CN105004638A - Speed-accurately controlled transparent solution phase-separation observation apparatus - Google Patents
Speed-accurately controlled transparent solution phase-separation observation apparatus Download PDFInfo
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Abstract
A speed-accurately controlled transparent solution phase-separation observation apparatus is disclosed. The apparatus comprises a set of accuracy transmission equipment, two temperature control modules, two high and low temperature cycling devices connected with the temperature control modules, a pedestal and a fixed support, a microscope and an acquisition and detection system. The apparatus is characterized in that a sample can move at an accurate speed in a horizontal temperature gradient field when driven by the accuracy transmission equipment; and as the sample moves accurately at the set speed, the action between a phase separation interface and movement behavior of a second phase droplet can be observed and recorded at real time by the microscope. The apparatus has the following advantages: by adjusting rotational speed of a motor, movement speed of a sample can be changed accurately with the speed range of 100 microns/s to 4.2 mm/s to adapt to migration, growing and coagulation processes of a second phase droplet at the phase separation interface at different movement speeds caused by different temperature gradients so as to obtain multilayered band microstructures and better understand the multilayered band microstructures and core-shell structure and morphology obtained in a metallic monotectic alloy.
Description
Technical field:
The present invention relates to the accurate controlled clear solution of a kind of speed to be separated observation device, belong to new material science and technology field, the process slowly occurred specifically by being separated in observation clear solution is to set forth a kind of experimental provision of quick phase separation in immiscible alloy system.
Background introduction:
About the focus that the monotectic material preparation technology with unique physical and mechanical properties is material science concern always.Such as prepare rich Fe phase Dispersed precipitate in the alloy of Cu matrix, Cu-Fe alloy has excellent electric conductivity, usually as excellent contact, tactile bridge and vacuum device material; When oarse-grained rich Fe phase is dispersed in Cu matrix, it shows giant magnetoresistance effect and special physical property.Equally, the alloy of even dispersion Al-In can manufacture superconductor, and Cu-Pb alloy has good lubricity and high-temperature stability because of it and is usually used as bearing shell.Metal system like this also has a lot, has potential application prospect in view of such material, and therefore, its dynamics Forming Mechanism of finer research is very necessary.
Monotectic alloy has a difficult miscible district at its hypermonotectic composition range, liquid-liquid phase separation can occur when the temperature decreases, this relate to a kind of liquid phase-second liquid phase-mother liquor mutually in formation.Under certain temperature field condition, drop can be moved to temperature end by low-temperature end by the effect of Marangoni convection current, and collision, the coalescence of drop can be there is and grows up in the moving interface of second-phase, this formation for solidified structure and final mechanical property have decisive role, and the monotectic alloy that the interface kinetics process therefore obtaining second-phase drop has ad hoc structure and performance for design is most important.This patent provides a kind of device utilizing lead screw transmission accurately to control phase interface translational speed, and research is separated this whole process and disclose further transition kinetics and become more clear visual.
The invention provides the accurate controlled clear solution of a kind of speed to be separated observation device, utilize the constant speed of motor and leading screw to move, second-phase liquid drop movement interface geo-stationary is within the scope of microscopic observation.Employing of the present invention and metal material solidify the similar clear solution of behavior to simulate phase separation in metal, although existing patent (publication number: CN1579606A) has invented a kind of transparent model alloy device before, pass through control temperature, regulate thermograde thus the process of in-situ observation Marangoni convection current, but its alloy chamber and Microexamination device all static, be difficult to the interface of following the tracks of second liquid phase, the home position observation of phase interface cannot be realized.
Apparatus of the present invention Observations Means is the method adopting optical microphotograph, the substantivity that visual field is observed brings great convenience to measuring Marangoni migration velocity, adopt a kind of gearing of the interface movement that is separated with precise speed follow-up simultaneously, second-phase drop translational speed and sample drawing velocity is made to keep synchronous, with this understanding, the be separated forward position at interface is in the range of observation of visual field all the time, is conducive to our accurate observation and record second-phase drop forming process, migration velocity, moving front, drop annex speed to the impact etc. be separated.Keep light microscopic original position motionless, print is with stabilized speed pull, make the picture observed in microscope steady and audible, this is for setting up the dynamic behavior model be separated, study the mechanism that is separated, explain segregation and lamination in metal alloy, it is very favourable for improving some structural behaviour of alloy.
Summary of the invention
The object of the present invention is to provide a kind of with motor and lead screw transmission and the accurate controlled real-time monitored clear solution phase-separating device of speed.In order to achieve the above object, the present invention realizes by the following technical solutions: the accurate controlled clear solution of a kind of speed is separated observation device, comprise base (1), two temperature control modules (2), support the fixed support (7) of temperature control module, microscope (5), Microscope base (9), thermopair (14), high temperature and low temperature circulating device (6), mobile example platform (3), motor (4), driveline support (8), transmission bracket (10), leading screw (11), big belt pulley (15), small belt pulley (12), belt (13).Fixed support (7), driveline support (8) and Microscope base (9) are fixed on base (1), the temperature control module (2) of four hollows is placed on fixed support (7), wherein temperature control module is relative between two, be screwed, centre is left certain space and is used for the sample be placed on mobile example platform (3) that placement needs to observe with microscope (4), between two relatively after temperature control module (2) be placed on microscope (4) both sides, high temperature and low temperature circulating device (6) is connected for precise control of temperature with temperature control module (2), leading screw (11) and transmission bracket (10) are fixedly connected on driveline support (8), mobile example platform (3) is connected for mobile example with transmission bracket (10), belt lace (12) is connected by belt (13) with big belt pulley (15), motor (4) is fixed on big belt pulley (15) place, small belt pulley (12) is connected with leading screw (11) and then the translational speed of accurate Quality control, accurate temperature measurement in the sample to which placed by thermopair (14).It is characterized in that: described temperature gradient field is level, the temperature at two ends, left and right is controlled by high temperature and low temperature circulating device; Sample can move with precise speed under the drive of motor device; Meanwhile, sample, with the speed accurately movement of setting, ensure that microscope equipment can be observed in slow mobile example in fixing position the interface that is separated and be in all the time in visual field; Microscope can real-time monitored record be separated interface and Marangoni migration effect under second-phase drop motor behavior between impact.
The be separated motor (4) of observation device of the accurate controlled clear solution of a kind of speed of the present invention can drive sample accurately movement, wherein in equipment, the tooth distance of leading screw (11) is 0.5mm, by the translational speed regulating the rotating speed of motor accurately can change sample, velocity range is approximately 100 μm/s to 4.2mm/s, contribute to the migration that we can observe be separated forward position, interface and second-phase drop in clear solution is separated whole process, grow up, coalescence process, obtain the band tissue of multilayer, in order to understand the multilayer band tissue and shell-core structure pattern that obtain in metal metaphosphate peritectic alloy better.
The be separated temperature of high temperature and low temperature circulating device (6) of observation device of the accurate controlled clear solution of a kind of speed of the present invention can set arbitrarily, this system temperature control is accurate, it is connected with hollow temperature control module (2), for temperature control module (2) provides different temperature gradient fields, distance wherein between temperature control module (2) also can regulate, and thermograde can reach 50K/mm.
The be separated base (1) of observation device of the accurate controlled clear solution of a kind of speed of the present invention is of a size of 800 × 280 × 15mm, this base quality is larger, effectively can reduce the impact of the microseismic activity in experimentation, microscope equipment display frame is stablized, clear.
The be separated recording geometry of observation device of the accurate controlled clear solution of a kind of speed of the present invention is microscope (5) with acquisition system, and be connected with computing machine, and corresponding Survey Software is equipped with, in order to accurate analysis drop migration, grow up, coalescence behavior.Meanwhile, microscopical objective lens is all transportable in XYZ direction, thus can regulate the different parts course of reaction of sample to be observed quickly.
The miscible transparent system of difficulty of what the accurate controlled clear solution of a kind of speed of the present invention was separated that the clear solution of observation device selects is similar density, selects the system object of similar density to be to reduce as far as possible the impact of natural convection.The phase separation that this transparent body ties up to the phase separation of immiscible range and immiscible alloy system immiscible range is similar, therefore can simulate the phase transition process of immiscible alloy immiscible range with it.
The invention has the beneficial effects as follows: motor device can drive sample with the movement that precise speed is stable in the temperature field module of accurate temperature controlling, can real-time monitored record the course of reaction that is separated of continuous mobile example inside.This device successfully utilizes the clear solution similar with immiscible alloy process of setting to simulate its process of setting.Tracing observation Marangoni migration moves second-phase, grow up, the impact of coalescence, discloses the mechanism in itself and phase separation.
Accompanying drawing illustrates:
Fig. 1 is that the accurate controlled clear solution of a kind of speed is separated the schematic diagram of observation device.
Fig. 2 is the microcosmic interphase of the multilayer band tissue obtained.
Fig. 3 and Fig. 4 is that or else sample organizes experimental result macrograph with the multilayer band obtained under translational speed.
In figure: 1. base 2. temperature control module 3. mobile example platform 4. motor 5. microscope 6. high temperature and low temperature circulating device 7. supports fixed support 8. driveline support 9. Microscope base 10. transmission bracket 11. leading screw 12. small belt pulley 13. belt 14. thermopair 15. big belt pulley of temperature control module
Embodiment:
Now the invention will be further described in conjunction with the embodiments:
Embodiment 1:
Step 1: it is SCN-50wt%H that the succinonitrile (SCN) of high purity water and purity 99.9% is at room temperature made into composition
2the solution of O, sample quality is about 3 grams.
Step 2: because sample is immiscible in room temperature, the temperature of this system critical point is at about 58 DEG C, therefore the hot bath first sample being placed on about 90 DEG C heats about 5 minutes, be injected in sample cavity with the syringe of 1ml after complete miscibility, and injection process must be slow, avoid air to enter in sample cavity, then install by modified acroleic acid rubber seal.
Step 3: the high temperature and low temperature circulating device heated with left end, refrigerating module is connected is set to 70 DEG C, heats with right-hand member, high temperature and low temperature circulating device that refrigerating module is connected is set to 20 DEG C, two heating, refrigerating module are spaced apart 10mm, and thermograde is 5K/mm.
Step 4: packaged sample is reheated after dissolving each other completely, put in the groove of heating, refrigerating module, to be separated interface and the interaction of moving with the Marangoni of second-phase drop thereof by microscopic, motor pulls sample to the right with the speed of 1mm/s simultaneously.
Obtain microcosmic interphase as shown in Figure 2, the 6 layers of laminated tissue of macroscopic view as shown in Figure 3.
Embodiment 2:
Step 1: the succinonitrile (SCN) of high purity water and purity 99.9% is at room temperature made into the solution that composition is SCN-50wt%H2O, and sample quality is about 3 grams.
Step 2: because sample is immiscible in room temperature, the temperature of this system critical point is at about 58 DEG C, therefore the hot bath first sample being placed on about 90 DEG C heats about 5 minutes, be injected in sample cavity with the syringe of 1ml after complete miscibility, and injection process must be slow, avoid air to enter in sample cavity, then install by modified acroleic acid rubber seal.
Step 3: the high temperature and low temperature circulating device heated with left end, refrigerating module is connected is set to 60 DEG C, heats with right-hand member, high temperature and low temperature circulating device that refrigerating module is connected is set to 20 DEG C, two heating, refrigerating module are spaced apart 10mm, and thermograde is 4K/mm.
Step 4: packaged sample is reheated after dissolving each other completely, put in the groove of heating, refrigerating module, to be separated interface and the interaction of moving with the Marangoni of second-phase drop thereof by microscopic, motor pulls sample to the right with the speed of 0.8mm/s simultaneously.
Obtain microcosmic interphase as shown in Figure 2, the 8 layers of laminated tissue of macroscopic view as shown in Figure 4.In an experiment by changing motor speed, what make sample pulls speed also not identical, can obtain similar microcosmic interphase and the laminated tissue of the different number of plies like this.
Claims (4)
1. the accurate controlled clear solution of speed is separated an observation device, comprises base (1), two temperature control modules (2) and relatively fixing, the fixed support (7), microscope (5), Microscope base (9), thermopair (14), high temperature and low temperature circulating device (6), mobile example platform (3), motor (4), driveline support (8), transmission bracket (10), leading screw (11), big belt pulley (15), small belt pulley (12), the belt (13) that support temperature control module between two.It is characterized in that: it is characterized in that: it is characterized in that: described temperature gradient field is level, the temperature at two ends, left and right is controlled by high temperature and low temperature circulating device; Sample can move with precise speed under the drive of motor device; Meanwhile, sample accurately moves forward with the speed of setting, ensure that microscope equipment can be observed in slow mobile example in fixing position the interface that is separated and be in all the time in visual field; Microscope can real-time monitored record be separated interface and Marangoni migration effect under second-phase drop motor behavior between impact.
2. to be separated observation device according to the accurate controlled clear solution of a kind of speed according to claim 1, it is characterized in that: the equipment of described driven by motor sample movement is fixed on base (1), can pass through transmission bracket (10) drives the sample be fixed on mobile example platform (3) to move with accurate speed, and velocity range is approximately 100 μm/s to 4.2mm/s.
3. to be separated observation device according to the accurate controlled clear solution of a kind of speed according to claim 1, it is characterized in that: two described temperature control modules (2) are relative between two, be screwed, but adjustment module spacing can be moved horizontally, leave certain space in the middle of module to be used for placing the sample needing observation, and being placed on base (1) by two fixed supports (7), the thermograde at temperature control module two ends can reach 50K/mm.
4. to be separated observation device according to the accurate controlled clear solution of a kind of speed according to claim 1, it is characterized in that: described system is that density difference is small, all temperature ranges are the clear solution system of-20-230 DEG C.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107057777A (en) * | 2017-03-01 | 2017-08-18 | 榆林学院 | A kind of use interface fluctuation induces the experimental provision that the high Buddhist nun of horse traction condenses |
| CN109000883A (en) * | 2018-08-03 | 2018-12-14 | 中国科学院力学研究所 | A kind of method of pressure and discharge relation in determining micron capillary tube passage |
| CN109142675A (en) * | 2018-08-03 | 2019-01-04 | 中国科学院力学研究所 | A kind of micron capillary column gas-liquid dynamic phase interface test device |
| CN112710681A (en) * | 2020-12-21 | 2021-04-27 | 中南大学 | Experimental device for solidification behavior is observed to normal position |
| CN113252626A (en) * | 2021-05-06 | 2021-08-13 | 江苏格罗瑞化学有限公司 | Fluorescent brightener automatic checkout device |
| CN114113078A (en) * | 2021-10-09 | 2022-03-01 | 温州大学 | Device and method for observing liquid-liquid phase separation |
| CN114460125A (en) * | 2022-01-21 | 2022-05-10 | 西安航空学院 | Experimental device and method for metal surface supercooling liquid drop solidification |
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| CN1579606A (en) * | 2003-08-01 | 2005-02-16 | 中国科学院金属研究所 | Transparent model alloy device |
| CN101571498A (en) * | 2009-06-05 | 2009-11-04 | 东南大学 | Micropore evolution real-time imaging device during alloy remelting and solidification |
| CN101811186A (en) * | 2010-05-27 | 2010-08-25 | 哈尔滨工业大学 | Device for driving solidification and crystallization process by using electrical effect |
| CN101832942A (en) * | 2010-05-27 | 2010-09-15 | 哈尔滨工业大学 | Observing method of electrical effect driving solidification crystallization process |
| JP5307539B2 (en) * | 2006-05-31 | 2013-10-02 | オリンパス株式会社 | Biological sample imaging method and biological sample imaging apparatus |
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2014
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| CN1579606A (en) * | 2003-08-01 | 2005-02-16 | 中国科学院金属研究所 | Transparent model alloy device |
| JP5307539B2 (en) * | 2006-05-31 | 2013-10-02 | オリンパス株式会社 | Biological sample imaging method and biological sample imaging apparatus |
| CN101571498A (en) * | 2009-06-05 | 2009-11-04 | 东南大学 | Micropore evolution real-time imaging device during alloy remelting and solidification |
| CN101811186A (en) * | 2010-05-27 | 2010-08-25 | 哈尔滨工业大学 | Device for driving solidification and crystallization process by using electrical effect |
| CN101832942A (en) * | 2010-05-27 | 2010-09-15 | 哈尔滨工业大学 | Observing method of electrical effect driving solidification crystallization process |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107057777A (en) * | 2017-03-01 | 2017-08-18 | 榆林学院 | A kind of use interface fluctuation induces the experimental provision that the high Buddhist nun of horse traction condenses |
| CN107057777B (en) * | 2017-03-01 | 2023-11-28 | 海口图腾新能源应用研发有限公司 | Experimental device for inducing marangoni condensation by adopting interface fluctuation |
| CN109000883A (en) * | 2018-08-03 | 2018-12-14 | 中国科学院力学研究所 | A kind of method of pressure and discharge relation in determining micron capillary tube passage |
| CN109142675A (en) * | 2018-08-03 | 2019-01-04 | 中国科学院力学研究所 | A kind of micron capillary column gas-liquid dynamic phase interface test device |
| CN112710681A (en) * | 2020-12-21 | 2021-04-27 | 中南大学 | Experimental device for solidification behavior is observed to normal position |
| CN113252626A (en) * | 2021-05-06 | 2021-08-13 | 江苏格罗瑞化学有限公司 | Fluorescent brightener automatic checkout device |
| CN114113078A (en) * | 2021-10-09 | 2022-03-01 | 温州大学 | Device and method for observing liquid-liquid phase separation |
| CN114460125A (en) * | 2022-01-21 | 2022-05-10 | 西安航空学院 | Experimental device and method for metal surface supercooling liquid drop solidification |
| CN114460125B (en) * | 2022-01-21 | 2023-11-03 | 西安航空学院 | Experimental device and method for solidifying supercooled liquid drops on metal surface |
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