CN101246111B - Fabric contact angle on-line measuring method and device - Google Patents
Fabric contact angle on-line measuring method and device Download PDFInfo
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- CN101246111B CN101246111B CN2008100348921A CN200810034892A CN101246111B CN 101246111 B CN101246111 B CN 101246111B CN 2008100348921 A CN2008100348921 A CN 2008100348921A CN 200810034892 A CN200810034892 A CN 200810034892A CN 101246111 B CN101246111 B CN 101246111B
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Abstract
The present invention belongs to the field of the measuring technique, specially is a fiber contact angle on-line measuring method and the device thereof. In the method the polymer solution is suspended on individual fiber with a shape of liquid drop, and the fiber is fixed in the suspension device, afterwards the suspension device is arranged in an optical transparent and temperature-controllable enclosed system, when the liquid drop has obtained balance the contract angle between the liquid drop of the polymer solution and the individual fiber can be measured. The concentration of liquid drop on the fiber is alternated by regulating the temperature, the pressure and the concentration of the solution in the balance groove, the method for combining the optical microscope and the vector calculation is adopted, the characteristic dimension and shape are processed and analyzed with a statistical averaging method, the contact angle is calculated thereby on-line measuring the contact angle of different-concentration liquid drop and the fiber is measured at the home position.
Description
Technical field
The invention belongs to field of measuring technique, be specifically related to a kind of On-line Measuring Method and device of fabric contact angle, specifically, relate to the surface tension that a kind of on-line measurement polymer solution causes with concentration change at fiber surface, measuring method and the measurement mechanism that contact angle changes.
Background technology
In various polymer matrix composites, the interface feature of fiber and polymeric matrix material directly influences hydrothermal aging, mechanical property and the electric property of compound substance.Interfacial failure is one of principal mode of compound substance hydrothermal aging, so the measurement of the contact angle of polymeric matrix and fiber has very important meaning to composite study.
Polymer matrix composite adopts polymer solution to soak into the method for fiber usually, and then carries out heating and pressurizing and obtain laminate behind solvent flashing.Because polymer solution can cause the variation of itself and fabric contact angle with concentration change, thereby may cause fiber interface defective or hole to occur, the performance and the use of material caused negative effect.Therefore, change with the contact angle that concentration change causes, just can improve the interfacial bond property of compound substance easily by online in site measurement polymer solution.
Because fiber is cylindrical usually, the technology of employing measurement plane contact angle is difficult to be applied to the measurement of single fiber contact angle.In addition, the wetting balance method is owing to the high viscosity and the high viscoelasticity of concentrated polymer solution also can't be carried out.At the measurement of solvent or polymer solution at the contact angle of fiber, people such as B.J.Carroll and J.I.Yamaki has proposed droplet profile method (B.J.Carroll, Journal of Colloid and Interface Science, 1976,57 (3): 488-495.J.I.Yamaki, Y.Katayama, Journal of Applied Polymer Science, 1975,19:2897-2909), this method obtains contact angle according to the droplet profile that is hanging on the fiber in conjunction with the Young-Laplace Equation for Calculating.Yet said method need be measured the data such as diameter length of drop, and the human factor in the measuring process is more, and the accuracy of data depends on gauger's individual skill to a great extent, therefore bigger error can occur.
In addition, the whole bag of tricks of bibliographical information all is limited to the contact angle test to particular fluid and fiber, lacks solution is caused measuring method and the device that contact angle changes with concentration change.
Summary of the invention
The objective of the invention is in order to overcome the shortcoming of prior art, improve instrument shooting precision, observation automation degree and data processing method, solve of the influence of in-situ tracking concentration change, thereby the surface tension that a kind of original position on-line measurement polymer solution causes with concentration change at fiber surface, assay method and the measurement mechanism that contact angle changes are provided contact angle.
Technical scheme of the present invention is:
Single fiber is fixed in fiber suspender (Fig. 3), utilize sprayer or micro syringe that the form of a certain amount of polymer solution with drop is suspended on the single fiber, with whole fiber suspender pack into (Fig. 4) in the transparent airtight quartzy box of adding a cover, Controllable Temperature in the quartzy box, box is embedded with compensating groove, injects the solvent of polymer solution system to be measured or the solution of debita spissitudo in the groove; Quartzy box places on the microscopical objective table, regulate temperature in the quartzy box, after treating that polymer solution droplets reaches balance on the fiber, can utilize the high-pixel camera machine that is used with microscope and the aspect graph of drop on the fiber under the computer acquisition equilibrium state that is connected with video camera.Fig. 2 is the device synoptic diagram of images acquired, and Fig. 1 is the synoptic diagram of the fiber droplet morphology figure that collects.By software for calculation droplet morphology figure is handled and analyzes, obtain and calculate the contact angle necessary parameter,, can calculate the contact angle of polymer solution and fiber by these parameters as fibre diameter, drop characteristic dimension etc.In addition, the concentration of drop when the concentration by regulating temperature in the quartzy box, pressure and compensating groove interpolymer solution can adjustment reaches the purpose of online in site measurement variable concentrations polymer solution and fabric contact angle.Can obtain the bulking value of liquid to the drop image integration, the concentration of polymer solution droplets when droplet size and drop initial volume and initial concentration just can calculate balance during the contrast balance.
The fabric contact angle on-line measuring device that the present invention proposes is made up of optical microscope, digital camera, computing machine, suspender and closed system; Wherein said suspender comprises: quartzy closed enclosure, single fiber suspender and temperature control, pressure control device; Wherein the single fiber suspender is positioned in the quartzy closed enclosure, is used for fixing single fiber; Temperature control, pressure control device are in order to regulate the temperature and pressure in the quartzy closed enclosure; Be embedded with the compensating groove of dress polymer solution or solvent in the quartzy closed enclosure.
The present invention compares with traditional technical scheme, has following effect:
The present invention has enlarged the usable range of fiber droplet profile method, has solved the existing methods personal error, as mensuration problem of drop axial length etc.;
The present invention can the in-situ continuous collecting concentration change the drop image, on the basis that guarantees accuracy, realized concentration change is caused the test that contact angle changes;
The contact angle determination method that the present invention proposes has novelty academicly, can be used for the theoretical research of relevant polymer solution.
Description of drawings
Fig. 1: the shape synoptic diagram of drop on single fiber during equilibrium state.
Fig. 2: contact angle measurement mechanism synoptic diagram.
Fig. 3: single fiber suspender (a) is a front view, (b) is vertical view.
Fig. 4: quartzy closed enclosure and single fiber suspender.
Number in the figure: 1. quartzy closed enclosure (comprising inner fiber suspender and temperature regulating device), 2. optical microscope, 3. digital camera (as video camera), 4. computing machine, 5. the drop that hangs on the fiber, 6. single fiber, 7. fiber suspender handle, the 8. Magnetic strip of fiber suspender, 9. the substrate of fiber suspender, 10. quartzy closed enclosure, 11. polymer solutions or solvent
Embodiment
As shown in Figure 2, obtain single fiber droplet morphology figure part and be made up of microscope 2, video camera 3 and computing machine 4, video camera 3 is the Cannon Digital Video, and microscope 2 and video camera 3 supporting uses connect by USB port between video camera 3 and the computing machine 4.
The fiber suspender adopts the steel plate of teflon plated film and magnet to constitute as shown in Figure 3, and steel plate is of a size of 50 * 30 * 3mm
3(length * wide * height), middle hollow out is of a size of 20 * 20 * 3mm
3(length * wide * height), magnet size is 30 * 5 * 3mm
3(length * wide * height).Single fiber is suspended on the hollow out position of steel plate by magnet.
The quartz glass closed enclosure is of a size of 100 * 40 * 30mm
3(length * wide * height), closed enclosure is inlayed flux bath apart from one side 20mm, adds solvent or the certain density solution identical with polymer solution therein.Connect the pressure control equipment and can regulate the pressure of enclosed system.
Adopt bisphenol A type epoxy resin to be dissolved in N, in N '-dimethyl formamide, be made into the solution of 50% (weight), a certain amount of polymer solution is suspended on the single fiber with droplet morphology with sprayer or micro syringe; The fiber suspending apparatus is positioned in the quartzy closed enclosure, and the two ends of quartzy closed enclosure inside are embedded with compensating groove, and are positioned in the temperature regulating device together.Regulate solution concentration in temperature, pressure and the compensating groove of enclosed system, the concentration of drop during with adjustment, when calculating variable concentrations polymer solution in the contact angle data of fiber surface, as shown in table 1.
The concrete computing method of contact angle:
As shown in Figure 1: according to the symmetry foundation rectangular coordinate system as shown in the figure of fiber and drop, the o point is the initial point of the symcenter and the rectangular coordinate system of figure, the outline of drop when camber line abc represents to reach equilibrium state, middle band oblique line is partly represented fiber, θ is the contact angle of drop and fiber.R is a fiber radius, and h is the maximum height of drop, and l is the maximum length of drop.The computing method of existing document generally are according to the above-mentioned numerical evaluation contact angle of measuring gained, have the bigger deficiency of personal error.
In the inventive method, take up an official post at the drop outline and to get 1 p (x, y), with h, x, y obtain characteristic H (h/r) divided by fiber radius r respectively, X (x/r), Y (y/r).When fiber is desirable cylindric, radius enough little (between 1～20 μ m), drop gravity can be ignored, and when drop reaches thermodynamic equilibrium, according to Young-Laplace equation (Young-Laplaceequation), put on the drop profile p (X Y) establishes an equation under meeting:
Wherein
F and E are respectively the first kind and second class Legendre (Legendre) standard elliptic integral.Can accurately obtain the maximum height H of drop on the droplet morphology figure that obtains from photomicrograph, and the coordinate of arbitrfary point p on the drop profile (removing the most high and low point) (X, Y).Because F, E can only utilize the method for numerical evaluation to obtain, so can't directly instead separate the explicit expression that obtains contact angle θ, has only by supposing a series of θ
sValue, in conjunction with H, it is θ that Y calculates contact angle
sThe time X value X
s, make X
sEqual the θ of measured value X
sThe contact angle θ that promptly is considered to drop and fiber.Promptly utilize the contact angle value θ of supposition
sWith value H substitution relational expression (3) value of obtaining a, utilize relational expression (4) value of obtaining k again, then can the value of obtaining with Y substitution formula (1)
At last by relational expression (2) calculate X
sIf, X
sConsistent with X, then think θ
sIt is exactly the contact angle of droplet solution and fiber.Simpler method is a constructed fuction
Because H, X, Y can obtain from the Treatment Analysis of droplet morphology figure, and function f is the function of a single variable of θ, and the θ that makes f obtain minimum value (minimum value is 0) is exactly the contact angle of drop and fiber.
By computing machine 20 to 50 points of picked at random on a drop outline, the mean value that calculates its contact angle is to reduce stochastic error.On this basis, the uncertainty of bringing to the result for the otherness that reduces different piece on the fiber, can measure the contact angle of at least 20 drops, calculate gained result's mean value as the solution droplets of this kind polymkeric substance under this concentration and the contact angle of fiber with these drops.
Optical microscope system can be ordinary optical microscope, inverted microscope and perflectometer; Because inverted microscope can be handled in quartzy closed enclosure size and single fiber stationary installation, adjusts focal length more easily, thereby the preferred inversion microscope.
Droplet profile obtain the digital image system that requires precision, adopt digital camera or video camera, its resolution can adopt colour or black and white camera lens greater than 3,000,000 pixels.
The single fiber suspender adopt steel plate as substrate, magnet as press strip, substrate and press strip surface coat poly tetrafluoroethylene, fluted on the substrate, can make the press strip stationkeeping, unlikely slip during use, can make things convenient for anchoring fiber thus, and assurance device is not subjected to pollution, the corrosion of each kind solvent and polymkeric substance.
Evenly, guarantee that the droplet morphology figure that obtains can not be distorted, be out of shape on the quartz glass closed enclosure optics.Closed enclosure links to each other with extraneous decompression system, keeps weighing apparatus level pressure power; Quartzy closed enclosure is positioned in the temperature regulating device so that regulate temperature in the box; Add solvent or debita spissitudo polymer solution in the embedded compensating groove of closed enclosure, make polymer solution droplets can reach thermodynamic equilibrium state, solution concentration can change the concentration of drop under the equilibrium condition, the variation of contact angle when being convenient for measuring variable concentrations in adjusting temperature, pressure and the change groove.
A plurality of drops can be hung on the single fiber, stochastic error can be reduced greatly as the net result of measuring with the mean value of the measurement result of a plurality of drops.
| Polymer concentration (wt%) | Contact angle (degree) | Standard deviation (30 points) |
| 50 | 38.68 | 0.41 |
| 52 | 37.12 | 0.31 |
| 54 | 36.07 | 0.36 |
| 56 | 35.06 | 0.45 |
| 58 | 33.86 | 0.36 |
| 60 | 32.64 | 0.34 |
| 62 | 32.34 | 0.24 |
| 64 | 32.28 | 0.36 |
| 66 | 32.85 | 0.35 |
| 68 | 33.45 | 0.44 |
| 70 | 34.23 | 0.36 |
| 72 | 35.61 | 0.30 |
| 74 | 37.35 | 0.58 |
| 76 | 39.11 | 0.25 |
| 78 | 41.56 | 0.52 |
| 80 | 44.03 | 0.49 |
Claims (1)
1. the On-line Measuring Method of a fabric contact angle is characterized in that: use single fiber droplet profile contact angle instrument, this analyzer comprises optical microscope, digital camera, computing machine, suspender and closed system; With sprayer or micro syringe the form of polymer solution with drop hung on the single fiber, and fiber is fixed on the suspender, suspender is placed in the enclosed system of optical clear and Controllable Temperature, enclosed system is embedded with compensating groove, injects polymer solution to be measured in the groove; The concentration of solution in temperature, pressure and the compensating groove of adjusting enclosed system, after treating that drop reaches balance, utilize optical microscope, digital camera and computing machine to obtain the aspect graph of drop on the fiber, and droplet morphology figure is handled and analyzes by software for calculation, obtain the characteristic dimension and the shape of drop, calculate the concentration and the contact angle of drop; Wherein:
The step of described calculating liquid-drop contact angle is as follows:
If the o point is the initial point of symcenter and the rectangular coordinate system of droplet profile figure, the outline of drop when camber line abc represents to reach equilibrium state, θ are the contact angle of drop and fiber, and r is a fiber radius, and h is the maximum height of drop, and l is the maximum length of drop;
The drop outline take up an official post get 1 p (x, y), with h, x, y obtain characteristic H (h/r) divided by fiber radius r respectively, X (x/r), Y (y/r); The coordinate X of point p on the drop profile, Y meets relational expression (1), (2):
Wherein
F and E are respectively the first kind and the second class Legendre standard elliptic integral; Can accurately obtain the maximum height H of drop on the droplet morphology figure that obtains from photomicrograph, (X Y), supposes a series of contact angle θ to the coordinate of arbitrfary point p on the drop profile
sValue is as θ, by the contact angle value θ of supposition
sWith value H by relational expression (3) value of calculating a, utilize relational expression (4) value of obtaining k again, then can the value of obtaining with Y substitution formula (1)
At last by relational expression (2) calculate X
sIf, X
sConsistent with X, then think θ
sIt is exactly the contact angle of droplet solution and fiber;
Constructed fuction
Function f is the function of a single variable of θ, and the θ that makes f obtain minimum value is exactly the contact angle of drop and fiber;
By computing machine 20 to 50 points of picked at random on a drop outline, the mean value that calculates its contact angle is as the solution droplets of this kind polymkeric substance under this concentration and the contact angle of fiber.
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|---|---|---|---|
| CN2008100348921A CN101246111B (en) | 2008-03-20 | 2008-03-20 | Fabric contact angle on-line measuring method and device |
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|---|---|---|---|
| CN2008100348921A CN101246111B (en) | 2008-03-20 | 2008-03-20 | Fabric contact angle on-line measuring method and device |
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| CN101246111B true CN101246111B (en) | 2011-04-06 |
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| CN106570300B (en) * | 2016-11-17 | 2019-09-20 | 中南大学 | A kind of acquisition methods of rule second order structure surface liquid-drop contact angle |
| CN107907450B (en) * | 2017-11-27 | 2020-06-09 | 深圳大学 | Two-dimensional nano material hydrophilic angle testing method based on atomic force microscope |
| 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 |
| CN109596464B (en) * | 2018-12-27 | 2021-06-08 | 北京航空航天大学 | Method for testing interface performance of carbon nanotube surface modified fiber |
| CN112284979B (en) * | 2020-09-22 | 2023-02-03 | 上海梭伦信息科技有限公司 | Method for measuring dynamic contact angle of droplet boundary |
| CN112284980A (en) * | 2020-09-30 | 2021-01-29 | 武汉理工大学 | Reagent asphalt static contact angle testing method, device and system |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101089680A (en) * | 2007-08-20 | 2007-12-19 | 友达光电（苏州）有限公司 | Device for measuring contact corner |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101089680A (en) * | 2007-08-20 | 2007-12-19 | 友达光电（苏州）有限公司 | Device for measuring contact corner |
Non-Patent Citations (3)
| Title |
|---|
| Bihai Song等.a generalized drop length-height method for determination of contact angle in drop-on-fiber systems.《journal of colloid and interface science》.1998,(第197期),68-77. * |
| JP特开平8-334455A 1996.12.17 |
| 王宜等.液滴形状法测量纤维接触角的研究.《合成纤维工业》.2004,第27卷(第2期),12-14. * |
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