CN101692011A - Method for synchronously measuring temperature and roll angle of droplet by controlling temperature and humidity - Google Patents
Method for synchronously measuring temperature and roll angle of droplet by controlling temperature and humidity Download PDFInfo
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Abstract
The invention belongs to the technical field of chemical measurement. A temperature and humidity control system is adopted to accurately control the environmental conditions in a sample case, namely the temperature ranges from minus 80 DEG C to plus 300 DEG C and the accuracy is +/-0.1 DEG C, the relative humidity ranges from 0% to 100% and the accuracy is +/-2%-+/-5%. A driver is adopted to accurately control the speed and angle of rotation, namely the rotating speed is 0.01 degree/S-10 degrees/S, the measurement ranges of the roll angle, advance angle and receding angle are between minus 180 degrees and plus 180 degrees and the accuracy is +/-0.01 degree. A high-speed data acquisition system and a high-speed camera system are adopted to synchronously measure the temperature and profile image of a droplet accurately. The sampling frequency of the temperature can be as high as 1MHz and the sampling speed of the image can reach 420 frames/s. Sample data are transmitted to a computing system through data lines and the temperature of the droplet is obtained. Software is adopted to analyze the image to obtain the temperature, roll angle, advance angle and receding angle of the droplet. The device has simple operation, high testing accuracy and good repeatability of experimental results and is suitable for synchronously measuring the temperature, roll angle, advance angle, receding angle and lag angle under the conditions of wide temperature and humidity ranges.
Description
Technical field
The present invention relates to a kind of wide temperature territory, the device of synchro measure drop temperature and roll angle belongs to technical field of chemical measurement under the full damp condition.
Background technology
Wetting phenomena is the surface of solid surface structure and properties, liquid and the macro manifestations of microscopic characteristics such as interfacial property and solid-liquid two-phase intermolecular interaction.The research of wetting phenomena can provide Useful Information for understanding nature of solid surface, and surface tension of liquid and contact angle are measured, can understand the interaction between solid-liquid, the liquid-liquid better, these interact for the cementability of understanding solid surface, material wetting state, biocompatibility and lubricity, and the wellability of liquid, washing performance, diffusion and absorption are very important.When adopting modern complex surfaces engineering to develop and improve liquid-solid surface, the measurement of surface tension and contact angle can provide needed information, so the measurement of different condition lower surface tension force and contact angle becomes the focus of research.
Natural plants blade (as lotus leaf, paddy rice leaf) often has super-hydrophobicity and special automatically cleaning effect, and promptly particle such as dust can be washed out from this surface at an easy rate by rainwater.This automatically cleaning effect is extremely important in actual applications, because the total surface that is exposed in the environment is can be contaminated, and super hydrophobic surface tends to lose its original hydrophobicity after contaminated.By research and imitation natural plants blade, the bionic surface that has good automatically cleaning effect in a large number emerges in an endless stream.If can more in depth understand the mechanism of action, for design with make novel super-hydrophobic, self-cleaning surface and have important directive function and practical value undoubtedly.Roll angle is the critical angle of drop when taking place to roll on inclined surface, and the moment of rolling, the advancing angle of drop, receding angle and drag angle are to judge the major criterion of dynamic super-hydrophobicity and automatically cleaning effect, therefore roll angle, advancing angle under the different condition, the measurement of receding angle and drag angle becomes the focus of research.
For example, application number 03121050.3, Granted publication number: the Chinese invention patent application of CN1265201C discloses the device of a kind of on-line measurement high-temperature fusant surface tension, contact angle and density.It is sent to sample in the quartzy Sealed casing pipe by sending into the sample quartz ampoule, with being about to quartzy Sealed casing pipe sealing, utilize the high temperature furnace pipe heated sample to fusion then, by the contour images of the online shooting melt of camera, start software and carry out Flame Image Process and calculate each numerical value such as surface tension, contact angle of melt constantly.But there is following defective in this device:
(1). lack the parts of measuring melt temperature in the quartzy Sealed casing pipe, only judge that by image viewing melt state is inaccurate;
(2). do not have accurately to control the device of temperature and humidity, the surface tension of measurement and contact angle numerical value are affected by environment bigger;
(3). can only measure the surface tension and the contact angle of melt, both limit the scope of application of temperature, limit the range of choice of test liquid again.
CAM 200 optics contact angle instrument are equipped with highly sensitive high speed and take the photograph phase system, can photograph the online dynamic image of high-quality drop, utilize the shape of software analysis drop to determine numerical value such as surface tension and contact angle simultaneously.Can measure room temperature condition and have a down dip angle in the roll angle of 0 °~+ 90 ° of range by installing manual tilting table additional, prior art is titration drop on sample earlier, and then tilting table is rotated to an angle.Such advantage is that baseline can remain horizontality, reduces greatly for the requirement of software development, but is to use such technology, can't write down the reciprocation between contact moment liquid and the sample surfaces.The drop temperature has than big-difference with environment temperature owing to be subjected to the influence of factors such as velocity of evaporation and phase transformation in addition, can't measure under existence conditions as one of important parameter.Tilting table only can change between 0~90 °, and making can't be to the limiting case of rolling---and hang phenomenon research by the feet, and only can the room temperature test have limited the measurement range of roll angle greatly, can't further investigate the dependence of roll angle for temperature.The humiture of surface tension and contact angle and measurement environment is closely related, sample bench directly is in communication with the outside, influenced seriously by extraneous humiture, measuring accuracy can't ensure, the drop temperature is owing to be subjected to the influence of factors such as velocity of evaporation and phase transformation in addition, have than big-difference with environment temperature, and under existence conditions, can't measure as one of important parameter.Can realize the measurement of room temperature~250 ℃ scope inside surface tension force and contact angle by installing electrical heating temperature control measuring chamber additional, but for high-volatile liquid because low temperature environment must be provided, under the prerequisite that reduces its rate of volatilization, measure, thereby limited the range of choice of test liquid greatly.
Summary of the invention
The objective of the invention is in order to break through the use restriction of existing measurement mechanism, realize the range of choice of temperature, humidity and the expansion test liquid of the accurate hierarchy of control, provide a kind of can be in wide temperature territory, in the full humidity range, the device of accurate temperature controlling degree, humidity synchro measure drop temperature, advancing angle, receding angle, roll angle, drag angle.
Technical scheme of the present invention:
A kind of wide temperature territory, full humidity range synchro measure drop temperature, advancing angle, receding angle, the device of roll angle, comprise: sample box (4), lifting table (3), frame (1), wheelwork (25), temperature-controlling system (12), the wet system (2) of control, high-speed data acquistion system (6), light source (9), take the photograph phase system (10) and computing system (11) at a high speed, high-speed data acquistion system, take the photograph phase system at a high speed, wheelwork, the wet system of control is connected with computing system by data line, sample box is fixed on the swinging mounting (30), be inserted on the lifting table by connecting link (24), light source with take the photograph mutually between the camera lens, lifting table can about, about, the front and back three-dimensional is adjusted position, light source, lifting table, high speed video system is installed on the frame.
The sample box shell is equipped with thermofin (23), and sample to be tested places sample box inner bottom part central authorities, thermopair (14) is housed in the sample box, micro thermocouple (7) is connected with high-speed data acquistion system; Humidity sensor (8) is connected with the wet system of control; Establish circulation line (15) in the sample box wall, the heat-conducting medium that flows in the pipeline, pipeline is connected with temperature-controlling system through conduit (13) by interface (17); Open gas piping import (18) on the sample box wall, outlet (19) is connected through the wet system of gas piping (20) and control; The rectangle window is opened in both sides, sample box opposite, and window is adorned double-deck optical glass (21), vacuumizes in the middle of the double glazing; Light source (9) illuminates test droplets (5) by window, and high speed video system obtains the test droplets view data by window, and light source, window, test droplets, pick-up lens are on the same level line; Temperature, humidity, view data, turn signal are connected with computing machine by data line, by temperature, humidity, wheelwork, the high speed video system of computer control sample box; The sample box loam cake is opened one and is connected narrow groove, and groove pours into soft silicon rubber, and test fluid is quantitatively dripped in sample to be tested (22) surface by syringe needle.
Described wheelwork comprises: swinging mounting (30), stepper motor (28), turbine (26), worm screw (27), driver (29); Stepper motor is realized the accurate speed governing of rolling by driver regulating impulse frequency, speed adjustable range is 0.01~10 °/s, can come pilot angle displacement realization roller tray accurately to locate by the regulating impulse number simultaneously, orientation range is-180 °~+ 180 °, precision pitch angle display precision and control accuracy be 0.01 ° ±.The static torque of stepper motor is 1200gcm, drives sample box by turbine and worm and rotates, and sample box is fixed on the swinging mounting, and swinging mounting is inserted on the lifting table by connecting link (24).
Described temperature-controlling system (12) comprising: low-temperature receiver, thermal source, conduit, heat-conducting medium, temperature measurement-control instrument; Temperature-controlling system (12) is connected with sample box interface (17) by conduit (13), temperature control method is that microcomputer temperature control+PID regulates, circulation by heat-conducting medium realizes temperature stabilization in the sample box, heat-conducting medium is selected according to actual probe temperature, the temperature control scope is-80 ℃~+ 300 ℃, precision is ± 0.1 ℃, and temperature fluctuation is ± 0.05 ℃.
The described control system (2) that wets comprising: dry gas, water, humidity measurement and control instrument; Relative humidity in humidity sensor (8) the monitoring sample box, the regulation and control of humidity measurement and control instrument are done, the humid gas flow proportional, to reach the condition of work of humidity requirement, the relative humidity scope is 0%~100%, (0~80%RH) precision is ± 2% to middle low humidity section, and (80~100%RH) precision are 5% to the high humility section.
Described high-speed data acquistion system (6) comprises high speed temperature data acquisition card, data processing software; The minisize thermoelectric dual diameter that connects is 0.01mm, or thinner, is used to measure the drop temperature, and test droplets (5) drops to the sample to be tested surface and contacts with micro thermocouple.Take the photograph phase system at a high speed and in record drop contour images, write down the drop temperature by high-speed data acquistion system (6).The thermopair (14) that connects is preset in the sample box respectively and in the wall, is used to measure in the sample box and the temperature of sample box wall, and the temperature sampling frequency is 1MHz, and resolution is 16bit.
Described high speed is taken the photograph phase system (10) and being comprised: high speed camcorder, image processing software; Taking the photograph phase velocity was 30~420 frame/seconds, and interframe is divided into 2ms ~ 1000s, and its camera lens is a focal length CCD camera lens far away, and enlargement factor is 0.7~20 times, image area 4 * 4mm
2Computer Image Processing software tool has high-speed capture, record, storage, analysis image function in real time.
Light source (9) is the background illumination of the blue look cold light source of LED.
Use temperature control provided by the invention wet synchro measure drop temperature, roll angle, advancing angle, receding angle device, can realize that temperature in the sample box is in the accurate control in 0%~100% scope of-80 ℃~+ 300 ℃ scopes, humidity, open high-speed data acquistion system, tourelle simultaneously, take the photograph phase system at a high speed by the data-triggered function, take the photograph phase system at a high speed and take drop in the clear contour images of specimen surface, by high speed temperature data collecting system record drop temperature variation.Image and temperature transfer to computing system by data line, and image is carried out match, obtain roll angle, advancing angle, the receding angle of drop under different humitures.Because the angle of inclination can reach 0.01 ° accurately, pitch velocity can be very slow (0.01 °/s), so can clearly observe the rolling phenomenon of drop when roller tray is light and slow to rotate.If know the required angle of inclination of experiment, then can set in advance the angle of camber roll platform, and then drop is dripped in sample surfaces, measure drop the free-running property on solid sample surface and with the reciprocation of sample.This device is simple to operate, temperature control and temperature measurement accuracy height, and the experimental result good reproducibility has been broken through the use restriction of existing measurement mechanism, can measure roll angle, advancing angle, receding angle under the different humitures, and the range of choice of test liquid is widened greatly also.
Use apparatus of the present invention, make the range of choice of test liquid extensive.
α: roll angle θ
A: advancing angle θ
D: receding angle
Apparatus of the present invention are measured water droplet roll angle, advancing angle, receding angle, drag angle at super hydrophobic surface under 40 ℃, RH=60% condition:
With the sample box sealing, 40 ℃ of temperature-controlling systems, control wetting phase are 60% to humidity, and behind the system stability, recording the sample box wall temperature by thermopair is 40.1 ℃, and temperature is 38.9 ℃ in the sample box, and relative humidity is 59%.Accurately drip 10.0 μ L water droplets by syringe to super hydrophobic surface, regulate lens focus and get a distinct image.The stepper motor rotational angle is preset as 0 °, velocity of rotation is preset as 0.05 °/s, open wheelwork simultaneously by the data-triggered function, high-speed data acquistion system and high speed are taken the photograph phase system, recording water droplet temperature by the 0.01mm micro thermocouple is 39.7 ℃, take the dynamic outline image that water droplet rotates with sample box at super hydrophobic surface by camera, transfer to computing system by data line, utilize software that image is analyzed, calculating water droplet roll angle at super hydrophobic surface under this temperature and humidity condition is 2.5 °, 158.4 ° of advancing angles, 148.6 ° of receding angles, 9.8 ° of drag angle.
Apparatus of the present invention are measured water droplet roll angle at super hydrophobic surface under 0 ℃, RH=85% condition:
With the sample box sealing, temperature control is 0 ℃, control is wet is 85%, and behind the system stability, the temperature that is recorded the sample box wall by thermopair is 0.0 ℃, and temperature is 1.1 ℃ in the sample box, and humidity is 86%.Accurately drip 10.0 μ L water droplets by syringe to super hydrophobic surface, regulate lens focus and get a distinct image.The stepper motor rotational angle is preset as 0 °, velocity of rotation is preset as 0.1 °/s, open wheelwork, high-speed data acquistion system simultaneously and take the photograph phase system at a high speed by the data-triggered function, recording water droplet temperature by the 0.01mm micro thermocouple is 0.7 ℃, take the dynamic outline image that water droplet moves with the sample box tumbler at super hydrophobic surface by camera, transfer to computing system by data line, utilize software that image is analyzed, calculating water droplet roll angle at super hydrophobic surface under this temperature and humidity condition is 59.1 °.
Apparatus of the present invention are measured water droplet roll angle at super hydrophobic surface under-10 ℃, RH=95% condition:
With the sample box sealing, temperature control is-10 ℃, control is wet is 95%, and behind the system stability, the temperature that is recorded the sample box wall by thermopair is-9.9 ℃, and temperature is-8.5 ℃ in the sample box, and humidity is 92%.Accurately drip 10.0 μ L water droplets by syringe to super hydrophobic surface, regulate lens focus and get a distinct image.The stepper motor rotational angle is adjusted into 0 °, velocity of rotation is preset as 1 °/s, open wheelwork, high-speed data acquistion system simultaneously and take the photograph phase system at a high speed by the data-triggered function, record water droplet temperature by the 0.01mm micro thermocouple and be-9.2 ℃, take the dynamic outline image that water droplet rotates with sample box at super hydrophobic surface by camera, transfer to computing system by data line, utilize software that image is analyzed, calculate water droplet and can't roll at super hydrophobic surface under this temperature and humidity condition, state is for hanging by the feet.
Description of drawings
Fig. 1 is the contour shape synoptic diagram of water droplet in the roll angle of super-hydrophobic solid surface;
Fig. 2 is the device synoptic diagram of synchro measure drop temperature and roll angle under the wet condition of temperature control of the present invention.
Fig. 3 is sample box and the swinging mounting diagrammatic cross-section in apparatus of the present invention
Fig. 4 is the swinging mounting right view of apparatus of the present invention
The drawing explanation:
1: frame 2: the wet system 3 of control: lifting platform 4: sample box 5: test droplets 6: high-speed data extraction system 7: micro thermocouple 8: humidity sensor 9: light source 10: take the photograph at a high speed phase system 11: computing system 12: temperature-controlling system 13: conduit 14: thermocouple 15: circulation line 17: interface 18: import 19: outlet 20: gas piping 21: double-deck optical glass 22: sample 23: thermal insulation layer 24: connecting rod 25: tumbler 26: turbine 27: worm screw 28: stepper motor 29: driver 30 swinging mountings
Embodiment
Embodiment 1, water droplet under 40 ℃, RH=60% condition at roll angle, advancing angle, the receding angle of super-hydrophobic solid surface
Sample box is fixed on the swinging mounting, swinging mounting is inserted on the lifting table by connecting link, light source with take the photograph mutually between the camera lens, sample to be tested is placed by sample box inner bottom part central authorities, adjust the lifting table position, make light source, the sample box window, specimen surface, video camera (Basler A6021-2, Computar Telecentric, Germany) be positioned at same line, light source illuminates test droplets by window, high speed video system obtains the test droplets view data by window, the thermopair that is equipped with in the sample box, (Personal Daq/3000Series, LOtech USA) connect for micro thermocouple and high-speed data acquistion system, humidity sensor is connected stepper motor (Haydon Switch﹠amp with the wet system's (DH6-HT01B humidity controller) of control; Instrument INC.) is connected with driver (StepDriverTM), circulation line is by interface, conduit and temperature-controlling system (SHP DL-4006 in the sample box wall, scientific instrument company limited weighs and consider in order to uphold justice in Shanghai) connect, gas piping import on the sample box wall, outlet is connected with the wet system of control, and high-speed data acquistion system, the wet system of control, temperature-controlling system, wheelwork are connected with computing system by data line.
With the sample box sealing, 40 ℃ of temperature-controlling systems, control wetting phase are 60% to humidity, and behind the system stability, recording the sample box wall temperature by thermopair is 40.1 ℃, and temperature is 38.9 ℃ in the sample box, and relative humidity is 59%.Accurately drip 10.0 μ L water droplets by syringe to super-hydrophobic solid surface, regulate lens focus and get a distinct image.The stepper motor rotational angle is preset as 0 °, velocity of rotation is preset as 0.05 °/s, open wheelwork simultaneously by the data-triggered function, high-speed data acquistion system and high speed are taken the photograph phase system, recording water droplet temperature by the 0.01mm micro thermocouple is 39.7 ℃, take the dynamic outline image that water droplet rotates with sample box at super hydrophobic surface by camera, transfer to computing system by data line, utilize software that image is analyzed, calculating water droplet roll angle at super hydrophobic surface under this temperature and humidity condition is 2.5 °, 158.4 ° of advancing angles, 148.6 ° of receding angles, 9.8 ° of drag angle.
Claims (9)
1. the device of wet synchro measure drop temperature of a temperature control and roll angle, comprise: lifting table (3), frame (1), wheelwork (25), temperature-controlling system (12), the wet system (2) of control, high-speed data acquistion system (6), light source (9), take the photograph phase system (10) and computing system (11) composition at a high speed, it is characterized in that: thermopair (14) is housed in the sample box (4), micro thermocouple (7) is connected with high-speed data acquistion system; Humidity sensor (8) is connected with the wet system of control; Establish circulation line (15) in the sample box wall, the heat-conducting medium that flows in the pipeline, pipeline is connected with temperature-controlling system through conduit (13) by interface (17); Open air pipe import (18) on the sample box wall, outlet (19) is connected through the wet system of gas piping (20) and control; The rectangle window is opened in both sides, sample box opposite, window is adorned double-deck optical glass (21), vacuumize in the middle of the double glazing, sample box is fixed on the swinging mounting (30), be inserted on the lifting table by connecting link (24), lifting table, light source and high speed video system are installed on the frame, and light source (9) illuminates test droplets (5) by window, and high speed video system obtains the test droplets view data by window; Temperature-controlling system, the wet system of control, high-speed data acquistion system, high speed video system, wheelwork are connected with computing system by data line, by computer system control temperature control, the wet system of control, wheelwork, camera system; The sample box loam cake is opened one and is connected narrow groove, and groove pours into soft silicon rubber, and test fluid is quantitatively dripped in sample to be tested (22) surface by syringe needle.
2. device according to claim 1 is characterized in that: the sample box shell is equipped with thermofin (23), and sample to be tested places sample box inner bottom part central authorities, and micro thermocouple (7) directly contacts with test droplets, obtains the drop temperature; Thermopair (14) all is housed in the sample box and in the wall to be obtained in the sample box and the temperature of box wall in real time.
3. device according to claim 1, it is characterized in that: the rotation system device comprises stepper motor (28), turbine (26), worm screw (27), driver (29), swinging mounting (30), stepper motor is realized speed governing and location by driver regulating impulse frequency and number, the static torque of stepper motor is 1200gcm, driving sample box by the gear interlock rotates, speed adjustable range is 0.01~10 °/s, orientation range is-180 °~+ 180 °, pitch angle display precision and control accuracy be ± and 0.01 °.
4. device according to claim 1, it is characterized in that: temperature-controlling system comprises low-temperature receiver, thermal source, conduit, heat-conducting medium, temperature measurement-control instrument, and temperature control method is that microcomputer temperature control+PID regulates, and the temperature control scope is-80 ℃~+ 300 ℃, precision is ± 0.1 ℃, and temperature fluctuation is ± 0.05 ℃.
5. device according to claim 1, it is characterized in that: the wet system of control comprises dry gas, water, humidity measurement and control instrument, the wet scope of control is 0%~100%, and (0~80%RH) precision is ± 2% to middle low humidity section, and (80~100%RH) precision are 5% to the high humility section.
6. device according to claim 1, it is characterized in that: high-speed data acquistion system comprises: high-speed data acquisition card, data processing software; The micro thermocouple diameter range that connects is 0.01mm~0.001mm, and the high-speed data acquisition card sample frequency is 1MHz, and resolution is 16bit, analog input channel band cold junction compensation.
7. device according to claim 1 is characterized in that: taking the photograph phase system comprises high speed camcorder and image processing software at a high speed; The phase velocity of taking the photograph of camera was 30~420 frame/seconds, and interframe is divided into 2ms~1000s, and its camera lens is a focal length CCD camera lens far away, and enlargement factor is 0.7~20 times.
8. device according to claim 1 is characterized in that: light source is the blue look cold light source of LED.
9. device according to claim 1 is characterized in that: computer system comprises devices such as data-triggered, data recording, data storage, data operation; Data-triggered can be opened high-speed data acquistion system, wheelwork simultaneously, be taken the photograph phase system, synchronous recording drop temperature, sample box humiture and test droplets image outline in real time at a high speed.
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Cited By (20)
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CN101692012B (en) * | 2009-09-08 | 2011-08-31 | 南京大学 | Device for synchronously measuring temperature, surface tension and contact angle of droplet by controlling temperature and humidity |
CN102621042A (en) * | 2012-04-27 | 2012-08-01 | 南京大学 | Device for measuring droplet contact angle and rolling angle under temperature control, humidity control and pressure control condition |
CN104330338A (en) * | 2014-11-06 | 2015-02-04 | 西北工业大学 | Device and method for measuring contact angle in hypergravity environment |
CN104697900A (en) * | 2013-12-05 | 2015-06-10 | 上海梭伦信息科技有限公司 | Method for measuring interface tension and contact angle under vacuum controlled-temperature conditions, and apparatus thereof |
WO2015107159A1 (en) * | 2014-01-17 | 2015-07-23 | Technische Universität Kaiserslautern | Device and method for determining the contact angle of a liquid body with a solid surface |
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