CN101430292B - Method for single metal droplet supercooling degree measurement by large cooling speed in situ fast thermal analysis - Google Patents
Method for single metal droplet supercooling degree measurement by large cooling speed in situ fast thermal analysis Download PDFInfo
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- CN101430292B CN101430292B CN2008102039852A CN200810203985A CN101430292B CN 101430292 B CN101430292 B CN 101430292B CN 2008102039852 A CN2008102039852 A CN 2008102039852A CN 200810203985 A CN200810203985 A CN 200810203985A CN 101430292 B CN101430292 B CN 101430292B
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Abstract
The invention relates to a method for mensurating supercooling degree by single metallic microsphere high cooling speed in-situ fast thermal analysis and belongs to the technical field of physical performance test and measurement. The method is characterized in that real-time in-situ fast thermal analysis test is carried out on the single metallic microsphere at a high heating-cooling speed, thereby directly obtaining the solidification supercooling degree of the metallic microsphere under the condition of high cooling speed by experimental means; and the method is different from the existing method which only can obtain the solidification supercooling degree of microsphere under the fast cooling condition by theoretical calculation. The invention uses a fast thermal analyzing device to measure the heating and cooling curves of the single metallic microsphere at real time; the heating-cooling speed is 1 to 1*10<4>K/s; the obtained heating and cooling curves are analyzed to obtain the melting and solidifying temperatures of the single metallic microsphere; and the real-time solidification supercooling degree of the single metallic microsphere can be obtained.
Description
Technical field
The present invention relates to a kind of method of single metal droplet supercooling degree measurement by large cooling speed in situ fast thermal analysis, belong to Physical Property of Metal thermometrically technical field.
Background technology
Degree of supercooling is the important characterization parameter of metal solidification process, and the degree of supercooling of solidifying by reasonable control metal bath can obtain the solidified structure of different shape, and obtains different material properties.Therefore, how the degree of supercooling of metal solidification process being estimated and characterized is wherein key.For the influence factor of fully realizing degree of supercooling in the metal solidification process and to the influence of aspects such as solidified structure, the researchist has carried out extensive studies.Because metal is non-transparent material, and in the heating process with high temperature, so the sign of process of setting often just can be carried out after the material preparation process is finished.Adopt laser confocal microscope, can realize in-situ observation to the material solidification tissue, utilize synchrotron radiation that the technology of the energy dispersion X-ray diffraction under the ray condition is provided, the degree of supercooling of the metal bath under also can in situ detection electromagnetic suspension condition, but the experiment of the metal freezing degree of supercooling under the big cooling rate condition to detect still be a difficult point.
Usually, the metal degree of supercooling can adopt traditional thermal analyzer such as differential scanning calorimeter (DifferentialScanning Calorimeter, DSC) or thermal analyzer (Differential Thermal Analyzer, DTA) etc. means are measured.But because the limitation of equipment itself, its maximum cooling velocity often can only reach the cooling power of the hundreds of K of per minute, therefore can't test the degree of supercooling of rapid solidification.For most metal solidification processes, the degree of supercooling of droplet then often the means by Theoretical Calculation obtain, thereby can't obtain direct test data the result of Theoretical Calculation is verified.
Summary of the invention
The method that the purpose of this invention is to provide a kind of supercooling degree measurement by large cooling speed in situ fast thermal analysis of single metal droplet.More particularly, the purpose of this invention is to provide a kind of metal droplet separates, with big firing rate and cooldown rate single metal droplet is carried out the quick thermoanalytical technology of real-time in-situ then, thereby non-traditional Theoretical Calculation is directly obtained metal freezing degree of supercooling under the rapid solidification condition with laboratory facilities.
The present invention relates to the method for single metal droplet supercooling degree measurement by large cooling speed in situ fast thermal analysis, it is characterized in that having following test process and step:
A. under optical microscope, required single metal is solidified droplet and pick out, and be positioned in the heating region of Rapid Thermal analytical equipment sensor;
B. will test the droplet location by optical microscope, guarantee that the position control of droplet is accurate, make it to be positioned at the top, center of sensor heating region, and determine the size of single droplet;
C. adopt the Rapid Thermal analytical equipment to measure the heating and the cooling curve of above-mentioned single metal droplet in real time, the heating cooldown rate is 1 * 10
3～1 * 10
4Any point among the K/s;
D. analyze the heating and the cooling curve of gained, obtain the fusing and the temperature of solidification of single metal droplet under above-mentioned different heating and the cooldown rate, what can directly obtain single metal droplet solidifies degree of supercooling (degree of supercooling=temperature of fusion-temperature of solidification) in real time.
The used isolated plant of the method for single metal droplet supercooling degree measurement by large cooling speed in situ fast thermal analysis is the Rapid Thermal analyte sensors, described sensor is made up of a well heater and a thermoelectric pile, its heating cooled region is the amorphous SiN film of 60 * 80 μ m, therebetween the thermoelectric pile of being made up of six thermopairs (being of a size of 13 * 34 μ m); The X1296 type thin film sensor product that described sensor is made for XensorIntegration company.
Described metal droplet when being fused into liquid state because of having stronger surface tension, and and the wetting state between the Rapid Thermal analyte sensors (material is SiN) is relatively poor, thereby make droplet keep geometrical shape stability in whole test process, promptly the change in size of droplet can be ignored.
Description of drawings
Fig. 1 places Rapid Thermal to analyze Sn-3.0Ag-0.5Cu (wt.%) the individual particle shape appearance figure of heating region center, and its position just in time is positioned at the top at the center of well heater, helps the detection of temperature variation signal, and the single droplet that solidifies is of a size of 47 μ m.
Fig. 2 is the single droplet Rapid Thermal of Sn-3.0Ag-0.5Cu (wt.%) analytic curve under different heating-cooldown rate, and its heating-cooling velocity is chosen as 1,10 respectively
2, 5 * 10
2, 1 * 10
3, 2 * 10
3, 3 * 10
3, 5 * 10
3And 1 * 10
4K/s.
Fig. 3 is (a) 10
3K/s and (b) the single many circulations of droplet of Sn-3.0Ag-0.5Cu (wt.%) the Rapid Thermal analytic curve under the 5K/s heating-cooldown rate.
Fig. 4 is the degree of supercooling of the single droplet in-situ test acquisition of Sn-3.0Ag-0.5Cu (wt.%) and the graph of a relation between the cooldown rate, and this graph of a relation is illustrated under the constant situation of droplet size, the relation of single metal droplet degree of supercooling and cooldown rate.
Fig. 5 is the Rapid Thermal analyte sensors, (a) is the sensor synoptic diagram, (b) is sensor heating cooling area schematic.
Embodiment
After now specific embodiments of the invention being described in.
Embodiment 1
It is the single metal droplet material that present embodiment is selected this typical leadless welding alloy of Sn-3.0Ag-0.5Cu (wt.%).
The concrete processing step of present embodiment is as follows:
(1) under optical microscope, required single metal is solidified droplet and pick out, and be positioned in the heating region of Rapid Thermal analytical equipment sensor;
(2) after droplet is had good positioning, amplify observation with optical microscope, accurate with the position control of guaranteeing droplet, be positioned at the top, center of sensor heating region, and determine the size of single droplet, it is of a size of 47 μ m, sees accompanying drawing 1;
(3) adopt the Rapid Thermal analytical equipment to measure the heating and the cooling curve of above-mentioned single metal droplet in real time, the heating cooldown rate is chosen as 1,1 * 10 respectively
2, 5 * 10
2, 1 * 10
3, 2 * 10
3, 3 * 10
3, 5 * 10
3And 1 * 10
4K/s sees accompanying drawing 2; 10
3Measure repeatedly round-robin thermal analysis curve under K/s and the 5K/s heating-cooldown rate, see accompanying drawing 3;
(4) analyze the heating and the cooling curve of gained, obtain the fusing and the temperature of solidification of single metal droplet under above-mentioned different heating and the cooldown rate, can directly obtain single metal droplet solidify in real time degree of supercooling and with the relation of cooldown rate, see accompanying drawing 4.
The Rapid Thermal analyte sensors is seen accompanying drawing 5.This sensor is the X1296 type thin film sensor product that Xensor Integration company makes.
Following table 1 is the cooling velocity and the average cold number of degrees value of Fig. 4 correspondence.
The pairing average degree of supercooling of table 1 different cooling rate
| Cooldown rate (K/s) | 10000 | 5000 | 3000 | 2000 | 1000 | 500 | 100 | 5 | 1 |
| Degree of supercooling (K) | 115.01 | 113.79 | 113.04 | 116.21 | 114.13 | 109.98 | 109.56 | 61.43 | 69.54 |
Claims (1)
1. the method for a single metal droplet supercooling degree measurement by large cooling speed in situ fast thermal analysis is characterized in that having following test process and step:
A. under optical microscope, required single metal is solidified droplet and pick out, and be positioned in the heating region of Rapid Thermal analytical equipment sensor;
B. will test the droplet location by optical microscope, guarantee that the position control of droplet is accurate, make it to be positioned at the top, center of sensor heating region, and determine the size of single droplet;
C. adopt the Rapid Thermal analytical equipment to measure the heating and the cooling curve of above-mentioned single metal droplet in real time, 1 * 10
3～1 * 10
4Measure repeatedly round-robin thermal analysis curve among the K/s under the heating cooldown rate of any point;
D. analyze the heating and the cooling curve of gained, obtain the fusing and the temperature of solidification of single metal droplet under different heating and the cooldown rate, what can directly obtain single metal droplet solidifies degree of supercooling in real time.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008102039852A CN101430292B (en) | 2008-12-04 | 2008-12-04 | Method for single metal droplet supercooling degree measurement by large cooling speed in situ fast thermal analysis |
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| CN2008102039852A CN101430292B (en) | 2008-12-04 | 2008-12-04 | Method for single metal droplet supercooling degree measurement by large cooling speed in situ fast thermal analysis |
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| CN101430292A CN101430292A (en) | 2009-05-13 |
| CN101430292B true CN101430292B (en) | 2011-05-04 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102914558A (en) * | 2012-10-25 | 2013-02-06 | 上海大学 | Method for testing TTT (Time,Temperature,Transformation) curve |
| CN104089972B (en) * | 2014-07-18 | 2017-02-15 | 大连理工常州研究院有限公司 | Method for determining condensate depression of metal micro-drops during rapid solidification process and device used by method |
| CN104889348B (en) * | 2015-06-19 | 2017-03-01 | 东方电气集团东方汽轮机有限公司 | The method of measurement high temperature alloy critical nuclei degree of supercooling |
| CN106623909A (en) * | 2016-11-16 | 2017-05-10 | 上海大学 | Method for simulating metal powder 3D printing |
| CN108614004B (en) * | 2016-12-09 | 2020-03-27 | 上海大学 | Fitting method and system of cooling curve |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4389904A (en) * | 1981-03-23 | 1983-06-28 | The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration | Method and apparatus for supercooling and solidifying substances |
| JP2000137011A (en) * | 1998-10-30 | 2000-05-16 | Kdk Corp | Freezing point depression measuring device and method thereof |
| CN1676249A (en) * | 2005-04-25 | 2005-10-05 | 北京科技大学 | Method and apparatus for preparing sheet-type metal pwoder by atomized drop deformation |
| US20070242722A1 (en) * | 2006-02-13 | 2007-10-18 | Toshihiko Nakamura | Freezing point temperature measuring method and temperature calibrating method in differential scanning calorimetry |
-
2008
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4389904A (en) * | 1981-03-23 | 1983-06-28 | The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration | Method and apparatus for supercooling and solidifying substances |
| JP2000137011A (en) * | 1998-10-30 | 2000-05-16 | Kdk Corp | Freezing point depression measuring device and method thereof |
| CN1676249A (en) * | 2005-04-25 | 2005-10-05 | 北京科技大学 | Method and apparatus for preparing sheet-type metal pwoder by atomized drop deformation |
| US20070242722A1 (en) * | 2006-02-13 | 2007-10-18 | Toshihiko Nakamura | Freezing point temperature measuring method and temperature calibrating method in differential scanning calorimetry |
Non-Patent Citations (2)
| Title |
|---|
| P.R. Algoso, et al.Solidification velocity of undercooled Ni-Cu alloys.ACTA MATERIALIA.2003,51(14),4307-4318. * |
| 高玉来,等.金属微滴快速凝固的过冷度研究.中国科学(E辑:信息科学).2006,36(1),24-28. * |
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