CN106501134A - The accurate measurement method of low-angle contact angle - Google Patents
The accurate measurement method of low-angle contact angle Download PDFInfo
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- CN106501134A CN106501134A CN201611228803.8A CN201611228803A CN106501134A CN 106501134 A CN106501134 A CN 106501134A CN 201611228803 A CN201611228803 A CN 201611228803A CN 106501134 A CN106501134 A CN 106501134A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
- G01N13/02—Investigating surface tension of liquids
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
- G01N13/02—Investigating surface tension of liquids
- G01N2013/0208—Investigating surface tension of liquids by measuring contact angle
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Abstract
The accurate measurement method of low-angle contact angle, is imaged from above sample；Led area sources using release directional light；Led light source overall brightnesses are consistent；Led light sources area is more than 1.2 times of test sample area；Angle of incidence and angle of reflection are respectively less than 45 degree；By directional light specimen surface focusing, in photoshop, all sample backgrounds chosen below of tolerance 20, so as to the differentiation of wetting liquid and sample background；The imaging of drop is realized using the difference between droplet surface scattering and specimen surface reflected in parallel；The calculating of drop occupied area is obtained so that the total pixel of drop accounts for the ratio of the total pixel of sample or indirect calculating of ratio between radius and actual samples length；After investigating drop area, by drop areal calculation droplet radius, contact angle is then calculated.The exact evaluation of little contact angle is the global problem for being difficult to capture, and the present invention is realized to little contact angle exact evaluation.
Description
Technical field：
Liquid is a kind of very important natural phenomena of nature in the wetting phenomena of the surface of solids, to the production of people and
Life has very important impact.This patent solves low-angle profit by changing imaging direction and complete householder methods
Wet cannot accurate measurement problem.
Background technology
When liquid is with solid contact, liquid can be along the surface of solids to external expansion, original solid and gas circle in simultaneity factor
Face and liquid gas interface are gradually replaced by new solid liquid interface, and this process is referred to as moistening.The journey of liquid versus solid surfaces moistening
Degree is referred to as the wettability of the surface of solids.
Wettability is one of key property of the surface of solids, plays important in industrial and agricultural production and people's daily life
Effect, such as oil exploitation, pesticide spraying and fabric waterproof and washing etc..Surface wettability depends primarily on the surface of solids
Roughness and surface free energy, contact angle of its size generally by drop and the surface of solids is weighing.In the state of the equilibrium, solid
Body, liquids and gases three-phase intersection do the tangent line of solid and liquid surface respectively, and two tangent lines are formed in liquid internal
Angle is contact angle (θ angle in Fig. 1).The accurate measurement of contact angle has very important effect for the research of association area.
Contact angle measurement is the visual plant of Contact-angle measurement.At present, conventional Contact-angle measurement be from image side faces,
Contact angle is directly read, as shown in Figure 2：
The characteristics of this measuring method, is directly found a view along surface of test piece horizontal direction, and method of testing does not directly have theory
Error.The main method of current Contact-angle measurement is become.But when contact angle smaller droplet is relatively large in diameter, the drop edge depth of field
Increase (as shown in Figure 3) with the growth of droplet radius.And due to liquid height limited, it is impossible to provide enough light anti-
Penetrate, drop edge imaging will appear from larger error so that final measurement error will be doubled and redoubled.
Content of the invention：
For these reasons, current contact angle test equipment can produce larger error under 10, contact angle more little then
Measurement error is bigger.When required precision is not high, when contact angle is spent less than 5-7, research worker often thinks liquid complete wetting, no
Furtherd investigate again.And although actually a lot of liquid can obtain less contact angle, wettability still has
Different.In near liquid excellent in select excellent, distinguish optimal moistening medium in particular surface, in super close moistened surface etc.
Most important in the research in field, but this needs is more advanced and high-precision measuring method is used as support.Current test
Although mechanism has carried out unremitting effort in the field such as stability of light source, method of testing and platform, due to method of testing
Limitation, the exact evaluation of little contact angle remain a global problem for being difficult to capture.Overcome the problems referred to above, to little contact
Angle exact evaluation is the main starting point of this patent.
The accurate measurement method of low-angle contact angle, it is characterised in that：It is imaged from above sample；
Contact angle testing light source and position include following four key element：
A) the Led area sources of directional light are discharged；
B) Led light sources overall brightness is consistent, and deviation is not more than 5%；
C) Led light sources area is more than 1.2 times of test sample area；
D) angle of incidence and angle of reflection are respectively less than 45 degree；
By directional light specimen surface focusing, in photoshop, all sample backgrounds chosen below of tolerance 20,
So as to wetting liquid and the differentiation of sample background；Realized using the difference between droplet surface scattering and specimen surface reflected in parallel
The imaging of drop；The calculating of drop occupied area is ratio or radius and the actual examination for accounting for the total pixel of sample with the total pixel of drop
Ratio between sample length is calculated indirectly and is obtained；After investigating drop area, by drop areal calculation droplet radius, then calculate and connect
Feeler.
Further, the low-angle moistening to contact angle less than less than 10 degree is evaluated.
Further, Contact-angle measurement realizes the single measurement requirement of particular point in time, or realizes a certain setting time section
The dynamic evaluation of lower drop wetting state；During dynamic evaluation, evaluation time is not less than 1 minute, and testing time is no less than 5 times.
Description of the drawings
Fig. 1 contact angle schematic diagrams
The conventional contact angle test view directions of Fig. 2 are arranged
Change of Fig. 3 contact angle detections depth of field with droplet radius
Fig. 4 contact angle view directions
Fig. 5 drop imaging schematic diagrams
The imaging picture of Fig. 6 moistening drops
Fig. 7 drops distinguish design sketch
Fig. 8 software set parameters
Contact angle of Fig. 9 n-butyric acies on silicon carbide ceramics surface changes over situation
Picture after Figure 10 process
Specific embodiment
The setting of 1 view direction
For the problem for existing above, be improved design to test philosophy, by image side faces be changed to from above sample into
Picture, so as to easily obtain the whole drop top view after drop spreads, then recycles the area of drop to be solved.So
Design solves the problems, such as that low-angle contact angle cannot accurately image.Concrete view direction is as shown in Figure 4：
This method of testing is changed to be imaged from above sample by the image side faces in the test of common contact angle, eliminates the depth of field pair
The impact of imaging, so that be readily available the whole droplet morphology after drop spreads, the moistening of accurate perception low-angle moistening drop
State.
2 light source illuminating method principles and design
Reagent is dropped on sample, most drop be transparent, approximate with print color, it is impossible to blur-free imaging.In test
One area source of middle offer, is allowed to cover whole sample, and drop is different with sample reflection ray angle, so as to clear in camera
Imaging.Schematic diagram such as Fig. 5
Wherein, θ and θ ' is angle of incidence and angle of reflection.
Contact angle testing light source needs to be specifically designed, and its most important feature includes following key element：
A) directional light can be discharged, rather than point source scattering.
B) Led light sources overall brightness is consistent, and deviation is not more than 5%.
C) Led light sources area is more than more than 1.2 times of test sample area.
D) angle of incidence and angle of reflection are less than 45 degree.
3rd, the preparation method of moistening print.
Digital imaging device is placed at Fig. 5 camera lenses, Wet Out of the liquid in specimen surface is obtained.Due to this test
Needs are continuously shot, and therefore, picture pick-up device should possess self-timing shoot function, and pixel meets wanting for blur-free imaging
Ask (pixel is more than 2,000,000).In today that digital equipment is flourishing, relevant device is a lot.For example, general slr camera and specially
Digital imaging device can realize such function.Due to not being the protected right content of invention, no longer deep here
Enter to introduce.By directional light specimen surface focusing so that moistening sample shoot after surface color be close to consistent (
When tolerance is less than 20 in photoshop, all sample figure viewed from behind colors can be extracted), as shown in Figure 6.
If investigating the Wet Out at a certain moment, it is only necessary to shoot a photo.Such as need to investigate drop in sample
The dynamic moisture process on surface, then need to shoot multiple pictures under time conditions at equal intervals.When investigating dynamic moisture process, see
The survey time should be greater than 1 minute, shoots photo number and is no less than 5.
The extraction of 3 drop wetting areas
In photoshop, following methods are adopted to remove drop with exterior domain.1st, artificial selection's non-wetted print is with outskirt
Domain simultaneously removes；2nd, it is 20 to select tolerance, selects all moistening print regions with magic wand tool and removes.Droplet morphology after differentiation
As shown in Figure 7:
The calculating of 3 contact angles
The calculating of contact angle includes following step：
By the pixel value of length of the wetted print in picture in scale functional measurement Fig. 6 in PS softwares, and utilize
Long * width calculates the total pixel of wetted print.
Physical length and the width of wetted print is measured, print real area is calculated.
Histogram module is opened in PS softwares, is selected drop and is read total pixel value of 4 dropping liquids drop in Fig. 7.
Can be in the hope of the area of 4 dropping liquids drop by the pixel ratio of drop and print.The area that 4 dropping liquids are dripped is obtained divided by 4
Average area to each of the droplets.
According to round area formula：A=π r2, you can try to achieve droplet radius r.Actual radius value can also pass through radius
Calculate with the proportionate relationship of print length.
Bring radius r into formula：
Contact angle of the reagent in specimen surface can be tried to achieve.
Wherein, v is droplet size.The value is the meansigma methodss that early stage tests each of the droplets volume；R is droplet radius；θ is to connect
Feeler.
As formula 1 is simple cubic equation, appropriate method accounting equation solution is needed.For example, using Excel in monotropic
Amount solving method or program calculation can realize this purpose.
Case:
Contact angle of the measurement n-butyric acie on silicon carbide ceramics surface.
1st, experimental situation
(1) temperature design
Due to experiment not just for single object of experiment, under condition of different temperatures the surface tension of organic chemical reagent and
Different in the spreadability of the surface of solids, it is to reduce the deviation that temperature is caused to the measurement result of wetting test, it is ensured that test data
True and reliable, test temperature must be constant.In this experiment, experimental site and temperature of reagent are manually set as 25 degree.Synthermal bar
Under part, different reagents can show more preferable comparability.
(2) dustfree environment
In process of the test, reagent droplet exposes in atmosphere, and the dust in inevitable air can fall in test solution drop
On, affect drop sprawls situation.For reducing the deviation that dust granules are caused to the measurement result of wetting test, it is ensured that test number
According to true and reliable, test need to be carried out under dustfree environment.This experiment is carried out after carrying out dust-removing process under enclosed environment.
(3) specimen surface is processed
Moistening surface needs the foreign substance for removing surface adhesion as much as possible.Silicon carbide ceramics sample warp in present case
Cross ultrasonic cleaning and high-temperature process.Experimental result is only responsible for this sample.
2nd, test equipment
Picture pick-up device：Canon's 700D single-lens reflex cameras
Moistening test platform：JGW-360r contact angles test platform and micro-sampling system
Light source：Three sections of brightness adjustable LED light sources
3 test processs and result
(1) slr camera is mounted on camera support, is connected with computer, camera is carried out using EOS Utility softwares
Connection.This testing setup camera parameter such as Fig. 8；
(2) by n-butyric acie suck microsyringe and be fixed on contact angle instrument micro-feed mechanism；
(3) average estimation is carried out per drop of liquid to microsyringe, and test drop number is not less than 50 drops；
(4) sample is positioned over test platform setting position, and is focused, at the same adjust podium level, make sample with
Suitable distance is kept between syringe；
(5) rotating screw knob, on print, drippage 4 drips reagent, and print is moved to photographed region by quick and stable；
(6) EOS Utility software start buttons are clicked on, is shot, shooting interval 10 seconds is continuously shot 15 (such as
Shown in Fig. 9)；
(6) using photoshop softwares, photo wetted portions in Fig. 9 are extracted.And record correlation computations information.
Picture after process is as shown in Figure 10：
(7) recorded by photoshop using contact angle of the associated information calculation n-butyric acie on silicon carbide ceramics surface
Auxiliary information is as shown in table 1：
1 contact angle of table calculates auxiliary information table
| Volume | 4.3 microlitre |
| Specimen length pixel | 1350 |
| Sample physical length | 49.8 |
| The ratio of length pixel and physical length | 27.10843 |
The moistening data recorded by photoshop and result of calculation are as shown in table 2：
2 contact angle of table calculates information table
From table 2 it can be seen that moistening of the n-butyl alcohol on silicon carbide ceramics surface is increased over time from initial 4.95
Degree is constantly decreased to 2.9 degree and keeps stable.
It is emphasized that in this test, it is 2.9 degree finally to keep stable contact angle on silicon carbide ceramics surface,
The contact angle cannot be measured in conventional contacts angle tester.As this patent is measured using top view, therefore moisten
Wetted surface is bigger, and contact angle is less, then certainty of measurement is higher, compensate for the deficiency of conventional contacts angle measuring method.
Additionally, during measurement contact angle, should carry out when wetting liquid is stable in theory, but different wetting liquids is reached
The time of steady statue is different.Method of this patent using Timing measurement, can preferably by the change of wet processes
Find stable wetting state.Avoid the long waiting time and the contact angle change for bringing that evaporates, improve measurement
Precision.
Claims (3)
1. the accurate measurement method of low-angle contact angle, it is characterised in that：It is imaged from above sample；
Contact angle testing light source and position include following four key element：
A) the Led area sources of directional light are discharged；
B) Led light sources overall brightness is consistent, and deviation is not more than 5%；
C) Led light sources area is more than 1.2 times of test sample area；
D) angle of incidence and angle of reflection are respectively less than 45 degree；
By directional light specimen surface focusing, in photoshop, all sample backgrounds chosen below of tolerance 20, so as to
Wetting liquid and the differentiation of sample background；Drop is realized using the difference between droplet surface scattering and specimen surface reflected in parallel
Imaging；The calculating of drop occupied area is that the ratio or radius and actual samples for accounting for the total pixel of sample with the total pixel of drop is long
Ratio between degree is calculated indirectly and is obtained；After investigating drop area, by drop areal calculation droplet radius, contact is then calculated
Angle.
2. method according to claim 1, it is characterised in that：Low-angle moistening of the contact angle less than less than 10 degree is carried out
Evaluate.
3. method according to claim 1, it is characterised in that：Contact-angle measurement realizes that the single measurement of particular point in time will
Ask, or realize the dynamic evaluation of drop wetting state under a certain setting time section；During dynamic evaluation, evaluation time is not less than 1
Minute, testing time is no less than 5 times.
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Cited By (10)
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| CN107817193A (en) * | 2017-10-27 | 2018-03-20 | 清华大学 | Super-hydrophobic surface of solids contact angle measuring method and system based on partial circle fitting |
| CN108398117A (en) * | 2017-02-08 | 2018-08-14 | 中国科学院物理研究所 | The method for detecting the surface smoothness of two-dimensional material |
| CN108982305A (en) * | 2018-05-03 | 2018-12-11 | 浙江工业大学 | A kind of calculation method of horizontal rule double roughness surface heavy-fluid drop profiles and contact angle |
| CN109709001A (en) * | 2017-10-25 | 2019-05-03 | 河北工业大学 | Based on optical Contact-angle measurement system |
| CN110501263A (en) * | 2018-05-16 | 2019-11-26 | 宝山钢铁股份有限公司 | A kind of tin plate sheet surface wettability evaluation method |
| CN110967280A (en) * | 2018-09-28 | 2020-04-07 | 财团法人工业技术研究院 | Surface wettability detection system and surface wettability detection method |
| CN112683734A (en) * | 2020-11-25 | 2021-04-20 | 江苏科技大学 | Hydrophobic surface performance testing device and method thereof |
| CN114113090A (en) * | 2021-11-22 | 2022-03-01 | 中国药科大学 | Dynamic characterization method for wettability of medicine powder |
| US11709133B2 (en) | 2018-09-28 | 2023-07-25 | Industrial Technology Research Institute | Solid surface wettability determination method |
| CN117153713A (en) * | 2023-10-25 | 2023-12-01 | 江苏惠达电子科技有限责任公司 | Method, system and equipment control method for detecting residual pollutants of frequency components |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108398117A (en) * | 2017-02-08 | 2018-08-14 | 中国科学院物理研究所 | The method for detecting the surface smoothness of two-dimensional material |
| CN109709001A (en) * | 2017-10-25 | 2019-05-03 | 河北工业大学 | Based on optical Contact-angle measurement system |
| CN107817193A (en) * | 2017-10-27 | 2018-03-20 | 清华大学 | Super-hydrophobic surface of solids contact angle measuring method and system based on partial circle fitting |
| CN107817193B (en) * | 2017-10-27 | 2020-12-04 | 清华大学 | Method and system for measuring contact angle of super-hydrophobic solid surface based on local circle fitting |
| CN108982305B (en) * | 2018-05-03 | 2020-07-28 | 浙江工业大学 | Method for calculating profile and contact angle of heavy liquid drop on horizontal regular double-roughness surface |
| CN108982305A (en) * | 2018-05-03 | 2018-12-11 | 浙江工业大学 | A kind of calculation method of horizontal rule double roughness surface heavy-fluid drop profiles and contact angle |
| CN110501263A (en) * | 2018-05-16 | 2019-11-26 | 宝山钢铁股份有限公司 | A kind of tin plate sheet surface wettability evaluation method |
| CN110501263B (en) * | 2018-05-16 | 2022-06-28 | 宝山钢铁股份有限公司 | Tin plate surface wettability evaluation method |
| CN110967280A (en) * | 2018-09-28 | 2020-04-07 | 财团法人工业技术研究院 | Surface wettability detection system and surface wettability detection method |
| US11326997B2 (en) | 2018-09-28 | 2022-05-10 | Industrial Technology Research Institute | Surface wettability determination method |
| US11709133B2 (en) | 2018-09-28 | 2023-07-25 | Industrial Technology Research Institute | Solid surface wettability determination method |
| CN112683734A (en) * | 2020-11-25 | 2021-04-20 | 江苏科技大学 | Hydrophobic surface performance testing device and method thereof |
| CN114113090A (en) * | 2021-11-22 | 2022-03-01 | 中国药科大学 | Dynamic characterization method for wettability of medicine powder |
| CN117153713A (en) * | 2023-10-25 | 2023-12-01 | 江苏惠达电子科技有限责任公司 | Method, system and equipment control method for detecting residual pollutants of frequency components |
| CN117153713B (en) * | 2023-10-25 | 2024-02-02 | 江苏惠达电子科技有限责任公司 | Method, system and equipment control method for detecting residual pollutants of frequency components |
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Application publication date: 20170315 |