CN103954534A - Device for synchronously measuring wetting angle and differential scanning calorimetry (DSC) curve of metals on substrate - Google Patents
Device for synchronously measuring wetting angle and differential scanning calorimetry (DSC) curve of metals on substrate Download PDFInfo
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- CN103954534A CN103954534A CN201410147683.3A CN201410147683A CN103954534A CN 103954534 A CN103954534 A CN 103954534A CN 201410147683 A CN201410147683 A CN 201410147683A CN 103954534 A CN103954534 A CN 103954534A
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Abstract
The invention relates to a device for synchronously measuring a wetting angle and a differential scanning calorimetry (DSC) curve of metals on a substrate. According to the technical problem to be solved in the invention, the invention provides a device for synchronously obtaining supercooling degree in a metal solidification process and the wetting angle varying with temperature. The device can work in a temperature range of 0-1,600 DEG C for a long time, the requirement of measuring most of metal phase change points through DSC can be met, and outlines of the metals and a substrate can be obtained in real time by adopting an optical imaging method in the device, so that the wetting angle is obtained through software. The device consists of a vacuum and inflation system, a horizontal heating furnace body system, a photographing and observing system, a DSC system and a data acquisition processing system. According to the device, the functions of DSC equipment and wetting angle measuring equipment are integrated, the limitation that traditional DSC equipment is invisible is overcome, and the defect that a sample heat effect cannot be captured by previous wetting angle equipment is overcome.
Description
Technical field
The present invention relates to the device of a kind of synchro measure metal at suprabasil wetting angle and DSC curve, belong to metal freezing technical field.
Background technology
Modern heat analysis refers under temperature programmed control, the temperature variant class technology of the physical property of measurement of species.The thermophysical property of people by detecting sample itself be with the variation of temperature or time, studies molecular structure, aggregated structure, the variation of molecular motion etc. of material.Differential scanning calorimetry (is differential scanning calorimetry, be called for short DSC) be the variation of research its physical quantity of material variation with temperature (Δ Q and Δ H) under temperature program(me) control, by the variation of programed temperature, measure the difference power (rate of heat flow) of sample and reference substance and the relation of temperature simultaneously.
Can do the research of following several respects by DSC.One, the glass transition of sample: (can be accompanied by the variation of specific heat in the process that is elastomeric state by glassy transition, be presented as the variation (inflection of curve) of baseline height on DSC curve at amorphous polymer.Analyze thus, can obtain glass transition temperature and the specific heat intensity of variation of material.Two, melting: the melting of crystal is first order phase transition is accompanied by endothermic effect in melting process.Use DSC, can measure this endothermic effect, obtain the information such as fusing point, melting enthalpy.Three, crystallization: use DSC, can test Tc and the crystallization heat content of crystal, DSC is the Tc the most accurately measuring method of study sample under different experimental conditions.Four, phase transition temperature: when solid-state phase changes, the transformation of material recurring structure in heating and cooling process is often accompanied by the variation of heat.Utilize DSC can obtain accurately the information such as heat of change of phase enthalpy, phase transition temperature.DSC can also research material in addition crystallinity, oxidation stability, specific heat, the characteristic of aspect such as solidify.
Wetting angle is analyzed, and is mainly used in measuring the contact angle of liquid to solid, i.e. the wellability of liquid to solid, the contact angle of the various liquid of such device measures to various materials.Can measurements and calculations surface tension/interfacial tension, CMC, droplet profile size, surface free energy.Can measure the contact angle of various liquid to various materials, such as bulk material, fibrous material, textile material etc.Research and production to industries such as oil, printing and dyeing, medicine, spraying, ore dressings has very important effect.The test mode of wetting angle has multiple, wherein pushes drop method, sessile drop method the most conventional.Fluid drips is fallen in specific substrate, is then taken and is obtained liquid profile in time and the variation of temperature by high-speed camera, and then by special software, final wetting angle value is measured, calculated to the picture of taking.
If can be in doing wetting angle experiment, in time and the DSC data of temperature variation, that will be more meaningful in synchronization gain.But, one, current DSC function both domestic and external is comparatively single, furnace binding is substantially all vertically, almost can not observe at side-wall hole, and the structure of DSC sensor also limits directly sample is observed at present.Two, the method for measuring at present both at home and abroad sample wetting angle has a variety of, is all often under the control of temperature program(me), to study sample wetting angle on some temperature spot over time, can not obtain the details of some crucial tr pts jumping characteristic.If DSC curve and the wetting angle curve changing with temperature, time can be combined being very large breakthrough, can ideally explain the phenomenon of curve in the time of flex point, for a new thinking is expanded out in the research in the field of solidifying.
Summary of the invention
For the deficiencies in the prior art part, the object of this invention is to provide the device of a kind of synchro measure metal at suprabasil wetting angle and DSC curve, measurement mechanism is easy and simple to handle, and data measured is accurately and reliably.
Be directed to the requirement of above-mentioned implementation method, designed special DSC furnace binding, sensor construction, the integrated apparatus of taking pictures fast.This device with the basis of traditional Wetness Angle Measuring Instrument at geometric similarity on, reduced the scale of device, and stable horizontal body of heater realized DSC temperature measurement function.Can synchronization gain contact angle and accurate DSC data in the process of cooling that heats up.Mainly comprise vacuum and gas charging system, horizontal heating furnace body system, the observing system of taking pictures, DSC system, data acquisition processing system and gas blow pipe, described vacuum and gas charging system mainly comprise vacuum pump and gas blow pipe, the whole body of heater of this device is in sealing state, body of heater can be evacuated to vacuum by vacuum pump, can be filled with protective atmosphere to body of heater through gas blow pipe by source of the gas and take office will and spirit pressure, through repeatedly bleeding and inflating, can make to have pure protective atmosphere environment in stove, also can directly under vacuum condition, test; Described horizontal heating furnace body system is made up of sensor, calandria, heat-insulation layer and furnace shell, described sensor is measured the temperature of sample in real time, and according to the real-time thermal value of temperature information control calandria, make the temperature of sample according to the heating-cooling change of program of setting, complete fusing, the process of setting of metal; The described observing system of taking pictures is made up of additional light source and quick video camera, additional light source is to the light of stove vivo sample direction transmitting characteristic frequency, the profile of the sharp image, particularly sample that the quick video camera that only receives this kind of light photographed sample and vary with temperature each time point after fusing; Described DSC system is mainly made up of DSC sample sensor and DSC reference substance sensor, identical substrate one and substrate two are put in respectively on DSC sample sensor and DSC reference substance sensor, again sample is placed in substrate one, substrate two is as reference substance, and in experimentation, DSC system is measured the temperature data of sample and substrate two in real time; Described data acquisition processing system connects observing system and the DSC system of taking pictures, according to the sample profile photo obtaining from the observing system of taking pictures, calculate the wetting angle data after sample fusing, according to the real time temperature data of the sample obtaining from DSC system and substrate two, draw DSC curve, actual temp point when accurately calculating sample and melt, solidify according to the endothermic peak on DSC curve and exothermic peak, reaches the object of synchro measure metal at suprabasil wetting angle and DSC curve.
Above-mentioned horizontal body of heater can horizontally slip along slide rail, slides to right side and exposes sensor, can load sample, substrate one and substrate two, slides to left side fire door and contacts furnace wall and sealed, and whole body of heater keeps sealing state.
Above-mentioned body of heater provides circulating water by cooling-water machine, and cooling-water machine water yield size is preferably 8-20L/min, and temperature range is preferably 10-25 DEG C.
The light that above-mentioned additional light source sends is preferably He-Ne laser.
The frequency acquisition of above-mentioned quick video camera is preferably 10-120 frame/second.
The experimental temperature scope of above-mentioned body of heater is preferably 0 DEG C-1600 DEG C, and temperature rate is preferably 1-30 DEG C/min, and temperature resolution is preferably ± 0.1 DEG C, and temperature accuracy is preferably ± and 0.3 DEG C.
Be preferably ± 10～± 1000uV of the differential thermal range of above-mentioned DSC system, differential thermal sensitivity is preferably 0.01 uV, and DSC noise is preferably 0.01uW.
The maximum vacuum of above-mentioned body of heater is preferably 4x10
-4pa.
The material of above-mentioned DSC sample sensor and DSC reference substance sensor is preferably selected platinum.
Above-mentioned body of heater is preferably in vacuum environment (can be low to moderate 10
-4and be filled with under the condition of various protective atmospheres (as argon gas and nitrogen) and test Pa).
The sliding scale of above-mentioned body of heater on guide rail is preferably 0-40cm.
Advantage of the present invention is as follows:
(1) obtain the suction heat release situation of sample in sample substrate by the meticulous calorimetric means of DSC, overcome traditional Wetness Angle Measuring Instrument and cannot catch the shortcoming of sample thermal effect.
(2) realize in the process heating up, lower the temperature and observe the pattern of sample and sample substrate by Wetness Angle Measuring Instrument, and measure its wetting angle, broken through the not visible limitation of traditional DSC.
Brief description of the drawings
Fig. 1 is the device of synchro measure metal at suprabasil wetting angle and DSC curve.
In figure: 1. quick video camera, 2. heat-insulation layer, 3. furnace shell, 4. gas blow pipe, 5. sensor, 6. substrate one, 7. sample, 8.DSC sample sensor, 9. substrate two, 10.DSC reference substance sensor, 11. heaters, 12. additional light sources, 13. data acquisition logging systems, 14. slide rails, 15. cooling-water machines, 16. vacuum pumps.
Fig. 2 is the DSC curve that uses the measured pure iron heating and cooling of this device.
Fig. 3 is the contour image using after the measured pure iron fusing of this device.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiment.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtaining under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment:
Referring to Fig. 1, synchro measure metal of the present invention, at the device of suprabasil wetting angle and DSC curve, comprises quick video camera 1, heat-insulation layer 2, furnace shell 3, gas blow pipe 4, sensor 5, substrate 1, sample 7, DSC sample sensor 8, substrate 29, DSC reference substance sensor 10, calandria 11, additional light source 12, data acquisition logging system 13, slide rail 14, cooling-water machine 15 and vacuum pump 16.
First opening cooling-water machine, body of heater is sliped off from slide rail, is Φ 8x0.5 and the Al that is oriented to (0001) two sizes
2o
3single crystal substrates is respectively placed on DSC sample sensor and DSC reference substance sensor, then the pure iron sample of the square bodily form of heavy 100mg is placed on DSC sample sensor, and body of heater closes.Body of heater is pumped to 5x10 with vacuum pump
-4pa, then be filled with high-purity argon gas to atmospheric pressure, the inflation three times of repeatedly bleeding, makes to be full of high-purity argon atmosphere and an atmospheric pressure of maintenance in stove, body of heater is passed into high-purity argon on one side subsequently, discharges furnace gas on one side with same traffic, keeps mobile atmosphere.
Setting program, makes body of heater arrive 1580 DEG C from room temperature with the heating rate of 20 DEG C/min, then drops to room temperature with the speed of 20 DEG C/min, and in whole experimentation, video camera is taken a photo, DSC system real-time rendering DSC curve every 1 DEG C fast.Fig. 2 is the pure iron that obtains in the experimentation Al in (0001) orientation
2o
3dSC curve in single crystal substrates, Fig. 3 is that the iron that pure iron photographs in the time cooling to 1553 DEG C drips photo, recording its wetting angle by software is 116.27 °.
Claims (10)
1. a synchro measure metal is at the device of suprabasil wetting angle and DSC curve, mainly comprise vacuum and gas charging system, horizontal heating furnace body system, the observing system of taking pictures, DSC system, data acquisition processing system (13), described vacuum and gas charging system mainly comprise vacuum pump (16) and gas blow pipe (4), described horizontal heating furnace body system is by sensor (5), calandria (11), heat-insulation layer (2) and furnace shell (3) composition, the described observing system of taking pictures is made up of additional light source (12) and quick video camera (1), take light path through sample (7), described DSC system is mainly made up of DSC sample sensor (8) and DSC reference substance sensor (10), substrate one (6) and substrate two (9) are put in respectively on DSC sample sensor (8) and DSC reference substance sensor (10), sample (7) is placed in substrate one (6), described data acquisition processing system (13) connects observing system and the DSC system of taking pictures.
2. the device at suprabasil wetting angle and DSC curve according to the synchro measure metal described in claims 1, it is characterized in that, whole horizontal body of heater can horizontally slip along slide rail (14), slide to right side and expose sensor (5), slide to fire door contact furnace wall, left side and after being sealed, whole body of heater keeps sealing state.
3. the device at suprabasil wetting angle and DSC curve according to the synchro measure metal described in claims 1, it is characterized in that, provide circulating water by cooling-water machine (15) to body of heater, cooling-water machine (15) water yield size is 8-20L/min, and temperature range is 10-25 DEG C.
4. the device at suprabasil wetting angle and DSC curve according to the synchro measure metal described in any one in claim 1～3, it is characterized in that, the light that described additional light source (12) sends is He-Ne laser, and the frequency acquisition of described quick video camera (1) is 10-120 frame/second.
5. the device at suprabasil wetting angle and DSC curve according to the synchro measure metal described in any one in claim 1～3, it is characterized in that, the experimental temperature scope of body of heater is 0 DEG C-1600 DEG C, temperature rate is 1-30 DEG C/min, the temperature resolution of body of heater is ± 0.1 DEG C, and temperature accuracy is ± 0.3 DEG C.
6. the device at suprabasil wetting angle and DSC curve according to the synchro measure metal described in any one in claim 1～3, it is characterized in that, the differential thermal range of DSC system is ± 10～± 1000uV, and differential thermal sensitivity is 0.01 uV, and DSC noise is 0.01uW.
7. the device at suprabasil wetting angle and DSC curve according to the synchro measure metal described in any one in claim 1～3, is characterized in that, the maximum vacuum of body of heater is 4x10
-4pa.
8. the device at suprabasil wetting angle and DSC curve according to the synchro measure metal described in any one in claim 1～3, is characterized in that, the material selection platinum of DSC sample sensor (8) and DSC reference substance sensor (10).
9. the device at suprabasil wetting angle and DSC curve according to the synchro measure metal described in any one in claim 1～3, is characterized in that, body of heater (is low to moderate 4x10 most in vacuum environment
-4and be filled with under the condition of various protective atmospheres (as argon gas and nitrogen) and test Pa).
10. the device at suprabasil wetting angle and DSC curve according to the synchro measure metal described in any one in claim 1～3, is characterized in that, the sliding scale of body of heater on guide rail (14) is 0-40cm.
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| CN201410147683.3A CN103954534A (en) | 2014-04-14 | 2014-04-14 | Device for synchronously measuring wetting angle and differential scanning calorimetry (DSC) curve of metals on substrate |
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| CN201410147683.3A CN103954534A (en) | 2014-04-14 | 2014-04-14 | Device for synchronously measuring wetting angle and differential scanning calorimetry (DSC) curve of metals on substrate |
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Cited By (6)
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| CN106181101A (en) * | 2016-07-13 | 2016-12-07 | 江苏科技大学 | A kind of observation instantaneous high-temperature wetting areas assay device |
| CN107505231A (en) * | 2017-09-04 | 2017-12-22 | 南昌大学 | The equipment at triple line movement and dynamic moisture angle during a kind of real-time synchronization monitoring brazing filler metal melts |
| CN108088871A (en) * | 2018-01-10 | 2018-05-29 | 上海工程技术大学 | A kind of test device and its test method of fiber assembly heat storage performance |
| CN109142406A (en) * | 2018-09-07 | 2019-01-04 | 上海大学 | A kind of metal phase change research device |
| CN112748108A (en) * | 2020-12-15 | 2021-05-04 | 中国科学院国家空间科学中心 | Real-time measuring system for wettability parameter of space high-temperature melt material |
| CN113324877A (en) * | 2021-06-01 | 2021-08-31 | 上海应用技术大学 | Ultra-low oxygen partial pressure sealing chamber seat dropping method for observing wetting angle of aluminum and magnesium melt |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106181101A (en) * | 2016-07-13 | 2016-12-07 | 江苏科技大学 | A kind of observation instantaneous high-temperature wetting areas assay device |
| CN107505231A (en) * | 2017-09-04 | 2017-12-22 | 南昌大学 | The equipment at triple line movement and dynamic moisture angle during a kind of real-time synchronization monitoring brazing filler metal melts |
| CN108088871A (en) * | 2018-01-10 | 2018-05-29 | 上海工程技术大学 | A kind of test device and its test method of fiber assembly heat storage performance |
| CN108088871B (en) * | 2018-01-10 | 2024-03-08 | 上海工程技术大学 | Device and method for testing heat storage performance of fiber aggregate |
| CN109142406A (en) * | 2018-09-07 | 2019-01-04 | 上海大学 | A kind of metal phase change research device |
| CN112748108A (en) * | 2020-12-15 | 2021-05-04 | 中国科学院国家空间科学中心 | Real-time measuring system for wettability parameter of space high-temperature melt material |
| CN113324877A (en) * | 2021-06-01 | 2021-08-31 | 上海应用技术大学 | Ultra-low oxygen partial pressure sealing chamber seat dropping method for observing wetting angle of aluminum and magnesium melt |
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Application publication date: 20140730 |