CN104697900A - Method for measuring interface tension and contact angle under vacuum controlled-temperature conditions, and apparatus thereof - Google Patents
Method for measuring interface tension and contact angle under vacuum controlled-temperature conditions, and apparatus thereof Download PDFInfo
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Abstract
The invention discloses an apparatus for measuring the interface tension and the contact angle under vacuum controlled-temperature conditions, and a method thereof. The apparatus comprises a vacuum controlled-temperature cavity made of quartz glass and having double side observation windows, a vacuum connecting fitting, a syringe pump, a syringe pump control part, a camera with a telecentric lens, and a parallel light source; and the contact angle and the interface tension are obtained through shooting the profile image of a liquid drop and adopting fitting Young-Laplace equation test. The apparatus and the method can be used to analyze the contact angle and the interface tension under different pressures, have extremely wide popularization prices in the fields of oilfields, petrochemical engineering and new material researches, allow the interface tension and the contact angle to be measured by stimulating the practical degree of vacuum and temperature of space especially in a space environment stimulation experiment, and are very effective.
Description
Technical field
The present invention relates to a kind of determinator and assay method of interface parameter, be specially a kind of measurement mechanism for test interface tension force and contact angle values under vacuum and controlled temperature conditions and method, belong to surface chemistry analysis field.
Background technology
Liquid-liquid interface tension force, liquid-basic index such as gas meter surface tension and solid-liquid contact angle values is the basic parameter characterizing material physicochemical property.Contact angle refer in solid level plane drip on a droplet drop, the solid-liquid on solid surface-gas three-phase point of interface place, the angle formed when its gas-liquid interface and solid-liquid interface two tangent line are clipped in liquid phase wherein, is shown in accompanying drawing 1.Contact angle test is the main means analyzing solid-liquid interface physicochemical property, by testing the contact angle values obtained, through Equation of state algorithm, the surface tension value (dyne value) only using a kind of drop just can analyze very accurately to draw solid.And liquid-liquid interface tension force and the capillary test of liquid-gas are also topmost physical indexs in physicochemical analysis.By theoretical analysis, we know, pressure and temperature is the main two indices affecting material surface chemical property.The singularity of testing contact angle and interfacial tension under vacuum condition is: vacuumize and liquid can be absorbed rapidly.Therefore, the general theoretic solution in existing patent cannot meet this respect demand at all.As the Chinese patent ZL200910034768.X device of synchro measure drop temperature, surface tension, contact angle " a kind of temperature control wet " and ZL201210127093.5 " measuring the device of liquid-drop contact angle and roll angle under wet, the pressure control condition of a kind of temperature control, control ", describe that a kind of temperature control, control are wet, measure the device of liquid-drop contact angle and roll angle under pressure control condition, that a kind of fuzzyyer theoretical property describes, concrete implementation detail is also that generality describes, from enforcement, particularly under vacuum, operability is not had.
At present, contact angle and interfacial tension testing tool are all instruments of standard design usually.As " measuring analyzer for dynamic characteristics of liquid surface and interface based on high rate burst communication " patent No. in existing Patent data storehouse: 200610050811.8 and 200620103753.6, " a kind of automatic testing method of static contact angle " patent No. 201010288857.X, " contact angle and surface energy measurement mechanism " patent No.: 201010600278.4, " measuring contact angle device " patent No.: 200710142656.7, " a kind of On-line Measuring Method of self clean glass contact angle " patent No.: 200710008521.1 etc.
On the algorithm of contact angle and interfacial tension, the content that Chinese patent data has part to mention to content of the present invention has certain similar, but there is larger difference in the realization of concrete summary of the invention.As, " a kind of measuring method of liquid-drop contact angle on solid surface and device " patent No.: 200910136101.0.In specific implementation, this patent have employed having discrete partial differential equation of second order to solve curve and adopting shooting method matching contact angle angle value of the rewriting of Young-Laplace equation, only propose the concept of the Young-Laplace equation model of a simple Liquid contact angle test, specific implementation process may not be high.A kind of measuring method of the liquid interfacial tension based on drop profile curve four measurement point is proposed in Chinese patent ZL201210566095.4 " measuring method based on the liquid interfacial tension of drop profile curve four measurement point ", the method is the picture under adopting the image capture device production picture sprawled on subtest platform upper surface of drop or drop to hang on the rotational symmetry additional bearing surface of horizontal positioned, carries out process extraction drop profile curve to picture; Drop profile curve is chosen four measurement points, measures the vertical distance between adjacent measurement points, each measurement point crosses the distance between the horizontal line of measurement point and the intersection point of drop profile curve, angle between the tangent line of the drop profile curve of each measurement point and horizontal line; The liquid volume relevant to four measurement points is calculated according to drop profile curve; The interfacial tension of liquid is gone out according to formulae discovery.Only that geometry conversion has been carried out to outline portion in algorithm, completely inconsistent with the innovative point of this patent.ZL201210594516.4 " a kind of computing method of static contact angle " proposes a kind of drop edge producing different volumes and contact angle based on the emulation of Young-Laplace equation; The contact angle of drop edge that computer sim-ulation produces, and then obtain the relation calculating gained contact angle, droplet size and actual contact angle; Take true Liquid particle image, the contact angle of computed image; According to calculating gained contact angle, droplet size and the relation at actual contact angle and the contact angle of real image, method of interpolation or similar approach is adopted to obtain contact angle accurately.This is a kind of simple application, and does not relate to concrete algorithm.
As a kind of method that optical method surface chemistry is analyzed, image analysis surface chemistry analytical technology has similar techniques in the world, usually occurs with the form of Young-Laplace equation model.But because algorithm and development of computer affect very large, these Young-Laplace matchings or adopt Bashforth-Adams look-up table or simple experience to solve (with Bashforth.F, Adams.J.C, Andreas, S. Hartland etc. are representative, or adopt based on DS/DE or base point (30 °, 45 °, 60 ° of angle values) algorithm of Select plane quick interface tension test of coordinate ratio, with Springer, F.K.Hansen etc. are representative, or adopt ALFI algorithm with the simple image analysis of empirical hypothesis, with Rotenberg, A.W.Neumann, O.I.del.RIO is representative, all there is open defect, the image analysis of the completely true drop profile (RealDrop) mentioned with this patent has certain difference.
In foreign patent, Jap.P. JP63210748A " contact angle お I び interface Zhang power Zi Move Measuring determines method " proposes a kind of method based on wide supreme people's court calculating contact angle values and this patent has obvious difference; In US Patent No. 5615276 " METHOD OF MEASURING LOW INTERFACIAL TENSION BY PENDANT DROP DIGITIZATION ", propose a kind of Young-Laplace and solve the method drawing interfacial tension and contact angle, its core algorithm adopted is identical with people such as F.K.Hansen, based on the Young-Laplace fitting technique under Select Plane algorithm, so, have any different with the algorithm mentioned by this patent.US Patent No. 5479816 " CAPTIVE DROPLET INTERFACIAL TENSIOMETER AND METHODS OF USE THEREOF " proposes a kind of very special Young-Laplace non trivial solution method, and the solution method mentioned with this patent is completely different.And other patents such as US4688938, US4953389, US5080484, US5115677, US5143744, US5394740, US7952698B2, US2003/0049863/Al, US2005/0012894/Al, WO0122058A1, US8151635B2 are all some special contact angle proving installation and application, completely different from the innovative point of this patent.
US Patent No. 4942760 " APPARATUS FOR THE MEASUREMENT OF INTERFACIAL TENSION " proposes the device having test interface tension force under pressure condition of a phase pairing approximation, but its patent main innovate point is can by the method for liquid-gas interface tension force under mechanism's testing high voltage condition of syringe needle of can changing online of a particular design, need to use two supercharge pumps although propose, but its principle of work is complete Stress control by the mode of pressure cycling, instead of inject two-way liquid, pass through simulation analysis, we also can reach a conclusion further, the sealing of such device is very general, the seal request under condition of high voltage cannot be completed, and the usual pressure of liquid-gas interface tension test is increased to some, and namely gas liquefy, and cannot complete test at all.From the mechanism design of needle exchange head, the testing algorithm of such device is most basic select plane algorithm, and the diameter of syringe needle directly can have influence on measured value result.So the content proposed in patent relatively backwardness, exploitativeness is general, also cannot solve that aforesaid UHV (ultra-high voltage), control are wet, the demand of high precision interfacial tension and contact angle measured value.
Summary of the invention
For problems of the prior art and deficiency, the invention provides a kind of for solving interfacial tension under vacuum and controlled temperature conditions and contact angle proving installation and method of testing, video camera and the source of parallel light of the vacuum temp control cavity of the bilateral view window that this device is made up of quartz glass, bonding in vacuum accessory, syringe pump and control assembly thereof, band telecentric lens form.After contour images by shooting drop, the test of matching Young-Laplace equation is adopted to obtain contact angle and interfacial tension value.
For realizing vacuum and temperature control (maximum temperature-50-200 degree, depend on the temperature of the Water Tank with Temp.-controlled of temperature control) complete high precision measurement under condition and have sticky all contact angles of product system and the object of interfacial tension, the invention provides measuring method and the device of interfacial tension and contact angle values under a kind of vacuum, controlled temperature conditions, concrete summary of the invention is as follows:
1, design the topology layout that combines general conditions and vacuum temp control condition image method contact angle and interfacial tension test, vacuum, the measurement mechanism of interfacial tension and contact angle values under controlled temperature conditions, as shown in Figure 2, comprise: pressure cap, upper cover plate, KF50 standard interface, quartz glass view window, kapillary, pressure cap, vacuum valve, microsyringe, syringe pump, Vertical dimension moves one dimensional optical translation stage, support, telecentric lens, camera lens set collar, video camera, electric control box (comprises stepper motor driver, motion control card, control circuit for light source etc.), LED source of parallel light, XYZ three-dimensional optical translation stage, KF16 vacuum interface, two-dimensional level adjustment platform, syringe needle, four horizontal adjustment pin, camera fixing support, the rear of vacuum cavity provides temperature sensor and recirculated water/conduction oil fast interface, the XY two-dimensional optical translation stage that one controls syringe needle right position is provided in syringe pump control structure.
Above-mentioned horizontal adjustment pin 21 is fixed on corner, frame lower end, frame two is provided with support 11 and electric control box 15, horizontal light source 16 is arranged at electric control box side, support 11 is provided with telecentric lens 12, camera lens set collar 13, video camera 14, camera lens set collar 13, a camera fixing support 22 is set below video camera 14, support 11 upper end is provided with Vertical dimension and moves one dimensional optical translation stage 10, Vertical dimension moves on one dimensional optical translation stage 10 and is fixed with syringe pump 9, syringe pump 9 connects an XY two-dimensional optical translation stage, syringe pump 9 lower end is connected with microsyringe 8, vacuum valve 7 is connected with below microsyringe 8, vacuum valve 7 connects kapillary 5 upper end by pressure cap 6, kapillary 5 lower end syringe needle 20 is through upper cover plate 2, in quartz observing window 4 window in KF50 vacuum interface 3 to vacuum temp control cavity 26, kapillary 5 by pressure cap 1 and with the pressure ring press seal of chamfering in both sides on upper cover plate 2, vacuum temp control cavity 26 connects two-dimensional level adjustment platform 19, is XYZ three-dimensional optical translation stage 17 below two-dimensional level adjustment platform 19.
2, for making drop profile reach sub-pixel, in the selection of camera lens and light source, following structure is adopted: (1), in the selection of camera lens, adopts telecentric lens, thus significantly promotes the sharpness of the depth of field and contour edge; (2) in the selection of background light source, adopt LED source of parallel light, thus significantly promote the sharpness of the depth of field and contour edge; (3) in the selection of video camera, broadcasting speed is selected to reach above high-speed camera 60 frames/second.
3, the measuring method of interfacial tension and contact angle values under vacuum, controlled temperature conditions, comprise: (1) proposes the Young-Laplace system of equations of discretize, (a sessile drop) dripped for the stopping during image analysing computer of side-looking method, bubble catches (Captive bubble) or hanging drop (pendant drop):
Wherein: θ is contact angle, s is arc length, R
0for the radius-of-curvature of vertex position, Δ ρ is that inside and outside phase density is poor, and z height, x is width, and V is volume, and A is area, and (x0, z0) is apex coordinate.
(2) solution that solves Young-Laplace discrete equation group is designed, specific as follows: use the discrete equation group as above mentioned by (1) when using the theoretical curve of Software on Drawing drop profile, utilize Long Gekula (Runge-Kutta) or position, Europe (Euler) method or similar method theory of solving curve, and the mode utilizing software to draw, show each coordinate points (x on corresponding theoretical curve and curve
i, y
i).
(3) a kind of method of drawing the actual curve of contact angle and interfacial tension drop profile is designed, specifically comprise: utilize CANNY or SOBEL algorithm, imaging system is utilized to take the change obtaining gray scale in rotating liquid drop contour images, reasonable threshold value is set, find out the edge of drop profile, and the edge utilizing Spline algorithm to do to search is optimized calculating, obtain the marginal point coordinate figure (X of drop profile
i, Y
i) and ordered arrangement, and the mode utilizing software to draw, marks searching the contour edge actual curve that limit obtains.
(4) design is a kind of adopts Newton method (Newton-Raphson method) or similar least square method algorithm, at input density difference Δ ρ, gravity coefficient g, after constant value, by radius of curvature R 0, contact angle values θ, interfacial tension value γ, the theoretical curve that arc length S draws as variable optimization Young-Laplace equation solution as above with search drop contour edge and the actual curve that obtains, and then obtain final vertex curvature radius R0, contact angle values θ, interfacial tension value γ, the parameters such as arc length S, and and then utilize integration to quadrature and the method for volume, try to achieve area and the isoparametric method of volume of drop.Specifically comprise: (1) is by directly optimizing the Young-Laplace Equation Theory curve of drop profile and searching actual curve test fluid-gas or the liquid-liquid interface tension value of edge gained; (2) have employed true sessile drop method (RealDrop) or image outline method (DIPM).Thus, need not demarcate as the experience of the Young-Laplace matching on Select plane algorithm basis.
(5) two kinds of particular algorithms for as above optimizing process described in 3 are designed, for optimization interfacial tension value γ and contact angle values θ:
The first, image outline method: it is characterized in that: utilize image processing algorithm, matched curve: as circle or ellipse, polynomial curve or Spline curve, calculate the algorithm of the radius-of-curvature value on summit.And then, by as above 5 optimized algorithms mentioned, optimize and draw the required test parameter such as contact angle values θ, interfacial tension value γ, arc length S.
The second, truly sessile drop method (RealDrop method): utilize zero dimension transformation equation and original discrete equation to carry out the algorithm of two suboptimization to contour curve, it is characterized by: optimizing process for the first time, optimizes and draws interfacial tension value γ and vertex curvature radius R
0between linear relation; Second time utilizes primary relational expression, after reducing variable, utilizes the iteration of interfacial tension value γ, optimizes and draws the required test parameter such as contact angle values θ, interfacial tension value γ, arc length S.
As above the dimensionless equation used of the optimization described in (2) group is as follows:
(formula: 8)
Wherein:
, X=x/R
0, Y=y/R
0, S=s/R
0
(6) solved the surface chemistry analytical approach of surface/interface tension value, contact angle values and liquid volume, area, drop radius-of-curvature and wetting line by drop image analysing computer, matching, optimization and software automatic Iterative variable element (drop image analysis), and utilize the measuring method solving area and the surface/interface tension analysis interfacial rheological characteristic matter obtained.
Drop utilizes the mode vacuumizing rear pressure differential, realizes in the mode of the hanging drop freely falling to dripping or stop syringe needle.
Device provided by the invention and method of testing can analyze contact angle and interfacial tension value etc. in different pressures (vacuum) situation, in oil field, the field such as petrochemical industry, new material research has extremely wide popularization price, special in space environment simulated experiment, by simulation space practical vacuum degree and temperature conditions and and then measured value interfacial tension and contact angle values, these apparatus and method are very effective.
Accompanying drawing explanation
Fig. 1: contact angle schematic diagram;
In Fig. 1: θ: contact angle
γ
s: the surface tension value of solid
γ
l: the surface tension value of solid
γ
sL: the interfacial tension value of solid and liquid
γ
S:γ
L?cosθ+γ
SL
Fig. 2: the front elevation of contact angle and interfacial tension test device under the vacuum described in this patent and controlled temperature conditions;
In Fig. 2: 1-pressure cap; 2-upper cover plate; 3-KF50 standard interface; 4-quartz glass view window; 5-kapillary; 6-pressure cap; 7-vacuum valve; 8-microsyringe; 9-syringe pump; 10-Vertical dimension moves one dimensional optical translation stage; 11-support; 12-telecentric lens; 13-camera lens set collar; 14-video camera; 15-electric control box; 16-LED source of parallel light; 17-XYZ three-dimensional optical translation stage; 18-KF16 vacuum interface; 19-two-dimensional level adjustment platform; 20-syringe needle; 21-tetra-horizontal adjustment pin; 22-camera fixing support, 26-vacuum temp control cavity.
Fig. 3: the rear view of contact angle and interfacial tension test device under the vacuum described in this patent and controlled temperature conditions;
In Fig. 3: 23-temperature sensor; 24-recirculated water/conduction oil fast interface.
Fig. 4: the vertical view of contact angle and interfacial tension test device under the vacuum described in this patent and controlled temperature conditions;
In Fig. 4: 25-XY two-dimensional optical translation stage.
Embodiment
For realizing vacuum and temperature control (maximum temperature-50-200 degree, depend on the temperature of the Water Tank with Temp.-controlled of temperature control) complete high precision measurement under condition and have sticky all contact angles of product system and the object of interfacial tension, the present invention carries out innovative design in total layout, spare parts purchasing, light path design, testing algorithm etc., and embodiment is as follows:
1, design the topology layout that combines general conditions and vacuum temp control condition image method contact angle and interfacial tension test, the measurement mechanism of interfacial tension and contact angle values under vacuum, controlled temperature conditions, as shown in Figure 2, specific embodiments is as follows:
(1) design a vacuum temp control cavity, cavity includes KF16 vacuum interface 18, two recirculated water/conduction oil fast interfaces 24 and a temperature sensor 23 of two quartz glass view windows, 4,1 standard; Meanwhile, this cavity envisaged underneath interlayer is used for heat insulation for the formation of recirculated water (not shown) and an interlayer, is filled with ceramic wool in interlayer; (2) this cavity is arranged on a union body with the four-dimensional optical translation platform 17 of XYZR and two-dimensional level adjustment platform 19, and cavity is removable; (3) the top laser bonding KF50 vacuum flange of a standard of this cavity; (4) anchor ear (not shown) is used to be tightly connected after being provided a centre standard K F50 vacuum upper cover plate 2 of an interior chamfering to fill O-ring seal with the flange of above-mentioned (3) is middle; (5) be about the kapillary of 2mm at above-mentioned (4) interstitial hole at insertion external diameter, and use the pressure ring of chamfering in pressure cap 1 and both sides by capillary pressure tightening seal on upper cover plate; Meanwhile, kapillary lower end occurs in view window, forms syringe needle 20 effect as shown in Figure 2.(6) upper end of kapillary is pressed to after on a vacuum valve 7 by pressure cap 6 and is connected with a micro-injection pump by vacuum valve; (7) microsyringe is installed to above the syringe pump 9 of an Electric Machine Control, and this syringe pump has Vertical dimension moves one dimensional optical translation stage 10 and XY two-dimensional optical translation stage 25, for controlling correct position and the focal position of syringe pump; (8) syringe pump and control union body thereof are installed on support 11; (9) telecentric lens 12, camera lens set collar 13, video camera 14, electric control box 15, LED source of parallel light 16, four horizontal adjustment pin 21, camera fixing supports 22 are designed with in system, electric control box 15 comprises stepper motor driver, motion control card, control circuit for light source etc., with the system of the imaging that realizes taking pictures.
Above-mentioned horizontal adjustment pin 21 is fixed on corner, frame lower end, frame two is provided with support 11 and electric control box 15, horizontal light source 16 is arranged at electric control box side, support 11 is provided with telecentric lens 12, camera lens set collar 13, video camera 14, camera lens set collar 13, a camera fixing support 22 is set below video camera 14, support 11 upper end is provided with Vertical dimension and moves one dimensional optical translation stage 10, Vertical dimension moves on one dimensional optical translation stage 10 and is fixed with syringe pump 9, syringe pump 9 connects an XY two-dimensional optical translation stage, syringe pump 9 lower end is connected with microsyringe 8, vacuum valve 7 is connected with below microsyringe 8, vacuum valve 7 connects kapillary 5 upper end by pressure cap 6, kapillary 5 lower end syringe needle 20 is through upper cover plate 2, in quartz observing window 4 window in KF50 vacuum interface 3 to vacuum temp control cavity 26, kapillary 5 by pressure cap 1 and with the pressure ring press seal of chamfering in both sides on upper cover plate 2, vacuum temp control cavity 26 connects two-dimensional level adjustment platform 19, is XYZ three-dimensional optical translation stage 17 below two-dimensional level adjustment platform 19.
2, to vacuumize and the implementation of vacuum degree control:
By the standard K F16 vacuum interface 18 of vacuum temp control cavity, O-ring seal is adopted to be connected a KF16 T-valve (not shown) with the mode that anchor ear seals, in another two mouths of this T-valve, connection can to carry out the vacuum tightness instrument of both-way communication with computing machine by RS485, one is connected to a vacuum valve (not shown); Another interface of vacuum valve is connected on a vacuum pump, by the operation of vacuum tightness instrument control vacuum pump, and the vacuum tightness in vacuum temp control cavity.
3, temperature controlled implementation:
The recirculated water interface of cavity and a circulating water chennel are controlled, system temperature thus tank temperature range determine.Temperature sensor 23 reads the temperature of current cavity, and carries out two-way communication by RS485 communications protocol and computing machine.
4, for making drop profile reach sub-pixel, in the selection of camera lens and light source, following structure is adopted: (1), in the selection of camera lens, adopts telecentric lens, thus significantly promotes the sharpness of the depth of field and contour edge; (2) in the selection of background light source, adopt LED source of parallel light, thus significantly promote the sharpness of the depth of field and contour edge; (3) in the selection of video camera, select the high-speed camera of USB2.0 or USB3.0 of German IDS company, broadcasting speed reaches 60 frames/more than second.
5, true sessile drop method or image fitting process matching Young-Laplace equation, and in order to test the embodiment of contact angle and interfacial tension value:
(1), when implementing true sessile drop method, by software systems control both optical imaging system, the real-time imaging of drop is captured in computer;
(2) the drop outline line edge of software systems automatic analysis real-time imaging data or the picture information of automatic analysis continuous capturing, picture information is the picture formats such as BMP, JPG, and real-time imaging data adopts the forms such as AVI, MPG;
(3) a kind of true sessile drop method test of design is used for have modified gravity system contact angle and interfacial tension value, comprising:
The first, propose the Young-Laplace system of equations of discretize, the stopping during image analysing computer of side-looking method dripped, bubble catches or hanging drop:
Wherein: θ is contact angle, s is arc length, R
0for the radius-of-curvature of vertex position, Δ ρ is that inside and outside phase density is poor, and z height, x is width, and V is volume, and A is area, and (x0, z0) is apex coordinate.
The second, the solution that solves Young-Laplace discrete equation group is designed, specific as follows: use the discrete equation group as above mentioned by (1) when using the theoretical curve of Software on Drawing drop profile, utilize Long Gekula or Ou Weifa or similar method theory of solving curve, and the mode utilizing software to draw, show each coordinate points (x on corresponding theoretical curve and curve
i, y
i).
Three, a kind of method of drawing the actual curve of contact angle and interfacial tension drop profile is designed, specifically comprise: utilize CANNY or SOBEL algorithm, imaging system is utilized to take the change obtaining gray scale in rotating liquid drop contour images, reasonable threshold value is set, find out the edge of drop profile, and the edge utilizing Spline algorithm to do to search is optimized calculating, obtain the marginal point coordinate figure (X of drop profile
i, Y
i) and ordered arrangement, and the mode utilizing software to draw, marks searching the contour edge actual curve that limit obtains.
4th, design and a kind ofly adopt Newton method or similar least square method algorithm, at input density difference Δ ρ, gravity coefficient g, after constant value, by radius of curvature R 0, contact angle values θ, interfacial tension value γ, the theoretical curve that arc length S draws as variable optimization Young-Laplace equation solution as above with search drop contour edge and the actual curve that obtains, and then obtain final vertex curvature radius R0, contact angle values θ, interfacial tension value γ, the parameters such as arc length S, and and then utilize integration to quadrature and the method for volume, try to achieve area and the isoparametric method of volume of drop.Specifically comprise: (1) is by directly optimizing the Young-Laplace Equation Theory curve of drop profile and searching actual curve test fluid-gas or the liquid-liquid interface tension value of edge gained; (2) have employed true sessile drop method or image outline method, thus, need not demarcate as the experience of the Young-Laplace matching on Select plane algorithm basis.
Five, two kinds of particular algorithms for as above (3) described optimizing process are designed, for optimization interfacial tension value γ and contact angle values θ:
One, image outline method: utilize image processing algorithm, matched curve (as circle or ellipse, polynomial curve or Spline curve), calculates the algorithm of the radius-of-curvature value on summit.And then the optimized algorithm mentioned by as above (5), is optimized and draws the required test parameter such as contact angle values θ, interfacial tension value γ, arc length S.
Two, true sessile drop method: utilize zero dimension transformation equation and original discrete equation to carry out the algorithm of two suboptimization to contour curve, it is characterized by: optimizing process for the first time, optimizes and draws interfacial tension value γ and vertex curvature radius R
0between linear relation; Second time utilizes primary relational expression, after reducing variable, utilizes the iteration of interfacial tension value γ, optimizes and draws the required test parameter such as contact angle values θ, interfacial tension value γ, arc length S.
As above its optimization dimensionless equation used group described in two is as follows:
(formula: 8)
Wherein:
, X=x/R
0, Y=y/R
0, S=s/R
0
Six, solve surface/interface tension value, contact angle values and liquid volume, area, drop radius-of-curvature and wetting line by drop image analysing computer, matching, optimization and software automatic Iterative variable element (drop image analysis), and utilization solves the area and surface/interface tension analysis interfacial rheological characteristic matter that obtain.
6, adopt this device to form drop and test the implementation of contact angle:
(1) vacuum valve 7 is closed; (2) in microsyringe, fluid to be measured is drawn; (3), after having connected vacuum pump, vacuum temp control cavity is vacuumized; (4) vacuum temp control cavity temperature reaches desired value; (5) after vacuum tightness and temperature reach desired value, close vacuum pump and be connected middle vacuum valve with cavity; (6) slowly open vacuum valve 7, drop can be drawn into rapidly vacuum temp control cavity due to pressure differential and drop onto the surface of solid sample; (7) use the lower video image of high-speed camera shooting, and Iamge Segmentation is become BMP picture.
6, this device is adopted to form drop and the implementation of test interface tension force:
(1) vacuum valve 7 is closed; (2) in microsyringe, fluid to be measured is drawn; (3), after having connected vacuum pump, vacuum temp control cavity is vacuumized; (4) vacuum temp control cavity temperature reaches desired value; (5) after vacuum tightness and temperature reach desired value, close vacuum pump and be connected middle vacuum valve with vacuum temp control cavity; (6) slowly open vacuum valve 7, drop can form a hanging drop from syringe needle rapidly due to pressure differential; (7) use the lower video image of high-speed camera shooting, and Iamge Segmentation is become BMP picture.
This patent is announced and is a kind ofly adopted the test contact angle of true sessile drop method or image fitting process matching Young-Laplace equation and the method for testing of interfacial tension value and a kind of proving installation testing contact angle and table/interfacial tension under vacuum and controlled temperature conditions.The vacuum temp control cavity of the bilateral view window that this device is made up of quartz glass, bonding in vacuum accessory (three-way valve, kapillary), syringe pump and control assembly thereof, video camera with telecentric lens and source of parallel light composition, after contour images by shooting drop, the test of matching Young-Laplace equation is adopted to obtain contact angle and interfacial tension value, this device and method of testing can analyze contact angle and interfacial tension value etc. in different pressures (vacuum) situation, in oil field, petrochemical industry, the fields such as new material research have extremely wide promotional value, special in space environment simulated experiment, by simulation space practical vacuum degree and temperature conditions and and then measured value interfacial tension and contact angle values, these apparatus and method are very effective.
Claims (6)
1. the measurement mechanism of interfacial tension and contact angle values under vacuum, controlled temperature conditions, its notable feature is: (1) include pressure cap, upper cover plate, KF50 standard interface, quartz glass view window, kapillary, (syringe pump, Vertical dimension move one dimensional optical translation stage, support, telecentric lens, camera lens set collar, video camera, electric control box, LED source of parallel light, XYZ three-dimensional optical translation stage, KF16 vacuum interface, two-dimensional level adjustment platform, syringe needle, four horizontal adjustment pin, camera fixing supports for vacuum valve, microsyringe; Meanwhile, the rear of vacuum cavity provides temperature sensor and recirculated water/conduction oil fast interface; The XY two-dimensional optical translation stage that one controls syringe needle right position is provided in syringe pump control structure;
Above-mentioned horizontal adjustment pin is fixed on corner, frame lower end, frame two is provided with support and electric control box, horizontal light source is arranged at electric control box side, support is provided with telecentric lens, camera lens set collar, video camera, camera lens set collar, a camera fixing support is set below video camera, pedestal upper end is provided with Vertical dimension and moves one dimensional optical translation stage, Vertical dimension moves on one dimensional optical translation stage and is fixed with syringe pump, syringe pump connects an XY two-dimensional optical translation stage, syringe pump lower end is connected with microsyringe, vacuum valve is connected with below microsyringe, vacuum valve connects kapillary upper end by pressure cap, kapillary lower end syringe needle is through upper cover plate, KF50 vacuum interface is in the quartz observing window window in vacuum temp control cavity, kapillary by pressure cap and with the pressure ring press seal of chamfering in both sides on upper cover plate, vacuum temp control cavity connects two-dimensional level adjustment platform, is XYZ three-dimensional optical translation stage below two-dimensional level adjustment platform.
2. the measurement mechanism of interfacial tension and contact angle values under vacuum according to claim 1, controlled temperature conditions, it is characterized in that, in the selection of camera lens, light source and video camera, have employed the remarkable structure as follows with profile test: (1) is in the selection of camera lens, adopt telecentric lens, thus significantly promote the sharpness of the depth of field and contour edge; (2) in the selection of background light source, adopt LED source of parallel light, thus significantly promote the sharpness of the depth of field and contour edge; (3) in the selection of video camera, choose the high-speed camera of USB2.0 or USB3.0 of German IDS company, broadcasting speed reaches 60 frames/more than second.
3. the measuring method of interfacial tension and contact angle values under the vacuum that make use of the measurement mechanism of interfacial tension and contact angle values under vacuum according to claim 1, controlled temperature conditions, controlled temperature conditions, it is characterized in that, have employed a kind of true sessile drop method test for have modified gravity system contact angle and interfacial tension value, its notable feature comprises:
(1) employ the Young-Laplace system of equations of discretize, (a sessile drop) dripped for the stopping during image analysing computer of side-looking method, bubble catches (Captive bubble) or hanging drop (pendant drop):
Wherein: θ is contact angle, s is arc length, R
0for the radius-of-curvature of vertex position, Δ ρ is that inside and outside phase density is poor, z height, and x is width, and V is volume, and A is area, and x0, z0 are apex coordinate;
(2) solution that solves Young-Laplace discrete equation group is employed, its notable feature comprises: use the discrete equation group as above mentioned by (1) when using the theoretical curve of Software on Drawing drop profile, utilize Long Gekula (Runge-Kutta) or position, Europe (Euler) method or similar method theory of solving curve, and the mode utilizing software to draw, show each coordinate points (x on corresponding theoretical curve and curve
i, y
i);
(3) a kind of method of drawing the actual curve of contact angle and interfacial tension drop profile is employed, its notable feature is: utilize CANNY or SOBEL algorithm, imaging system is utilized to take the change obtaining gray scale in rotating liquid drop contour images, reasonable threshold value is set, find out the edge of drop profile, and the edge utilizing Spline algorithm to do to search is optimized calculating, obtain the marginal point coordinate figure (X of drop profile
i, Y
i) and ordered arrangement, and the mode utilizing software to draw, marks searching the contour edge actual curve that limit obtains;
(4) a kind of employing Newton method (Newton-Raphson method) or similar least square method algorithm is employed, at input density difference Δ ρ, gravity coefficient g, after constant value, by radius of curvature R 0, contact angle values θ, interfacial tension value γ, the theoretical curve that arc length S draws as variable optimization Young-Laplace equation solution as above with search drop contour edge and the actual curve that obtains, and then obtain final vertex curvature radius R0, contact angle values θ, interfacial tension value γ, the parameters such as arc length S, and and then utilize integration to quadrature and the method for volume, try to achieve area and the isoparametric method of volume of drop,
Its notable feature comprises: (1) is by directly optimizing the Young-Laplace Equation Theory curve of drop profile and searching actual curve test fluid-gas or the liquid-liquid interface tension value of edge gained; (2) have employed true sessile drop method (RealDrop) or image outline method (DIPM), thus, need not demarcate as the experience of the Young-Laplace matching on Select plane algorithm basis;
(5) one in the following two kinds method is employed, for the particular algorithm of as above optimizing process described in 3, for optimization interfacial tension value γ and contact angle values θ:
The first, image outline method (DIPM:Drop image profile method): it is characterized in that: utilize image processing algorithm, matched curve (as circle or ellipse, polynomial curve or Spline curve), calculate the algorithm of the radius-of-curvature value on summit, and then, by optimized algorithm as mentioned above, optimize and draw the required test parameter such as contact angle values θ, interfacial tension value γ, arc length S;
Or,
The second, truly sessile drop method (RealDrop method): utilize zero dimension transformation equation and original discrete equation to carry out the algorithm of two suboptimization to contour curve, it is characterized by: optimizing process for the first time, optimizes and draws interfacial tension value γ and vertex curvature radius R
0between linear relation; Second time utilizes primary relational expression, after reducing variable, utilizes the iteration of interfacial tension value γ, optimizes and draws the required test parameter such as contact angle values θ, interfacial tension value γ, arc length S;
As above the dimensionless equation used of the optimization described in (2) group is as follows:
(formula: 8)
Wherein:
, X=x/R
0, Y=y/R
0, S=s/R
0
(6) employ the surface chemistry analytical approach being solved surface/interface tension value, contact angle values and liquid volume, area, drop radius-of-curvature and wetting line by drop image analysing computer, matching, optimization and software automatic Iterative variable element (drop image analysis), and utilize the measuring method solving area and the surface/interface tension analysis interfacial rheological characteristic matter obtained.
4. a kind of vacuum, measuring method of interfacial tension and contact angle values under controlled temperature conditions that make use of the measurement mechanism of interfacial tension and contact angle values under vacuum according to claim 1, controlled temperature conditions according to claim 3, it is characterized in that, the mode of contact angle drop and interfacial tension drop is formed under a kind of vacuum condition, its notable feature is: drop utilizes the mode vacuumizing rear pressure differential, realizes in the mode of the hanging drop freely falling to dripping or stop syringe needle.
5. a kind of vacuum, measuring method of interfacial tension and contact angle values under controlled temperature conditions that make use of the measurement mechanism of interfacial tension and contact angle values under vacuum according to claim 1, controlled temperature conditions according to claim 3, it is characterized in that, form drop and the implementation of test interface tension force:
1) vacuum valve is closed; 2) in microsyringe, fluid to be measured is drawn; 3), after having connected vacuum pump, vacuum temp control cavity is vacuumized; 4) vacuum temp control cavity temperature reaches desired value; 5) after vacuum tightness and temperature reach desired value, close vacuum pump and be connected middle vacuum valve with vacuum temp control cavity; 6) slowly open vacuum valve, drop can form a hanging drop from syringe needle rapidly due to pressure differential; 7) use the lower video image of high-speed camera shooting, and Iamge Segmentation is become BMP picture.
6. a kind of vacuum, measuring method of interfacial tension and contact angle values under controlled temperature conditions that make use of the measurement mechanism of interfacial tension and contact angle values under vacuum according to claim 1, controlled temperature conditions according to claim 3, it is characterized in that, form drop and test the implementation of contact angle:
1) vacuum valve is closed; 2) in microsyringe, fluid to be measured is drawn; 3), after having connected vacuum pump, vacuum temp control cavity is vacuumized; 4) vacuum temp control cavity temperature reaches desired value; 5) after vacuum tightness and temperature reach desired value, close vacuum pump and be connected middle vacuum valve with cavity; 6) slowly open vacuum valve, drop can be drawn into rapidly vacuum temp control cavity due to pressure differential and drop onto the surface of solid sample; 7) use the lower video image of high-speed camera shooting, and Iamge Segmentation is become BMP picture.
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