CN103994952B - The device of extrusion synchro measure metal angle of wetting and DSC curve - Google Patents
The device of extrusion synchro measure metal angle of wetting and DSC curve Download PDFInfo
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- CN103994952B CN103994952B CN201410212036.6A CN201410212036A CN103994952B CN 103994952 B CN103994952 B CN 103994952B CN 201410212036 A CN201410212036 A CN 201410212036A CN 103994952 B CN103994952 B CN 103994952B
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Abstract
The present invention relates to a kind of extrusion synchro measure metal angle of wetting and the device of DSC curve, belong to metal freezing technical field.Device of the present invention mainly includes horizontal heating furnace body system, observing system of taking pictures, vacuum and inflation system, DSC systems, data acquisition logging system and extruding drippage system.The present apparatus has not only gathered DSC equipment and the function of Wetness Angle Measuring Instrument, and extruding drippage system through the hole on body of heater and and furnace sealing, keep vertical and bottom face DSC sample sensor pallets.In experimentation, metal melts in alundum tube, is then extruded to drop onto and is placed in the substrate on DSC sample sensor pallets, effectively the oxide-film of metal surface has been filtered out during drippage, so as to more accurately measure the data of its transformation temperature and angle of wetting.
Description
Technical field
The present invention relates to a kind of extrusion synchro measure metal angle of wetting and the device of DSC curve, belong to metal freezing technology
Field.
Background technology
Modern heat analysis refers under temperature programmed control, the class technology that the physical property of measurement of species is varied with temperature.People
Thermophysical property by detecting sample itself with the change of temperature or time, to study molecular structure, the state of aggregation of material
Structure, change of molecular motion etc..DSC be research under temperature program(me) control its physical quantity of material variation with temperature (Δ Q and
Δ H) change, i.e., by the change of programed temperature, while temperature change, measurement sample and reference substance difference power
The relation of (rate of heat flow) and temperature.
By DSC, we can do the research of following several respects.First, the glass transition of sample：In amorphous polymer
（, along with the change of specific heat, the change of baseline height is presented as on DSC curve by glassy transition for meeting during elastomeric state
Change（The inflection of curve）.Thus analyzed, you can obtain the glass transition temperature and specific heat intensity of variation of material.2nd, melt
Melt：The melting of crystal is first order phase transition, along with endothermic effect in melting process., can be to the endothermic effect using DSC
It is measured, obtains the information such as fusing point, melting enthalpy.3rd, crystallize：Using DSC, crystallization temperature and the crystallization of crystal can be tested
Heat content, DSC is the most accurate measuring method of crystallization temperature of the study sample under different experimental conditions.4th, phase transition temperature：Phase
Change is the transformation of material recurring structure in heating and cooling process, and it is usually associated with the change of heat.Can be accurately using DSC
Obtain the information such as phase in version heat content, phase transition temperature.Other DSC can also the crystallinity of research material, oxidation stability, ratio
Characteristic in terms of heat, solidification.
Angle of wetting is analyzed, and is mainly used in measuring the wellability of the contact angle, i.e. liquid versus solid of liquid versus solid, such instrument
Device can measure contact angle of the various liquid to various materials.Measurable and gauging surface tension force/interfacial tension, CMC, droplet profile
Size, surface free energy.Various liquid can be measured to the contact angle of various materials, such as bulk material, fibrous material, weaving
Material etc..There is very important effect to the research and production of the industries such as oil, printing and dyeing, medicine, spraying, ore dressing.The survey of angle of wetting
Examination mode has a variety of, wherein extruding drop method, sessile drop method are the most commonly used.Liquid is dropped onto on specific matrix, then by a high speed
Video camera shoots the change for obtaining liquid profile with time and temperature, and then the picture of shooting is carried out by special software again
Measurement, calculating obtain final wetting angle value.
If can be while angle of wetting experiment is done, synchronization gain be with time and the DSC data of temperature change, and that will
It is more meaningful.However, one, current DSC functions both domestic and external are more single, it is vertical that furnace binding is substantially, almost
It can not be observed in side-wall hole, and the structure of DSC sensors also limits directly sample is observed at present.2nd, current state
The method at interior external pelivimetry sample wetness angle has many kinds, is all often that some temperature are studied under the control of temperature program(me) jumping characteristic
The angle of wetting change for the sample that changes with time is spent on point, it is impossible to obtain the details of some Key Transformation points.Therefore by DSC
It will be very big breakthrough that curve combines with the wetting angular curve with temperature, time change, can ideally explain that curve is being turned
Phenomenon during point.
And current DSC and Wetness Angle Measuring Instrument are that sample is placed on into measuring table in advance in experimentation, nearly all
On substrate on, allow sample to heat fusing with body of heater, obtain its DSC curve or wetting angular data, but this method exist
Following shortcoming：In temperature-rise period, although the oxygen content in protective atmosphere is extremely low, but due to sample can be stopped in high temperature section it is longer
Time, oxidation still easily occurs, and causes the place of sample surfaces and sample and substrate contact to generate oxide-film, the DSC measured
Situation in curve and wetting angular data and imagination has relatively large deviation, and the device that the present invention is provided overcomes this problem,
Metal accurate angle of wetting and phase transformation point data in substrate can precisely be obtained.
The content of the invention
In view of the deficiencies of the prior art, it is an object of the invention to provide a kind of extrusion synchro measure metal angle of wetting
With the device of DSC curve, measurement apparatus is easily operated, and data measured is accurately credible.
Be directed to the requirement of above-mentioned implementation method, devise special DSC furnace bindings, sensor construction, snapshots,
Extrude the integrated apparatus such as drippage system.The present apparatus on the basis of geometric similarity, reduces dress with traditional Wetness Angle Measuring Instrument
The complexity put, and the device of extruding drippage is combined, DSC function is realized in stable horizontal body of heater, in the mistake of experiment
Can synchronization gain metal accurate contact angle and phase transformation point data in substrate in journey.Mainly include horizontal heating furnace body system,
DSC systems, observing system of taking pictures, vacuum and inflation system, data acquisition logging system and extruding drippage system, the level add
Hot system of bf body is made up of sensor, calandria, heat-insulation layer and furnace shell, and calandria produces heat in experimentation, and passes through
Sensor Real-time Feedback temperature information, makes the heating and cooling process of sample be run in strict accordance with setting program；The DSC systems are main
It is made up of DSC sample sensors pallet and DSC reference sensor pallets, DSC sample sensors pallet and DSC reference sensor supports
Disk keeps level and each on DSC sample sensors pallet and DSC reference sensor pallets in sustained height, experimentation
A piece of identical substrate is placed, when body of heater rises to target temperature, metal sample is dropped on DSC sample sensor pallets
In substrate, in temperature-fall period, heat can be released when metal sample solidifies, so that generation one is small between causing two pallets
Temperature difference, and can be accurately reflected on DSC curve, curve importing software can be measured into the accurate transformation temperature of sample；It is described
Observing system of taking pictures is made up of laser generator and fast camera, the pickup light curb horizontal direction of the system, and passes through DSC
Sample sensor pallet, it is ensured that in experimentation after sample drippage, accurately photograph the contour images of spherical sample, will scheme
As importing in software, its accurately wetting angular data can be measured；The vacuum and inflation system mainly include vavuum pump and stove
Body air inlet pipe, vacuum pumps up the effect for extracting furnace gas out, and body of heater air inlet pipe rises and is filled with protective atmosphere（Such as argon gas, nitrogen）'s
Effect；The data acquisition logging system connects real-time acquisition and recording sample in observing system and the DSC systems of taking pictures, experimentation
DSC curve and wetting angular data；The extruding drippage system keeps sealing through the hole on body of heater and with body of heater, keeps hanging down
It is straight and bottom faces DSC sample sensor pallets, it is ensured that sample is accurately dropped on DSC sample sensor pallets during extruding
Substrate center.
Extruding drippage system and body of heater realize that dynamic sealing is connected, and extruding drippage system is beaten by rotary handle, pressure ram, bottom
Foraminate alundum tube composition, pressure ram is located inside alundum tube, and sample is previously placed between alundum tube and pressure ram, and and sample
The pressure ram bottom material of product contact is graphite, rotates rotary handle, pressure ram can be made to be moved up and down in alundum tube, is tested
During, with the progress of heating, the metal sample in alundum tube can gradually melt, but due to its surface oxidation layer tension compared with
Greatly, metal bath will not flow out from aperture, when being continuously heating to target temperature, rotate rotary handle, pressure ram is oppressed metal
Melt, allows it to be flowed out from aperture, drops in the substrate on DSC sample sensor pallets, during drippage, oxide-film is by aperture
Filtering, the molten drop surface fallen down be not present oxide-film, so as to ensure the DSC curve measured and wetting angular data can
By property.
Body of heater connecting sliding rail, whole horizontal body of heater can horizontally slip along slide rail, slide to right side and expose sensor, now can
Substrate is enough loaded, leftmost side bell is slided to and is in close contact sealing ring and is enclosed whole body of heater, keep air-tight state, this state
Under can be tested.
Cooling-water machine connects body of heater, and cooling circulating water is provided for it, and the water size of cooling-water machine is preferably 8-20L/min,
Water temperature range is preferably 10-25 DEG C.
The light that laser generator is sent is preferably He-Ne laser, and the frequency acquisition of fast camera is preferably 10-120
Frame/second, fast camera is preferably able to realize left-right and front-back continuous moving, and moving range is preferably 0-40mm.
Sensor is preferably with Type B thermocouple, and the operating temperature of body of heater is preferably 0-800 DEG C, and temperature rate is preferably
0.1-30 DEG C/s, temperature resolution is preferably ± 0.1 DEG C, and temperature accuracy is preferably ± 0.1 DEG C.
The differential thermal range of DSC systems is preferably ± 10- ± 1000uV, and differential thermal sensitivity is preferably 0.01 uV, DSC noises
Preferably 0.01uW.
It is evacuated by vavuum pump, the maximum vacuum of body of heater is preferably 5x10-4Pa。
Body of heater is evacuated and charge operation by controlling vavuum pump and body of heater air inlet pipe to realize, it is desirable to realize
Under vacuum or the angle of wetting under the inert atmosphere protection such as argon gas, nitrogen and transformation temperature measurement.
Alundum tube bottom part aperture diameter is preferably 0.3-1mm, and pressure ram is moving up and down to preferably range from 0-25mm.
Brief description of the drawings
Fig. 1 is the device of extrusion synchro measure metal angle of wetting and DSC curve.
In figure：1. cooling-water machine, 2. fast cameras, 3. bells, 4. sealing rings, 5. body of heater air inlet pipe, 6. sensors, 7. squeeze
Press drippage system, 8.DSC sample sensor pallets, 9..DSC reference sensor pallets, 10. laser generators, 11. data acquisitions
Record system, 12. vavuum pumps, 13. calandrias, 14. heat-insulation layers, 15. furnace shells, 16. slide rails.
Fig. 2 is the DSC curve before and after being dripped using the fine aluminium measured by the device.
Fig. 3 is to drip contour images using the aluminium after the fine aluminium drippage measured by the 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 carried out clear, complete
Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.It is based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of creative work is not made
Embodiment, belongs to the scope of protection of the invention.
Embodiment
Referring to Fig. 1, the device of extrusion synchro measure metal angle of wetting of the present invention and DSC curve mainly adds including level
Hot system of bf body, DSC systems, observing system of taking pictures, vacuum and inflation system, data acquisition logging system 11 and extruding drippage system
System 7, the horizontal heating furnace body system is made up of sensor 6, calandria 13, heat-insulation layer 14 and furnace shell 15, the DSC systems
Mainly it is made up of DSC sample sensors pallet 8 and DSC reference sensors pallet 9, DSC sample sensors pallet 8 and DSC references
Sensor pallet 9 keeps level and in sustained height, and the observing system of taking pictures is by laser generator 10 and fast camera 2
Composition, the pickup light curb horizontal direction of the system, and by DSC sample sensors pallet 8, the vacuum and inflation system master
To include vavuum pump 12 and body of heater air inlet pipe 5, the data acquisition logging system 11 connects observing system and the DSC systems of taking pictures,
The extruding drippage system 7 keeps sealing through the hole on body of heater and with body of heater, keeps vertical and bottom faces DSC samples
Sensor pallet 8.
Extruding drippage system 7 and body of heater realize that dynamic sealing is connected, and extruding drippage system 7 is by rotary handle, pressure ram, bottom
The alundum tube composition being with holes, pressure ram is located inside alundum tube, and sample is previously placed between alundum tube and pressure ram, and and
The pressure ram bottom material of sample contact is graphite, rotates rotary handle, pressure ram is moved up and down in alundum tube.
Body of heater connecting sliding rail 16, whole horizontal stove physical efficiency horizontally slips along slide rail 16, slides to right side and exposes sensor 6,
Slide to leftmost side bell 3 to be in close contact sealing ring 4 and be enclosed whole body of heater, keep air-tight state.
Cooling-water machine 1 connects body of heater, and cooling circulating water is provided for it, and the water size of cooling-water machine 1 is 8-20L/min, water
Warm scope is 10-25 DEG C.
The light that the laser generator 10 is sent is He-Ne laser, and the frequency acquisition of the fast camera 2 is 10-
120 frames/second, fast camera 2 can realize left-right and front-back continuous moving, and moving range is 0-40mm.
Sensor 6 uses Type B thermocouple, and the operating temperature of body of heater is 0-800 DEG C, and temperature rate is 0.1-30 DEG C/s,
Temperature resolution is ± 0.1 DEG C, and temperature accuracy is ± 0.1 DEG C.
The differential thermal range of DSC systems is ± 10- ± 1000uV, and differential thermal sensitivity is 0.01 uV, and DSC noises are 0.01uW
。
It is evacuated by vavuum pump 12, the maximum vacuum of body of heater is 5 × 10-4Pa。
Body of heater is evacuated and charge operation, is realized true by controlling vavuum pump 12 and body of heater air inlet pipe 5 to realize
Angle of wetting and transformation temperature measurement under empty condition or under inert atmosphere protection.
Alundum tube bottom part aperture diameter is 0.3-1mm, and pressure ram scope moving up and down is 0-25mm.
Using the present invention and its special purpose device, the experiment done for rafifinal is completed, its experimental conditions and result are chatted
State as follows：
Cooling-water machine is opened, then high-purity aluminium block of 1 gram of weight is put into extruding drippage system, and two panels is oriented to
（0001）Disc Al2O3Single-chip (size is Φ 8x0.5) is individually placed to DSC sample sensors pallet and DSC references sensing
On device pallet, closed body of heater.With the air in vacuum pumping body of heater, high-purity argon gas is then allowed to flow into stove from body of heater air inlet pipe
Body, then open the gas in vacuum pumped stove, repeatedly after prepurging 3 times, allows high-purity argon gas constantly to be flowed into from body of heater air inlet pipe,
And be discharged to identical flow velocity for normal pressure in outdoor, holding furnace body, after after steady air current, startup setting program is by body of heater with 20
DEG C/min speed is warming up to 800 DEG C, and is incubated 30min.Then operation extruding drippage system, rotates rotary handle, allows aluminium liquid
Extrude, and drop onto on the single-chip on DSC sample sensor pallets, the drippage and liquid of sample from the aperture under alundum tube
The angle of wetting situation of drop is recorded in real time by data acquisition logging system, after soaking time terminates, and body of heater starts with 20 DEG C/min's
Speed cools, and DSC curve produces exothermic peak when being down to sample solidification, and the position of exothermic peak, size and shape reflect sample
Solidify the physico-chemical parameters such as transformation temperature.Fig. 2 is the DSC curve before and after being dripped using the fine aluminium measured by the device, and Fig. 3 should to use
Aluminium drop contour images after fine aluminium drippage measured by device.
Claims (8)
1. the device of a kind of extrusion synchro measure metal angle of wetting and DSC curve, mainly including horizontal heating furnace body system,
DSC systems, observing system of taking pictures, vacuum and inflation system, data acquisition logging system (11) and extruding drippage system (7), institute
State horizontal heating furnace body system to be made up of sensor (6), calandria (13), heat-insulation layer (14) and furnace shell (15), the DSC systems
Mainly be made up of DSC sample sensors pallet (8) and DSC reference sensors pallet (9), DSC sample sensors pallet (8) and
DSC reference sensors pallet (9) keeps level and in sustained height, the observing system of taking pictures by laser generator (10) and
Fast camera (2) is constituted, the pickup light curb horizontal direction of the system, and by DSC sample sensors pallet (8), it is described
Vacuum and inflation system mainly include vavuum pump (12) and body of heater air inlet pipe (5), data acquisition logging system (11) connection
Observing system of taking pictures and DSC systems, the extruding drippage system (7) keep sealing through the hole on body of heater and with body of heater, protect
Hold vertical and bottom and face DSC sample sensors pallet (8), the extruding drippage system (7) and body of heater realize that dynamic sealing connects
Connect, the alundum tube that extruding drippage system (7) is with holes by rotary handle, pressure ram, bottom is constituted, pressure ram is located at alundum tube
Inside, sample is previously placed between alundum tube and pressure ram, and the pressure ram bottom material contacted with sample is graphite, rotates rotation
Handle is changed hands, pressure ram is moved up and down in alundum tube, the body of heater connecting sliding rail (16), whole horizontal stove physical efficiency is along slide rail
(16) horizontally slip, slide to right side and expose sensor (6), slide to leftmost side bell (3) and be in close contact sealing ring (4) and make whole
Body of heater is enclosed, and keeps air-tight state.
2. the device of extrusion synchro measure metal angle of wetting according to claim 1 and DSC curve, it is characterised in that
Cooling-water machine (1) connects body of heater, and cooling circulating water is provided for it, and the water size of cooling-water machine (1) is 8-20L/min, water temperature model
Enclose for 10-25 DEG C.
3. the device of extrusion synchro measure metal angle of wetting according to claim 1 and DSC curve, it is characterised in that
The light that the laser generator (10) sends is He-Ne laser, and the frequency acquisition of the fast camera (2) is 10-120
Frame/second, fast camera (2) can realize left-right and front-back continuous moving, and moving range is 0-40mm.
4. the device of extrusion synchro measure metal angle of wetting according to claim 1 and DSC curve, it is characterised in that
Sensor (6) uses Type B thermocouple, and the operating temperature of body of heater is 0-800 DEG C, and temperature rate is 0.1-30 DEG C/s, temperature point
Resolution is ± 0.1 DEG C, and temperature accuracy is ± 0.1 DEG C.
5. the device of extrusion synchro measure metal angle of wetting according to claim 1 and DSC curve, it is characterised in that
The differential thermal range of DSC systems is ± 10~± 1000uV, and differential thermal sensitivity is 0.01uV, and DSC noises are 0.01uW.
6. the device of extrusion synchro measure metal angle of wetting according to claim 1 and DSC curve, it is characterised in that
It is evacuated by vavuum pump (12), the maximum vacuum of body of heater is 5 × 10-4Pa。
7. the device of extrusion synchro measure metal angle of wetting according to claim 1 and DSC curve, it is characterised in that
Body of heater is evacuated and charge operation, is realized in vacuum bar by controlling vavuum pump (12) and body of heater air inlet pipe (5) to realize
Angle of wetting and transformation temperature measurement under part or under inert atmosphere protection.
8. the device of extrusion synchro measure metal angle of wetting according to claim 1 and DSC curve, it is characterised in that
Alundum tube bottom part aperture diameter is 0.3-1mm, and pressure ram scope moving up and down is 0-25mm.
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| CN105181735B (en) * | 2015-10-21 | 2019-03-08 | 广州纤维产品检测研究院 | The discrimination method of composite fibre |
| CN105954144A (en) * | 2016-05-13 | 2016-09-21 | 江苏科技大学 | Density measurement equipment and method for variable-temperature metal |
| CN106706473B (en) * | 2017-01-13 | 2019-04-02 | 浙江师范大学 | A kind of device of quick obtaining polymer melt surface contact angle |
| CN107796737B (en) * | 2017-09-15 | 2020-04-17 | 深圳大学 | Metal melt wetting test device and substrate wetting performance test method |
| CN109142406B (en) * | 2018-09-07 | 2020-10-16 | 上海大学 | Metal phase transition research device |
| CN109443251A (en) * | 2018-12-18 | 2019-03-08 | 上海大恒光学精密机械有限公司 | The test device and measurement method of high-temp solid material at high temperature contact angle |
| CN109540742A (en) * | 2018-12-20 | 2019-03-29 | 山东大学 | A kind of multifunctional access feeler in-situ test pond and its application for measuring surface wettability matter |
| CN112903540A (en) * | 2021-01-14 | 2021-06-04 | 湖南师范大学 | High-temperature liquid drop contact angle testing device and testing method |
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| JP2001183319A (en) * | 1999-12-27 | 2001-07-06 | Shimadzu Corp | Thermal analyzer |
| CN101986134B (en) * | 2010-09-20 | 2012-08-15 | 华北电力大学（保定） | Automatic detection method of static contact angle |
| US8858070B2 (en) * | 2011-06-03 | 2014-10-14 | The Aerospace Corporation | System and method for measuring glass transition temperature |
| CN102353620B (en) * | 2011-06-21 | 2013-09-25 | 吉林大学 | Apparatus and method for determining high temperature wettability |
| CN103128454B (en) * | 2013-02-01 | 2015-07-29 | 河南科技大学 | Improve the method for solder wetting, device and test experience method and apparatus thereof |
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