CN102621042A - Device for measuring droplet contact angle and rolling angle under temperature control, humidity control and pressure control condition - Google Patents
Device for measuring droplet contact angle and rolling angle under temperature control, humidity control and pressure control condition Download PDFInfo
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Abstract
The invention belongs to the technical field of chemical measurement and in particular relates to a device for measuring a droplet contact angle and a rolling angle under a temperature control, humidity control and pressure control condition. A temperature control system is used for accurately controlling the temperature in a specimen box within a range from -20 DEG C to +200 DEG C; a humidity control system is used for controlling the relative humidity range at 0-100%; a vacuum/pressure control system comprises a high pressure system and a vacuum system; the pressure control range is from 10-6 Pa to 8.5 MPa; an anti-fogging device is used for preventing the surface of a glass window from fogging; a high speed image pickup system is used for obtaining a testing droplet contour image; the image sampling speed can reach 1400 thousand frames per second; the highest resolution reaches 1280x800; image sampling data is transmitted to a computer system by a data wire; and the image is fitted by using software according to a Young-Laplace equation so as to the contact angle, rolling angle, advancing angle, backing angle and viscoelastic property of the droplet. The device provided by the invention has the advantages of high automatic degree, testing accuracy, good experiment result repeatability, suitability for a wide temperature range, broad humidity, high pressure and negative pressure system to measure the contact angle, rolling angle, advancing angle, backing angle and lag angle of the droplet.
Description
Technical field
The present invention relates to a kind of wide temperature territory, wide humidity, high pressure, condition of negative pressure and measure the device of liquid-drop contact angle and roll angle down, belong to technical field of chemical measurement.
Technical background
Super-hydrophobic phenomenon is extensively to exist at occurring in nature, and for example: the surface of lotus leaf just has very strong hydrophobicity and self-cleaning net work can; The feather of the wing of butterfly, the pin of water skipper, aquatic bird all has superpower hydrophobic performance.Through research and imitation natural plants blade, the bionic surface that has good automatically cleaning effect in a large number emerges in an endless stream at present.If can more in depth understand the mechanism of action of super hydrophobic surface, 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 on inclined surface, taking place to roll; 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, so roll angle, advancing angle under the different condition, and the measurement of receding angle and drag angle becomes the focus of research.
Simultaneously, at present research direction mainly is the variation of material surface contact angle and roll angle under different temperature and damp condition, to the research of contact angle under the different pressures and roll angle seldom.Aircraft residing surrounding air when high aerial flight of several kms is thin, and air pressure is to be lower than standard atmospheric pressure; Equally the residing pressure of submarine of work has tens to a hundreds of atmospheric pressure at the deep-sea, so if the deep enough research pressure of ability to the influence of surface contact angle and roll angle, has important directive significance for the research of the surface coating of aircraft and submarine.
For example: application number is 200910034768.5, and Granted publication number is the Chinese invention patent of CN 101692011 B, discloses the device of wet synchro measure drop temperature of a kind of temperature control and roll angle.This device is accurately controlled environment temperature and humidity in the sample box through temperature, wet control system; Speed and the angle of utilizing driver control to rotate; High-speed data acquistion system and high speed video system are accurately measured the temperature and the contour images of drop synchronously; Utilize software that image is analyzed, obtain temperature, roll angle, advancing angle, the receding angle of drop.But there is following defective in this device:
(1). only can under normal pressure, test, limit the test specification of contact angle and roll angle, can't obtain contact angle and roll angle under the pressure-changed condition.
(2). under very low temperature conditions such as-20 ℃; Even double-deck its outside surface of quartz glass also can be tied very serious water smoke; The usefulness that need not stop is dipped in the cotton balls wiping window surface of anti freezing solution; The process of wiping can be blocked the camera lens filming image of video camera, and the direction that the water smoke of staying quartz glass surface simultaneously can change light path makes the image that photographed be distorted and brings error to the result.
(3). the high-speed camera prestissimo that is adopted had only for 420 frame/seconds, can't real-time follow-up low temperature under water droplet in the freezing process of super hydrophobic surface or water droplet spring, viscoelastic process at super hydrophobic surface.
Summary of the invention
The objective of the invention is in order to break through the use restriction of existing apparatus; Realize in the accurate hierarchy of control pressure, window condensation when preventing low temperature, improve the degree of accuracy of photographic images, thereby provide that a kind of temperature control, control are wet, measure the device of liquid-drop contact angle and roll angle under the pressure control condition.
The parent of ideal surfaced, lyophobicity depend on the chemical property of solid surface fully, shown in the Young equation.
Cosθ
Y?=?(γ
SV－γ
SL)/?γ
LV
Drop in the situation of sprawling of smooth flat shown in accompanying drawing 1, θ
YBe YoungShi contact angle, γ
SVBe solid/aerosphere face free energy, γ
SLBe solid/liquid interfaces free energy, γ
LVBe the liquid/gas interfacial free energy.
When pressure changes, γ
SVAnd γ
LVSize all will change, can make that so also contact angle changes thereupon.
Technical scheme of the present invention is:
A kind of temperature control, control are wet, measure the device of liquid-drop contact angle and roll angle under the pressure control condition, comprising: frame (10), temperature-controlling system (1), the wet system (2) of control, vacuum/pressurized control system (3), rotation system, LED cold light source (4), high speed video system (9) and computer system (11).Temperature-controlling system, the wet system of control, vacuum/pressurized control system, rotation system are connected with computer system with high speed video system.Sample box (6) is fixed on the frame through swinging mounting (5), between LED cold light source and pick-up lens, can adjust the position by three-dimensional in top to bottom, left and right, front and rear, and LED cold light source, swinging mounting, high speed video system are installed on the frame.
Sample box is equipped with heat-insulation layer (20) outward; Can effectively reduce the heat interchange between the system and surrounding; Heat-insulation layer has one deck stainless steel protection shell (19) outward simultaneously; Columniform sample chamber (8) is arranged in the sample box, and optical quartz glass window (17) is equipped with in both sides, diametric(al) opposite, sample locular wall upper edge, and the optical quartz glass window is equipped with outward and prevents the glass window surface device (14) of mist with fixed attention; Sample box has and is communicated with sample chamber and the outer pipeline (27) of sample box, and its interface (23) is connected with vacuum/pressurized control system with the wet system of control respectively; Temperature sensor (12) is housed in the sample box to be connected with computer system through data line with humidity sensor (13); Establish circulation line (21) in the sample box wall, pipeline includes mobile heat-conducting medium, through conduit circulation line inlet (24), outlet (22) is connected with temperature-controlling system; Liquid droping port (18) is arranged on the sample box, experimental liquid is dripped on the testing sample surface through liquid droping port; The LED cold light source illuminates test droplets through the optical quartz glass window, and high speed video system obtains the test droplets view data through the optical quartz glass window on opposite; Temperature, humidity, pressure, view data, turn signal are delivered to computer system through data line, by computing system control temperature-controlling system, the wet system of control, vacuum/pressurized control system, rotation system and high speed video system.LED cold light source, optical quartz glass window, test droplets, high-speed camera camera lens are on same horizontal line.
Described temperature-controlling system comprises: low-temperature receiver, thermal source, conduit, temperature sensor; Be connected with temperature-controlling system with outlet (22) through the circulation line inlet (24) of conduit sample box; Temperature control method is regulated for the microcomputer temperature control adds PID, and through temperature stabilization in the circulation realization sample box of heat-conducting medium, heat-conducting medium is selected according to actual probe temperature; Temperature control scope-20 ℃～200 ℃, control accuracy is ± 0.1 ℃.
The wet system of described control comprises: dry gas, water, humidity controller, humidity sensor; Relative humidity in the humidity sensor test samples box, the regulation and control of humidity measurement and control instrument are done, the humid gas flow proportional, and to reach the condition of work of humidity requirement, the wet scope of control is 0%～100%, and control accuracy is ± 5%.
Described vacuum/pressurized control system comprises: pressure gas cylinder/vacuum pump, accumulator, pressure transducer (26), solenoid valve (25).Through withstand voltage copper pipe vacuum/pressurized control system is connected with the interface (23) of sample box, the force value that the real-time test sample of pressure transducer is indoor is regulated the pressure size through the switch of computer system control solenoid valve, pressure control range 10
-6Pa～8.5MPa, control accuracy is ± 1%.Wherein accumulator is connected with them through withstand voltage copper pipe between pressure gas cylinder and sample box; When whole compression system does not operate for a long time, and will keep in the test box for constant pressure the time, available accumulator comes leakages, thereby makes the sample box internal pressure constant and guarantee not fall in 24 hours pressure; Simultaneously accumulator can keep the pressure equilibrium in the sample box, make the pressure surge scope 1%, when in sample box, pressurizeing suddenly, can relax compression shock and guarantee that the sample in the sample chamber can be because of adding the air pressure impact suddenly and rocking.
Described high speed video system (9) comprising: high-speed camera and image processing software; The high-speed camera prestissimo can reach for 1,400,000 frame/seconds, and highest resolution 1280 * 800 has nearly long distance camera function, can follow the tracks of spring, the viscoelastic process of water droplet at super hydrophobic surface at a high speed; Image processing software has functions such as real-time monitoring, image download, file management, Flame Image Process, motion analysis.
Describedly prevent that glass window surface from coagulating the device (14) of mist is a ring-shaped air chamber; Be fixed on the outer sample box of optical quartz glass window, the air chamber inwall has 2～12 gas holes (16), and the angle of gas hole is α=20～45 °; Bore dia is 0.5～5mm; To guarantee that the gas that blows out can cover whole glass window surface, gas hole connects the purging silica glass window surface that dry nitrogen does not stop through inflatable mouth (15), prevents the surperficial mist that coagulates of glass window.
Described rotation system comprises: swinging mounting (5) and rotary driver (7); Swinging mounting links to each other with frame; Rotation axis and light source, sample, high-speed camera are on the same straight line, and rotary electric machine is realized speed governing and location through rotary driver regulating impulse frequency and number, and speed adjustable range is 0.01～10 °/s; Orientation range is-180 °～+ 180 °, pitch angle display precision and control accuracy be ± and 0.01 °.
Temperature control provided by the invention, control are wet, measure the device of liquid-drop contact angle, roll angle, advancing angle, receding angle under the pressure control condition, can realize in the sample box temperature in-20 ℃～+ 200 ℃ scopes, humidity at 0%～100% scope, pressure 10
-6The accurate control of Pa～8.5MPa scope can be opened temperature-controlling system, the wet system of control, vacuum/pressurized control system, rotation system, high speed video system simultaneously, and high-speed camera is taken the clear contour images of drop in different solid surface.The figure sampled data transfers to computing system through data line; The simultaneous computer system obtains temperature, humidity, the pressure of system; Utilize software image to be carried out match, obtain contact angle, roll angle, advancing angle, the receding angle of drop according to the Young-Laplace equation.This plant automation degree is high, and testing precision is high, and the experimental result favorable repeatability is applicable to wide temperature territory, wide humidity, high pressure, the measurement of negative pressure system liquid-drop contact angle, roll angle, carries out angle, receding angle, drag angle.
Description of drawings
Fig. 1 is that water droplet is at desirable wetting of surfaces form synoptic diagram
Fig. 2 is that temperature control, control are wet, measure the device synoptic diagram of liquid-drop contact angle and roll angle under the pressure control condition
Fig. 3 is the sample box front elevational schematic
Fig. 4 is that synoptic diagram is looked on the sample box right side
Fig. 5 is that high-speed camera is followed the tracks of the water droplet free-falling and the process synoptic diagram that bounces on the inclined-plane
6 pictures from left to right are followed successively by among Fig. 5: water droplet begins to fall during 0ms, water droplet tumbled out sample surfaces when water droplet bounced to peak and 167ms when water droplet had just left sample surfaces, 60ms when water droplet spread into maximum gauge, 41.7ms when water droplet had just contacted sample surfaces, 33ms during 28ms.
The drawing explanation:
1: The temperature control system? 2: Wet control system? 3: Vacuum / pressure control system? 4: LED cold light source? 5: Rotating Stand? 6: Sample Box? 7: Turn the drive 8: sample chamber? 9: high-speed camera system? 10: Rack? 11: computer System? 12: Temperature sensor? 13: humidity sensor? 14: to prevent the glass surface of the window fogging device? 15: blowing mouth? 16: blowing holes? 17: optical quartz glass window? 18: dripping mouth? 19: protective housing? 20: insulation? 21: circulation line? 22: circulation pipeline exports? 23: aerated Interface? 24: circulation pipeline population? 25: Solenoid valve? 26 : pressure sensor? 27: tubing.
Embodiment
Embodiment 1: water droplet under 40 ℃, relative humidity 60%, 0.5MPa pressure condition in contact angle, roll angle, advancing angle, receding angle and the drag angle of super hydrophobic surface.
Sample box is fixed on the swinging mounting; Swinging mounting is between light source and high-speed camera camera lens; Sample to be tested is placed by central authorities in the sample box; Adjustment swinging mounting position; Make LED cold light source, optical quartz glass window, specimen surface, high-speed camera (Phantom V12.0) be positioned at same line, the LED cold light source illuminates test droplets through the optical quartz glass window, and high speed video system obtains the test droplets view data through the optical quartz glass window; The temperature sensor that is equipped with on the sample box, humidity sensor and pressure transducer are connected with computer system; Stepper motor (Haydon Switch & Instrument INC.) is connected with driver (StepDriver TM), and circulation line connects through interface, conduit and temperature-controlling system (SHP DL-4006, scientific instrument company limited weighs and consider in order to uphold justice in Shanghai) in the sample box wall; The wet system of control is connected with sample box with vacuum/pressurized control system, and high speed video system and rotation system pass through data line and computer system swap data and by computer control.
Regulating 40 ℃ of temperature-controlling systems, controlling wetting phase is 60% to humidity, and behind the system stability, recording the sample indoor temperature by temperature sensor is 39.9 ℃, and relative humidity is 58%.Accurately drip 10.0 μ L water droplets through syringe to super hydrophobic surface, the sealing sample box, and open lentamente and close the high pressure nitrogen cylinder valve after the high pressure nitrogen cylinder valve makes the interior pressure of system rise to 0.5MPa stably.The adjusting lens focus gets a distinct image.The stepper motor rotational angle is preset as 0 °, and velocity of rotation is preset as 0.05 °/s, opens wheelwork and high speed video system simultaneously through the data-triggered function; Take the dynamic outline image that water droplet rotates with sample box at super hydrophobic surface by video camera; Transfer to computing system through data line, utilize software that image is analyzed, calculating water droplet contact angle at super hydrophobic surface under this temperature, humidity and pressure condition is 160.5 °; Roll angle is 5.5 °; 163.2 ° of advancing angles, 158.0 ° of degree of receding angle, 5.2 ° of drag angle.
Instance 2: water droplet is in the contact angle and the roll angle of glass surface under the 0.1kpa condition at 0 ℃, vacuum tightness
Sample box is fixed on the swinging mounting; Swinging mounting is between LED cold light source and high-speed camera camera lens; Sample to be tested is placed by central authorities in the sample box, and adjustment swinging mounting position makes LED cold light source, optical quartz glass window, specimen surface, high-speed camera be positioned at same line; The lED cold light source illuminates test droplets through the optical quartz glass window; High speed video system obtains the test droplets view data through window, and the temperature sensor that is equipped with on the sample box, humidity sensor and pressure transducer are connected with computer system, and stepper motor is connected with driver; Circulation line is connected with temperature-controlling system through interface, conduit in the sample box wall; Vacuum pump is connected with sample box, and the anti-condensation gas outlet on optical quartz glass surface links to each other with the nitrogen steel cylinder of drying, and high speed video system and rotation system pass through data line and computer system swap data and by computer control.
Regulate 0 ℃ of temperature-controlling system; Open purging optical quartz glass surface that the drying nitrogen valve do not stop and prevent that window from tying water smoke at low temperatures; Behind the system stability, record the sample indoor temperature by temperature sensor and be-9.8 ℃, accurately drip 10.0 μ L water to super hydrophobic surface through syringe; The sealing sample box is opened lentamente and is closed vacuum pump after the vacuum tightness variable valve makes the interior pressure of system drop to 0.1kPa stably.The adjusting lens focus gets a distinct image.The stepper motor rotational angle is preset as 0 °; Velocity of rotation is preset as 1 °/s, opens wheelwork and high speed video system simultaneously through the data-triggered function, takes the dynamic outline image that water droplet rotates with sample box at glass by high-speed camera; Transfer to computing system through data line; Utilize software that image is analyzed, calculating water outlet contact angle at glass surface under this condition is 53.2 °, and water is not hung by the feet or not can be tumbled at glass surface.
Instance 3: at-10 ℃, relative humidity is 50%, under the condition of normal pressure, follows the tracks of water droplet highly falls at the angle of inclination super hydrophobic surface that is 10 ° from 0.5cm spring process at a high speed
Sample box is fixed on the swinging mounting; Swinging mounting is between LED cold light source and high-speed camera camera lens; Sample to be tested is placed by central authorities in the sample box; Adjustment swinging mounting position makes LED cold light source, optical quartz glass window, specimen surface, high-speed camera be positioned at same line, and the LED cold light source illuminates test droplets through the optical quartz glass window; High speed video system obtains the test droplets view data through window; The temperature sensor that is equipped with on the sample box is connected with computer system with humidity sensor, and circulation line is connected with temperature-controlling system through interface, conduit in the sample box wall, and high speed video system passes through data line and computer system swap data and by computer control.
Adjustment sample box angle is 10 °; Regulate temperature-controlling system-10 ℃, the control wetting phase is 50% to humidity; Open purging optical quartz glass surface that the drying nitrogen valve do not stop and prevent that window from tying water smoke at low temperatures; Behind the system stability, record the sample indoor temperature by temperature sensor and be-9.8 ℃, relative humidity is 48%.The adjustment syringe is apart from sample surfaces height 0.5cm; Open the shooting speed that high speed video system uses 3000 frames/s through the data-triggered function; Regulate camera lens and obtain suitable focal length; Accurately dripping 10.0 μ L water droplets drops on the sample surfaces; Take the process of whole free-falling of water droplet and spring by high-speed camera, the result is shown in accompanying drawing 5, and 6 pictures from left to right are followed successively by: water droplet begins to fall during 0ms, water droplet tumbled out sample surfaces when water droplet bounced to peak and 167ms when water droplet had just left sample surfaces, 60ms when water droplet spread into maximum gauge, 41.7ms when water droplet had just contacted sample surfaces, 33ms during 28ms.
Claims (4)
1. measure the device of liquid-drop contact angle and roll angle under wet, the pressure control condition of a temperature control, control; Comprise: in frame (10), temperature-controlling system (1), the wet system (2) of control, rotation system, LED cold light source (4), high speed video system (9), computer system (11), the sample box (6) temperature sensor (12) is housed and is connected with computer system with humidity sensor (13); It is characterized in that having in the sample box columniform sample chamber (8); Sample box has and is communicated with the sample chamber to the outer pipeline (27) of sample box, and its interface (23) is connected with vacuum/pressurized control system (3) with the wet system of control respectively; Optical quartz glass window (17) is equipped with in both sides, diametric(al) opposite, sample locular wall upper edge, and the optical quartz glass window is equipped with outward and prevents the glass window surface device (14) of mist with fixed attention; Liquid droping port (18) is arranged on the sample box, experimental liquid is dripped to the testing sample surface through liquid droping port; Sample box is fixed on the frame through swinging mounting (5), between LED cold light source and pick-up lens; LED cold light source, swinging mounting, high speed video system are installed on the frame; The LED cold light source illuminates test droplets through the optical quartz glass window, and high speed video system obtains the test droplets view data through the optical quartz glass window on opposite; Temperature, humidity, pressure, view data, turn signal pass to computer system through data line, by computer system control temperature-controlling system, the wet system of control, vacuum/pressurized control system, rotation system and high speed video system.
2. device according to claim 1 is characterized in that vacuum/pressurized control system comprises: pressure gas cylinder/vacuum pump, accumulator, pressure transducer (26), solenoid valve (25), pressure control range 10
-6Pa～8.5MPa, control accuracy is ± 1%.
3. device according to claim 1; It is characterized in that preventing that the glass window surface from coagulating the device of mist is a ring-shaped air chamber; Be fixed on the outer sample box of optical quartz glass window, the inboard of air chamber has 2～12 gas holes (16), and the angle of gas hole is α=20～45 °; The diameter in hole is 0.5～5mm; Can cover whole silica glass window surface with the gas that guarantees to blow out, it is surperficial that gas hole connects dry nitrogen purging quartz glass through inflatable mouth (15), prevents that the optical quartz glass window surface from coagulating mist.
4. device according to claim 1 is characterized in that high speed video system comprises high-speed camera and image processing software; The high-speed camera motor speeds reaches 1,400,000 frame/seconds, highest resolution 1280 * 800; Image processing software has real-time monitoring, image download, file management, Flame Image Process, motion analysis function.
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