CN102703986A - Method for transforming columnar crystal-orienting isometric crystal of directional solidified alloy with strong static magnetic field induction - Google Patents
Method for transforming columnar crystal-orienting isometric crystal of directional solidified alloy with strong static magnetic field induction Download PDFInfo
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Abstract
The invention relates to a method for transforming a columnar crystal-orienting isometric crystal of a directional solidified alloy with strong static magnetic field induction and belongs to the technical field of an alloy metallographic structure controlled by a physical field. According to the method, the growth morphology of an alloy treelike crystal is controlled by utilizing a thermoelectric magnetic effect generated under the mutual action of the strong static magnetic field and a temperature gradient generated on a solid liquid interface during a directional solidifying process. The method provided by the invention is characterized in that a 10-14T strong static magnetic field is utilized; a typical Bridgman directional solidifying device is adopted; the solid liquid interface of a melt is designed as being in a central position of the strong static magnetic field; the whole solidifying process is finished under the strong static magnetic field; a lathy alloy bar is adopted; the temperature gradient of the solid liquid interface of a sample is changed following the change in furnace temperature and alloy variety; the directional solidifying is performed under the condition of a downward drawing speed of the alloy bar at 10-120 microns per second; and after a crystal grows to a stable stage, the crystal is quickly pulled into a cooling medium for quenching, so that a special isometric crystal alloy structure is finally obtained under the directional solidifying condition.
Description
Technical field
The present invention relates to a kind of method of under strong static magnetic field, inducing alloy directionally solidified tissue to change to equiax crystal by column crystal; Provide a kind of and existing through the different induced orientation solidified structure pattern of mechanical oscillation, electromagnetic oscillation method by column crystal to the novel process that equiax crystal changes, belong to alloy structure Control Study technical field.
Background technology
Dendrite is a kind of style of organizing the most common in the material prepn forming process, and its size and form have very important influence to the final performance of material.Under normal conditions, people hope that generally dendrite can grow with the equiax crystal mode, because by the equiax crystal resulting polycrystalline material of growing; Non-anisotropy with performance; When stress deformation, owing to have the mutual coordinative role of polycrystalline grain distortion, and inner a large amount of crystal boundaries can improve resistance to deformation on the one hand; Can block simultaneously the development of crackle again, therefore have higher intensity and plasticity usually.This shows in the material solidification process control of column crystal and equiax crystal growth to be had very important influence to the final use properties of material.
In order to obtain the equiaxed grain structure of refinement, investigators have carried out a large amount of explorations and research.The mode of action according to control melt means is different, can these means be divided into thermodynamic control mode, chemical control mode and kinetic control mode.
The principle of thermodynamic control mode is theoretical based on the crystallography of solidifying, and Johnson-Mei Er equation can be derived, and counts P (t) and nucleation rate at the nucleus that t formed in the time
NAnd growth rate
v g Between relation:
Can know nucleation rate by following formula
NBig more, crystal grain is tiny more.Commaterial
NWith
v g All depend on condensate depression, increase condensate depression,
NIncrease rapidly, and ratio
v g Faster, therefore, under general curing condition, increase condensate depression and can make the grain refining after solidifying.The chemical control mode is through in melt, adding nucleating agent, and actual solidifying all be heterogeneous nucleation, is the raising nucleation rate, can adding can be as the artificial nucleating agent of heterogeneous nucleation substrate before liquation solidifies.
Compare with preceding two kinds of methods, utilize the kinetics function crystal grain thinning, promote column crystal to be that segregation is less, not introduce impurity element to the equiax crystal transformation.Commonly used comprises two big types: 1. mechanical vibration 2. physical fields.Mechanical vibration comprise: mechanical stirring, vibration, swing etc.; Physical field comprises: alternating electric field, UW, travelling-magnetic-field, rotatingfield and electromagnetic complex field.The effect in outfield can cause column crystal fracture usually, in free and the melt, the transformation of column crystal to equiax crystal takes place, and the time crystal grain generation refinement.These methods can effectively promote melt flow, make temperature field homogenizing in the melt,
But still there are a lot of defectives in above-mentioned outfield.The mechanical oscillation method need contact with melt and could oscillation force be reached melt through vibrator, causes the pollution of molten metal, and simultaneously, the thinning effect of vibration mainly concentrates near the vibrator, and the tissue odds that obtains is even.The defective of sonic oscillation is that sound wave dissipates seriously in high-temperature fusant, the refinement zone is limited.Pulsed current (magnetic field) can produce thermal agitation at short notice, but excessive then being prone to of electric current causes melt to splash, and electric current is too little, can make crystal grain remelting in high-temperature fusant of new formation, the reduction thinning effect.
For this reason, high-intensity magnetic field seminar of Shanghai University inserts pair of electrodes through metal melt top in mold; And feeding alternating-current; The mold outside applies strong static magnetic field, utilizes near the rapid forming core of melt of self cooling electrode-induced electrode, combines electromagnetic oscillation to impel nucleus to launch in the metal melt simultaneously; Form the core main body of metal freezing thereafter, obtain fine grained texture's material.But this method, complex equipments is difficult to carry out in industrial production; Electrode contacts with melt, still can pollution metal liquid; Electrode need feed high-frequency current simultaneously, needs to consume mass energy, also has obstacle so industry is promoted.
Summary of the invention
To the deficiency that prior art exists, the purpose of this invention is to provide a kind of method of under strong static magnetic field, inducing alloy directionally solidified tissue generation column crystal to change to equiax crystal.
The method that a kind of strong static magnetic field induced orientation of the present invention solidified structure generation column crystal changes to equiax crystal; It is characterized in that solid-liquid interface in the directional freeze is placed the strong static magnetic field central position; Effect through thermoelectric magnetic effect is brought into play under the dendrite size interrupts dendrite, increases nucleation rate in the forward position, interface; Finally cause column crystal to change, make crystal grain obtain refinement to equiax crystal.This method does not need complex apparatus, only need apply strong static magnetic field, thereby industrial generalization is strong; The thermoelectric magnetic force that produces through magnetic field causes the fracture of dendrite, has really accomplished pollution-freely, can be used for preparing highly purified fine grained texture.Generally speaking, this method is simple to operate, be easy to realize, for promoting that column crystal changes to equiax crystal, thereby the excellent equiaxed grain structure of obtained performance provides a kind of new approaches.
The characteristics and the principle of the inventive method are described below:
The used device for directionally solidifying of method that a kind of strong static magnetic field induced orientation of the present invention solidified structure generation column crystal changes to equiax crystal; It is the conventional device of tradition, includes water-cooling jacket, process furnace, alloy bar, superconduction kicker magnet, alloy bar and has solidified part, quenching bath and pull bar; It is characterized in that device for directionally solidifying is as in the superconduction kicker magnet; One water-cooling jacket is set in the middle of superconduction kicker magnet and process furnace; The solid-liquid interface of sample is in the steady magnetic field zone of kicker magnet.
The principle of the invention is based on the thermoelectric magnetomechanical effects of strong static magnetic field.Thermoelectric magnetomechanical effects derives from the interaction of the thermoelectric current on magnetic field and the dendrite, and the principle that thermoelectric current produces is the Seebeck effect, as two Seebeck coefficient (η
s , η
l ) different metallic is connected to together at two ends up and down; And has thermograde Δ T between two nodes; Will form thermoelectric current in the loop; Produce a thermoelectric force and in alloy directionally solidified process, apply axial strong static magnetic field, under the certain temperature gradient effect, find that the phenomenon that is changed to equiax crystal by column crystal has taken place oriented freezing organization.Compare to the technology that equiax crystal changes with the existing column crystal of inducing, present method is through in the directional freeze process, applying static magnetic field, and is most advanced and sophisticated because thermoelectric magnetic effect produces potential difference Δ V at the dendrite in forward position, interface, as shown in Figure 2.The thermoelectric force size that connects the metal two ends is suc as formula shown in (1), and the Seebeck coefficient difference of two kinds of materials is big more, and the temperature difference is big more, and thermoelectric force that produces in the loop and thermoelectric current are just big more.
ΔV=（η
s -η
l ）ΔT…………………………………………………………………(1)
When alloy is grown with the dendrite mode,, can there be bigger thermograde in solid-liquid interface along the dendritic growth direction in the directional freeze process; And different its Seebeck coefficients that cause with interdendritic liquid composition of dendrite solid phase are different; Therefore can form thermocouple, produce thermoelectric current, cause thermoelectric magnetic force; Owing to, can only make that solid phase dendrite is stressed than the flowing of magnetic field inhibited liquid phase fluid under the high-intensity magnetic field.In the directional freeze process, as long as thermoelectric magnetic force is enough big, the thermoelectric magnetic force on the dendrite just can make dendritic arm rupture, and broken dendritic arm becomes the heterogeneous core of equi-axed crystal again, and these equi-axed crystal still can receive the effect of power under the effect in magnetic field.These equi-axed crystal are through merging, grow and then forming equiaxed grain structure as shown in the figure.This thermoelectric magnetomechanical effects of dendrite for the binary alloy in the experiment is remarkable, for the superalloy that uses in the aircraft industry, because interpolation alloying element kind is many; Quantity is big, generally has more than 10 kind of alloying element, addition even reach 30-40wt%; So superalloy solid phase dendrite and on every side liquid composition differ bigger, its Seebeck coefficient difference can be bigger, solid phase dendrite is stressed more obvious; Under big thermograde and magneticstrength effect, more be prone to this effect of performance.Rationally be utilized in the heterogeneous forming core of solid-liquid interface leading portion, and then make the dendrite pattern, can a kind of new thinking be provided for optimizing the alloy over-all properties by the effect of column crystal to the equiax crystal transformation.
It is characterized in that having following process and step:
A. adopt the conventional Bridgman method device for directionally solidifying of typical tradition; Alloy bar sample with Al-Cu or different systems such as Pb-Sn or Al-Si; In the corundum crucible in the encapsulation device for directionally solidifying; And it is contained on the pull bar, make it in the process furnace in the device, make vertical shifting by pull;
B. device for directionally solidifying is put into superconduction strong static magnetic field generation body, and the magneticstrength that superconducting magnet produces requires at 10-14T, makes the solid-liquid interface of directional freeze be in the steady zone in magnetic field;
C. process furnace heats the alloy test rod, and the heat-eliminating medium in the quenching bath is liquid Ga-In-Sn alloy, and the magneticstrength of superconduction kicker magnet all keeps stable during the course, and process furnace is also fixing; The thermograde in forward position, freezing interface changes with furnace temp; Temperature gradient of solid-liquid interface is more than 40K/cm generally speaking, and the withdrawing rate variation range is (drawing velocity of different-alloy is different) below the 120 μ m/s; Guarantee that in the pull process solid-liquid interface is in the steady magnetic field district, during with sample pull certain-length to stable growth zone, draw in the quenching bath rapidly and quench.
D. through the pattern of alloy grain after the observation directional freeze, explain that oriented freezing organization column crystal has taken place changed to equiax crystal, and estimate the situation of this transformation of alloy thus.
Description of drawings
Fig. 1 is the legal simple structure synoptic diagram to coagulation system of Bridgman under the used high-intensity magnetic field of the inventive method.Wherein 1-water-cooling jacket, 2-process furnace, 3-alloy bar melt, 4-superconduction kicker magnet, 5-alloy bar have solidified part, 6-quenching bath, 7-pull bar, 8-corundum crucible.
Fig. 2 is the principle schematic of the inventive method, and dendrite is most advanced and sophisticated because temperature difference heat electromotive force effect receives the effect of thermoelectric magnetic force; The fracture to such an extent as to deform; Become new forming core point, and hinder the further growth of column crystal, make tissue that column crystal take place and change to equiax crystal.
Fig. 3 for pulling rate be 20 μ m/s and thermograde when being 52K/cm Pb-80wt% Sn hypereutectic alloy at (a) 0T, (b) microtexture of vertical section under the 12T magneticstrength.
Fig. 4 for pulling rate be 10 μ m/s and thermograde when being 62.8K/cm Al-4.5wt% Cu hypoeutectic alloy at (a) 0T, (b) microtexture of vertical section under the 10T magneticstrength.
Fig. 5 for pulling rate be 120 μ m/s and thermograde when being 40K/cm Al-7wt% Si hypoeutectic alloy at (a) 0T, (b) microtexture of vertical section under the 12T magneticstrength.
Embodiment
After specific embodiment of the present invention being described at present.
Embodiment one
(1) selecting alloying constituent for use is the slicker solder hypereutectic alloy of Pb-80wt% Sn, and the purity of Pb and Sn is 99.99%, and it is that 3mm, length are the alloy bar of 20cm that the method for behind vacuum induction melting, casting through the negative pressure suction obtains diameter, and it is encapsulated in the alundum tube;
(2) utilize the device for directionally solidifying (see figure 1) of typical B ridgman method, above-mentioned alundum tube is fixed on the pull bar, and rises in the process furnace; The vertical strong static magnetic field that adopts the superconduction kicker magnet to produce makes the solid-liquid interface of sample be in the steady magnetic field zone, and controlling magnetic field intensity is 12T (tesla);
(3) energized is opened process furnace, and alloy bar is heated, and the process furnace core temperature is 600 ℃, and insulation 30min, learns that through measuring the thermograde in liquid-solid interface the place ahead is 52K/cm; The alloy bar sample moves down with the drawing velocity of 20 μ m/s, when sample directional solidification growth length reaches 80mm, draws in rapidly in the Ga-In-Sn heat-eliminating medium and quenches; Finally obtain the equiax crystal alloy structure under the directional freeze condition.
Embodiment two: process in the present embodiment and step and the foregoing description 1 are identical, and different is: alloy is an Al-4.5wt% Cu hypoeutectic alloy; The core temperature of process furnace is 900 ℃; The drawing velocity of pull bar is 10 μ m/s; The thermograde in sample solid-liquid interface forward position is 62.8K/cm in the stove; The magneticstrength that superconducting magnet produces is 10T.
Embodiment three: process in the present embodiment and step and the foregoing description 2 are identical, and different is: alloy system is an Al-7wt% Si hypoeutectic alloy; The process furnace core temperature is 900 ℃, and sample solid-liquid interface temp gradient at front edge is through being measured as 40K/cm; The drawing velocity of pull bar is 120 μ m/s.
The microstructure observation of alloy bar sample solidified structure dendrite
With the sample of directional freeze gained vertically symmetry section, and be taken near the sample the solid-liquid interface; With its grinding and polishing, corrode then, the employed etching reagent of Pb-Sn alloy sample is oxalic acid and hydrogen peroxide mixed solution, volume ratio is 3:1; The used etching reagent of Al-Cu and Al-Si alloy sample is H
2O:HF mixing solutions, both volume ratios are water: HF=1000:5.
In order to oppose frequently, the sample of the foregoing description 1,2,3 has also correspondingly adopted the sample for applying magneticstrength (0T) to detect contrast in testing process.
The microcosmic microstructure result of embodiment 1,2,3 samples is referring to Fig. 3, Fig. 4 and Fig. 5.
From figure, contrast and can know, the equiax crystal of the microtexture that applies sample vertical section behind the magnetic field for rupturing of gained compared with the dendritic structure of continuous growth under the no magnetic field condition in the embodiment of the invention, and the transformation of tangible column crystal to equiax crystal taken place.
Claims (2)
1. a strong static magnetic field induced orientation solidified superalloy column crystal is characterized in that having following process and step to the method that equiax crystal changes:
A. adopt typical traditional conventional Bridgman method device for directionally solidifying; Alloy bar sample with Al-Cu or different systems such as Pb-Sn or Al-Si; In the corundum crucible in the encapsulation device for directionally solidifying; And it is contained on the pull bar, make it in the process furnace in the device, make vertical shifting by pull;
B. device for directionally solidifying is put into superconduction strong static magnetic field generation body, and the static magnetic field strength that superconducting magnet produces can make the solid-liquid interface of directional freeze be in the steady zone in magnetic field at 10-14T;
C. process furnace heats the alloy test rod; Heat-eliminating medium in the quenching bath is liquid Ga-In-Sn alloy; The magneticstrength of superconduction kicker magnet will keep stable in implementation process, and process furnace is also fixing, and the thermograde in forward position, freezing interface changes with furnace temp; The process furnace center furnace temperature of Al-Cu alloy is 900 ℃, and thermograde is 45K/cm, and withdrawing rate is less than 10 μ m/s; The process furnace center furnace temperature of Pb-Sn alloy is 600 ℃, and thermograde is 52K/cm, and withdrawing rate is less than 50 μ m/s; The process furnace center furnace temperature of Al-Si alloy is 900 ℃, and thermograde is 40K/cm, and withdrawing rate is less than 150 μ m/s; Guarantee that in the pull process solid-liquid interface is in the steady magnetic field district; During with sample pull certain-length to stable growth zone, draw in the quenching bath rapidly and quench.
2. a strong static magnetic field induced orientation solidified structure generation column crystal is to the used conventional device for directionally solidifying of tradition of method that equiax crystal changes, and includes water-cooling jacket (1), process furnace (2), alloy bar melt (3), superconduction kicker magnet (4), alloy bar and solidified part (5), quenching bath (6), pull bar (7) and corundum crucible (8); It is characterized in that device for directionally solidifying is as in the superconduction kicker magnet (4); One water-cooling jacket (1) is set in the middle of superconduction kicker magnet (4) and process furnace (2); Alloy bar melt (3) has solidified the steady magnetic field zone that part (5) junction is positioned over kicker magnet (4) with alloy bar.
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Cited By (12)
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| CN103056347A (en) * | 2013-01-09 | 2013-04-24 | 上海大学 | Method for controlling dendritic crystal orientation of oriented solidification structure by high-intensity magnetic field |
| CN104416252A (en) * | 2013-08-28 | 2015-03-18 | 中国科学院金属研究所 | Preparation method of preferred orientation texture welding spots |
| CN104785739A (en) * | 2015-04-21 | 2015-07-22 | 上海大学 | Method and device for grain refinement in secondary cooling area in continuous casting process under steady-state magnetic field condition |
| CN104862777A (en) * | 2015-05-19 | 2015-08-26 | 上海大学 | Method and device for controlling crystal orientation in steady-state magnetic field through directional solidification |
| CN105970133A (en) * | 2016-04-27 | 2016-09-28 | 上海大学 | Method for preparing metastable metal material through stable-state magnetic field and application thereof |
| CN107385513A (en) * | 2017-09-06 | 2017-11-24 | 中国科学院金属研究所 | A kind of directional solidification furnace is heated with center and central cooling device |
| CN108655375A (en) * | 2018-05-17 | 2018-10-16 | 上海大学 | The method and its device for directionally solidifying of functionally graded material are prepared using axial homogeneous magnetic field |
| CN112695263A (en) * | 2020-12-08 | 2021-04-23 | 上海大学 | Method for eliminating solidification material segregation in strong magnetostatic field |
| CN113957276A (en) * | 2021-10-26 | 2022-01-21 | 西北工业大学 | Liquid deep supercooling and solid phase change duplex coordination control method and device for metal material |
| CN114164495A (en) * | 2021-10-27 | 2022-03-11 | 上海大学 | Multi-mode magnetostatic field controlled single crystal high-temperature alloy directional solidification growth device, method and application thereof |
| CN114182352A (en) * | 2021-12-13 | 2022-03-15 | 西北工业大学 | Preparation method of multi-stage directional growth metal material under multi-field action |
| CN115090860A (en) * | 2022-06-20 | 2022-09-23 | 上海大学 | Method for regulating peritectic phase volume fraction in peritectic alloy |
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| CN103056347A (en) * | 2013-01-09 | 2013-04-24 | 上海大学 | Method for controlling dendritic crystal orientation of oriented solidification structure by high-intensity magnetic field |
| CN104416252A (en) * | 2013-08-28 | 2015-03-18 | 中国科学院金属研究所 | Preparation method of preferred orientation texture welding spots |
| CN104416252B (en) * | 2013-08-28 | 2016-08-10 | 中国科学院金属研究所 | A kind of preparation method of preferred orientation texture solder joint |
| CN104785739A (en) * | 2015-04-21 | 2015-07-22 | 上海大学 | Method and device for grain refinement in secondary cooling area in continuous casting process under steady-state magnetic field condition |
| CN104862777A (en) * | 2015-05-19 | 2015-08-26 | 上海大学 | Method and device for controlling crystal orientation in steady-state magnetic field through directional solidification |
| CN104862777B (en) * | 2015-05-19 | 2018-03-02 | 上海大学 | The method and device of directional solidification control crystal orientation under steady magnetic field |
| CN105970133A (en) * | 2016-04-27 | 2016-09-28 | 上海大学 | Method for preparing metastable metal material through stable-state magnetic field and application thereof |
| CN107385513B (en) * | 2017-09-06 | 2023-11-10 | 中国科学院金属研究所 | Central heating and central cooling device for directional solidification furnace |
| CN107385513A (en) * | 2017-09-06 | 2017-11-24 | 中国科学院金属研究所 | A kind of directional solidification furnace is heated with center and central cooling device |
| CN108655375A (en) * | 2018-05-17 | 2018-10-16 | 上海大学 | The method and its device for directionally solidifying of functionally graded material are prepared using axial homogeneous magnetic field |
| CN112695263A (en) * | 2020-12-08 | 2021-04-23 | 上海大学 | Method for eliminating solidification material segregation in strong magnetostatic field |
| CN113957276A (en) * | 2021-10-26 | 2022-01-21 | 西北工业大学 | Liquid deep supercooling and solid phase change duplex coordination control method and device for metal material |
| CN113957276B (en) * | 2021-10-26 | 2022-07-26 | 西北工业大学 | Liquid deep undercooling and solid phase change duplex coordination control method and device for metal material |
| CN114164495A (en) * | 2021-10-27 | 2022-03-11 | 上海大学 | Multi-mode magnetostatic field controlled single crystal high-temperature alloy directional solidification growth device, method and application thereof |
| CN114164495B (en) * | 2021-10-27 | 2024-05-14 | 上海大学 | Multi-mode static magnetic field controlled single crystal superalloy directional solidification growth device, method and application thereof |
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| CN115090860A (en) * | 2022-06-20 | 2022-09-23 | 上海大学 | Method for regulating peritectic phase volume fraction in peritectic alloy |
| CN115090860B (en) * | 2022-06-20 | 2023-08-18 | 上海大学 | Method for regulating and controlling volume fraction of peritectic phase in peritectic alloy |
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Application publication date: 20121003 |