CN107052282A - A kind of preparation method of the twin dendrite of Al 40%Zn alloys - Google Patents

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

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Publication number
CN107052282A
CN107052282A CN201710281993.8A CN201710281993A CN107052282A CN 107052282 A CN107052282 A CN 107052282A CN 201710281993 A CN201710281993 A CN 201710281993A CN 107052282 A CN107052282 A CN 107052282A
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dendrite
heating
pumping rod
thermal insulation
alloys
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CN107052282B (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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    • 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

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention belongs to the preparation field of metal material, and in particular to a kind of preparation method of the twin dendrite of Al 40%Zn alloys.The preparation method selects high Zn content Al Zn alloys(40%Zn)Composition design, using directional solidification technique, choose high directional solidification withdrawing rate(900~1100μm/s), using the convection current formed in directional solidification process in melt, it is successfully prepared the twin dendrite of Al 40%Zn alloys.The present invention chooses Al 40%Zn alloys as the alloy system for preparing twin dendrite, different from low content Zn in research report(Below 30%Zn)Al Zn alloy systems, this is not reported into component selections, overcomes technology prejudice.

Description

A kind of preparation method of the twin dendrite of Al-40%Zn alloys
Technical field
The invention belongs to the preparation field of metal material, and in particular to a kind of preparation side of the twin dendrite of Al-40%Zn alloys Method.
Background technology
Twin dendrite, also known as Feather-like Crystal(Feathery grains), also referred to as twin crystal, twin, basaltiform be brilliant Deng belonging to one kind of twin(Growth 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, is referred to as the 3rd class dendrite in casting.It is twin why it is referred to as featheriness Dendrite, is due to that this kind of dendrite its pattern in two-dimentional microstructure is similar to feather.Research shows that twin dendrite is certain Under the conditions of a kind of obtained cast sturcture, the speed of its maximum growth axially carries out, has with axially in parallel twin dendrite There is most strong competitiveness, so the dendrite in other directions is easy to be suppressed.Thus, its direction of growth substantially with it is axially in parallel, With strong anisotropy, and it is not susceptible to deform in pressing process and crushes, so its microcosmic group to alloy Knit and play a part of optimization with mechanical property.Zhou Yao and et al. it is brilliant to single Shu Yuzhuan brilliant with 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 network structure that multi beam pinniform crystalline substance is formed when intersecting strengthens the continuity of sample in the stretching direction so that mechanical property Significantly improve.Therefore large area twin dendrite being obtained in alloy casting process and turning into improves the key of alloy property, to it Research has important value in solidification theory research and commercial Application.
And found in the research of the Forming Mechanism in twin dendrite, because twin dendrite is the temperature in crystallization front liquid 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 produce.Based on this, the thermograde for thinking high and strong convection are generally studied at present, are that twin dendrite is produced Necessary condition.Because Al has weak anisotropy such as in Al-Zn alloys, coarse boundary is easily formed during conventional coagulation Face, in the absence of strong growth competitiveness, is unfavorable for the formation of twin dendrite, but is found by studying, under certain specific condition, As in high-temperature gradient and strong convection environment, certain twin dendrite can also be formed.Directional solidification technique is as special There is higher thermograde, cooldown rate and convection environment in nonequilibrium freezing technology, its process of setting, be Al-Zn alloys The formation of twin dendrite provides preparation condition.However, current study show that in Al-Zn alloys when Zn contents reach 40%, it is twin Raw dendrite is not re-formed, and this turns into the bottleneck of the twin dendrite preparation process of Al-Zn alloys.Accordingly, it is capable to no in high Zn content Al-Zn Twin dendrite is prepared in alloy turns into research emphasis prepared by material.
The content of the invention
It is an object of the invention to provide a kind of preparation method of the twin dendrite of Al-40%Zn alloys.
To achieve the above object, the technical scheme that the present invention takes is as follows:
A kind of preparation method of the twin dendrite of Al-40%Zn alloys, the preparation method uses a device for directionally solidifying, and the orientation is coagulated It is fixedly mounted with induction coil, inverted trapezoidal graphite cannula, the cylindrical earthenware put including pumping rod, heating and thermal insulation stove and among its inner chamber Crucible, "convex" shaped connecting tube, collet, the small end of connecting tube is adapted with crucible, end greatly is adapted with pumping rod, heating and thermal insulation The side wall of stove is respectively communicated with provided with Ar tracheaes and vacuum tube with its inner chamber, and Ar tracheaes are connected with Ar gas tanks, and vacuum tube is sequentially connected There are molecular pump, mechanical pump, the bottom of heating and thermal insulation stove, which is sealed against, is connected with crystallizer, and Ga-In-Sn alloys are filled with crystallizer Liquid, crystallizer top is among heating and thermal insulation furnace chamber, remainder is then located at outside heating and thermal insulation stove, and collet is located at knot On brilliant device, graphite cannula is located on collet, and induction coil is around graphite cannula surrounding is located at, and induction coil is with being arranged on heating Induction power supply outside holding furnace is connected, and crucible is located among graphite cannula, and crucible and pumping rod are inserted by the small end of connecting tube The upper end realization connection that crucible lower end, big end are enclosed on pumping rod is located at, pumping rod is sealed through collet, knot successively from top to bottom Brilliant device, pumping rod bottom is connected with drawing device;
Preparation process is as follows:
(1), prepare the cylindrical Al-40%Zn alloy samples that are adapted with crucible shape;
(2), sand paper polishing, acetone cleaning sample, to remove the oxide layer and impurity on surface;Sample is put into crucible, passed through Drawing device moves down pumping rod until the bottom of the small end of connecting tube is just concordant with the top of collet, hold then stretch out greatly Collet is simultaneously immersed in the Ga-In-Sn aluminium alloys in crystallizer;
(3), respectively vacuumized using mechanical pump and molecular pump, until the vacuum of heating and thermal insulation stove is to 7 × 10-3 More than Pa, so Ar gas formation protective gas environment is filled with backward heating and thermal insulation stove, the vacuum after Ar gas in heating and thermal insulation stove is filled and is maintained at 350~400 Pa;
(4), open induction power supply, heated by induction coil, be heated to above 80 ~ 150 DEG C of sample fusing point, be now in sense The sample of coil effective heating area is answered to melt, and the sample outside induction coil effective heating area does not melt, Insulation(30 ~60min), make melt temperature uniformly, stably;
(5), adjustment pumping rod drawing velocity be 900 ~ 1100 μm/s, start pull be oriented solidification experiments, by melt from Drawn under above in Ga-In-Sn aluminium alloys and realize directional solidification;
(6), after after melt directional solidification, then it is 90 ~ 110 mm/s to adjust the drawing velocity of pumping rod, and whole sample is drawn completely Enter and quenched in Ga-In-Sn aluminium alloys, simultaneously close off heating and thermal insulation stove, open fire door, the furnace temperature in holding furnace to be heated from So it is cooled to after room temperature, pumping rod is moved up by drawing device, whole sample is ejected into Ga-In-Sn aluminium alloys completely, taken Go out, produce the twin dendrite of Al-40%Zn alloys.
Preferably, the drawing velocity of adjustment pumping rod is preferably 1000 μm/s
Preferably, the crucible is preferably high-purity(99.9%Al2O3)Aluminum oxide alundum tube.
Beneficial effect:
1st, the present invention chooses Al-40%Zn alloys as the alloy system for preparing twin dendrite, different from low content Zn in research report (Below 30%Zn)Al-Zn alloy systems, this is not reported into component selections.And existing research before making the present invention(Yang Lu Progress [J] the Rare Metals Materials and engineering of twin dendrite in rock, Li Shuanming, Gao Ka, Zhong Hong, Fu Heng will aluminium alloys, 2015, 44(07): 001809-1814)Think that Al-Zn alloys can not possibly prepare twin dendrite when Zn contents are more than 40% Alloying component, therefore instant invention overcomes technology prejudice;
2nd, high Zn content Al-Zn alloys are selected in the present invention(40%Zn)Composition design, employ directional solidification technique, choose High directional solidification withdrawing rate(900~1100μm/s), using the convection current formed in directional solidification process in melt, successfully make For the twin dendrite of high Zn content Al-Zn alloys, the extensive preparation for the twin dendrite of Al-Zn alloys provides test basis.In addition, By twin dendrite made from the inventive method, Hirschfeld-Klinger reaction only occurs for organization internal, and precipitated phase is simple, and whole operation process Simply, experimental expenses is relatively low.
Brief description of the drawings
Fig. 1:Oriented coagulation forming device:1- heating and thermal insulation stoves, 2- induction coils, 3- graphite cannulas, 4- crucibles, 5- connections Pipe, 6- collets, 7-Ar tracheaes, 8- vacuum tubes, 9- crystallizers, 10-Ga-In-Sn aluminium alloys, 11- pumping rods, 12- samples.
Fig. 2:The longitudinal section analysis of the twin dendrite of Al-40%Zn alloys made from embodiment 1:(a)Micro-organization chart;(b)For (a)Middle solid-line rectangle frame regional enlarged drawing;(c)For(b)The EBSD pole figures that middle dotted rectangle region is tested.
Fig. 3:The brilliant longitudinal section analysis of Al-40%Zn alloys plain cylindrical made from reference examples 1:(a)Micro-organization chart;(b) For(a)The EBSD pole figures that middle dotted rectangle region is tested.
Fig. 4:The brilliant longitudinal section analysis of Al-40%Zn alloys plain cylindrical made from reference examples 2:(a)Micro-organization chart;(b) For(a)Middle solid-line rectangle frame regional enlarged drawing;(c)For(b)The EBSD pole figures that middle dotted rectangle region is tested.
Embodiment
With reference to specific embodiment, the present invention is further elaborated, and used raw material is in following examples This area general chemical.
Embodiment 1
A kind of preparation method of the twin dendrite of Al-40%Zn alloys, the preparation method uses a device for directionally solidifying, such as Fig. 1 institutes Show, the device for directionally solidifying includes pumping rod 11, heating and thermal insulation stove 1 and induction coil 2, inverted trapezoidal stone among its inner chamber Ink set 3, cylindrical crucible 4(It is high-purity(99.9%Al2O3)Aluminum oxide alundum tube), "convex" shaped connecting tube 5, collet 6, connecting tube 5 small end is adapted with crucible 4, end greatly is adapted with pumping rod 11, and the side wall of heating and thermal insulation stove 1 is respectively communicated with its inner chamber to be set There are Ar tracheaes 7 and vacuum tube 8, Ar tracheaes 7 are connected with Ar gas tanks, and vacuum tube 8 is connected with molecular pump, mechanical pump in turn, and heating is protected The bottom of warm stove 1, which is sealed against, is connected with crystallizer 9, and Ga-In-Sn aluminium alloys 10, the upper bit of crystallizer 9 are filled with crystallizer 9 Among the inner chamber of heating and thermal insulation stove 1, remainder then be located at heating and thermal insulation stove 1 outside, collet 6 be located at crystallizer 9 on, stone Ink set 3 is located on collet 6, and induction coil 2 is around the surrounding of graphite cannula 3 is located at, and induction coil 2 is with being arranged on heating and thermal insulation stove Induction power supply outside 1 is connected, and crucible 4 is located among graphite cannula 3, and crucible 4 and pumping rod 11 are inserted by the small end of connecting tube 5 The upper end realization connection that the lower end of crucible 4, big end are enclosed on pumping rod 11 is located at, pumping rod 11 is sealed through heat-insulated successively from top to bottom Set 6, crystallizer 9, the bottom of pumping rod 11 is connected with drawing device;
Preparation process is as follows:
(1), by 60: 40 mass ratio weigh high-purity (99.99%) Al and Zn metals, match somebody with somebody, cut into by the way that high-frequency induction heating is molten The cylindrical Al-40%Zn alloy samples 12 being adapted with the shape of crucible 4;
(2), sand paper polishing, acetone cleaning sample 12, to remove the oxide layer and impurity on surface;Sample 12 is put into crucible 4, Pumping rod 11 is moved down by drawing device until the bottom of the small end of connecting tube 5 is just concordant with the top of collet 6, big Collet 6 and the Ga-In-Sn aluminium alloys immersed in crystallizer 9 are then stretched out in end(Mass percent is constituted:Ga 10%、In 45%、 Sn 45%)In 10;
(3), respectively vacuumized using mechanical pump and molecular pump, until the vacuum of heating and thermal insulation stove 1 is to 7 × 10-3 Pa, then Ar gas formation protective gas environment is filled with into heating and thermal insulation stove 1, the vacuum after Ar gas in heating and thermal insulation stove 1 is filled and is maintained at 400 Pa;
(4), open induction power supply, heated by induction coil 2, be heated to above 80 DEG C of 12 fusing point of sample, be now in sensing The sample 12 of the effective heating area of coil 2 melts, and the sample 12 outside the effective heating area of induction coil 2 does not melt Change, be incubated 30min, make melt temperature uniformly, stably;
(5), adjustment pumping rod 11 drawing velocity be 1000 μm/s, start pull and be oriented solidification experiments, by melt from upper And under draw in Ga-In-Sn aluminium alloys 10 and realize directional solidification;
(6), after after melt directional solidification, then it is 100mm/s to adjust the drawing velocity of pumping rod 11, and whole sample 12 is drawn completely Enter and quenched in Ga-In-Sn aluminium alloys 10, simultaneously close off heating and thermal insulation stove 1, the stove opened in fire door, holding furnace 1 to be heated Temperature is naturally cooled to after room temperature, and pumping rod 11 is moved up by drawing device, by whole sample 12 ejection Ga-In-Sn completely Aluminium alloy 10, takes out, produces the twin dendrite of Al-40%Zn alloys.
Fig. 2 is the longitudinal section analysis of the twin dendrite of Al-40%Zn alloys:(a)Micro-organization chart;(b)For(a)Middle solid line square Shape frame regional enlarged drawing;(c)For(b)The EBSD pole figures that middle dotted rectangle region is tested.Fig. 2(a)It can be seen that:In sample Portion forms the Feather-like Crystal tissue of prosperity, and twin dendritic growth uniformity is obvious.In Fig. 2 (b), a dendrite of twin dendrite Do now obvious symmetrical interface, as shown by the solid line, dendrite both sides on this Twin Interface symmetric growth, secondary dendrite with it is twin About 60 ° of angles are presented in interface.In addition, dendrite has obvious crystal boundary in Fig. 2 (b).Analyzed by further EBSD, such as Fig. 2 (c) shown in, it may be determined that gained arborescent structure is twin dendrite, twin plane is(111)Face, dry main shaft of dendrite of dendrite and secondary The dendritic arm direction of growth is<110>Direction, this finds the increase meeting of Zn constituent contents in aluminium alloy with Gonzales and Rappaz Change solid liquid interface can anisotropy so that the direction of growth of conventional dendrite by<100>It is changed into<110>, be conducive to<110>Side To the formation of twin dendrite, this conclusion is consistent.
Reference examples 1
Difference with embodiment 1 is:Inverted trapezoidal graphite cannula, and preparation process are saved in device for directionally solidifying(5)In, adjustment The drawing velocity of pumping rod 11 is 800 μm/s, other equal be the same as Examples 1.
The longitudinal section analysis of product made from the reference examples is as shown in Figure 3:(a)Micro-organization chart;(b)For(a)Middle dotted line The EBSD pole figures that rectangle frame region is tested.Fig. 3(a)It can be seen that:Feather-like Crystal tissue, Al-40% are not formed inside sample Zn alloys 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 due to the drawing velocity without use inverted trapezoidal graphite cannula and 800 μm/s(Less than the drawing velocity in the present invention), it is impossible to Convection environment strong inside melt is produced, column crystal is each along direction of heat flow is solidified perpendicular to quenching interface growth, without Fig. 2 The twin dendrite of middle lateral growth occurs, and the brilliant secondary dendrite of plain cylindrical is done with dendrite and 60 ° of angles, such as Fig. 3 are not presented(a) It is shown.Analyzed by further EBSD, shown in such as Fig. 3 (b), it may be determined that gained arborescent structure is common dendrite, not twin Interface occurs, and the dry main shaft direction of growth of dendrite of dendrite is<100>Direction, be not<110>Direction.Institute in Fig. 3 can be illustrated Conventional common dendrite is shown as, is not twin dendrite.
Reference examples 2
Difference with embodiment 1 is:Inverted trapezoidal graphite cannula, and preparation process are saved in device for directionally solidifying(5)In, adjustment The drawing velocity of pumping rod 11 is 1500 μm/s, other equal be the same as Examples 1.
The longitudinal section analysis of product made from the reference examples is as shown in Figure 4:(a)Micro-organization chart;(b)For(a)Middle solid line Rectangle frame regional enlarged drawing;(c)For(b)The EBSD pole figures that middle dotted rectangle region is tested.In this reference examples experimentation Inverted trapezoidal graphite cannula is not used, and uses 1500 μm/s pull degree of hastening(Higher than the drawing velocity in the present invention).Fig. 4 (a)It can be seen that:Sample interior tissue is the conventional plain cylindrical crystalline substance tissue of Al-Zn alloys, and dendrite is dry and a dendrite does not have plumage The shape characteristic of the twin dendrite of hairy, column crystal is 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 °, such as Fig. 4(b)It is shown.EBSD analysis results show:The dry main shaft life of dendrite of dendrite Length direction is<100>Direction, be not<110>Direction, occurs without Twin Interface, shown in such as Fig. 4 (c), it may be determined that this reference examples The arborescent structure of gained is common dendrite.
It was found from embodiment 1 and reference examples 1-2:It could only be made using the drawing velocity and preparation scheme in the present invention It is standby go out the twin dendrite of Al-40%Zn alloys.It is described herein to be:Inventor finally determines the present invention's by creative work Technical scheme, the present invention also simply enumerates the representational reference examples of two of which and is explained, but is not exhaustive.

Claims (3)

1. a kind of preparation method of the twin dendrite of Al-40%Zn alloys, it is characterised in that:The preparation method uses a directional solidification Device, the device for directionally solidifying includes pumping rod, heating and thermal insulation stove and induction coil, inverted trapezoidal graphite among its inner chamber Set, cylindrical crucible, "convex" shaped connecting tube, collet, the small end of connecting tube are adapted with crucible, hold mutually fitted with pumping rod greatly Match somebody with somebody, side wall and its inner chamber of heating and thermal insulation stove are respectively communicated with provided with Ar tracheaes and vacuum tube, and Ar tracheaes are connected with Ar gas tanks, vacuum Pipe is connected with molecular pump, mechanical pump in turn, and the bottom of heating and thermal insulation stove, which is sealed against, is connected with crystallizer, is filled with crystallizer Ga-In-Sn aluminium alloys, crystallizer top is among heating and thermal insulation furnace chamber, remainder is then located at outside heating and thermal insulation stove, Collet is located on crystallizer, and graphite cannula is located on collet, and induction coil surrounds and is located at graphite cannula surrounding, induction coil It is connected with the induction power supply being arranged on outside heating and thermal insulation stove, crucible is located among graphite cannula, crucible and pumping rod pass through even The small end of adapter is plugged in the upper end realization connection that crucible lower end, big end are enclosed on pumping rod, and pumping rod is sealed successively from top to bottom Through collet, crystallizer, pumping rod bottom is connected with drawing device;
Preparation process is as follows:
(1), prepare the cylindrical Al-40%Zn alloy samples that are adapted with crucible shape;
(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, collet and the Ga- immersed in crystallizer are then stretched out in big end In In-Sn aluminium alloys;
(3), respectively vacuumized using mechanical pump and molecular pump, until the vacuum of heating and thermal insulation stove is to 7 × 10-3 More than Pa, so Ar gas is filled with backward heating and thermal insulation stove, the vacuum after Ar gas in heating and thermal insulation stove is filled and is maintained at 350 ~ 400 Pa;
(4), open induction power supply, heated by induction coil, be heated to above 80 ~ 150 DEG C of sample fusing point, be now in sense The sample of coil effective heating area is answered to melt, and the sample outside induction coil effective heating area does not melt, Insulation, makes melt temperature uniformly, stably;
(5), adjustment pumping rod drawing velocity be 900 ~ 1100 μm/s, melt is drawn in Ga-In-Sn aluminium alloys from top to bottom In realize directional solidification;
(6), after after melt directional solidification, then it is 90 ~ 110 mm/s to adjust the drawing velocity of pumping rod, and whole sample is drawn completely Enter and quenched in Ga-In-Sn aluminium alloys, simultaneously close off heating and thermal insulation stove, open fire door, the furnace temperature in holding furnace to be heated from So it is cooled to after room temperature, pumping rod is moved up by drawing device, whole sample is ejected into Ga-In-Sn aluminium alloys completely, taken Go out, produce the twin dendrite of Al-40%Zn alloys.
2. preparation method as claimed in claim 1, it is characterised in that: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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Publication number Priority date Publication date Assignee Title
CN111570515A (en) * 2020-05-20 2020-08-25 中国科学院上海应用物理研究所 Metal composite plate rolling process optimization method and design method

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