CN100509217C - Equipment for preparing monotectic alloy shell type composite tissue powder and use method thereof - Google Patents

Equipment for preparing monotectic alloy shell type composite tissue powder and use method thereof Download PDF

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CN100509217C
CN100509217C CNB2006100478216A CN200610047821A CN100509217C CN 100509217 C CN100509217 C CN 100509217C CN B2006100478216 A CNB2006100478216 A CN B2006100478216A CN 200610047821 A CN200610047821 A CN 200610047821A CN 100509217 C CN100509217 C CN 100509217C
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drop
liquid
trigger
crucible furnace
type composite
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CN101147974A (en
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赵九洲
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Institute of Metal Research of CAS
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Institute of Metal Research of CAS
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Abstract

The present invention relates to an equipment for preparing monotectic alloy powder with shell mold composite structure and its application. Said equipment includes from top to bottom arranged liquid-drop production device, liquid-drop charging device and cabin body. The liquid-drop production device includes crucible furnace, vibration exciter device capable of making the melt liquid flow flowed out from flow guide hole positioned in the bottom portion of said crucible furnace produce vibration and liquid-drop charging device. In the described cabin interior are set an infrared temperature-measuring instrument for measuring liquid-drop temperature, a nucleation trigger device and a nucleation trigger device position regulation mechanism. The nucleation trigger device and nucleation trigger device position regulation mechanism include trigger, trigger target material, slide block screw-rod for regulating trigger and target material position and motor. Said invention utilizes said liquid-drop production device to produce liquid-drop with uniform size, in the course of cooling liquid-drop uses the nucleation trigger device to make surface trigger nucleation, and impel that the supersaturation degree of liquid-drop surface in the course of liquid-liquid phase transition is smaller, the solute in the liquid-drop interior can be continuously migrated towards surface, so that the monotectic alloy powder with shell mold composite structure can be formed.

Description

Be used to prepare the equipment and the using method thereof of monotectic alloy shell type composite tissue powder
Technical field
The invention belongs to monotectic type alloy powder technology of preparing, specifically a kind of equipment and using method thereof that is used to prepare monotectic alloy shell type composite tissue powder.
Background technology
The signal phasor of monotectic type alloy as shown in Figure 1.Such alloy exists constituent element unmixing temperature range (L in liquid state 1+ L 2).When the alloy melt of homogeneous is cooled to L 1+ L 2In the time of in the district, liquid-liquid phase will take place and become (L → L in it 1+ L 2).Such alloy is very extensive, and wherein many have special mechanics and a physical property, have good application prospects industrial, so its research attracted more and more people's attention.In order deeply to be familiar with the coagulating property of such alloy, the material science worker has successively done a large amount of experimental study work, and has carried out theoretical modeling widely under ground and space microgravity condition both at home and abroad.Discover that when preparing the monotectic alloy powder with the gas atomization method, the shell mould that obtains having top layer and core through regular meeting is organized powder, shown in Fig. 2 a-b.This powder has an important purposes industrial.For example, alloy powder with low melting point top layer, high-strength highly-conductive electrical inner layer complex tissue is desirable electronics industry high-performance scolder, can guarantee to have good welding performance, can guarantee that again solder joint has the high-strength highly-conductive electrical characteristics, can improve the performance of integrated circuit significantly.
The formation mechanism of this shell mould tissue is listed in the mystery of science always.Recently, the applicant discovers that the formation of such tissue on the atomized drop surface heterogeneous forming core takes place by disperse phase (separating out liquid phase earlier) in the liquid-liquid phase change process and causes.So-called heterogeneous forming core just is meant that disperse phase depends on exogenous impurity or surperficial process of carrying out forming core, and it is corresponding with the homogeneous forming core, and the homogeneous forming core is meant the process of spontaneous nucleation in homogeneous free from admixture melt.Compare with the homogeneous forming core, heterogeneous forming core is easier to carry out.
Summary of the invention
The present invention proposes a kind of surface that utilizes and triggers equipment and using method thereof that the forming core technology prepares monotectic alloy shell type composite tissue powder.Its objective is and utilize the surface to trigger the forming core technology, make disperse phase be easier to forming core on the atomized drop surface, therefore, in the atomized drop cooling procedure, disperse phase just begins at atomized drop surface forming core under less degree of supersaturation, and forming core speed is very high.This makes that in whole process of setting, the atomized drop surface all has lower degree of supersaturation, thereby solute constantly carries out diffusive migration to the drop surface, impels the formation with shell mould complex tissue powder.
Technical scheme of the present invention is:
A kind of equipment that is used to prepare monotectic alloy shell type composite tissue powder, comprise the drop generation device that is provided with from top to bottom, the drop charge device, the cabin body, the drop generation device comprises crucible furnace, to the exciting device that vibrates from the molten body fluid flow of crucible furnace bottom pod apertures outflow, the drop charge device, the drop charge device is installed on melt exit, crucible furnace bottom, be provided with the infrared radiation thermometer of measuring the drop temperature in the body of cabin, forming core triggers and position regulator, and forming core triggers and position regulator comprises the trigger that can produce electron beam or ion beam, corresponding with trigger and produce the target that drop triggers bundle, adjust the slide block leading screw of trigger and target position, motor.
The described equipment that is used to prepare monotectic alloy shell type composite tissue powder is provided with water-cooling circulating system above exciting device, the crucible furnace top is connected with the gas charging system that melt in the crucible furnace is exerted pressure by pipeline.
The described equipment that is used to prepare monotectic alloy shell type composite tissue powder, exciting device adopt exciting rod to place the interior melt of crucible furnace.
The described equipment that is used to prepare monotectic alloy shell type composite tissue powder, the crucible furnace bottom offers pod apertures, establishes the thermocouple that is used to measure melt temperature in the crucible furnace in the crucible furnace.
The described equipment that is used to prepare monotectic alloy shell type composite tissue powder is established the infrared radiation thermometer that is used to measure the shooting speed measuring device of liquid drop speed and is used to measure the drop temperature in the body of cabin.
The described equipment that is used to prepare monotectic alloy shell type composite tissue powder, the cabin body is connected with vavuum pump and gas charging system.
The described equipment that is used to prepare monotectic alloy shell type composite tissue powder is provided with observation window and observation camera at the crucible furnace top.
The described using method that is used to prepare the equipment of monotectic alloy shell type composite tissue powder, concrete steps are as follows:
(1) melt monotectic alloy with crucible furnace, and make the alloy melt temperature rise to constituent element to dissolve each other more than the temperature, insulation forms the homogeneous melt;
(2) in crucible furnace, inflate, force liquid metal to flow out from pod apertures, by using exciting device to make liquid stream under the effect of exciting ripple, be atomized into the drop of size homogeneous, adopt the drop charge device that drop is applied electric field, the drop that forms has like charges, repel mutually, collision merging phenomenon between drop can not take place;
(3) in the droplets fall process, measure the drop temperature with infrared radiation thermometer, according to measured temperature, determine the position of trigger and target, guarantee that reducing to the constituent element liquid state temperature line of dissolving each other when the drop temperature begins to trigger forming core when following;
(4) in liquid-liquid phase change process, the electron beam or the ion beam that produce by trigger impact on target, target is produced trigger bundle, drop is triggered forming core, the result who triggers forming core is that disperse phase is at drop surface forming core, the solute of drop inside causes the formation of disperse phase enriched layer or shell mould complex tissue to the drop diffusion into the surface.
The described using method that is used to prepare the equipment of monotectic alloy shell type composite tissue powder, target is selected the pure constituent element corresponding to disperse phase for use.
The invention has the beneficial effects as follows:
1, the present invention is provided with the drop generation device, use exciting device to make liquid stream under the effect of exciting ripple, be atomized into the drop of size homogeneous, size droplet diameter is a micron order, scope at several micron to hundreds of micron, and in the drop cooling procedure, it is carried out surface triggering forming core with triggering the forming core device, impel the degree of supersaturation on drop surface in liquid-liquid phase change process less, the inner solute of drop causes having the formation of shell mould complex tissue monotectic alloy powder constantly to the diffusion into the surface migration.
2, the present invention to drop charge, applies electric field to liquid stream by the drop charge device near the outlet of crucible furnace bottom liquid stream, makes the drop band like charges of formation, can avoid collision mutually between drop.
3, monotectic alloy smelting temperature of the present invention will be higher than the constituent element temperature of dissolving each other, the atomized drop free-falling, speed progressively increases, in dropping process, adopt infrared radiation thermometer to measure the drop temperature, thereby adjust the position of trigger and target, when drop reaches the liquid-liquid phase alternating temperature and spends, it is carried out surface and trigger forming core, the formation of promotion shell mould complex tissue monotectic alloy powder.
4, the present invention is applicable to that monotectic alloy (as: Al-Pb, Al-Bi, Al-Sn-Bi, Cu-Pb, Cu-Sn-Bi or the like) shell mould organizes the preparation of powder.
Description of drawings
Fig. 1 is the signal phasor of monotectic type alloy.
Fig. 2 a-c is the monotectic alloy shell type composite tissue powder schematic diagram.The typical shell mould complex tissue of Fig. 2 a powder is a cutaway view; Fig. 2 b is typical shell mould complex tissue powder partial cutaway schematic; Fig. 2 c is the Al-Pb alloy powder organization chart with shell mould complex tissue.
Fig. 3 is the special equipment schematic diagram of monotectic alloy shell type composite tissue powder preparation.
Fig. 4 involves it to liquid stream atomizing schematic diagram for exciting device among Fig. 3 forms exciting.
Among the figure, 1 crucible furnace; 2 observation windows; 3 exciting devices; 4 cameras; 5 cooling water pipes; 6 water-cooling circulating systems; 7 gas charging systems; 8 shooting speed measuring devices; 9 vavuum pumps; 10 infrared radiation thermometers; 11 motors; 12 slide block leading screws; 13 forming cores trigger and position regulator; 14 targets; 15 triggers; 16 drop charge devices; 17 pod apertures; 18 thermocouples; 19 drop generation devices; 20 microns drops; 21 trigger bundle; 22 cabin bodies.
The specific embodiment
Embodiment 1
As shown in Figure 3, equipment proposed by the invention mainly is made up of the single-size drop generation device 19, drop charge device 16, the cabin body 22 that are provided with from top to bottom.Wherein, single-size drop generation device 19 comprises crucible furnace 1, exciting device 3, water-cooling circulating system 6, be opened in the crucible furnace bottom pod apertures 17, be used to measure the thermocouple 18 of melt temperature in the crucible furnace, in the melt in the exciting device 3 employing exciting rods insertion crucible furnaces 1, above exciting device 3, be provided with water-cooling circulating system 6, cool off by 5 pairs of exciting devices 3 of cooling water pipe, the crucible furnace top is connected with gas charging system 7 by pipeline, melt in the close crucible stove is exerted pressure, impel melt to flow out crucible furnace.Dc source or drop charge device 16 make the drop band like charges of formation by near the outlet of crucible furnace bottom liquid stream liquid stream being applied electric field, avoid collision mutually between drop.Forming core triggers and position regulator 13 comprises the trigger 15 that can produce electron beam or ion beam, corresponding with trigger and produce the target 14 that drop triggers bundle, slide block leading screw 12, the motor 11 of adjusting trigger and target position, and the triggering bundle 21 of target 14 generations is relative with micron drop 20 after trigger 15 triggers.Be used for that high-speed camera speed measuring device 8, infrared radiation thermometer 10, forming core that micron drop tests the speed trigger and position regulator 13 places in the cabin body 22; cabin body 22 is connected with vavuum pump 9 and gas charging system; can be vacuum state or protective gas state in the cabin body 22, decide according to concrete alloy.Also be provided with observation window 2 and observation at cabin body 22 tops with camera 4, can observe working condition in the body of cabin.
The preparation method of present embodiment monotectic alloy shell type composite tissue powder is as follows:
(1) fusing monotectic alloy, and make the alloy melt temperature rise to constituent element to dissolve each other more than the temperature, insulation forms the homogeneous melt;
(2) in crucible furnace 1, inflate (as argon gas, nitrogen etc., the gas charging system the blowing pressure can be adjusted as required), force liquid metal to flow out from pod apertures, by using exciting device 3 to make liquid stream under the effect of exciting ripple, be atomized into the drop of size homogeneous, owing to applied electric field with drop charge device 16, the drop that forms has like charges, repels mutually, and collision merging phenomenon between drop can not take place.
(3) can be vacuum in the cabin body 22, also can fill protective gas (as argon gas, nitrogen etc.), decide according to alloy.In the droplets fall process, measure the drop temperature with infrared radiation thermometer 10, measure droplets fall speed with shooting speed measuring device 8 (as high-speed camera), according to measured temperature, determine the position of trigger and target, guarantee that reducing to the constituent element liquid state temperature line of dissolving each other when the drop temperature begins to trigger forming core when following.
(4) in liquid-liquid phase change process, electron beam that produces by trigger or ion beam impact that (target is generally selected the pure constituent element corresponding to disperse phase for use on target, as: for the Al-Pb alloy, when disperse phase or first precipitated phase are rich Pb phase time, target can be selected pure Pb for use), target is produced trigger bundle 21 (ion beam of present embodiment is the lead ion bundle), drop is triggered forming core.The result who triggers forming core is a disperse phase (the rich Pb phase in the present embodiment) under extremely low degree of supercooling (constituent element dissolve each other between temperature and drop actual temperature poor) promptly at the surperficial forming core of drop, and the number density of nuclear is very high, this makes that the degree of supersaturation on drop surface is lower all the time in whole liquid-liquid phase change process, therefore, the solute of drop inside (Pb in this example) causes the formation of disperse phase enriched layer or shell mould complex tissue to the drop diffusion into the surface.
The course of work of the present invention is as follows:
Behind the alloy melting, produce the monotectic alloy drop by drop generation device 19, under the effect of exciting device 3, drop forms exciting ripple (Fig. 4), near pod apertures 17, produce the micron drop 20 of single-size (granularity be several microns to the hundreds of micron), at the drop charge device in pod apertures 17 outsides to drop charge, make between the drop mutually exclusive because of the band like charges, avoid drop that collision mutually takes place in dropping process, by decision triggers the rational position of forming core to it to the drop thermometric, by slide block leading screw 12, motor 11 is adjusted the position of trigger 15 and target 14, in place forming core is triggered on the drop surface, in liquid-liquid phase change process, form triggering forming core phase enriched layer, promptly form the shell mould complex tissue on the drop surface.
Fig. 2 c has a complex tissue Al-Pb alloy powder for preparation in the applicant research, and skin is plumbous, and internal layer is an aluminium.

Claims (9)

1, a kind of equipment that is used to prepare monotectic alloy shell type composite tissue powder, it is characterized in that: comprise the drop generation device (19) that is provided with from top to bottom, drop charge device (16), cabin body (22), drop generation device (19) comprises crucible furnace (1), to the exciting device (3) that vibrates from the molten body fluid flow of crucible furnace bottom pod apertures outflow, drop charge device (16), drop charge device (16) is installed on melt exit, crucible furnace bottom, be provided with the infrared radiation thermometer (10) of measuring the drop temperature in the cabin body (22), forming core triggers and position regulator (13), and forming core triggers and position regulator (13) comprises the trigger (15) that can produce electron beam or ion beam, corresponding with trigger and produce the target (14) that drop triggers bundle, adjust the slide block leading screw (12) of trigger and target position, motor (11).
2, according to the described equipment that is used to prepare monotectic alloy shell type composite tissue powder of claim 1, it is characterized in that: be provided with water-cooling circulating system (6) in exciting device (3) top, the crucible furnace top is connected with the gas charging system (7) that melt in the crucible furnace is exerted pressure by pipeline.
3, according to the described equipment that is used to prepare monotectic alloy shell type composite tissue powder of claim 1, it is characterized in that: exciting device (3) adopts exciting rod to place the interior melt of crucible furnace (1).
4, according to the described equipment that is used to prepare monotectic alloy shell type composite tissue powder of claim 1, it is characterized in that: crucible furnace (1) bottom offers pod apertures (17), establishes the thermocouple (18) that is used to measure melt temperature in the crucible furnace in the crucible furnace (1).
5, according to the described equipment that is used to prepare monotectic alloy shell type composite tissue powder of claim 1, it is characterized in that: establish the infrared radiation thermometer (10) that is used to measure the shooting speed measuring device (8) of liquid drop speed and is used to measure the drop temperature in the cabin body (22).
6, according to the described equipment that is used to prepare monotectic alloy shell type composite tissue powder of claim 1, it is characterized in that: the cabin body is connected with vavuum pump and gas charging system.
7, according to the described equipment that is used to prepare monotectic alloy shell type composite tissue powder of claim 1, it is characterized in that: observation window (2) and observation camera (4) are set at crucible furnace (1) top.
8, a kind of according to the described using method that is used to prepare the equipment of monotectic alloy shell type composite tissue powder of claim 1, it is characterized in that concrete steps are as follows:
(1) melt monotectic alloy with crucible furnace, and make the alloy melt temperature rise to constituent element to dissolve each other more than the temperature, insulation forms the homogeneous melt;
(2) in crucible furnace, inflate, force liquid metal to flow out from pod apertures, by using exciting device to make liquid stream under the effect of exciting ripple, be atomized into the drop of size homogeneous, adopt the drop charge device that drop is applied electric field, the drop that forms has like charges, repel mutually, collision merging phenomenon between drop can not take place;
(3) in the droplets fall process, measure the drop temperature with infrared radiation thermometer, according to measured temperature, determine the position of trigger and target, guarantee that reducing to the constituent element liquid state temperature line of dissolving each other when the drop temperature begins to trigger forming core when following;
(4) in liquid-liquid phase change process, the electron beam or the ion beam that produce by trigger impact on target, target is produced trigger bundle, drop is triggered forming core, the result who triggers forming core is that disperse phase is at drop surface forming core, the solute of drop inside causes the formation of disperse phase enriched layer or shell mould complex tissue to the drop diffusion into the surface.
9, according to the described using method that is used to prepare the equipment of monotectic alloy shell type composite tissue powder of claim 8, it is characterized in that: target is selected the pure constituent element corresponding to disperse phase for use.
CNB2006100478216A 2006-09-20 2006-09-20 Equipment for preparing monotectic alloy shell type composite tissue powder and use method thereof Expired - Fee Related CN100509217C (en)

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CN103077647B (en) * 2013-01-29 2015-01-07 中国科学院合肥物质科学研究院 Droplet falling control device
CN109128206B (en) 2018-09-25 2020-11-24 中国人民解放军陆军装甲兵学院 Device and method for efficiently preparing superfine spherical metal powder by droplet-by-droplet centrifugal atomization method

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5400851A (en) * 1990-02-02 1995-03-28 Metallgesellschaft Aktiengesellschaft Process of producing monotectic alloys
CN1121452A (en) * 1994-10-26 1996-05-01 中国科学院金属研究所 Controllable casting technology for monotectic alloy antifriction bearing material
CN1299719A (en) * 1999-12-14 2001-06-20 中国科学院金属研究所 Monotectic alloy making process
US20040089437A1 (en) * 2000-08-11 2004-05-13 Zhongyung Fan Method and apparatus for making metal alloy castings
CN200984642Y (en) * 2006-09-20 2007-12-05 中国科学院金属研究所 Device for preparing monotectic alloy shuck type composite tissue powder

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5400851A (en) * 1990-02-02 1995-03-28 Metallgesellschaft Aktiengesellschaft Process of producing monotectic alloys
CN1121452A (en) * 1994-10-26 1996-05-01 中国科学院金属研究所 Controllable casting technology for monotectic alloy antifriction bearing material
CN1299719A (en) * 1999-12-14 2001-06-20 中国科学院金属研究所 Monotectic alloy making process
US20040089437A1 (en) * 2000-08-11 2004-05-13 Zhongyung Fan Method and apparatus for making metal alloy castings
CN200984642Y (en) * 2006-09-20 2007-12-05 中国科学院金属研究所 Device for preparing monotectic alloy shuck type composite tissue powder

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