CN107052282B - A kind of preparation method of the twin dendrite of Al-40%Zn alloy - Google Patents

A kind of preparation method of the twin dendrite of Al-40%Zn alloy Download PDF

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Publication number
CN107052282B
CN107052282B CN201710281993.8A CN201710281993A CN107052282B CN 107052282 B CN107052282 B CN 107052282B CN 201710281993 A CN201710281993 A CN 201710281993A CN 107052282 B CN107052282 B CN 107052282B
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heating
alloy
dendrite
thermal insulation
twin
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CN107052282A (en
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高卡
赵彪
白中义
宋文正
刘军威
郭晓琴
张锐
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Zhengzhou University of Aeronautics
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Zhengzhou University of Aeronautics
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22DCASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D11/00Continuous casting of metals, i.e. casting in indefinite lengths
    • B22D11/04Continuous casting of metals, i.e. casting in indefinite lengths into open-ended moulds
    • B22D11/049Continuous casting of metals, i.e. casting in indefinite lengths into open-ended moulds for direct chill casting, e.g. electromagnetic casting
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22DCASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D11/00Continuous casting of metals, i.e. casting in indefinite lengths
    • B22D11/001Continuous casting of metals, i.e. casting in indefinite lengths of specific alloys
    • B22D11/003Aluminium alloys
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22DCASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D11/00Continuous casting of metals, i.e. casting in indefinite lengths
    • B22D11/10Supplying or treating molten metal
    • B22D11/11Treating the molten metal
    • B22D11/112Treating the molten metal by accelerated cooling
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium
    • C22C21/10Alloys based on aluminium with zinc as the next major constituent

Abstract

The invention belongs to the preparation fields of metal material, and in particular to a kind of preparation method of the twin dendrite of Al-40%Zn alloy.The preparation method selects the ingredient design of high Zn content Al-Zn alloy (40%Zn), using directional solidification technique, high directional solidification withdrawing rate (900 ~ 1100 μm/s) are chosen, intracorporal convection current is melted using being formed in directional solidification process, is successfully prepared the twin dendrite of Al-40%Zn alloy.The present invention choose Al-40%Zn alloy be used as the alloy system for prepare twin dendrite, be different from study report in low content Zn(30%Zn or less) Al-Zn alloy system, this is not reported at component selections, overcomes technology prejudice.

Description

A kind of preparation method of the twin dendrite of Al-40%Zn alloy
Technical field
The invention belongs to the preparation fields of metal material, and in particular to a kind of preparation side of the twin dendrite of Al-40%Zn alloy Method.
Background technique
Twin dendrite, also known as Feather-like Crystal (Feathery grains), also referred to as twin crystal, twin, basaltiform are brilliant Deng belonging to one kind (Growth twin) of twin.Be originally found in semi-continuous casting aluminium alloy, be totally different from it is common A kind of abnormal grain of column crystal and dendrite, referred to as the third class dendrite in casting.It is twin why it is referred to as featheriness Dendrite is that its pattern is similar to feather in two-dimentional microstructure due to this kind of dendrite.Research shows that twin dendrite is certain Under the conditions of a kind of obtained cast sturcture, the speed of maximum growth axially carries out, has with axial parallel twin dendrite There is strongest competitiveness, so the dendrite in other directions is easy to be suppressed.Thus, the direction of growth is substantially parallel with axial direction, It with strong anisotropy, and is not susceptible to deform in pressing process and be crushed, so its microcosmic group to alloy It knits and plays the role of optimization with mechanical property.Zhou Yao and et al. it is brilliant to single Shu Yuzhuan crystalline substance and multi beam pinniform in last century the eighties Mechanical property did the work of more system, and analyze influence of the pinniform crystal layer piece spacing to mechanical property, they have found The reticular structure that multi beam pinniform crystalline substance is formed when intersecting strengthens the continuity of sample in the stretching direction, so that mechanical property It significantly improves.Therefore in alloy casting process obtain the twin dendrite of large area become improve alloy property key, to it Research has important value in solidification theory research and industrial application.
And found in the research of the Forming Mechanism in twin dendrite, since twin dendrite is the temperature in crystallization front liquid It is generated in the case that degree gradient is very precipitous, to cross cold belt extremely narrow.Therefore, when the overtemperature of melt is very high, ingot casting Cooling velocity is exceedingly fast, hot-fluid from crystallization be diffused towards single direction and melt in effective active particle it is few when, it is twin Raw dendrite is easy to generate.Based on this, it is that twin dendrite generates that generally high temperature gradient and strong convection are thought in research at present Necessary condition.Since Al has weak anisotropy such as in Al-Zn alloy, coarse boundary is easily formed during conventional coagulation Face is unfavorable for the formation of twin dendrite there is no strong growth competitiveness, but passes through the study found that under certain specific condition, In high-temperature gradient and strong convection environment, certain twin dendrite can also be formed.Directional solidification technique is as special Nonequilibrium freezing technology, temperature gradient, cooling rate and convection environment with higher in process of setting are Al-Zn alloy The formation of twin dendrite provides preparation condition.However, current study show that in Al-Zn alloy when Zn content reaches 40%, it is twin Raw dendrite does not re-form, this becomes the bottleneck of the twin dendrite preparation process of Al-Zn alloy.It therefore, can be in high Zn content Al-Zn Twin dendrite is prepared in alloy becomes the research emphasis of material preparation.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of twin dendrite of Al-40%Zn alloy.
To achieve the above object, the technical solution adopted by the present invention is as follows:
A kind of preparation method of the twin dendrite of Al-40%Zn alloy, the preparation method use a device for directionally solidifying, this is fixed It include pumping rod, heating and thermal insulation furnace and induction coil, inverted trapezoidal graphite cannula, cylinder among its inner cavity to coagulation system Crucible, "convex" shaped connecting tube, collet, the small end of connecting tube is adapted with crucible, big end is adapted with pumping rod, and heating is protected The side wall of warm furnace and its inner cavity are respectively communicated with equipped with Ar tracheae and vacuum tube, and Ar tracheae is connected with Ar gas tank, and vacuum tube successively connects It is connected to molecular pump, mechanical pump, the bottom of heating and thermal insulation furnace is sealedly connected with crystallizer with it, and Ga-In-Sn conjunction is filled in crystallizer Golden liquid, crystallizer top is located among heating and thermal insulation furnace chamber, remainder is then located at heating and thermal insulation furnace exterior, and collet is located at On crystallizer, graphite cannula is located on collet, and induction coil is adding around graphite cannula surrounding, induction coil is located at setting Induction power supply except hot holding furnace is connected, and crucible is located among graphite cannula, the small end that crucible and pumping rod pass through connecting tube Be plugged in the lower end of the crucible, big end cap pumping rod upper end realize connection, pumping rod from top to bottom successively sealing through collet, Crystallizer, pumping rod bottom are connected with drawing device;
Preparation step is as follows:
(1), cylinder Al-40%Zn alloy sample compatible with crucible shape is prepared;
(2), sand paper polishing, acetone cleaning sample, to remove the oxide layer and impurity on surface;Sample is put into crucible, Move down pumping rod by drawing device until the small end of connecting tube bottom is just concordant with the top of collet, big end then It stretches out collet and immerses in the Ga-In-Sn aluminium alloy in crystallizer;
(3), it is vacuumized respectively using mechanical pump and molecular pump, until the vacuum degree of heating and thermal insulation furnace is to 7 × 10-3Pa with On, it is then filled with Ar gas into heating and thermal insulation furnace and forms protective gas environment, fills the vacuum degree after Ar gas in heating and thermal insulation furnace and protects It holds in 350 ~ 400 Pa;
(4), induction power supply is opened, is heated by induction coil, is heated to above 80 ~ 150 DEG C of sample fusing point, locates at this time Sample in induction coil effective heating area melts, and the sample except induction coil effective heating area does not melt Change, keep the temperature (30 ~ 60min), keeps melt temperature uniform, stable;
(5), the drawing velocity for adjusting pumping rod is 900 ~ 1100 μm/s, starts pull and is oriented solidification experiments, will melt Body draws in Ga-In-Sn aluminium alloy from top to bottom and realizes directional solidification;
(6), after melt directional solidification, then adjusting the drawing velocity of pumping rod is 90 ~ 110 mm/s, and entire sample is complete It draws in Ga-In-Sn aluminium alloy and is quenched entirely, simultaneously close off heating and thermal insulation furnace, open fire door, the furnace in holding furnace to be heated After temperature naturally cools to room temperature, pumping rod is moved up by drawing device, entire sample is ejected into Ga-In-Sn alloy completely Liquid takes out to get the twin dendrite of Al-40%Zn alloy.
Preferably, the drawing velocity for adjusting pumping rod is preferably 1000 μm/s
Preferably, the preferably high-purity (99.9%Al of the crucible2O3) aluminium oxide alundum tube.
The utility model has the advantages that
1, the present invention chooses Al-40%Zn alloy as the alloy system for preparing twin dendrite, contains different from low in research report Measure Zn(30%Zn or less) Al-Zn alloy system, this is not reported at component selections.And existing research before making the present invention (in Yang Luyan, Li Shuanming, Gao Ka, Zhong Hong, Fu Heng will aluminium alloy progress [J] the Rare Metals Materials of twin dendrite with Engineering, 2015,44 (07): 001809-1814) think that Al-Zn alloy can not be prepared twin when Zn content is greater than 40% The alloying component of raw dendrite, therefore the present invention overcomes technology prejudice;
2, the ingredient design that high Zn content Al-Zn alloy (40%Zn) is selected in the present invention, uses directional solidification technique, High directional solidification withdrawing rate (900 ~ 1100 μm/s) are chosen, melt intracorporal convection current using being formed in directional solidification process, at Function is prepared for the twin dendrite of high Zn content Al-Zn alloy, provides test basis for the extensive preparation of the twin dendrite of Al-Zn alloy. In addition, Hirschfeld-Klinger reaction only occurs for twin dendrite obtained, organization internal by the method for the invention, precipitated phase is simple, and entire behaviour It is simple to make process, experimental expenses is lower.
Detailed description of the invention
Fig. 1: oriented coagulation forming device: 1- heating and thermal insulation furnace, 2- induction coil, 3- graphite cannula, 4- crucible, 5- connection Pipe, 6- collet, 7-Ar tracheae, 8- vacuum tube, 9- crystallizer, 10-Ga-In-Sn aluminium alloy, 11- pumping rod, 12- sample.
Fig. 2: the longitudinal section analysis of the twin dendrite of Al-40%Zn alloy made from embodiment 1 :(a) micro-organization chart;(b) it is (a) solid-line rectangle frame region enlarged drawing in;(c) the EBSD pole figure tested for dashed rectangle frame region in (b).
Fig. 3: the longitudinal section analysis of Al-40%Zn alloy plain cylindrical crystalline substance made from reference examples 1 :(a) micro-organization chart;(b) The EBSD pole figure tested for dashed rectangle frame region in (a).
Fig. 4: the longitudinal section analysis of Al-40%Zn alloy plain cylindrical crystalline substance made from reference examples 2 :(a) micro-organization chart;(b) For solid-line rectangle frame region enlarged drawing in (a);(c) the EBSD pole figure tested for dashed rectangle frame region in (b).
Specific embodiment
The present invention is further elaborated combined with specific embodiments below, and used raw material is in following embodiment This field general chemical.
Embodiment 1
A kind of preparation method of the twin dendrite of Al-40%Zn alloy, the preparation method use a device for directionally solidifying, such as Fig. 1 Shown, which includes pumping rod 11, heating and thermal insulation furnace 1 and the induction coil 2 among its inner cavity, inverted trapezoidal Graphite cannula 3, the high-purity (99.9%Al of cylinder crucible 4(2O3) aluminium oxide alundum tube), "convex" shaped connecting tube 5, collet 6, connection The small end of pipe 5 is adapted with crucible 4, big end is adapted with pumping rod 11, and the side wall of heating and thermal insulation furnace 1 is respectively communicated with its inner cavity Equipped with Ar tracheae 7 and vacuum tube 8, Ar tracheae 7 is connected with Ar gas tank, and vacuum tube 8 is connected with molecular pump, mechanical pump in turn, heating The bottom of holding furnace 1 is sealedly connected with crystallizer 9 with it, and Ga-In-Sn aluminium alloy 10,9 top of crystallizer are filled in crystallizer 9 Among 1 inner cavity of heating and thermal insulation furnace, remainder be then located at outside heating and thermal insulation furnace 1, collet 6 is located on crystallizer 9, Graphite cannula 3 is located on collet 6, and induction coil 2 is around 3 surrounding of graphite cannula is located at, and induction coil 2 and setting are in heating and thermal insulation Induction power supply except furnace 1 is connected, and crucible 4 is located among graphite cannula 3, the small end that crucible 4 and pumping rod 11 pass through connecting tube 5 Be plugged in 4 lower end of crucible, big end cap pumping rod 11 upper end realize connection, pumping rod 11 from top to bottom successively sealing through every Hot jacket 6, crystallizer 9,11 bottom of pumping rod are connected with drawing device;
Preparation step is as follows:
(1), high-purity (99.99%) Al and Zn metal is weighed by 60: 40 mass ratio, is melted by high-frequency induction heating and matches, cuts It is cut into cylinder Al-40%Zn alloy sample 12 compatible with 4 shape of crucible;
(2), sand paper polishing, acetone cleaning sample 12, to remove the oxide layer and impurity on surface;Sample 12 is put into crucible In 4, top flat of the pumping rod 11 up to the bottom of the small end of connecting tube 5 just with collet 6 is moved down by drawing device Together, big end then stretches out collet 6 and immerses the (mass percentage composition: Ga 10%, In of the Ga-In-Sn aluminium alloy in crystallizer 9 45%, Sn 45%) in 10;
(3), it is vacuumized respectively using mechanical pump and molecular pump, until the vacuum degree of heating and thermal insulation furnace 1 is to 7 × 10-3Pa, Then it is filled with Ar gas into heating and thermal insulation furnace 1 and forms protective gas environment, fills the vacuum degree after Ar gas in heating and thermal insulation furnace 1 and keeps In 400 Pa;
(4), induction power supply is opened, is heated by induction coil 2, is heated to above 80 DEG C of 12 fusing point of sample, is now in The sample 12 of 2 effective heating area of induction coil melts, and the sample 12 except 2 effective heating area of induction coil is not sent out Raw fusing, keeps the temperature 30min, keeps melt temperature uniform, stable;
(5), the drawing velocity for adjusting pumping rod 11 is 1000 μm/s, starts pull and is oriented solidification experiments, by melt It is drawn in Ga-In-Sn aluminium alloy 10 from top to bottom and realizes directional solidification;
(6), after melt directional solidification, then adjusting the drawing velocity of pumping rod 11 is 100mm/s, and entire sample 12 is complete It draws in Ga-In-Sn aluminium alloy 10 and is quenched entirely, simultaneously close off heating and thermal insulation furnace 1, open fire door, in holding furnace 1 to be heated Furnace temperature naturally cool to room temperature after, pumping rod 11 is moved up by drawing device, by the ejection Ga- completely of entire sample 12 In-Sn aluminium alloy 10 takes out to get the twin dendrite of Al-40%Zn alloy.
Fig. 2 is the longitudinal section analysis of the twin dendrite of Al-40%Zn alloy :(a) micro-organization chart;It (b) is solid line square in (a) Shape frame region enlarged drawing;(c) the EBSD pole figure tested for dashed rectangle frame region in (b).Fig. 2 (a) is it can be seen that in sample Portion forms flourishing Feather-like Crystal tissue, and twin dendritic growth consistency is obvious.In Fig. 2 (b), a dendrite of twin dendrite Do now apparent symmetrical interface, as shown by the solid line, dendrite two sides about this Twin Interface symmetric growth, secondary dendrite with it is twin About 60 ° of angles are presented in interface.In addition, dendrite has apparent crystal boundary in Fig. 2 (b).It is analyzed by further EBSD, such as Fig. 2 (c) shown in, it may be determined that gained arborescent structure is twin dendrite, and twin plane is (111) face, the dry main shaft of dendrite of dendrite and secondary The dendritic arm direction of growth is<110>direction, the increase meeting of this and Zn constituent content in Gonzales and Rappaz discovery aluminium alloy Change the anisotropy of solid liquid interface energy, so that the direction of growth of conventional dendrite becomes<110>from<100>, is conducive to<110>side To the formation of twin dendrite, this conclusion is consistent.
Reference examples 1
The difference from embodiment 1 is that: inverted trapezoidal graphite cannula is saved in device for directionally solidifying, and in preparation step (5), The drawing velocity for adjusting pumping rod 11 is 800 μm/s, other with embodiment 1.
The longitudinal section analysis of product made from the reference examples is as shown in Figure 3 :(a) micro-organization chart;It (b) is dotted line in (a) The EBSD pole figure that rectangle frame region is tested.Fig. 3 (a) is it can be seen that sample inside and not formed Feather-like Crystal tissue, Al-40% Zn alloy microstructure is conventional plain cylindrical crystalline substance tissue, and dendrite is dry and a dendrite does not have the feature of the twin dendrite of featheriness. And it, cannot due to there is no the drawing velocity (lower than the drawing velocity in the present invention) using inverted trapezoidal graphite cannula and 800 μm/s Generate strong convection environment inside melt, column crystal each along solidification direction of heat flow perpendicular to quenching interface growth, without Fig. 2 The twin dendrite of middle lateral growth occurs, and the secondary dendrite of plain cylindrical crystalline substance and dendrite are done and 60 ° of angles is not presented, such as Fig. 3 (a) It is shown.It is analyzed by further EBSD, as shown in Fig. 3 (b), it may be determined that gained arborescent structure is common dendrite, not twin Interface occurs, and it is not<110>direction that the dry main shaft direction of growth of dendrite of dendrite, which is<100>direction,.It can illustrate institute in Fig. 3 It is shown as conventional common dendrite, is not twin dendrite.
Reference examples 2
The difference from embodiment 1 is that: inverted trapezoidal graphite cannula is saved in device for directionally solidifying, and in preparation step (5), The drawing velocity for adjusting pumping rod 11 is 1500 μm/s, other with embodiment 1.
The longitudinal section analysis of product made from the reference examples is as shown in Figure 4 :(a) micro-organization chart;It (b) is solid line in (a) Rectangle frame regional enlarged drawing;(c) the EBSD pole figure tested for dashed rectangle frame region in (b).In this reference examples experimentation It does not use inverted trapezoidal graphite cannula, and uses the pull degree of hastening of 1500 μm/s (higher than the drawing velocity in the present invention).Fig. 4 (a) it can be seen that sample interior tissue is Al-Zn alloy routine plain cylindrical crystalline substance tissue, dendrite is dry and a dendrite does not have plumage The shape characteristic of hairy twin dendrite, column crystal each along solidification direction of heat flow perpendicular to quenching interface growth, the two of column crystal Secondary dendrite and the dry angle of dendrite are not 60 °, as shown in Figure 4 (b).EBSD analysis the result shows that: the dry main shaft of dendrite of dendrite is raw Length direction is<100>direction, is not<110>direction, is occurred without Twin Interface, as shown in Fig. 4 (c), it may be determined that this reference examples Resulting arborescent structure is common dendrite.
From it was found from embodiment 1 and reference examples 1-2: only using drawing velocity and preparation method in the present invention that could make The standby twin dendrite of Al-40%Zn alloy out.Described herein to be: inventor is finally determined of the invention by creative work Technical solution, the present invention also only enumerate the representational reference examples of two of them and are explained, but are not exhaustions.

Claims (3)

1. a kind of preparation method of the twin dendrite of Al-40%Zn alloy, it is characterised in that: the preparation method uses a directional solidification Device, the device for directionally solidifying include pumping rod, heating and thermal insulation furnace and induction coil, inverted trapezoidal graphite among its inner cavity Set, cylindrical crucible, "convex" shaped connecting tube, collet, the small end of connecting tube is adapted with crucible, big end and pumping rod are mutually fitted Match, the side wall of heating and thermal insulation furnace is respectively equipped with Ar tracheae and vacuum tube and is connected to the inner cavity of heating and thermal insulation furnace, and Ar tracheae is connected with Ar gas tank, vacuum tube are connected with molecular pump, mechanical pump in turn, and the bottom of heating and thermal insulation furnace is sealedly connected with crystallizer with it, knot Ga-In-Sn aluminium alloy is filled in brilliant device, crystallizer top is located among heating and thermal insulation furnace chamber, remainder is then located at heating Outside holding furnace, collet is located on crystallizer, and graphite cannula is located on collet, and induction coil surrounds and is located at graphite cannula four Week, induction coil are connected with the induction power supply being arranged in except heating and thermal insulation furnace, and crucible is located among graphite cannula, crucible and pumping Pull rod by the small end of connecting tube be plugged in the lower end of the crucible, big end cap pumping rod upper end realize connection, pumping rod from up to Under successively sealing run through collet, crystallizer, pumping rod bottom is connected with drawing device;
Preparation step is as follows:
(1), cylinder Al-40%Zn alloy sample compatible with crucible shape is prepared;
(2), sand paper polishing, acetone cleaning sample;Sample is put into crucible, by drawing device move down pumping rod until The bottom of the small end of connecting tube is just concordant with the top of collet, big end then stretches out collet and immerses the Ga- in crystallizer In In-Sn aluminium alloy;
(3), it is vacuumized respectively using mechanical pump and molecular pump, until the vacuum degree of heating and thermal insulation furnace is to 7 × 10-3Pa or more, so It is filled with Ar gas in backward heating and thermal insulation furnace, the vacuum degree after Ar gas in heating and thermal insulation furnace is filled and is maintained at 350 ~ 400 Pa;
(4), induction power supply is opened, is heated by induction coil, is heated to above 80 ~ 150 DEG C of sample fusing point, is now in sense The sample of coil effective heating area is answered to melt, and the sample except induction coil effective heating area does not melt, Heat preservation keeps melt temperature uniform, stable;
(5), the drawing velocity for adjusting pumping rod is 900 ~ 1100 μm/s, and melt is drawn in Ga-In-Sn aluminium alloy from top to bottom Middle realization directional solidification;
(6), after melt directional solidification, then adjusting the drawing velocity of pumping rod is 90 ~ 110 mm/s, and entire sample is drawn completely Into being quenched in Ga-In-Sn aluminium alloy, simultaneously closes off heating and thermal insulation furnace, opens fire door, the furnace temperature in holding furnace to be heated is certainly After being so cooled to room temperature, pumping rod is moved up by drawing device, entire sample is ejected into Ga-In-Sn aluminium alloy completely, is taken Out to get the twin dendrite of Al-40%Zn alloy.
2. preparation method as described in claim 1, it is characterised in that: in step (5), the drawing velocity for adjusting pumping rod is 1000 μm/s。
3. preparation method as claimed in claim 1 or 2, it is characterised in that: the crucible is high purity aluminium oxide alundum tube.
CN201710281993.8A 2017-04-26 2017-04-26 A kind of preparation method of the twin dendrite of Al-40%Zn alloy Expired - Fee Related CN107052282B (en)

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