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 PDF

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CN102914490A
CN102914490A CN 201210380819 CN201210380819A CN102914490A CN 102914490 A CN102914490 A CN 102914490A CN 201210380819 CN201210380819 CN 201210380819 CN 201210380819 A CN201210380819 A CN 201210380819A CN 102914490 A CN102914490 A CN 102914490A
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liquid
solid
contact angle
method
magnetic resonance
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CN 201210380819
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朱未琴
高雪峰
江雷
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中国科学院苏州纳米技术与纳米仿生研究所
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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.

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CN 102914490 A CN 102914490 A

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不透明或封闭空间内固液接触角测量方法 The method of solid-liquid contact angle measurement in an opaque enclosure or

[0001]【技术领域】 [0001] TECHNICAL FIELD

本发明涉及测量技术领域,具体涉及表征材料浸润性的固液接触角测量方法。 The present invention relates to the field of measuring technology, particularly relates to a solid-liquid contact angle measuring method to characterize the material wettability. [0002]【背景技术】 [0002] BACKGROUND

浸润性是固体重要的表面性质,在矿石浮选、建材涂料、防腐防水等等方面有着重要的应用。 Invasive nature of the solid surface is important, has important applications in ore flotation, architectural coatings, waterproofing, etc., anti-corrosion. 由于其在科学研究及实际应用中的重要地位,固体表面浸润性研究一直都是物理化学领域的热点内容。 Because of its important role in scientific research and practical applications, solid surface wettability of research has been a hot field of physical chemistry content. 其中,接触角测量作为浸润性研究最基本的组成部分,对于表面/界面科学领域的理论研究及生产实践有着重要的价值。 Wherein the contact angle measurements as part of invasive basic research has important value for surface / interface theoretical research and production practice of science.

[0003] 随着技术进步和研究的深入,已相继开发出多种测量接触角的方法,如Wilhelmy吊片法、悬滴法、气泡捕获法等等。 [0003] With the development of research and technological advances, we have been developed a variety of methods of measuring the contact angle, such as by Wilhelmy plate method, the hanging drop method, the bubble trap method and the like. 由于操作简便等优点,悬滴法在接触角测量中的应用最为广泛,其主要原理是通过光学成像得到微液滴在固体表面上的外形图像,通过对液滴轮廓进行拟合分析,最终得到接触角数值。 Since the advantages of simple operation, the hanging drop method in the application contact angle measurements are most widely used, its main principle is to give micro-droplets on a solid surface shape image by optical imaging, by contour droplet fit analysis finally obtained The contact angle values. 目前绝大多数的接触角测量仪都基于此原理。 At present, most of the contact angle measurement are based on this principle.

[0004] 然而,由于该方法是以光学成像为基本条件的,这就势必要求接触角测量必须在透明和开放体系中进行。 [0004] However, since this method is based on optical imaging as the basic conditions, which will require that a contact angle measurements must be carried out in a transparent and open system. 而在实际应用中,各种浸润行为往往是在不透明或封闭的情况下发生的,例如有害液体表面张力的测量、液体输运管道内流体控制、微流控体系等等,这些都是浸润性研究的重要应用方向,但由于体系本身的不透明及封闭性,传统的接触角测量手段无法应用于此类研究,这对于表面界面科学的理论发展及实际应用造成了很大的阻碍。 In practical applications, various wetting behavior often occurs in the case of an opaque or closed, e.g., noxious liquid surface tension of the liquid transport line fluid control, microfluidic systems, etc., which are invasive important application direction of research, but the system itself is opaque and closed, the traditional means of contact angle measurements can not be applied to such research, which has created a significant obstacle to the development of theory and practical application of surface and interface science.

[0005] 例如,聚四氟乙烯及聚酰胺是常用的液体管道输运材料,管道内液体的润湿状态对于流体参数及输运效率有着重要影响。 [0005] For example, polytetrafluoroethylene and polyamides are commonly used in liquid conduit transport material, the wet state conduit for liquid transport and fluid parameters have an important impact efficiency. 因此,得到流体在管道内的接触角,对于深入了解流体状态及进一步对流体进行调控有重要作用。 Thus, to obtain the contact angle of the fluid in the pipe, and fluid state for a further understanding of the important role in the regulation of fluid. 然而,由于材料的不透明性,采用传统的光学方法对液体在管道内的浸润状态无从了解。 However, since the opacity of the material, using methods conventional optical state of wetting liquid in the pipeline no way of knowing.

[0006] 因此亟需一种新的技术,用以实现对不透明及封闭体系内液体浸润性的研究。 [0006] Thus the need of a new technology, research to achieve an opaque liquid wettability and a closed system.

[0007]【发明内容】 [0007] [DISCLOSURE]

本发明要解决的技术问题是:开发一种能够测量不透明或封闭空间内部固液接触角的方法。 The present invention is to solve the technical problem: to develop a method capable of measuring opaque or enclosed space inside the solid-liquid contact angle.

[0008] 本发明提供一种用于测量不透明或封闭固液体系内部接触角的方法,其中固体由非铁磁性材料构成,液体含有核自旋量子数等于1/2的原子核,所述固体构成的空间内充有所述液体及空气,所述方法包括: [0008] The present invention provides a method for measuring blocking opaque or solid-liquid contact angle of the internal system, wherein the solid consists of non-ferromagnetic material, a liquid containing a nuclear spin quantum number of nuclei is equal to 1/2, the solid configuration filled with the liquid and air in the space, the method comprising:

SI放置所述固液体系至核磁共振成像仪的样品腔; SI placing the sample chamber to said solid-liquid system is magnetic resonance imaging device;

S2从至少一个方向对所述固液体系样品中的液体进行预成像,并对图像对比分析,以确定液气界面位置、方向及液气界面中心点; Pre-S2 system imaging the solid-liquid sample from at least one direction, image contrast analysis and to determine the liquid-gas interface position, direction and the center point of the liquid-air interface;

S3从至少一个方向,在垂直于所述液气界面方向且过所述液气界面中心点的平面,对所述固液体系样品中的液体进行核磁共振成像,并对图像对比分析,以得到液体过液气界面中心轴的剖面图; S3 from at least one direction, in a direction perpendicular to the liquid-gas interface of the plane through the center of the liquid-gas interface of said solid-liquid system liquid sample MRI, contrast and image analysis, to give sectional view of the liquid through the liquid-air interface of the central axis;

S4根据所述剖面图,得到固液和液气界面的轴心剖面曲线; S4 according to the cross-sectional view, axial sectional curves to obtain a solid-liquid and liquid-gas interface;

S5对所述轴心剖面曲线进行拟合,并通过测量或计算,得到固液接触角。 S5 fitting the axial cross-sectional profile, and by measurement or calculation, the solid-liquid contact angle.

3[0009] 固体可由任何非铁磁性材料构成,例如玻璃、聚四氟乙烯、聚酰胺,或其它非铁磁性材料。 3 [0009] The solid may be any non-ferromagnetic material, such as glass, polytetrafluoroethylene, polyamide, or other non-ferromagnetic material.

[0010] 液体可选自水性液体、油性液体或水油混合物。 [0010] Alternatively liquid from an aqueous liquid, an oily liquid or an oil mixture of water. 其中水性液体可以是水,或水溶液,或可溶于水中的液体,包括醇类等。 Wherein the aqueous liquid may be water, or an aqueous solution, liquid or soluble in water, including alcohols and the like. 油性液体可以为烷烃、芳香烃、酯类、脂肪酸等有机化合物;水油混合物是指水与各种有机化合物混合形成的液体,若二者互溶则为溶液,若互不相溶则形成乳液或分层形态。 The oily liquid may be an alkane, an aromatic hydrocarbon, esters, fatty acids and other organic compounds; refers to a liquid mixture of water and oil and water formed by mixing various organic compounds, compared to if the two immiscible solutions, if an emulsion is formed or immiscible layered form.

[0011] 所述不透明空间可为封闭或开放的空间,并且空间可为任意形状,例如管形、锥形 [0011] The opaque space may be closed or open space, and the space may be of any shape such as tubular, conical

坐寸O Sit inch O

[0012] 该方法的步骤S5中,所述拟合为多项式拟合、圆拟合或椭圆拟合等方式。 Step [0012] This process S5, the polynomial fit to the circle or ellipse fitting the fitting or the like.

[0013] 固液接触角的测量或计算可采用量角法或量高法进行。 [0013] protractor method can be measured or calculated or amount of the solid-liquid contact angle for the Supreme Court.

[0014] 拟合与测量或计算的过程可以通过接触角拟合及测量软件进行。 [0014] fit to the measured or calculated process may be carried out by measuring the contact angle and fitting software.

[0015] 现有的接触角拟合及测量软件有Drop Shape Analysis System (Kriiss,Germany)>Surftens (SURFTENS Universal,Germany)>SCA20 (Dataphysics, Germany)等。 [0015] The fitting and conventional contact angle measurement software Drop Shape Analysis System (Kriiss, Germany)> Surftens (SURFTENS Universal, Germany)> SCA20 (Dataphysics, Germany) and the like.

[0016] 本发明的有益效果在于:与基于光学成像的接触角测量方法相比,本发明利用核磁共振作为成像手段,利用核磁共振技术独特的内部成像功能,不仅可以测量常规的透明或开放空间体系内的固-液接触角,还可以测量不透明或封闭空间体系内的固-液接触角。 [0016] Advantageous effects of the present invention is that: compared with the contact angle measurement based on optical imaging, the present invention is the use of magnetic resonance imaging as a means of using unique internal nuclear magnetic resonance imaging function can measure not only the conventional transparent or open space the solid in the system - liquid contact angle, can also be measured in an opaque or solid enclosed space system - liquid contact angle. 应用范围得以拓宽,对于更符合液体浸润性表征的实际环境。 To broaden the range of applications, more in line with the actual environment of the liquid wettability characterization.

[0017]【附图说明】 [0017] BRIEF DESCRIPTION

图I为根据本发明的固液接触角测量方法的流程图。 Figure I is a flow chart solid-liquid contact angle measuring method according to the present invention.

[0018] 图2所示为光学成像与核磁共振成像对不透明空间成像的对比。 [0018] FIG. 2 shows a comparison of the optical imaging and MRI imaging of the opaque space.

[0019] 图3为采用本发明的方法对不同形状的不透明空间成像的图。 [0019] FIG. 3 is a method of the present invention, FIG opaque spatial imaging of different shapes.

[0020] 图4所示为采用圆形拟合测量接触角的示意图。 [0020] FIG. 4 is a schematic view of the contact angle is measured using a circular fitting.

[0021]【具体实施方式】 [0021] DETAILED DESCRIPTION OF THE INVENTION

核磁共振成像(MRI)技术是通过外加梯度磁场检测氢核所发射出的电磁波而得到物体内部结构图像的一种技术。 Magnetic resonance imaging (MRI) technology is electromagnetic wave emitted by hydrogen nuclear detecting gradient magnetic field is applied to give a technical structure of the interior of the object image. 磁共振是一种物理现象,由Block与Purcell于1946年首次报道并将其应用于波谱学。 Magnetic resonance is a physical phenomenon by Block and Purcell was first reported in 1946 and applied spectroscopy. 之后在20世纪70年代初,PC Lauterbur和P. Mansfield在MRI领域取得突破性进展,为MRI的成功应用奠定了基础。 After the early 1970s, PC Lauterbur and P. Mansfield breakthrough in the field of MRI, laid the foundation for the successful application of MRI.

[0022] 近年来,核磁共振成像技术发展十分迅速,已日臻成熟完善。 [0022] In recent years, magnetic resonance imaging technology developed rapidly, has matured perfect. 由于其良好的无损及非侵入性,磁共振成像技术已被广泛应用于医疗诊断、石油勘探、材料表征等各个领域中。 Because of its good all areas of destructive and non-invasive, magnetic resonance imaging technology has been widely applied to medical diagnosis, oil exploration, material characterization, and the like.

[0023] 从成像原理来看,核磁共振成像技术通过直接采集氢核的磁共振信号而成像,对研究体系的光学透明性不做任何要求,因此非常适合于不透明环境及封闭体系中固/液界面现象的研究。 [0023] From the point of view imaging principle, it is imaged by magnetic resonance imaging of hydrogen nuclei directly acquired magnetic resonance signals, the optical transparency of the research system without any requirements, making it ideal for closed systems and the solid opaque environment / liquid study interfacial phenomena.

[0024] 发明人以聚四氟乙烯管和聚酰胺管中水的浸润性研究为例,阐述不透明条件下浸润性表征的原理。 [0024] The inventors to investigate wettability PTFE tube and water tube for example polyamide, characterized wettability opaque under the conditions set forth principles. 在本发明中,我们通过借助磁共振成像技术可在不透明条件下成像的优势,成功实现了不透明聚四氟乙烯及聚酰胺管道内液体的成像,并通过对图像中的界面曲线进行分析测量,从而获得光学方法难以得到的接触角数值。 In the present invention, we can by means of magnetic resonance imaging in the imaging conditions advantage opaque, the opaque imaging successfully polytetrafluoroethylene and polyamide line liquids, and measured by analyzing the image of the boundary curve, thereby obtaining a contact angle values ​​obtained by the optical method is difficult.

[0025] 下面结合附图和具体实施例对本发明作进一步详细说明。 [0025] conjunction with the accompanying drawings and the following specific embodiments of the present invention is described in further detail.

[0026] 图I所示为根据本发明的固液接触角测量方法的流程图。 As shown in a flowchart [0026] I FIG solid-liquid contact angle measuring method according to the present invention. 从图中可见,测量过程主要包括以下五个步骤:首先是步骤SI,将固液体系样品放至核磁共振成像仪的样品腔中,固体界面形貌及形状可以为任何形貌和形状,实验前不需对样品进行特殊处理。 Seen from the figure, the measuring process includes the following five steps: first step of the SI, the discharge chamber to the sample in the magnetic resonance imaging system of a solid-liquid sample, and morphology solid interface shape may be any shape and morphology, experimental The samples were before without special treatment. 由于接触角计算是通过量取气液界面及固液界面之间的夹角来实现的,因此,无论界面形状多么复杂,只要能够准确得到气液及固液界面曲线形状,均可通过拟合计算得到接触角数值。 Since the contact angle is calculated taking the angle between the gas-liquid interface and the solid-liquid interface by an amount to achieve, therefore, no matter how complicated the shape of the interface, as long as the liquid can accurately obtain the shape of the curve and the solid-liquid interface, can be fitted through The contact angle values ​​calculated.

[0027] 在步骤S2,从至少一个方向对所述固液体系样品中的液体进行预成像,并对图像对比分析,以确定液气界面位置、方向及液气界面中心。 [0027] In step S2, the pre-image of a solid-liquid system, the liquid sample from at least one direction, image contrast analysis and to determine the position of the liquid-air interface, and the direction of the central liquid-air interface. 为了测量精确,需要获得固液和气液界面的轴心剖面曲线。 For accurate measurement, it is necessary to obtain the axial cross-sectional profile of a solid-liquid and gas-liquid interface.

[0028] 当空间形状和表面形貌规则,或是空间为透明空间时,判断液体轴心剖面曲线就相对容易的多,可以通过肉眼判断,并直接根据空间形状来设置成像参数。 [0028] When the spatial shape and surface morphology rules, transparent space or a space, the liquid is determined relatively easy axial sectional curve more, it can be judged by eye, and to set the imaging parameters directly from the spatial shape. 从而可以仅从一个方向对液体进行成像,成像过程相对简单,仅需一次即可获得所需图像。 So that the liquid can be imaged from only one direction, the imaging process is relatively simple, only a desired image can be obtained.

[0029] 然而,当空间为不透明时,由于对空间内部状况不清楚,就需要首先进行预成像,并对图像对比分析,来确定液气界面位置、方向及液气界面中心。 [0029] However, when the space is opaque, since the internal space of unknown status, would need to be pre-imaged, and the image contrast analysis, to determine the position of the liquid-air interface, and the direction of the central liquid-air interface. 有可能需要从多个方向成像,才能得到准确合适的结果。 There may be imaged from multiple directions, the right to get accurate results.

[0030] 然后,在步骤S3,由于已经确定了液气界面位置、方向及液气界面中心,此时可以调整核磁共振成像仪的参数,以从至少一个方向,在垂直于液气界面且过液气界面中心点的平面(即,在过液体中心轴的平面),对所述固液体系样品中的液体进行核磁共振成像,并对图像对比分析,以得到适合进一步分析的液体过中心轴的剖面图。 [0030] Then, at step S3, it has been determined due to the liquid-gas interface position, direction and the center of the liquid air interface, then you can adjust the parameters of the magnetic resonance imager, from at least one direction, perpendicular to and through the liquid-air interface liquid-air interface of the center point of the plane (i.e., in a plane through the central axis of the liquid), a solid-liquid system, the liquid sample is magnetic resonance imaging, contrast and image analysis, to give a liquid through the central axis for further analysis the cross-sectional view.

[0031] 之后,在步骤S4,可以根据得到的剖面图,得到准确的固液和液气界面的轴心剖面曲线。 After [0031] In step S4, according to a cross-sectional view taken, accurate axial cross-sectional profile of a solid-liquid and liquid-gas interface.

[0032] 最后,在步骤S5,对所述轴心剖面曲线进行拟合,并通过测量或计算,得到固液接触角。 [0032] Finally, in step S5, the axial cross-sectional curve fitting, and by measurement or calculation, the solid-liquid contact angle.

[0033] 以下具体实施例中,发明人以玻璃核磁管、聚四氟乙烯管和聚酰胺管中水、十二烷的浸润性研究为例,阐述固液体系中固液接触角测量,即液体浸润性表征的原理。 [0033] The following specific examples, the inventors glass NMR tube, PTFE tube and water tube polyamide, wettability studies dodecane example, describes a solid-liquid solid-liquid contact angle measurement system, i.e., liquid wettability characterized principle.

[0034] 仪器与材料 [0034] Apparatus and Materials

采用苏州纽迈电子科技有限公司生产的匪120-Analyst磁共振成像分析仪对液体进行成像。 Suzhou Niumai using Electronic Technology Co. bandit 120-Analyst magnetic resonance imaging for imaging a liquid analyzer.

[0035] 采用接触角测量软件SCA20 (Dataphysics, Germany)对核磁共振图像中的固液界面曲线进行拟合。 [0035] The contact angle measurement software SCA20 (Dataphysics, Germany) magnetic resonance curve for the solid-liquid interface in the image fit.

[0036] 固体:聚四氟乙烯管(Φ12,长度为约3. 5 cm);聚酰胺管(Φ 12,长度为约3. 5 cm);玻璃核磁管(Φ5和Φ15)。 [0036] Solid: PTFE tube (Φ12, a length of about 3. 5 cm); polyamide tube (Φ 12, a length of about 3. 5 cm); NMR glass tube (phi] 5 and Φ15).

[0037] 液体:二次去离子水;十二烷。 [0037] Liquid: Secondary deionized water; dodecane.

[0038] 实施例I [0038] Example I

固液体系准备:依次采用丙酮、乙醇及二次去离子水对聚四氟乙烯管超声洗涤15分钟,烘干后备用;将二次去离子水注入聚四氟乙烯管中,根据管径计算注入水量,控制水量使得管内水柱高度不大于2 cm。 Preparing a solid-liquid system: successively using acetone, ethanol, and washed with deionized water secondary Teflon tube sonicated for 15 minutes, drying standby; secondary Teflon tube of deionized water were calculated in accordance with the diameter injection of water, control of water column height such that the inner tube is not greater than 2 cm.

[0039] 液体高度的控制是为了满足本实验所用设备对样品高度的要求,应理解,在采用其他固液体系、不同形状的空间、或在其他核磁共振成像仪上测量时,该参数可以适当调整,而不影响本发明的范围。 [0039] Control of the liquid level in order to meet the equipment used for this test sample height requirements should be appreciated that when using other solid-liquid systems, the space of different shapes, or other measurements on magnetic resonance imaging device, this parameter can be suitably adjustment, without affecting the scope of the present invention.

[0040] 核磁共振成像:将水-聚四氟乙烯管体系竖直放入核磁共振成像仪中,选择z轴 [0040] Magnetic Resonance Imaging: water - Teflon tubing system of vertically placed magnetic resonance imaging device, the selected z-axis

5或X轴为成像方向,磁场强度为O. 5 T,以多层自旋回波序列为成像序列,重复采样等待时间1000 ms,累加次数32次,对聚四氟乙烯管中的水进行成像。 5 is an imaging or X-axis direction, the magnetic field strength is O. 5 T, a multi-layer spin-echo sequence is an imaging sequence, repeated sampling wait time 1000 ms, the accumulated number of times 32, the water tube polytetrafluoroethylene imaging .

[0041] 液体轴心剖面曲线:调整图像亮度及对比度,从图中得到水-聚四氟乙烯及空气-水相界面曲线。 [0041] Liquid axial sectional curve: adjusting image brightness and contrast, to obtain water from the drawing - and polytetrafluoroethylene air - aqueous phase interface curve.

[0042] 拟合及测量计算:通过接触角测量软件SCA20 (Dataphysics, Germany)对水-聚四氟乙烯及空气-水相界面进行拟合,并对接触角进行测量,得到该管道内水的接触角为107. 5 ± I. 1°。 [0042] Fitting and measuring and calculating: water contact angle measurement software SCA20 (Dataphysics, Germany) - and polytetrafluoroethylene air - aqueous phase interface fit, and the contact angle was measured to give the water contact with the duct angle of 107. 5 ± I. 1 °.

[0043] 实施例2 [0043] Example 2

除了使用聚酰胺管代替聚四氟乙烯管以外,步骤与实施例I类似。 Except that in place of the polyamide PTFE tube outside tube, similar to the procedure of Example I.

[0044] 通过接触角测量软件SCA20 (Dataphysics, Germany)对水-聚酰胺及空气-水相界面进行拟合,并对接触角进行测量,得到该管道内水的接触角为69. 4 ± 1.9°。 [0044] by a contact angle measurement software SCA20 (Dataphysics, Germany) water - for fitting aqueous phase interface, and the contact angle was measured to obtain the contact angle of water within the duct 69. 4 ± 1.9 ° - Polyamide and air .

[0045] 实施例3 [0045] Example 3

除了使用十二烷代替二次去离子水以外,步骤与实施例I类似。 Except that instead of the secondary dodecane than deionized water, similar to the procedure of Example I. 其中核磁共振成像过程中,重复采用等待时间为500 ms ο Wherein the magnetic resonance imaging procedure is repeated using the waiting time is 500 ms ο

[0046] 通过接触角测量软件SCA20(Dataphysics, Germany)对十二烧-聚四氟乙烯及空气-十二烷相界面进行拟合,并对接触角进行测量,得到该管道内十二烷的接触角为45. 7± 2.0。 [0046] by a contact angle measurement software SCA20 (Dataphysics, Germany) for twelve burn - dodecane phase interface for fitting, and the contact angle was measured to obtain the contact within the duct dodecane - PTFE and air angle of 45. 7 ± 2.0. .

[0047] 实施例4 [0047] Example 4

除了使用十二烷代替二次去离子水以外,步骤与实施例2类似。 Except that instead of the secondary dodecane than deionized water, similar to the procedure of Example 2. 其中核磁共振成像过程中,重复采用等待时间为500 ms ο Wherein the magnetic resonance imaging procedure is repeated using the waiting time is 500 ms ο

[0048] 通过接触角测量软件SCA20 (Dataphysics, Germany)对十二烧-聚酰胺及空气-十二烷相界面进行拟合,并对接触角进行测量,得到该管道内十二烷的接触角为41. 3+ 3. 6° 。 [0048] by a contact angle measurement software SCA20 (Dataphysics, Germany) for twelve burn - dodecane phase interface for fitting, and the contact angle was measured to obtain the contact angle of the dodecane duct - Air polyamide and 41. 3+ 3. 6 °.

[0049] 实施例5 [0049] Example 5

除了使用Φ5核磁管代替聚四氟乙烯管以外,步骤与实施例I类似。 Except that instead of the PTFE tube Φ5 NMR tube except that steps similar to Example I.

[0050] 通过接触角测量软件SCA20 (Dataphysics, Germany)对水-玻璃及空气_水相界面进行拟合,并对接触角进行测量,得到该管道内水的接触角为24. 3 ± 2.7°。 [0050] The water contact angle measurement software SCA20 (Dataphysics, Germany) - _ glass and air interface to fit the aqueous phase, and the contact angle was measured to obtain the contact angle of water within the duct 24. 3 ± 2.7 °.

[0051] 实施例6 [0051] Example 6

除了使用十二烷代替二次去离子水以外,步骤与实施例5类似。 Except that instead of the secondary dodecane than deionized water, similar to the procedure of Example 5. 其中核磁共振成像过程中,重复采用等待时间为500 ms ο Wherein the magnetic resonance imaging procedure is repeated using the waiting time is 500 ms ο

[0052] 通过接触角测量软件SCA20 (Dataphysics, Germany)对十二烧-玻璃及空气-十二烷相界面进行拟合,并对接触角进行测量,得到该管道内十二烷的接触角为24. 5± 2.8。 [0052] by a contact angle measurement software SCA20 (Dataphysics, Germany) for twelve burning - glass and air - for fitting dodecane phase interface, and the contact angle was measured to obtain the contact angle of the dodecane to the duct 24 . 5 ± 2.8. .

[0053] 实施例7 [0053] Example 7

除了使用Φ15核磁管代替Φ5核磁管以外,步骤与实施例5类似。 Except that instead of Φ15 NMR tube outside Φ5 NMR tube, similar to the procedure of Example 5.

[0054] 通过接触角测量软件SCA20 (Dataphysics, Germany)对水-玻璃及空气_水相界面进行拟合,并对接触角进行测量,得到该管道内水的接触角为29. I ± 5.6°。 [0054] The water contact angle measurement software SCA20 (Dataphysics, Germany) - _ glass and air interface to fit the aqueous phase, and the contact angle was measured to obtain the contact angle of water within the duct 29. I ± 5.6 °.

[0055] 实施例8 [0055] Example 8

除了使用十二烷代替二次去离子水以外,步骤与实施例7类似。 Except that instead of the secondary dodecane than deionized water, similar to the procedure of Example 7.

6[0056] 通过接触角测量软件SCA20 (Dataphysics, Germany)对十二烧-玻璃及空气-十二烷相界面进行拟合,并对接触角进行测量,得到该管道内十二烷的接触角为33. 7+ 6. 3° ο [0057] 实施例1-4是对不透明条件下固液接触角的测量;实施例5-8是对透明条件下固液接触角的测量。 6 [0056] by a contact angle measurement software SCA20 (Dataphysics, Germany) for twelve burn - dodecane phase interface for fitting, and the contact angle was measured to obtain the contact angle of the dodecane duct - glass and air 33. 7+ 6. 3 ° ο [0057] Examples 1-4 for solid-liquid contact angle was measured under conditions opaque; Example 5-8 for solid-liquid contact angle was measured under the conditions of transparency. 可见根据本发明基于核磁共振成像的接触角测量方法对固体的透明性无任何要求,大大拓宽了液体浸润性的研究范围。 The measuring method of the contact angle can be seen on magnetic resonance imaging of the present invention without any requirements for transparent solid, greatly broadens the coverage of the liquid wettability.

[0058] 为了说明与现有基于光学成像方法相比,本发明基于核磁共振成像的固液接触角测量方法的优越性,本发明人对聚四氟乙烯管中的水分别进行了光学成像和核磁共振成像。 [0058] To illustrate, compared with the conventional methods based on optical imaging, the method of the present invention is based on the advantages of solid-liquid contact angle measurements of magnetic resonance imaging, the present invention is polytetrafluoroethylene tube water respectively and the optical imaging magnetic resonance imaging. 所得图像示于图2中,其中a)为光学成像的图像;b)为核磁共振成像的图像。 The resulting images are shown in Figure 2, wherein a) an image of an optical imaging; b) of the MRI images.

[0059] 从图中明显可见,由于聚四氟乙烯管不透明,传统的光学法难以了解到水在聚四氟乙烯管中的润湿行为,而通过磁共振成像则可清楚地观察到水在聚四氟乙烯管中的浸润状态。 [0059] As is evident from the figure, since the PTFE tube opaque, conventional optical method is difficult to understand the behavior of water wet Teflon tube, while clearly observed in the water may be by magnetic resonance imaging infiltration state Teflon tube. 因此本发明的方法可以有效克服光学成像法在不透明空间中无法成像的缺陷,尤其适于不透明空间中固液接触角的测量,进而有助于了解不透明空间中液体对固体的浸润性。 Thus the method of the present invention can be effectively overcome the optical imaging method in the opaque space can not image defects, particularly suitable for solid-liquid contact angle measurement space opaque, thereby helping to understand the wettability of a liquid on a solid opaque space.

[0060] 图3所示为采用核磁共振成像,对Φ5圆柱形玻璃核磁管(a),以及圆锥形玻璃容器(b)中的水进行成像,得到的图像。 [0060] Figure 3 is a nuclear magnetic resonance imaging, for Φ5 cylindrical glass NMR tube (A), and a conical glass container (b) water is imaged, the image obtained.

[0061] 可见本发明的方法对空间的形状没有限制,其可以是柱形、锥形,或是其他任何形状。 [0061] The method of the present invention can be seen there is no limitation on the shape of the space, which may be cylindrical, conical, or any other shape. 图中的图像清楚地反映出玻璃的亲水特性。 FIG clearly reflects the image of the hydrophilic properties of the glass.

[0062] 图4举例说明了通过采用圆形拟合测量接触角β的示意图。 [0062] FIG 4 illustrates a schematic view of a circular fitting by using a contact angle β is measured.

[0063] 以上,我们通过借助磁共振成像技术可在不透明条件下成像的优势,成功实现了在不透明的聚四氟乙烯和聚酰胺管道、以及在透明的玻璃核磁管内液体的成像,并通过对图像中的界面曲线进行分析测量,从而获得光学方法难以得到的接触角数值。 [0063] above, we can by means of magnetic resonance imaging in the imaging conditions advantages opaque, opaque successfully achieved polytetrafluoroethylene and polyamide pipe, and an imaging fluid within the transparent glass NMR tube, and by boundary curve image analysis measurements, thereby obtaining the contact angle values ​​obtained by the optical method is difficult. 因此,本发明的方法对空间的是否透明、空间形状是否规则均无要求,大大拓展了固液接触角测量,及液体浸润性表征的应用范围。 Thus, the method of the present invention is transparent to the space, whether the space requirements no regular shape, greatly expand the solid-liquid contact angle measurement, and the scope of application of liquid wettability characterized.

[0064] 以上所述本发明的具体实施方式,并不构成对本发明保护范围的限定。 [0064] DETAILED DESCRIPTION embodiment of the present invention described above, do not limit the scope of the present invention. 任何根据本发明的技术构思所作出的各种其他相应的改变与变形,均应包含在本发明权利要求的保护范围内。 Any of various technical concept of the present invention to make corresponding changes and other modification, should be included within the scope of the claims of the invention.

Claims (8)

  1. 1. 一种用于测量不透明或封闭空间内固液接触角的方法,其中固体由非铁磁性材料构成,液体含有核自旋量子数等于1/2的原子核,所述空间内充有所述液体及空气,所述方法包括:Si放置固液体系样品至核磁共振成像仪的样品腔中;S2从至少一个方向对所述固液体系样品中的液体进行预成像,并对图像对比分析,以确定液气界面位置、方向及液气界面中心;S3从至少一个方向,在垂直于所述液气界面且过所述液气界面中心点的平面,对所述固液体系样品中的液体进行核磁共振成像,并对图像对比分析,以得到液体过液气界面中心轴的剖面图;S4根据所述剖面图,得到固液和液气界面的轴心剖面曲线;S5对所述轴心剖面曲线进行拟合,并通过测量或计算,得到固液接触角。 CLAIMS 1. A method for measuring the space opaque or solid-liquid contact angle closure, wherein the solid consists of non-ferromagnetic material, a liquid containing a nuclear spin quantum number of nuclei is equal to 1/2, the space filled with the liquid and air, said method comprising: Si solid-liquid system, the sample is placed into the sample chamber of the magnetic resonance imager; S2 from a direction of said solid-liquid system, the liquid sample is subjected to at least pre-image, and the image contrast analysis, the liquid air interface in order to determine the position, direction and the center of the liquid-gas interface; S3 from at least one direction, perpendicular to the liquid-gas interface and the plane through the center of the liquid-gas interface of said solid-liquid system, the liquid sample nuclear magnetic resonance imaging, contrast and image analysis, to give a cross-sectional view of the liquid through the liquid-gas interface of the central axis; S4 according to the cross-sectional view, axial sectional curves to obtain a solid-liquid and liquid-gas interface; the axial S5 sectional curve fitting, and by measurement or calculation, the solid-liquid contact angle.
  2. 2.根据权利要求I所述的方法,其中,所述固体由选自玻璃、聚四氟乙烯、聚酰胺的材料构成。 2. The method according to claim I, wherein the solid selected from glass, polytetrafluoroethylene, a polyamide material.
  3. 3.根据权利要求I所述的方法,其中,所述液体选自水性液体、油性液体或水油混合液。 3. The method of claim I, wherein said liquid is selected from aqueous liquid, an oily liquid or a mixture of water and oil.
  4. 4.根据权利要求I所述的方法,其中,所述不透明空间为封闭或开放的空间。 4. The method of claim I, wherein the opaque space is closed or open space.
  5. 5.根据权利要求I所述的方法,其中,所述空间的形状包括管形、锥形。 The method according to claim I, wherein the shape of said space comprises a tubular, cone.
  6. 6.根据权利要求I所述的方法,其中,步骤S5中,所述拟合为多项式拟合、圆拟合或椭圆拟合。 6. The method of claim I, wherein, in step S5, the fit to a polynomial fit, or circle fitting ellipse fitting.
  7. 7.根据权利要求I所述的方法,其中,步骤S5中,固液接触角的测量或计算采用量角法或量高法进行。 7. The method of claim I, wherein, in step S5, the measurement or calculation method using protractor or amount of solid-liquid contact angle for the Supreme Court.
  8. 8.根据权利要求I所述的方法,其中,步骤S5采用接触角拟合及测量软件进行。 8. The method of claim I, wherein the fitting step S5 using the contact angle and measurement software.
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Cited By (6)

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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
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
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