e) TiB2Energy spectrum analysis；Figure 10: (a) TiAl3 scanning electron microscope, (b) TiAl3Energy spectrum analysis, (c) α-Al energy Spectrum analysis, (d) TiB2Scanning electron microscope, (e) TiB2 energy spectrum analysis；Figure 11: (a) TiAl3With TiB2 scanning electron microscope, (b) TiAl3Energy Spectrum analysis, (c) α-Al energy spectrum analysis, (d) TiB2Energy spectrum analysis；Figure 12: the Surface scan region (a), (b) Al scanning distribution, (c) Ti Scanning distribution, (d) B-scan is distributed.
Specific embodiment
The present invention will be further described below in conjunction with specific embodiments.
Embodiment 1
A method of improving al-ti-b refiner structure property, comprising the following steps: Al-5Ti-1B intermediate alloy is taken, It is put into graphite crucible to be placed in shaft furnace, heats up after 10 DEG C/min of heating rate and 720 DEG C of set temperature are set, reach setting 10min is kept the temperature after temperature, then takes out graphite crucible, is put into low frequency magnetic field coil, and electromagnetism, machine are carried out under heat-retaining condition Tool coupled stir 5min, wherein mechanical stirring is that ceramic stirring rod preheats 15min at 600 DEG C in electromagnetism, mechanical couplings stirring After be stirred, it is cooling by water cooled copper mould after stirring to obtain the final product.Wherein, the magnetic field strength of low frequency magnetic field coil is 12000AT；Mechanical stirring frequency is 2Hz in electromagnetism, mechanical couplings stirring.
Embodiment 2
A method of improving al-ti-b refiner structure property, comprising the following steps: Al-5Ti-1B intermediate alloy is taken, It is put into graphite crucible to be placed in shaft furnace, heats up after 15 DEG C/min of heating rate and 820 DEG C of set temperature are set, reach setting 20min is kept the temperature after temperature, then takes out graphite crucible, is put into low frequency magnetic field coil, and electromagnetism, machine are carried out under heat-retaining condition Tool coupled stir 15min, wherein mechanical stirring is that ceramic stirring rod preheats at 700 DEG C in electromagnetism, mechanical couplings stirring It is stirred after 20min, it is cooling by water cooled copper mould after stirring to obtain the final product.Wherein, the magnetic field strength of low frequency magnetic field coil is 15000AT；Mechanical stirring frequency is 3Hz in electromagnetism, mechanical couplings stirring.
Embodiment 3
A method of improving al-ti-b refiner structure property, comprising the following steps: Al-5Ti-1B intermediate alloy is taken, It is put into graphite crucible to be placed in shaft furnace, heats up after 12 DEG C/min of heating rate and 760 DEG C of set temperature are set, reach setting 15min is kept the temperature after temperature, then takes out graphite crucible, is put into low frequency magnetic field coil, and electromagnetism, machine are carried out under heat-retaining condition Tool coupled stir 10min, wherein mechanical stirring is that ceramic stirring rod preheats at 650 DEG C in electromagnetism, mechanical couplings stirring It is stirred after 18min, it is cooling by water cooled copper mould after stirring to obtain the final product.Wherein, the magnetic field strength of low frequency magnetic field coil is 14000AT；Mechanical stirring frequency is 2.5Hz in electromagnetism, mechanical couplings stirring.
Embodiment 4
A method of improving al-ti-b refiner structure property, comprising the following steps: Al-5Ti-1B intermediate alloy is taken, It is put into graphite crucible to be placed in shaft furnace, heats up after 13 DEG C/min of heating rate and 780 DEG C of set temperature are set, reach setting 17min is kept the temperature after temperature, then takes out graphite crucible, is put into low frequency magnetic field coil, and electromagnetism, machine are carried out under heat-retaining condition Tool coupled stir 8min, wherein mechanical stirring is that ceramic stirring rod preheats 19min at 620 DEG C in electromagnetism, mechanical couplings stirring After be stirred, it is cooling by water cooled copper mould after stirring to obtain the final product.Wherein, the magnetic field strength of low frequency magnetic field coil is 13000AT；Mechanical stirring frequency is 2Hz in electromagnetism, mechanical couplings stirring.
Embodiment 5
A method of improving al-ti-b refiner structure property, comprising the following steps: Al-5Ti-1B intermediate alloy is taken, It is put into graphite crucible to be placed in shaft furnace, heats up after 11 DEG C/min of heating rate and 770 DEG C of set temperature are set, reach setting 13min is kept the temperature after temperature, then takes out graphite crucible, is put into low frequency magnetic field coil, and electromagnetism, machine are carried out under heat-retaining condition Tool coupled stir 14min, wherein mechanical stirring is that ceramic stirring rod preheats at 680 DEG C in electromagnetism, mechanical couplings stirring It is stirred after 16min, it is cooling by water cooled copper mould after stirring to obtain the final product.Wherein, the magnetic field strength of low frequency magnetic field coil is 15000AT；Mechanical stirring frequency is 3Hz in electromagnetism, mechanical couplings stirring.
Embodiment 6
A method of improving al-ti-b refiner structure property, comprising the following steps: Al-5Ti-1B intermediate alloy is taken, It is put into graphite crucible to be placed in shaft furnace, heats up after 14 DEG C/min of heating rate and 765 DEG C of set temperature are set, reach setting 16min is kept the temperature after temperature, then takes out graphite crucible, is put into low frequency magnetic field coil, and electromagnetism, machine are carried out under heat-retaining condition Tool coupled stir 9min, wherein mechanical stirring is that ceramic stirring rod preheats 17min at 660 DEG C in electromagnetism, mechanical couplings stirring After be stirred, it is cooling by water cooled copper mould after stirring to obtain the final product.Wherein, the magnetic field strength of low frequency magnetic field coil is 12000AT；Mechanical stirring frequency is 2Hz in electromagnetism, mechanical couplings stirring.
Embodiment 7
A method of improving al-ti-b refiner structure property, comprising the following steps: Al-5Ti-1B intermediate alloy is taken, It is put into graphite crucible to be placed in shaft furnace, heats up after 11 DEG C/min of heating rate and 740 DEG C of set temperature are set, reach setting 15min is kept the temperature after temperature, then takes out graphite crucible, is put into low frequency magnetic field coil, and electromagnetism, machine are carried out under heat-retaining condition Tool coupled stir 13min, wherein mechanical stirring is that ceramic stirring rod preheats at 600 DEG C in electromagnetism, mechanical couplings stirring It is stirred after 19min, it is cooling by water cooled copper mould after stirring to obtain the final product.Wherein, the magnetic field strength of low frequency magnetic field coil is 13500AT；Mechanical stirring frequency is 2.5Hz in electromagnetism, mechanical couplings stirring.
Embodiment 8
A method of improving al-ti-b refiner structure property, comprising the following steps: Al-5Ti-1B intermediate alloy is taken, It is put into graphite crucible to be placed in shaft furnace, heats up after 15 DEG C/min of heating rate and 800 DEG C of set temperature are set, reach setting 12min is kept the temperature after temperature, then takes out graphite crucible, is put into low frequency magnetic field coil, and electromagnetism, machine are carried out under heat-retaining condition Tool coupled stir 14min, wherein mechanical stirring is that ceramic stirring rod preheats at 700 DEG C in electromagnetism, mechanical couplings stirring It is stirred after 18min, it is cooling by water cooled copper mould after stirring to obtain the final product.Wherein, the magnetic field strength of low frequency magnetic field coil is 14000AT；Mechanical stirring frequency is 3Hz in electromagnetism, mechanical couplings stirring.

Claims (3)

1. a kind of method for improving al-ti-b refiner structure property, it is characterised in that: the following steps are included: taking Al-5Ti-1B Intermediate alloy is put into graphite crucible and is placed in shaft furnace, and setting heating rate is 10 DEG C/min~15 DEG C/min and setting temperature Degree heats up after being 720 DEG C~820 DEG C, keeps the temperature 10min~20min after reaching set temperature, then takes out graphite crucible, put Enter in low frequency magnetic field coil, electromagnetism, mechanical couplings stirring are carried out under heat-retaining condition, it is cooling by water cooled copper mould after stirring To obtain the final product；The magnetic field strength of the low frequency magnetic field coil is 12000 ~ 15000AT；Machinery stirs in the electromagnetism, mechanical couplings stirring Mixing frequency is 2 ~ 3Hz；The mixing time is 5~15min, and whipping temp is 760 DEG C~780 DEG C.
2. the method for the improvement al-ti-b refiner structure property according to claim 1, it is characterised in that: the electricity Mechanical stirring refers in magnetic, mechanical couplings stirring is stirred with the ceramic stirring rod after preheating.
3. improving the method for al-ti-b refiner structure property according to claim 2, it is characterised in that: ceramics stirring Stick preheats 15~20min at 600~700 DEG C.
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CN102990046A (en) * 2012-12-26 2013-03-27 常州大学 Method for refining pure aluminum from Al-5% Ti-1%B intermediate alloy
CN104498746A (en) * 2015-01-21 2015-04-08 广西大学 Method for preparing Al-5Ti-1B-1(La+Ce) intermediate alloy grain refiner having different content of lanthanum and cerium

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CN101708531A (en) * 2009-09-23 2010-05-19 清华大学 Method for improving fluidity of alloy melt and rotating electromagnetic field generation device
CN102990046A (en) * 2012-12-26 2013-03-27 常州大学 Method for refining pure aluminum from Al-5% Ti-1%B intermediate alloy
CN104498746A (en) * 2015-01-21 2015-04-08 广西大学 Method for preparing Al-5Ti-1B-1(La+Ce) intermediate alloy grain refiner having different content of lanthanum and cerium

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