CN102914490A - Solid-liquid contact angle measuring method in non-transparent or sealed space - Google Patents
Solid-liquid contact angle measuring method in non-transparent or sealed space Download PDFInfo
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- CN102914490A CN102914490A CN2012103808196A CN201210380819A CN102914490A CN 102914490 A CN102914490 A CN 102914490A CN 2012103808196 A CN2012103808196 A CN 2012103808196A CN 201210380819 A CN201210380819 A CN 201210380819A CN 102914490 A CN102914490 A CN 102914490A
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Abstract
The invention relates to a method for measuring a liquid contact angle in non-transparent or sealed space. An optical imaging method in the prior art is replaced by the nuclear magnetic resonance imaging technology; through directly collecting a magnetic resonance signal of a liquid with nuclear spin quantum number of 1/2 of atomic nucleus number, a liquid section passing through an axis of a gas-liquid interface is imaged; and then through fitting an axis section curve of an image and through further measurement or calculation, a solid-liquid contact angle is obtained. As nuclear magnetic resonance imaging has no requirement on optical transparency of a research system, the defect that the traditional solid-liquid contact angle measuring method based on optical imaging only can measure solid-liquid contact angles in transparent and open space is eliminated. The method for measuring the liquid contact angle in the non-transparent or sealed space, provided by the invention, is especially suitable for researches on solid/liquid interface phenomenon in non-transparent environments or sealed systems.
Description
[technical field]
The present invention relates to field of measuring technique, be specifically related to the infiltrating solid-liquid contact angle measuring method of exosyndrome material.
[background technology]
Wellability is the important surface nature of solid, aspect ore floatation, building materials coating, anticorrosion waterproof etc. important application is being arranged.Because its critical role in scientific research and practical application, the research of solid surface wellability always is the Hot Contents in physical chemistry field.Wherein, contact angle is measured as the most basic ingredient of wellability research, for theoretical research and the production practices of surface/interface scientific domain important value is arranged.
Along with going deep into of technical progress and research, in succession develop the method for multiple measurement contact angle, hang sheet method, sessile drop method, bubble prize law etc. such as Wilhelmy.Since the advantage such as easy and simple to handle, sessile drop method being most widely used in contact angle is measured, and its cardinal principle is to obtain the outside drawing picture of little drop on solid surface by optical imagery, by the drop profile being carried out Fitting Analysis, finally obtains contact angle numerical value.Most contact angle measurements is all based on this principle at present.
Yet because the method is take optical imagery as pacing items, this necessity of making use of momentum is asked contact angle to measure must to carry out in transparent and open system.And in actual applications, various infiltration behaviors often in the situation that opaque or sealing occur, the for example capillary measurement of harmful liquid, the control of liquid transport pipeline inner fluid, micro-fluidic system etc., these all are the important application directions of wellability research, but because the opaque and closure of system itself, traditional contact angle measurement means can't be applied to this type of research, and this theoretical developments and practical application for the surface interface science has caused very large obstruction.
For example, teflon and polyamide are the fluid pipeline conveying materials of commonly using, and the wetting regime of the interior liquid of pipeline is for fluid parameter and transport the efficient important.Therefore, obtain the contact angle of fluid in pipeline, for understanding fluid state in depth and further convection cell is regulated and control to play an important role.Yet, because the opacity of material adopts traditional optical means that the wet face state of liquid in pipeline had no way of understanding.
Therefore need a kind of new technology badly, in order to realize the research to liquid-soaked in opaque and the closed system.
[summary of the invention]
The technical problem to be solved in the present invention is: develop a kind of can measurement for opaque or the method for the inner solid-liquid contact angle of enclosure space.
The invention provides a kind of method for measurement for opaque or sealing solid-liquid system internal interface feeler, wherein solid is made of nonferromugnetic material, liquid contains the atomic nucleus that nuclear-spin quantum number equals 1/2, is filled with described liquid and air in the space that described solid consists of, and described method comprises:
S1 places described solid-liquid system to the sample cavity of NMR imaging instrument;
S2 carries out pre-imaging from least one direction to the liquid the described solid-liquid system sample, and to the image comparison analysis, to determine liquid gas interface position, direction and liquid gas interface central point;
S3 is from least one direction, on the plane perpendicular to described liquid gas interface direction and the described liquid gas interface central point of mistake, liquid in the described solid-liquid system sample is carried out Magnetic resonance imaging, and to the image comparison analysis, cross the sectional view of liquid gas interface central shaft to obtain liquid;
S4 obtains the axle center section curve of solid-liquid and liquid gas interface according to described sectional view;
S5 carries out match to described axle center section curve, and by measuring or calculating, obtains solid-liquid contact angle.
Solid can be made of any nonferromugnetic material, for example glass, teflon, polyamide, or other nonferromugnetic material.
Liquid can be selected from waterborne liquid, oil-based liquid or water oil mixture.Wherein waterborne liquid can be water, or aqueous solution, or the liquid in the water soluble, comprises alcohols etc.Oil-based liquid can be the organic compounds such as alkane, aromatic hydrocarbon, ester class, fatty acid; The water oil mixture refers to that water mixes the liquid that forms with various organic compounds, if the two dissolves each other then for solution, if immiscible emulsion or the layered morphology of then forming.
Described opaque space can be sealing or open space, and the space can be arbitrary shape, such as tubular, taper etc.
Among the step S5 of the method, the described modes such as fitting of a polynomial, circle match or ellipse fitting that fit to.
The measurement of solid-liquid contact angle or calculating can adopt goniometry or amount supreme people's court to carry out.
The process of match and measurement or calculating can be undertaken by contact angle match and Survey Software.
Existing contact angle match and Survey Software have Drop Shape Analysis System(Kr ü ss, Germany), Surftens(SURFTENS Universal, Germany), SCA20(Dataphysics, Germany) etc.
Beneficial effect of the present invention is: compare with the contact angle measuring method based on optical imagery, the present invention utilizes nuclear magnetic resonance as imaging means, utilize the internal imaging function of nuclear magnetic resonance technique uniqueness, not only can measure the solid-liquid contact angle in the conventional transparent or open space system, can also measurement for opaque or the interior solid-liquid contact angle of enclosure space system.Range of application is widened, for the actual environment that more meets the liquid-soaked sign.
[description of drawings]
Fig. 1 is the process flow diagram according to solid-liquid contact angle measuring method of the present invention.
Figure 2 shows that optical imagery and Magnetic resonance imaging are to the contrast of opaque space imaging.
Fig. 3 is for adopting method of the present invention to the figure of difform opaque space imaging.
Figure 4 shows that the schematic diagram that adopts circular fit to measure contact angle.
[embodiment]
Magnetic resonance imaging (MRI) technology is to detect a kind of technology that electromagnetic wave that proton launches obtains the internal structure of body image by adding gradient magnetic.Magnetic resonance is a kind of physical phenomenon, by Block and Purcell in nineteen forty-six reported first and be applied to Wave Spectrum.In early 1970s, P. C. Lauterbur and P. Mansfield make a breakthrough in the MRI field afterwards, for the successful Application of MRI is laid a good foundation.
In recent years, the nmr imaging technique development is very rapid, ripe perfect day by day.Because its good nothing undermines Noninvasive, mr imaging technique has been widely used in the every field such as medical diagnosis, petroleum prospecting, material sign.
From image-forming principle, imaging is not done any requirement to the optical transparence of research system to nmr imaging technique by directly gathering the magnetic resonance signal of proton, therefore is very suitable for the research of solid/liquid interfaces phenomenon in opaque environment and the closed system.
The inventor sets forth the principle that wellability characterizes under the opaque condition take the wellability research of polyfluortetraethylene pipe and polyamide Guan Zhongshui as example.In the present invention, our advantage by can imaging under opaque condition by mr imaging technique, successfully realized the imaging of liquid in opaque teflon and the polyamide pipeline, and by the border curve in the image is carried out analysis to measure, thereby obtain the contact angle numerical value that optical means is difficult to obtain.
Below in conjunction with the drawings and specific embodiments the present invention is described in further detail.
Figure 1 shows that the process flow diagram according to solid-liquid contact angle measuring method of the present invention.As seen from the figure, measuring process mainly comprises following five steps:
At first be step S1, the solid-liquid system sample is put to the sample cavity of NMR imaging instrument, solid interface pattern and shape can be any pattern and shape, do not need before the experiment sample is carried out special processing.Because contact angle calculate to be that angle between liquid-gas interface and the solid-liquid interface realizes by measuring, therefore, no matter the interface shape how complicated as long as can accurately obtain gas-liquid and solid-liquid interface curve shape, all can obtain contact angle numerical value by the Fitting Calculation.
At step S2, from least one direction the liquid the described solid-liquid system sample is carried out pre-imaging, and to the image comparison analysis, to determine liquid gas interface position, direction and liquid gas interface center.In order to measure accurately, need to obtain the axle center section curve of solid-liquid and liquid-gas interface.
When spatial form and surface topography rule, or the space is when being transparent space, judges that liquid axle center section curve with regard to relatively easy many, can judge by naked eyes, and directly according to spatial form imaging parameters is set.Thereby can only carry out imaging from a direction to liquid, imaging process is relatively simple, only needs once can obtain required image.
Yet, when space when being opaque, since unclear to the interior volume situation, just pre-imaging be need at first carry out, and to the image comparison analysis, liquid gas interface position, direction and liquid gas interface center determined.Might need from a plurality of direction imagings, just can obtain accurately suitable result.
Then, at step S3, owing to having determined liquid gas interface position, direction and liquid gas interface center, can adjust the parameter of NMR imaging instrument this moment, with from least one direction, perpendicular to liquid gas interface and the plane of crossing the liquid gas interface central point (namely, on the plane of crossing liquid center's axle), liquid in the described solid-liquid system sample is carried out Magnetic resonance imaging, and to the image comparison analysis, cross the sectional view of central shaft with the liquid that obtains being fit to further to analyze.
Afterwards, at step S4, can be according to the sectional view that obtains, obtain the accurately axle center section curve of solid-liquid and liquid gas interface.
At last, at step S5, described axle center section curve is carried out match, and by measuring or calculating, obtain solid-liquid contact angle.
In the following specific embodiment, the inventor sets forth solid-liquid contact angular measurement, the i.e. principle of liquid-soaked sign in the solid-liquid system take the wellability research of glass core magnetic tube, polyfluortetraethylene pipe and polyamide Guan Zhongshui, dodecane as example.
Instrument and material
The NMI20-Analyst magnetic resonance imaging analysis instrument that adopts Suzhou Niumai Electronics Co., Ltd. to produce carries out imaging to liquid.
Adopt contact angle Survey Software SCA20(Dataphysics, Germany) the solid-liquid interface curve in the nuclear magnetic resonance image is carried out match.
Solid: polyfluortetraethylene pipe (
Φ12, length is about 3.5 cm); The polyamide pipe (
Φ12, length is about 3.5 cm); The glass core magnetic tube (
Φ5 Hes
Φ15).
Liquid: secondary deionized water; Dodecane.
Embodiment 1
Solid-liquid system is prepared: adopt successively acetone, ethanol and secondary deionized water to polyfluortetraethylene pipe supersound washing 15 minutes, and for subsequent use after the oven dry; Secondary deionized water is injected polyfluortetraethylene pipe, and according to the PIPE DIAMETER CALCULATION volume of water input, the control water yield is so that the interior water colunm height of pipe is not more than 2 cm.
The control of liquid height is in order to satisfy this experiment device therefor to the requirement of height of specimen, should understand, adopting other solid-liquid systems, difform space or when other NMR imaging instrument were measured, this parameter can suitably be adjusted, and does not affect scope of the present invention.
Magnetic resonance imaging: water-polyfluortetraethylene pipe system is vertically put into NMR imaging instrument, selecting z axle or x axle is imaging direction, magnetic field intensity is 0.5 T, take the multilayer spin-echo sequence as imaging sequence, repeated sampling stand-by period 1000 ms, accumulative frequency 32 times carries out imaging to the water in the polyfluortetraethylene pipe.
Liquid axle center section curve: adjust brightness of image and contrast, from figure, obtain water-teflon and Air-Water phase interface curve.
Match and measurement are calculated: by contact angle Survey Software SCA20(Dataphysics, Germany) water-teflon and Air-Water phase interface are carried out match, and contact angle measured, the contact angle that obtains water in this pipeline is 107.5 ± 1.1 °.
Embodiment 2
Except using the polyamide pipe belt for the polyfluortetraethylene pipe, step is similar to Example 1.
By contact angle Survey Software SCA20(Dataphysics, Germany) water-polyamide and Air-Water phase interface are carried out match, and contact angle is measured, the contact angle that obtains water in this pipeline is 69.4 ± 1.9 °.
Embodiment 3
Except using dodecane replacement secondary deionized water, step is similar to Example 1.Wherein in the Magnetic resonance imaging process, the repeated using stand-by period is 500 ms.
By contact angle Survey Software SCA20(Dataphysics, Germany) dodecane-teflon and air-dodecane phase interface are carried out match, and contact angle is measured, the contact angle that obtains dodecane in this pipeline is 45.7 ± 2.0 °.
Except using dodecane replacement secondary deionized water, step is similar to Example 2.Wherein in the Magnetic resonance imaging process, the repeated using stand-by period is 500 ms.
By contact angle Survey Software SCA20(Dataphysics, Germany) dodecane-polyamide and air-dodecane phase interface are carried out match, and contact angle is measured, the contact angle that obtains dodecane in this pipeline is 41.3 ± 3.6 °.
Except using
Φ5 nuclear magnetic tubes replace beyond the polyfluortetraethylene pipe, and step is similar to Example 1.
By contact angle Survey Software SCA20(Dataphysics, Germany) water-glass and Air-Water phase interface are carried out match, and contact angle is measured, the contact angle that obtains water in this pipeline is 24.3 ± 2.7 °.
Embodiment 6
Except using dodecane replacement secondary deionized water, step is similar to Example 5.Wherein in the Magnetic resonance imaging process, the repeated using stand-by period is 500 ms.
By contact angle Survey Software SCA20(Dataphysics, Germany) dodecane-glass and air-dodecane phase interface are carried out match, and contact angle is measured, the contact angle that obtains dodecane in this pipeline is 24.5 ± 2.8 °.
Embodiment 7
Except using
Φ15 nuclear magnetic tubes replace
Φ Beyond 5 nuclear magnetic tubes, step is similar to Example 5.
By contact angle Survey Software SCA20(Dataphysics, Germany) water-glass and Air-Water phase interface are carried out match, and contact angle is measured, the contact angle that obtains water in this pipeline is 29.1 ± 5.6 °.
Embodiment 8
Except using dodecane replacement secondary deionized water, step is similar to Example 7.
By contact angle Survey Software SCA20(Dataphysics, Germany) dodecane-glass and air-dodecane phase interface are carried out match, and contact angle is measured, the contact angle that obtains dodecane in this pipeline is 33.7 ± 6.3 °.
Embodiment 1-4 is the measurement to solid-liquid contact angle under the opaque condition; Embodiment 5-8 is the measurement to solid-liquid contact angle under the transparent condition.As seen according to transparent without any requirement to solid of the contact angle measuring method that the present invention is based on Magnetic resonance imaging, greatly widened the research range of liquid-soaked.
To compare based on optical imaging method in order illustrating with existing, to the present invention is based on the superiority of the solid-liquid contact angle measuring method of Magnetic resonance imaging, the inventor has carried out respectively optical imagery and Magnetic resonance imaging to the water in the polyfluortetraethylene pipe.The gained image is shown among Fig. 2, a) is the image of optical imagery wherein; B) be the image of Magnetic resonance imaging.
Obviously as seen, because polyfluortetraethylene pipe is opaque, traditional optical method is difficult to recognize the wetting behavior of water in polyfluortetraethylene pipe, then can clearly observe the wet face state of water in polyfluortetraethylene pipe by magnetic resonance imaging from figure.Therefore method of the present invention can effectively overcome the defective that the optical imagery method can't imaging in opaque space, is particularly suited for the measurement of solid-liquid contact angle in the opaque space, and then helps to understand in the opaque space liquid to the wellability of solid.
Figure 3 shows that the employing Magnetic resonance imaging, right
Φ5 cylindrical glass nuclear magnetic tubes (a), and the water in the conical glass container (b) carries out imaging, the image that obtains.
As seen method of the present invention is to the not restriction of shape in space, and it can be cylindricality, taper, or other any shapes.Image among the figure clearly reflects the water-wet behavior of glass.
Fig. 4 for example understands by adopting circular fit to measure contact angle
θSchematic diagram.
Above, our advantage by can imaging under opaque condition by mr imaging technique, successfully realized in opaque teflon and polyamide pipeline and the imaging of liquid in transparent glass core magnetic tube, and by the border curve in the image is carried out analysis to measure, thereby obtain the contact angle numerical value that optical means is difficult to obtain.Therefore, method of the present invention has been expanded the solid-liquid contact angular measurement greatly to the whether all no requirement (NR)s of rule of whether transparent, the spatial form in space, and the range of application of liquid-soaked sign.
The above the specific embodiment of the present invention does not consist of the restriction to protection domain of the present invention.Various other corresponding changes and distortion that any technical conceive according to the present invention has been done all should be included in the protection domain of claim of the present invention.
Claims (8)
1. method that is used for solid-liquid contact angle in measurement for opaque or the enclosure space, wherein solid is made of nonferromugnetic material, and liquid contains the atomic nucleus that nuclear-spin quantum number equals 1/2, is filled with described liquid and air in the described space, and described method comprises:
S1 places the solid-liquid system sample to the sample cavity of NMR imaging instrument;
S2 carries out pre-imaging from least one direction to the liquid the described solid-liquid system sample, and to the image comparison analysis, to determine liquid gas interface position, direction and liquid gas interface center;
S3 is from least one direction, on the plane perpendicular to described liquid gas interface and the described liquid gas interface central point of mistake, liquid in the described solid-liquid system sample is carried out Magnetic resonance imaging, and to the image comparison analysis, cross the sectional view of liquid gas interface central shaft to obtain liquid;
S4 obtains the axle center section curve of solid-liquid and liquid gas interface according to described sectional view;
S5 carries out match to described axle center section curve, and by measuring or calculating, obtains solid-liquid contact angle.
2. method according to claim 1, wherein, described solid is made of the material that is selected from glass, teflon, polyamide.
3. method according to claim 1, wherein, described liquid is selected from waterborne liquid, oil-based liquid or water-oil mixture.
4. method according to claim 1, wherein, described opaque space is sealing or open space.
5. method according to claim 1, wherein, the shape in described space comprises tubular, taper.
6. method according to claim 1, wherein, among the step S5, described fitting of a polynomial, circle match or the ellipse fitting of fitting to.
7. method according to claim 1, wherein, among the step S5, the measurement of solid-liquid contact angle or calculate and adopt goniometry or amount supreme people's court to carry out.
8. method according to claim 1, wherein, step S5 adopts contact angle match and Survey Software to carry out.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103852403A (en) * | 2014-03-13 | 2014-06-11 | 深圳大学 | Method for measuring contact angle and surface energy of cement-based material |
| CN104132871A (en) * | 2014-05-30 | 2014-11-05 | 中国石油化工股份有限公司 | Method for measuring surface contact angle between opaque liquid and solid |
| CN104634805A (en) * | 2013-11-13 | 2015-05-20 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for measuring underwater contact angle of water strider leg simulated structure |
| CN105452842A (en) * | 2013-10-30 | 2016-03-30 | 京瓷医疗株式会社 | Contact-angle measurement method, contact-angle measurement device, bioprosthetic-member inspection device, program, and storage medium |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105452842A (en) * | 2013-10-30 | 2016-03-30 | 京瓷医疗株式会社 | Contact-angle measurement method, contact-angle measurement device, bioprosthetic-member inspection device, program, and storage medium |
| CN105452842B (en) * | 2013-10-30 | 2019-03-29 | 京瓷株式会社 | Contact angle measuring method, apparatus for measuring contact angle, organism patchery component check device and storage medium |
| CN104634805A (en) * | 2013-11-13 | 2015-05-20 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for measuring underwater contact angle of water strider leg simulated structure |
| CN104634805B (en) * | 2013-11-13 | 2017-05-03 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for measuring underwater contact angle of water strider leg simulated structure |
| CN103852403A (en) * | 2014-03-13 | 2014-06-11 | 深圳大学 | Method for measuring contact angle and surface energy of cement-based material |
| CN103852403B (en) * | 2014-03-13 | 2016-05-11 | 深圳大学 | The measuring method of a kind of cement-based material contact angle and surface energy |
| CN104132871A (en) * | 2014-05-30 | 2014-11-05 | 中国石油化工股份有限公司 | Method for measuring surface contact angle between opaque liquid and solid |
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Application publication date: 20130206 |