CN114034607B - Device and method for measuring contact angle of micro round tube - Google Patents

Device and method for measuring contact angle of micro round tube Download PDF

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CN114034607B
CN114034607B CN202111333316.9A CN202111333316A CN114034607B CN 114034607 B CN114034607 B CN 114034607B CN 202111333316 A CN202111333316 A CN 202111333316A CN 114034607 B CN114034607 B CN 114034607B
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contact angle
water tank
measuring
projection
image
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CN114034607A (en
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赵玉刚
张晓东
顾恬
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University of Shanghai for Science and Technology
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N13/00Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
    • G01N13/02Investigating surface tension of liquids
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N13/00Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
    • G01N13/02Investigating surface tension of liquids
    • G01N2013/0208Investigating surface tension of liquids by measuring contact angle

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  • Life Sciences & Earth Sciences (AREA)
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Abstract

The invention relates to a measuring method of contact angle, in particular to a measuring device and a measuring method of contact angle of a tiny circular tube, comprising a light source, a water tank, a projection plate and an image recording device; the light source, the water tank and the image recording device are sequentially and vertically arranged on the same straight line; the projection plate is arranged at the bottom of the water tank. Compared with the prior art, the device is very simple, when the device is used, the sample on the sample rack can be replaced to obtain projection images of different samples, corresponding projection widths are obtained through processing, and the accurate calculation of the contact angle of the sample tube to be measured can be simply and rapidly realized through correlation to obtain the function relation between the projection widths and the contact angle. The measuring result has good stability and high accuracy, and the device is simple to operate and is suitable for practical use.

Description

Device and method for measuring contact angle of micro round tube
Technical Field
The invention relates to a measuring method of a contact angle, in particular to a measuring device and a measuring method of a contact angle of a tiny circular tube.
Background
Prior to the day, there are relatively sophisticated methods for measuring planar contact angles, generally two: firstly, an appearance image analysis method; and the second is a weighing method. The latter may also be referred to as a wetting balance or a penetrometer contact angle. The most widely applied method is the appearance image analysis method which is the most direct and accurate of the measured value. Principle of outline image analysis: the liquid drop is dropped on the surface of the solid sample, the appearance image of the liquid drop is obtained through a microscope lens and a camera, and then the contact angle of the liquid drop in the image is calculated by using digital image processing and some algorithms.
However, the contact angle measuring device and method for small samples are not perfect, the limit amount width can not meet the industry requirement, and especially for the contact angle measurement of a single round tube, the measurement can not be basically carried out. When the droplet size is too large to exceed the sample diameter, the measured data does not truly reflect the contact angle of the sample. The lens of the contact angle measuring instrument cannot amplify the magnification specifically, or after the magnification, the imaging outline is unclear, and the contact angle of the sample cannot be accurately measured.
The existing measuring method of the tiny circular tube has the following obvious defects:
1. Only transparent capillaries can be measured, but opaque metallic or non-metallic materials cannot be measured;
2. the contact angle of the outer surface of the circular tube cannot be used as the force, and only the internal contact angle can be measured;
3. The measuring method is complex and the manufacturing cost is high.
Disclosure of Invention
The invention aims to solve at least one of the problems, and provides a device and a method for measuring the contact angle of a micro circular tube, which establish a functional relation between projection width and contact angle and realize accurate measurement of the contact angle of the micro circular tube.
The aim of the invention is achieved by the following technical scheme:
the first aspect of the invention discloses a measuring device for the contact angle of a tiny circular tube, which comprises a light source, a water tank, a projection plate and an image recording device;
The light source, the water tank and the image recording device are sequentially and vertically arranged on the same straight line; the projection plate is arranged at the bottom of the water tank.
Preferably, the light source is a parallel light generator.
Preferably, the image recording device is a CCD or CMOS camera.
Preferably, the measuring device further comprises a sample holder, wherein the sample holder is arranged between the light source and the water tank and is arranged on the same straight line with the light source and the water tank.
The invention discloses a measuring method of a contact angle of a tiny circular tube, which comprises the following steps:
s1: taking a group of flaky materials with the contact angles distributed in a step manner, vertically inserting the flaky materials into a water tank respectively, obtaining rectangular projections at a light shielding plate at the bottom of the water tank, recording the projections by an image recording device, and carrying out gray scale processing on the recorded images;
s2: measuring contact angles of the materials respectively;
S3: fitting by taking the projection width as an independent variable and the contact angle of the material as an independent variable to obtain a functional relation between the projection width and the contact angle;
S4: and (3) vertically inserting the sample tube to be tested into the water tank, recording annular projection at the projection plate at the bottom of the water tank by using the image recording device, carrying out gray processing on the image, and substituting the projection width into the functional relation obtained in the step (S3) to obtain the sample tube contact angle to be tested.
Preferably, the sheet material with the group of contact angles distributed in a step manner is the same as the material of the sample tube to be tested, and comprises a hydrophobic material and/or a hydrophilic material, wherein the hydrophobic material is obtained by silane chemical vapor deposition of a base material; the hydrophilic material is obtained by cleaning a substrate by plasma.
Preferably, the substrate is glass, PMMA, silicon, copper or aluminum.
Preferably, the gas introduced in the plasma cleaning process is air or oxygen, and the cleaning time is 0.5-60min.
Preferably, the gray scale processing is sequentially performed by image subtraction, image clipping and gray scale transformation. Preferably, MATLAB is used to sequentially perform image subtraction, image cropping and gray scale transformation on the image. The image subtraction is to subtract the background and eliminate the background effect; image cropping is to obtain the desired area; the gray scale transformation is to convert the RGB image into a gray scale image to extract the projection width.
Preferably, the contact angle of each material measured in step S2 is measured by a contour image analysis method or a wilfory method. Preferably, the image recording device is placed horizontally and fixed, a droplet is placed on the material with a syringe and photographed to obtain a side view of the droplet, and then the actual contact angle size is obtained with ImageJ.
Preferably, the liquid level in the water tank is fixed in the test process, and the measurement result is not affected.
The working principle of the invention is as follows:
A group of flaky materials with the contact angles distributed in a step mode are vertically inserted into a water tank respectively, a concave area or a convex area formed by the materials and the liquid level forms rectangular projection on a light shielding plate at the bottom of the water tank under the irradiation of light emitted by a light source, and the rectangular projection is recorded and gray-scale processed through an image recording device. And respectively measuring the contact angles of the materials, taking the projection width at the projection depth dividing line as an independent variable, and fitting the contact angle of the materials as a dependent variable to obtain the functional relation between the projection width and the contact angle.
The sample tube is vertically inserted into the water tank, the circular projection is recorded through the image recording device, gray processing is carried out, the projection width is substituted into the function relation obtained in the previous, and the contact angle of the sample tube can be obtained.
The concave or convex parts formed by different contact angles in the water are different, and due to refraction of light, circular projection with light intensity and light intensity distribution is formed on the bottom surface, the projection width is determined by the hydrophilicity/hydrophobicity of the material in the water, and the contact angle of the sample tube to be measured can be obtained through the functional relation between the associated projection width and the contact angle.
Compared with the prior art, the invention has the following beneficial effects:
1. the device adopted by the invention is very simple, when in use, the samples on the sample rack can be replaced to obtain projection images of different samples, corresponding projection widths are obtained by processing, and the accurate calculation of the contact angle of the sample tube to be detected can be simply and rapidly realized by correlating the obtained function relation of the projection widths and the contact angle. The measuring result has good stability and high accuracy, and the device is simple to operate and is suitable for practical use.
2. The measuring method of the invention can measure the contact angle of various types of tiny round pipes, including but not limited to the measurement of the contact angle of tiny round pipes made of opaque metal or nonmetal materials, the measurement of the contact angle of the outer surface of the round pipes and the measurement of the contact angle of tiny round pipes with different pipe diameters.
3. The functional relation established by the invention can be reused in the subsequent test of the same material, and the experimental strength of the test can be greatly reduced on the basis of ensuring the accuracy of the result after the functional relation is established.
Drawings
FIG. 1 is a schematic structural view of a measuring device for the contact angle of a tiny circular tube;
FIG. 2 is a schematic representation of the hydrophobic optical path when the device and method of the present invention are used to determine hydrophobic materials;
FIG. 3 is a schematic view of a hydrophilic optical path when hydrophilic materials are measured using the apparatus and method of the present invention;
FIG. 4 is a graph showing the relationship between the projection width and the contact angle fitted by the apparatus and method of the present invention in example 2;
In the figure: 1-a light source; 2-a sample holder; 3-a water tank; 4-an image recording device; 5-device holder.
Detailed Description
The invention will now be described in detail with reference to the drawings and specific examples.
The measuring device of the contact angle of the tiny circular tube comprises a light source 1, a water tank 3, a projection plate and an image recording device 4, as shown in figure 1; the light source 1, the water tank 3 and the image recording device 4 are vertically arranged on the same straight line in sequence; the projection plate is arranged at the bottom of the water tank 3. Wherein, the light source 1 is a parallel light generator; the image recording device 4 is a CCD or CMOS camera. A sample holder 2 is further arranged between the light source 1 and the water tank 3, the sample holder 2 is arranged on the same straight line with the light source 1 and the water tank 3, and a sample to be measured is arranged on the sample holder 2. The light source 1, the water tank 3 and the image recording device 4 are all fixed on the device bracket 5, and the three are ensured to be in a straight line.
When the micro round tube needs to be measured, the method comprises the following steps:
S1: taking a group of flaky materials with the contact angles distributed in a step manner, vertically inserting the flaky materials into a water tank 3 respectively, obtaining rectangular projections at a light shielding plate at the bottom of the water tank 3, recording the projections by an image recording device 4, and sequentially carrying out image subtraction, image shearing and gray level conversion on the recorded images by adopting MATLAB; the image subtraction is to subtract the background and eliminate the background effect; image cropping is to obtain the desired area; the gray scale transformation is to convert the RGB image into a gray scale image to extract the projection width;
s2: horizontally placing and fixing the image recording device 4, respectively placing a liquid drop on the materials by using a syringe, shooting to obtain a side view of the liquid drop, and then obtaining the actual contact angle by using imageJ;
S3: fitting by taking the projection width as an independent variable and the contact angle of the material as the dependent variable to obtain a function relation between the projection width and the contact angle, wherein the obtained curve can be seen from the curve shown in figure 4;
S4: and (3) vertically inserting the sample tube to be tested into the water tank 3, recording annular projection at the light shielding plate at the bottom of the water tank 3 by using the image recording device 4, carrying out gray scale processing on the image, and substituting the projection width into the functional relation obtained in the step (S3) to obtain the sample tube contact angle to be tested.
Wherein, the sheet material with the group of contact angles distributed in a step manner can be made of different materials, such as glass, PMMA, silicon, copper, aluminum and the like.
The super-hydrophilic material is obtained by plasma cleaning, and preferably, the gas introduced in the plasma cleaning process is air or oxygen, and the cleaning time is 0.5-60 min.
The hydrophobic material is obtained by a chemical vapor deposition method, and the super-hydrophobic material can be obtained by oxidizing the copper surface into CuO and then performing the chemical vapor deposition method.
In fig. 4, a negative value of the x-axis refers to the projected width of the hydrophilic surface, and a positive value refers to the projected width of the hydrophobic surface.
In the test process, the liquid level in the water tank 3 needs to be kept constant, so that the measurement result is not affected.
The working principle of the invention is as follows:
A group of flaky materials with the contact angles distributed in a step manner are vertically inserted into the water tank 3 respectively, and concave or convex areas formed by the materials and the liquid level form rectangular projections on a projection plate at the bottom of the water tank 3 under the irradiation of light emitted by the light source 1, and the rectangular projections are recorded and subjected to gray scale treatment by the image recording device 4. And respectively measuring the contact angles of the materials, taking the projection width as an independent variable, and fitting the contact angles of the materials as dependent variables to obtain the functional relation between the projection width and the contact angle.
The sample tube is vertically inserted into the water tank 3, the circular projection is recorded and gray-scale processed by the image recording device 4, and the contact angle of the sample tube can be obtained by substituting the projection width into the function relation obtained before.
As shown in fig. 2 and fig. 3, the concave or convex portions formed by the different contact angles in the water are different, and due to refraction of light, a circular projection of light intensity light-shade distribution is formed on the bottom surface, and the projection width of the light-shade boundary line is determined by the hydrophilicity/hydrophobicity of the material in the water, so that the contact angle of the sample tube to be measured can be obtained through the function relation between the projection width and the contact angle.
Example 1
Measurement of contact angle of aluminum micro round tube:
step (1): taking a group of flaky materials with the contact angles distributed in a step manner, vertically inserting the flaky materials into a water tank 3 respectively, obtaining rectangular projections at a light shielding plate at the bottom of the water tank 3, recording the projections by an image recording device 4, and sequentially carrying out image subtraction, image shearing and gray level conversion on the recorded images by adopting MATLAB; the image subtraction is to subtract the background and eliminate the background effect; image cropping is to obtain the desired area; the gray scale transformation is to convert the RGB image into a gray scale image to extract the projection width;
Step (2): horizontally placing and fixing the image recording device 4, respectively placing a liquid drop on the materials by using a syringe, shooting to obtain a side view of the liquid drop, and then obtaining the actual contact angle by using imageJ;
step (3): fitting by taking the projection width as an independent variable and the contact angle of the material as an independent variable to obtain a functional relation between the projection width and the contact angle;
Step (4): polishing an aluminum tiny circular tube by sand paper, and then sequentially cleaning the aluminum tiny circular tube by acetone, IPA (isopropyl alcohol) and ultrapure water (or deionized water) for 10min by ultrasonic waves;
Step (5): vertically inserting an aluminum tiny circular tube into the water tank 3, and recording annular projection at the projection plate and profile of side meniscus (bulge formed by the aluminum tiny circular tube and the water surface) by using a CCD camera;
step (6): and (3) carrying out image subtraction, image shearing and gray level transformation on the image obtained in the step (5) by using MATLAB in sequence to obtain the projection width. Tangential line is made on the contact point position of the side meniscus and the aluminum tiny circular tube, and the contact angle of the profile analysis method is 40+/-2 degrees;
Step (7): taking the projection width as an independent variable, substituting a projection width-contact angle curve fitted before to obtain a contact angle of 41.5+/-2 degrees, which is similar to the contact angle under the contour analysis method, so that the method has accurate measurement result and can be used for practical application;
Step (8): the steps (1) - (4) are repeated twice, the results of the two steps are respectively substituted into the projection width-contact angle curve, the contact angles are calculated to be 41+/-2 degrees and 41.7+/-2 degrees, and the stability of the result obtained by the measurement of the method is good, the same result can be obtained by repeated test, the method has high reliability, and the method is suitable for practical use.
Example 2
Silanized copper tube contact angle measurement:
step (1): taking a group of flaky materials with the contact angles distributed in a step manner, vertically inserting the flaky materials into a water tank 3 respectively, obtaining rectangular projections at a light shielding plate at the bottom of the water tank 3, recording the projections by an image recording device 4, and sequentially carrying out image subtraction, image shearing and gray level conversion on the recorded images by adopting MATLAB; the image subtraction is to subtract the background and eliminate the background effect; image cropping is to obtain the desired area; the gray scale transformation is to convert the RGB image into a gray scale image to extract the projection width;
Step (2): horizontally placing and fixing the image recording device 4, respectively placing a liquid drop on the materials by using a syringe, shooting to obtain a side view of the liquid drop, and then obtaining the actual contact angle by using imageJ;
Step (3): fitting the projection width as an independent variable and the contact angle of the material as a dependent variable to obtain a function relation between the projection width and the contact angle (namely, a curve in fig. 4, wherein a negative value of an x axis refers to the projection width of a hydrophilic surface and a positive value refers to the projection width of a hydrophobic surface);
Step (4): sequentially ultrasonically cleaning the silanized copper tube with acetone, IPA (isopropyl alcohol) and ultrapure water (or deionized water) for 10min;
step (5): vertically inserting the silanized copper tube into the water tank 3, and recording the annular projection at the projection plate and the profile of the side meniscus (the projection formed by the silanized copper tube and the water surface) by using a CMOS camera;
Step (6): and (3) carrying out image subtraction, image shearing and gray level transformation on the image obtained in the step (5) by using MATLAB in sequence to obtain the projection width. Tangential line is made on the contact point position of the side meniscus and the silanized copper pipe, and the contact angle of the surface contour analysis method is 103+/-3 degrees;
step (7): taking the projection width as an independent variable, substituting a projection width-contact angle curve fitted before to obtain a contact angle of 105+/-3 degrees, which is similar to the contact angle under the contour analysis method, so that the method has accurate measurement result and can be used for practical application;
Step (8): the steps (1) - (4) are repeated twice, the results of the two steps are respectively substituted into the projection width-contact angle curve, the contact angles are calculated to be 105.5+/-3 degrees and 104.6+/-3 degrees, the stability of the result obtained by the measurement of the method is good, the same result can be obtained by repeated tests, the method has high reliability, and the method is suitable for practical use.
The previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present invention. It will be apparent to those skilled in the art that various modifications can be readily made to these embodiments and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments, and those skilled in the art, based on the present disclosure, should make improvements and modifications without departing from the scope of the present invention.

Claims (9)

1. The measuring method of the contact angle of the tiny circular tube adopts a measuring device of the contact angle of the tiny circular tube, and is characterized in that the measuring device comprises a light source (1), a water tank (3), a projection plate and an image recording device (4);
the light source (1), the water tank (3) and the image recording device (4) are sequentially and vertically arranged on the same straight line; the projection plate is arranged at the bottom of the water tank (3);
The measuring method comprises the following steps:
S1: taking a group of flaky materials with the contact angles distributed in a step manner, vertically inserting the flaky materials into a water tank (3) respectively, obtaining rectangular projections at a light shielding plate at the bottom of the water tank (3), recording the projections by an image recording device (4), and carrying out gray scale processing on the recorded images;
s2: measuring contact angles of the materials respectively;
S3: fitting by taking the projection width as an independent variable and the contact angle of the material as an independent variable to obtain a functional relation between the projection width and the contact angle;
S4: and (3) vertically inserting the sample tube to be tested into the water tank (3), recording annular projection at the projection plate at the bottom of the water tank (3) by using the image recording device (4), carrying out gray processing on the image, and substituting the projection width into the functional relation obtained in the step (S3) to obtain the sample tube contact angle to be tested.
2. The method for measuring the contact angle of the tiny circular tube according to claim 1, wherein the light source (1) is a parallel light generator.
3. The method for measuring the contact angle of the tiny circular tube according to claim 1, wherein the image recording device (4) is a CCD or CMOS camera.
4. The method for measuring the contact angle of the tiny circular tube according to claim 1, wherein the measuring device further comprises a sample holder (2), and the sample holder (2) is arranged between the light source (1) and the water tank (3) and is arranged on the same straight line with the light source (1) and the water tank (3).
5. The method for measuring the contact angle of the micro circular tube according to claim 1, wherein the flaky materials with the stepwise distribution of the contact angles are the same as the material of the sample tube to be measured, and the flaky materials comprise hydrophobic materials and/or hydrophilic materials, and the hydrophobic materials are obtained by silane chemical vapor deposition of a base material; the hydrophilic material is obtained by cleaning a substrate by plasma.
6. The method of claim 5, wherein the substrate is glass, PMMA, silicon, copper or aluminum.
7. The method for measuring the contact angle of a tiny circular tube according to claim 5, wherein the gas introduced in the plasma cleaning process is air or oxygen, and the cleaning time is 0.5-60 min.
8. The method for measuring the contact angle of the micro round tube according to claim 1, wherein the gray scale processing is sequentially performed by image subtraction, image shearing and gray scale transformation.
9. The method according to claim 1, wherein the contact angle of each material is measured in step S2 by a profile image analysis method or a wilfory method.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102654442A (en) * 2011-03-04 2012-09-05 中国人民解放军军事医学科学院毒物药物研究所 Surface tension detection device and method
CN108956384A (en) * 2018-05-30 2018-12-07 陕西科技大学 A kind of optical means of synchro measure liquid surface tension coefficient and contact angle

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102654442A (en) * 2011-03-04 2012-09-05 中国人民解放军军事医学科学院毒物药物研究所 Surface tension detection device and method
CN108956384A (en) * 2018-05-30 2018-12-07 陕西科技大学 A kind of optical means of synchro measure liquid surface tension coefficient and contact angle

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
《Dynamic measurement of low contact angles by optical microscopy》;James Campbell et al.;《ACS Applied Materials & Interfaces》;第第10卷卷;第16894页左栏第2段-第16896页左栏第1段及图3-4 *

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