CN114624150A - Contact angle measuring method for micro and macro simultaneous measurement and mutual verification - Google Patents
Contact angle measuring method for micro and macro simultaneous measurement and mutual verification Download PDFInfo
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- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
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Abstract
The invention relates to the technical field of liquid drop infiltration research, and discloses a contact angle measuring method for simultaneously measuring and mutually verifying a micro surface and a macro surface, which comprises the following steps of: s1, adjusting the temperature to a target working condition; s2, adjusting the pressure to a target working condition; s3, enabling the computer to normally receive the image; s4, carrying out a water drop experiment; s5, processing the image to obtain a macroscopic contact angle and a microscopic contact angle; s6, verifying the macroscopic contact angle as the microscopic contact angle. The method simultaneously measures the liquid drop on the surface of the solid through two orthogonal visual angles, and corrects the sampling angle, thereby not only ensuring the accuracy of the measuring process, but also simultaneously measuring the microcosmic and macroscopical images; uncontrollable factors such as laboratory humidity, air flow and the like are avoided, the measurement environment is more stable, the contact angle is verified by utilizing the relation between the microscopic contact angle and the macroscopic contact angle, and the value with the minimum error is selected as a measured value, so that the contact angle value of the liquid drop on the surface of the solid is measured more accurately, conveniently and truly.
Description
Technical Field
The invention relates to the technical field of droplet infiltration research, in particular to a contact angle measuring method for simultaneously measuring microcosmic and macroscopical dimensions and mutually verifying the microcosmic and macroscopical dimensions.
Background
The surface wettability of the material has wide application, the material not only exists around people at all times, such as ink and wash calligraphy and painting, lotus leaf surface self-cleaning, but also is widely applied to various industrial fields such as spray cooling, micro-fluidic chips, ink-jet printing and the like, and the material essentially belongs to a liquid drop infiltration phenomenon and is one of the hot spots and difficult problems of current scientific research; the contact angle is an important parameter in the research of liquid drop infiltration, and the hydrophilic and hydrophobic properties of the surface of the material can be judged according to the size of the contact angle. The droplet contact angle occurs at the intersection of the three phases solid-liquid-gas, which is the result of the equilibrium of the three phase interfacial tensions.
At present, the mainstream methods for measuring the contact angle by the traditional experiment are divided into two categories: measuring macroscopic parameters of the liquid drops, and calculating according to a geometric relationship to obtain a result; the other is processing the image by a computer, and obtaining a result after fitting; although the measurement results can be obtained by the two methods, the traditional measurement method only measures the angle in one direction, so that the sampling angle is single, and the simultaneous measurement of the microscopic contact angle and the macroscopic contact angle cannot be realized.
Chinese patent discloses a surface contact angle measuring method (publication No. CN110286063A), which can photograph by using a variable-focus webcam and calculate a liquid drop contact angle with high precision and high accuracy, but it cannot measure micro and macro contact angles at the same time.
Disclosure of Invention
The invention aims to provide a contact angle measuring method for simultaneously measuring microcosmic and macroscopical surfaces and mutually verifying the microcosmic and macroscopical surfaces so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a contact angle measurement method for microscopic and macroscopic simultaneous measurement and mutual verification, comprising the steps of:
s1, temperature adjustment: loading the surface-treated sample into a visual pressure container, entering a working condition monitoring area, operating a thermostat to enable a thermocouple to enter a working state, and adjusting the temperature to a target working condition;
s2, pressure regulation: entering a pressure control area, sequentially opening an air compressor, a gas tank and a high-pressure plunger pump, and adjusting the pressure in the container to a target working condition through a pressure control console;
s3, image receiving and debugging: respectively turning on two groups of light sources and two groups of cameras, adjusting the objective table to be horizontal, and checking whether the computer can normally receive images;
s4, water drop test: entering a water drop supply area, opening a water pump and a water stop valve, operating a water flow control console to enable liquid drops in the stainless steel injector to drop on the material sample, and sequentially closing the water pump, the water stop valve and the water flow control console;
s5, image processing: taking a picture of the liquid drops dropping on the material sample, uploading the picture to a computer, and processing the picture uploaded to the computer by using software to obtain a macroscopic contact angle and a microscopic contact angle;
s6, contact angle verification: the macroscopic contact angle was verified by obtaining the microscopic contact angle by the step of S5.
As a still further scheme of the invention: the method of processing an image in the step S5 includes the steps of:
s51, setting the shooting time of the camera according to the temperature of the experiment; when the experiment temperature is below 200 ℃, liquid drops are deposited on the material sample for 2-3 s, and the material sample is shot; when the experiment temperature is above 200 ℃, the liquid drops are dripped on the material sample for 0.3-1 s, and the material sample is shot;
s52, transmitting the pictures shot by the two groups of cameras to a computer, carrying out threshold-based segmentation on the pictures, selecting a threshold, and carrying out binarization on the pictures so as to automatically obtain the outline of the liquid drop;
and S53, compiling by using MATLAB software based on an inflection point real-time detection algorithm in the binary image to respectively obtain a macroscopic contact angle and a microscopic contact angle.
As a still further scheme of the invention: the contact angle verification method in the step S6 comprises the following steps:
s61, calculating by using the microscopic contact angle obtained in the step S5 and a corresponding calculation formula according to the contact state of the liquid drop and the material sample to obtain a macroscopic contact angle;
and S62, analyzing the error between the macroscopic contact angle calculated by the microscopic contact angle and the macroscopic contact angle obtained in the step S5 to obtain the real measured contact angle.
As a still further scheme of the invention: the calculation of the macroscopic contact angle in the step S61 conforms to the Young equation, and theta is recordedY；
The calculation of the microscopic contact angle in the step S61 is as follows: observing the liquid drop through a microscopic camera, and if the liquid drop is in wet contact with the rough surface, the wetting state of the liquid drop is Wenzel state, and the microscopic contact angle is recorded as thetaWThe calculation formula is as follows:
cosθW＝r cosθY (1)
if the liquid drop and the rough surface do not form wet contact, the liquid drop soaks in Cassie state, and the micro contact angle is recorded as thetaCThe calculation formula is as follows:
cosθC＝φS(cosθY+1)-1 (2)
in the above formulae (1) and (2), θCMicroscopic contact angle in the Cassie state; thetaWMicro contact angle in Wenzel state, [ phi ]SAnd r is the roughness, i.e., the wetted surface to projected surface area ratio.
As a still further scheme of the invention: the calculation formula of the error in the step S61 is as follows:
in the above formula (3), θ'YiAnd thetaYiRespectively representing a plurality of macroscopic contact angles calculated by microscopic contact angles and corresponding known macroscopic contact angles, wherein the set of data having the smallest error between the calculated macroscopic contact angle and the corresponding known macroscopic contact angle represents the closest match with the true contact angle of the liquid dropThe corresponding contact angle of the liquid drop and the surface of the sample is the measured contact angle under the set working condition.
As a still further scheme of the invention: in the step S5, photographing needs to be carried out from two orthogonal directions, and the sampling angle is corrected, so that the accuracy of the measurement process is ensured, and the microscopic and macroscopic measurement is realized simultaneously.
Compared with the prior art, the invention has the beneficial effects that:
the method simultaneously measures the liquid drop on the surface of the solid through two orthogonal visual angles, and corrects the sampling angle, thereby not only ensuring the accuracy of the measuring process, but also simultaneously measuring the microcosmic and macroscopical images; uncontrollable factors such as humidity and air flow in a laboratory are avoided, the measurement environment is more stable, the contact angle is verified by utilizing the relation between the microscopic contact angle and the macroscopic contact angle, and the value with the minimum error is selected as the measured value, so that the contact angle value of the liquid drop on the surface of the solid is measured more accurately, conveniently and truly.
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FIG. 1 is a schematic view showing the structure of a measuring device in a contact angle measuring method in which microscopic and macroscopic measurements are simultaneously performed and mutually verified;
FIG. 2 is a left side view of a pressure vessel in a measuring device in a contact angle measuring method in which microscopic and macroscopic measurements are simultaneously made and mutually verified;
FIG. 3 is a top view of a pressure vessel in a measuring device for contact angle measurement in which microscopic and macroscopic measurements are made simultaneously and mutually verified;
FIG. 4 is a schematic representation of two wetting morphologies in a contact angle measurement method with simultaneous microscopic and macroscopic measurements and mutual validation.
In the figure: 1. a reservoir; 2. a water pump; 3. a water stop valve; 4. a water flow console; 5. a water pipe; 6. an air compressor; 7. a gas tank; 8. a high pressure plunger pump; 9. a pressure console; 10. an air tube; 11. a condenser and a high-pressure gas storage tank; 12. a pressure gauge; 13. a thermostat; 14. a cable; 15. a pressure detection probe; 16. a temperature detection probe; 17. a vibration isolation platform; 18. visualizing the pressure vessel; 19. an adjustable support; 20. an object stage; 21. a sample of material; 22. a droplet; 23. a stainless steel syringe; 24. a light-transmitting hole; 25. a thermocouple; 26. a first light source; 27. a CCD camera; 28. a computer; 29. a second light source; 30. a micro-camera.
Detailed Description
Referring to fig. 1 to 4, in an embodiment of the present invention, a contact angle measurement method for simultaneously measuring and mutually verifying a microscopic contact angle and a macroscopic contact angle includes the following steps:
s1, temperature adjustment: loading the surface-treated sample into a visual pressure container, entering a working condition monitoring area, operating a thermostat to enable a thermocouple to enter a working state, and adjusting the temperature to a target working condition;
s2, pressure regulation: entering a pressure control area, opening an air compressor, a gas tank and a high-pressure plunger pump in sequence,
adjusting the pressure in the container to a target working condition through a pressure control console;
s3, image receiving and debugging: respectively turning on two groups of light sources and two groups of cameras, adjusting the objective table to be horizontal, and checking whether the computer can normally receive images;
s4, water drop test: entering a water drop supply area, opening a water pump and a water stop valve, operating a water flow control console to enable liquid drops in the stainless steel injector to drop on the material sample, and sequentially closing the water pump, the water stop valve and the water flow control console;
s5, image processing: taking a picture of the liquid drop dropped on the material sample, uploading the picture to a computer, and processing the picture uploaded to the computer by using software to obtain a macroscopic contact angle and a microscopic contact angle;
s6, contact angle verification: the macroscopic contact angle was verified by obtaining the microscopic contact angle by the step of S5.
Preferably, the method of processing an image in step S5 includes the steps of:
s51, setting the shooting time of the camera according to the temperature of the experiment; when the experiment temperature is below 200 ℃, liquid drops are deposited on the material sample for 2-3 s, and the material sample is shot, so that the adverse effects of initial transient state and evaporation are avoided; when the experiment temperature is above 200 ℃, the liquid drops are shot on the material sample for 0.3-1 s, so that the evaporation of the liquid drops in a short time is avoided;
s52, transmitting the pictures shot by the two groups of cameras to a computer, segmenting the pictures based on a threshold value, selecting a threshold value, and binarizing the pictures to automatically obtain the contour line of the liquid drop;
and S53, compiling by using MATLAB software based on a real-time detection algorithm of an inflection point in the binary image to respectively obtain a macroscopic contact angle and a microscopic contact angle.
Preferably, the contact angle verification method in the step S6 includes the following steps:
s61, according to the contact state of the liquid drop and the material sample, adopting a corresponding calculation formula, and calculating by using the microscopic contact angle obtained in the step S5 to obtain a macroscopic contact angle, wherein multiple groups of data are required to be calculated;
and S62, analyzing the error between the macroscopic contact angle calculated by the microscopic contact angle and the macroscopic contact angle obtained in the step S5 to obtain the real measured contact angle.
Preferably, the calculation of the macroscopic contact angle in the step S61 conforms to Young' S equation, and is recorded as thetaY；
The microscopic contact angle in step S61 was calculated as follows: observing the liquid drop through a microscopic camera, and if the liquid drop is in wet contact with the rough surface, the wetting state of the liquid drop is Wenzel state, and the microscopic contact angle is recorded as thetaWThe calculation formula is as follows:
cosθW＝r cosθY (1)
if the liquid drop and the rough surface do not form wet contact, the liquid drop soaks in Cassie state, and the micro contact angle is recorded as thetaCThe calculation formula is as follows:
cosθC＝φS(cosθY+1)-1 (2)
in the above formulae (1) and (2), θCMicroscopic contact angle in Cassie state; theta.theta.WIs the micro contact angle in the Wenzel state, phiSAnd r is the roughness, i.e., the wetted surface to projected surface area ratio.
Preferably, the error in step S61 is calculated as follows:
in the above formula (3), θ'YiAnd thetaYiRespectively representing a plurality of macroscopic contact angles calculated through microscopic contact angles and corresponding known macroscopic contact angles, wherein in the plurality of groups of data, the group of data with the smallest error between the calculated macroscopic contact angles and the corresponding known macroscopic contact angles represents the closest match with the real contact angle of the liquid drop, and the corresponding contact angle is the measured contact angle of the liquid drop and the surface of the sample under the set working condition.
Preferably, the photographing in the step S5 needs to be performed from two orthogonal directions, and the sampling angle is corrected, so that the accuracy of the measurement process is ensured, and the microscopic and macroscopic measurements are performed simultaneously; uncontrollable factors such as humidity and air flow in a laboratory are avoided, and the measuring environment is more stable.
In order to better illustrate the technical effects of the invention, it is illustrated by the following examples:
with CO2-The contact angle of a water-rock system is measured as an example, and the measurement method is as follows;
s21, placing a rock sample into the visual pressure container 18, entering a working condition monitoring area, enabling the thermocouple 25 to enter a working state by operating the thermostat 13, adjusting the temperature to 200 ℃, collecting temperature data by the temperature detection probe 16 and transmitting the data to the thermostat 13, and carrying out the next step after the temperature is stable, wherein the thermocouple 25 is made of nickel-chromium-nickel-silicon, the code WRN, the measurement range is 0-1300 ℃, and the allowable error is +/-1.5 ℃;
s22, entering a pressure control area, sequentially opening an air compressor 6, a gas tank 7 and a high-pressure plunger pump 8, and adjusting the pressure in a visual pressure container 18 to 15MPa through a pressure control console 9; CO is stored in the gas tank 72Gas, the gas supplied by the gas tank 7 maintaining the container at a predetermined system pressure; in order to ensure the safe operation of the high-voltage experiment, an explosion-proof glass protective cover is arranged on the light hole 24; for pressure-detecting probes 15The pressure in the visual pressure container 18 is monitored, the measuring range can reach 30MPa, the precision is 0.25%, the conveying pressure of the high-pressure plunger pump 8 is 25-30 MPa, the supply flow is 0.1cc/min, the pressure resistance of the visual pressure container 18 is 15MPa, and the size is 50mm multiplied by 150 mm.
S23, turning on the first light source 26, the CCD camera 27, the second light source 29 and the microscopic camera 30, and adjusting the objective table 20 to be horizontal through the adjustable bracket 19 to ensure that the image processing of 640 multiplied by 480 pixels can be normally transmitted to the personal computer 28; the test board uses a stainless steel 304 board with the surface area of 20 multiplied by 20mm and the thickness of 0.5mm as a material sample 21, the surface of the rock is pretreated before the experiment, the rock is washed clean by deionized water, and the rock is dried in a constant temperature box for 10min and then used; the first light source 26 and the second light source 29 are both LED flat lamps, and light passes through a light guide plate with high light transmittance to form a uniform light emitting plane, so that the uniformity of illumination is good, and light rays are soft;
s24, entering a water drop supply area, opening a water pump 2 and a water stop valve 3, operating a water flow control console 4 to control the volume of the water drops to be about 0.05ml, flowing through a stainless steel injector 23 to drip on a material sample, and sequentially closing the water pump 2, the water stop valve 3 and the water flow control console 4, wherein the stainless steel injector 23 adopts a thin SS (suspended solid) tube with the inner diameter of 0.5mm as a drip needle, and the needle head is suspended above the center of the surface of the sample by about 5 mm;
s25, starting to shoot the liquid drops from two directions at 0.5S after the liquid drops drop, wherein the shooting time is 0.5S, and a clear picture is selected every 0.1S; the computer 28 segments each pixel and its neighborhood pixels in the image based on the threshold value, and then selects an inflection point according to the processing result; the microscopic camera 30 observes the liquid drop infiltration state, judges whether the liquid drop infiltration state is Wenzel state or Cassie state, and uses MATLAB software to compile and calculate the inflection angle to respectively obtain five groups of macroscopic contact angles thetaYiAnd micro contact angle thetaWiOr is θCiWherein i is 1, 2, 3, 4, 5.
S26, verifying the macroscopic contact angle by using the microscopic contact angle, wherein the macroscopic contact angle is as follows:
1) calculating a macroscopic contact angle by using the microscopic contact angle, and calculating five groups of data;
wherein, the calculation formula of the Wenzel state is as follows: cos θW＝r cosθYThe Cassie state conversion formula is as follows: cos θC＝φS(cosθY+1) -1, five sets of data were all calculated, and the calculated macroscopic contact angle is θ'Yi；
2) Using formulas
And calculating the error value of the macro contact angle calculated by the micro contact angle and the corresponding known macro contact angle, wherein the smallest error value is the measured contact angle of the liquid drop and the rock surface under the set working condition.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention are equivalent to or changed within the technical scope of the present invention.
Claims (6)
1. A contact angle measurement method for microscopic and macroscopic simultaneous measurement and mutual verification, comprising the steps of:
s1, temperature adjustment: loading the surface-treated sample into a visual pressure container, entering a working condition monitoring area, operating a thermostat to enable a thermocouple to enter a working state, and adjusting the temperature to a target working condition;
s2, pressure regulation: entering a pressure control area, sequentially opening an air compressor, a gas tank and a high-pressure plunger pump, and adjusting the pressure in the container to a target working condition through a pressure control console;
s3, image receiving and debugging: respectively turning on two groups of light sources and two groups of cameras, adjusting the objective table to be horizontal, and checking whether the computer can normally receive images;
s4, water drop test: entering a water drop supply area, opening a water pump and a water stop valve, operating a water flow control console to enable liquid drops in the stainless steel injector to drop on the material sample, and sequentially closing the water pump, the water stop valve and the water flow control console;
s5, image processing: taking a picture of the liquid drop dropped on the material sample, uploading the picture to a computer, and processing the picture uploaded to the computer by using software to obtain a macroscopic contact angle and a microscopic contact angle;
s6, contact angle verification: the macroscopic contact angle was verified by obtaining the microscopic contact angle by the step of S5.
2. The method for contact angle measurement for microscopic and macroscopic simultaneous measurement and mutual authentication as claimed in claim 1, wherein the method for image processing in the step of S5 comprises the steps of:
s51, setting the shooting time of the camera according to the temperature of the experiment; when the experiment temperature is below 200 ℃, liquid drops are deposited on the material sample for 2-3 s, and the material sample is shot; when the experiment temperature is above 200 ℃, the liquid drops are dropped on the material sample for 0.3-1 s, and the material sample is shot;
s52, transmitting the pictures shot by the two groups of cameras to a computer, carrying out threshold-based segmentation on the pictures, selecting a threshold, and carrying out binarization on the pictures so as to automatically obtain the outline of the liquid drop;
and S53, compiling by using MATLAB software based on an inflection point real-time detection algorithm in the binary image to respectively obtain a macroscopic contact angle and a microscopic contact angle.
3. The method for measuring contact angle according to claim 1, wherein the contact angle verification method in step S6 comprises the following steps:
s61, according to the contact state of the liquid drop and the material sample, adopting a corresponding calculation formula, and calculating by using the microscopic contact angle obtained in the step S5 to obtain a macroscopic contact angle;
and S62, analyzing the error between the macroscopic contact angle calculated by the microscopic contact angle and the macroscopic contact angle obtained in the step S5 to obtain the real measured contact angle.
4. The method of claim 3The contact angle measurement method for micro and macro simultaneous measurement and mutual verification is characterized in that the calculation of the macro contact angle in the step S61 conforms to the Young equation, and theta is recordedY；
The calculation of the microscopic contact angle in the step S61 is as follows: observing the liquid drop through a microscopic camera, and if the liquid drop is in wet contact with the rough surface, the wetting state of the liquid drop is Wenzel state, and the microscopic contact angle is recorded as thetaWThe calculation formula is as follows:
cosθW＝r cosθY (1)
if the liquid drop is not in wet contact with the rough surface, the wetting state of the liquid drop is Cassie state, and the microscopic contact angle is recorded as thetaCThe calculation formula is as follows:
cosθC＝φS(cosθY+1)-1 (2)
in the above formulae (1) and (2), θCMicroscopic contact angle in Cassie state; thetaWIs the micro contact angle in the Wenzel state, phiSAnd r is the roughness, i.e., the wetted surface to projected surface area ratio.
5. The method for contact angle measurement for microscopic and macroscopic simultaneous measurement and mutual authentication as claimed in claim 3, wherein the error in the step of S61 is calculated as follows:
in the above formula (3), θ'YiAnd thetaYiRespectively representing a plurality of macroscopic contact angles calculated through microscopic contact angles and corresponding known macroscopic contact angles, wherein in the plurality of groups of data, the group of data with the smallest error between the calculated macroscopic contact angles and the corresponding known macroscopic contact angles represents the closest match with the real contact angle of the liquid drop, and the corresponding contact angle is the measured contact angle of the liquid drop and the surface of the sample under the set working condition.
6. The method for contact angle measurement of microscopic and macroscopic simultaneous measurement and mutual authentication as claimed in claim 1, wherein the photographing in step S5 is performed from two orthogonal directions, and the sampling angle is corrected, so as to ensure the accuracy of the measurement process and achieve the microscopic and macroscopic simultaneous measurement.
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| CN115979901A (en) * | 2023-03-20 | 2023-04-18 | 中国科学院国家空间科学中心 | System for electrowetting experimental study based on variable force field generated by centrifugal machine platform |
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