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 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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contact angle
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朱未琴
高雪峰
江雷
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Suzhou Institute of Nano Tech and Nano Bionics of CAS
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Suzhou Institute of Nano Tech and Nano Bionics of CAS
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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

不透明或封闭空间内固液接触角测量方法Measurement method of solid-liquid contact angle in opaque or closed space

【技术领域】 【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 invention relates to the technical field of measurement, in particular to a solid-liquid contact angle measurement method for characterizing wettability of materials.

【背景技术】 【Background technique】

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。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。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。 Wettability is an important surface property of solids, and it has important applications in ore flotation, building material coatings, anti-corrosion and waterproofing, etc. Due to its important position in scientific research and practical application, the study of solid surface wettability has always been a hot topic in the field of physical chemistry. Among them, contact angle measurement, as the most basic component of wettability research, is of great value to theoretical research and production practice in the field of surface/interface science.

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。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。目前绝大多数的接触角测量仪都基于此原理。 With the advancement of technology and the deepening of research, a variety of methods for measuring contact angle have been developed, such as Wilhelmy hanging plate method, pendant drop method, bubble capture method and so on. Due to the advantages of easy operation and other advantages, the pendant drop method is the most widely used in the measurement of contact angle. Its main principle is to obtain the shape image of the micro-droplet on the solid surface through optical imaging, and through the fitting analysis of the droplet profile, finally get contact angle value. Most current contact angle measuring instruments are based on this principle.

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。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。 However, since this method is based on optical imaging, it is bound to require that the contact angle measurement must be carried out in a transparent and open system. In practical applications, various wetting behaviors often occur in opaque or closed conditions, such as the measurement of the surface tension of harmful liquids, fluid control in liquid transportation pipelines, microfluidic systems, etc., which are all wetting properties. However, due to the opacity and closure of the system itself, traditional contact angle measurement methods cannot be applied to this type of research, which has caused great obstacles to the theoretical development and practical application of surface interface science.

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。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。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。 For example, polytetrafluoroethylene and polyamide are commonly used liquid pipeline transportation materials, and the wetting state of the liquid in the pipeline has an important influence on the fluid parameters and transportation efficiency. Therefore, obtaining the contact angle of the fluid in the pipeline plays an important role in understanding the state of the fluid and further regulating the fluid. However, due to the opacity of the material, it is impossible to understand the wetting state of the liquid in the pipe by using traditional optical methods.

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。 Therefore, a new technology is urgently needed to realize the research on liquid wettability in opaque and closed systems.

【发明内容】 【Content of invention】

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 technical problem to be solved by the invention is to develop a method capable of measuring the solid-liquid contact angle inside an opaque or closed space.

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: The invention provides a method for measuring the internal contact angle of an opaque or closed solid-liquid system, wherein the solid is made of a non-ferromagnetic material, the liquid contains an atomic nucleus whose nuclear spin quantum number is equal to 1/2, and the space formed by the solid Filled with said liquid and air, said method comprising:

S1 放置所述固液体系至核磁共振成像仪的样品腔; S1 Place the solid-liquid system into the sample cavity of the nuclear magnetic resonance imager;

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; S2 Pre-image the liquid in the solid-liquid system sample from at least one direction, and compare and analyze the images to determine the position and direction of the liquid-gas interface and the center point of the liquid-gas 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, on a plane perpendicular to the direction of the liquid-gas interface and passing through the center point of the liquid-gas interface, perform nuclear magnetic resonance imaging on the liquid in the solid-liquid system sample, and compare and analyze the images to obtain The cross-sectional view of the central axis of the liquid passing through the liquid-air interface;

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 Obtain the axial profile curve of the solid-liquid and liquid-gas interface according to the profile;

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 Fit the axial section curve, and obtain the solid-liquid contact angle through measurement or calculation.

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。 The solid can be composed of any non-ferromagnetic material, such as glass, polytetrafluoroethylene, polyamide, or other non-ferromagnetic materials.

液体可选自水性液体、油性液体或水油混合物。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。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 liquid may be selected from aqueous liquids, oily liquids or water-oil mixtures. Wherein the aqueous liquid can be water, or an aqueous solution, or a liquid soluble in water, including alcohols and the like. Oily liquids can be organic compounds such as alkanes, aromatic hydrocarbons, esters, fatty acids, etc.; water-oil mixtures refer to liquids formed by mixing water and various organic compounds. layered form.

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、锥形等。 The opaque space may be a closed or open space, and the space may be of any shape, such as a tube, a cone, and the like.

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。 In step S5 of the method, the fitting is in the form of polynomial fitting, circle fitting or ellipse fitting.

固液接触角的测量或计算可采用量角法或量高法进行。 The measurement or calculation of the solid-liquid contact angle can be carried out by the angle measurement method or the height measurement method.

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。 The process of fitting and measuring or calculating can be carried out by contact angle fitting and measuring software.

现有的接触角拟合及测量软件有Drop Shape Analysis System(Krüss, Germany)、Surftens(SURFTENS Universal,Germany)、SCA20(Dataphysics, Germany)等。 The existing contact angle fitting and measurement software includes Drop Shape Analysis System (Krüss, Germany), Surftens (SURFTENS Universal, Germany), SCA20 (Dataphysics, Germany), etc.

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。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。 The beneficial effect of the present invention is that: compared with the contact angle measurement method based on optical imaging, the present invention uses nuclear magnetic resonance as an imaging means, utilizes the unique internal imaging function of nuclear magnetic resonance technology, not only can measure the contact angle in a conventional transparent or open space system The solid-liquid contact angle can also measure the solid-liquid contact angle in opaque or closed space systems. The scope of application is broadened, for the actual environment that is more in line with the characterization of liquid wettability.

【附图说明】 【Description of drawings】

图1为根据本发明的固液接触角测量方法的流程图。 Fig. 1 is a flow chart of the method for measuring solid-liquid contact angle according to the present invention.

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。 Figure 2 shows a comparison of optical imaging and MRI imaging of opaque spaces.

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。 Fig. 3 is a diagram of imaging of opaque spaces of different shapes using the method of the present invention.

图4所示为采用圆形拟合测量接触角的示意图。 Figure 4 is a schematic diagram of the measurement of contact angle using circular fitting.

【具体实施方式】 【Detailed ways】

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。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。之后在20世纪70年代初,P. C. 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。 Magnetic resonance imaging (MRI) technology is a technology that obtains images of the internal structure of objects by detecting the electromagnetic waves emitted by hydrogen nuclei with an external gradient magnetic field. Magnetic resonance is a physical phenomenon first reported by Block and Purcell in 1946 and applied to spectroscopy. Then in the early 1970s, P. C. Lauterbur and P. Mansfield made a breakthrough in the field of MRI, which laid the foundation for the successful application of MRI.

近年来,核磁共振成像技术发展十分迅速,已日臻成熟完善。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。 In recent years, nuclear magnetic resonance imaging technology has developed very rapidly and has become more mature and perfect. Due to its good non-destructive and non-invasive properties, magnetic resonance imaging technology has been widely used in various fields such as medical diagnosis, oil exploration, and material characterization.

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。 From the point of view of imaging principle, nuclear magnetic resonance imaging technology directly collects the magnetic resonance signals of hydrogen nuclei, and does not require any optical transparency of the research system, so it is very suitable for solid/liquid interface phenomena in opaque environments and closed systems. Research.

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。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。 The inventor took the study of the wettability of water in polytetrafluoroethylene tubes and polyamide tubes as an example to illustrate the principle of wettability characterization under opaque conditions. In the present invention, we have successfully realized the imaging of liquids in opaque polytetrafluoroethylene and polyamide pipelines by taking advantage of the advantages of magnetic resonance imaging technology in opaque conditions, and by analyzing and measuring the interface curves in the images, In this way, the contact angle value that is difficult to obtain by optical methods can be obtained.

下面结合附图和具体实施例对本发明作进一步详细说明。 The present invention will be described in further detail below in conjunction with the accompanying drawings and specific embodiments.

图1所示为根据本发明的固液接触角测量方法的流程图。从图中可见,测量过程主要包括以下五个步骤: FIG. 1 is a flowchart of a method for measuring solid-liquid contact angle according to the present invention. As can be seen from the figure, the measurement process mainly includes the following five steps:

首先是步骤S1,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。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。 The first is step S1. Put the solid-liquid system sample into the sample cavity of the MRI instrument. The appearance and shape of the solid interface can be any shape and shape, and no special treatment is required for the sample before the experiment. Since the calculation of the contact angle is realized by measuring the angle between the gas-liquid interface and the solid-liquid interface, no matter how complicated the interface shape is, as long as the curve shape of the gas-liquid and solid-liquid interface can be accurately obtained, it can be obtained by fitting Calculate the contact angle value.

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。为了测量精确,需要获得固液和气液界面的轴心剖面曲线。 In step S2, pre-image the liquid in the solid-liquid system sample from at least one direction, and compare and analyze the images to determine the position and direction of the liquid-air interface and the center of the liquid-air interface. In order to measure accurately, it is necessary to obtain the axial profile curves of the solid-liquid and gas-liquid interfaces.

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。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。 When the space shape and surface topography are regular, or the space is a transparent space, it is relatively easy to judge the liquid axis section curve, which can be judged by naked eyes, and the imaging parameters can be set directly according to the space shape. Therefore, the liquid can be imaged from only one direction, the imaging process is relatively simple, and the desired image can be obtained only once.

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。有可能需要从多个方向成像,才能得到准确合适的结果。 However, when the space is opaque, because the internal conditions of the space are not clear, it is necessary to perform pre-imaging first, and compare and analyze the images to determine the position, direction and center of the liquid-gas interface. It may be necessary to image from multiple directions to get accurate and suitable results.

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。 Then, in step S3, since the position and direction of the liquid-gas interface and the center of the liquid-gas interface have been determined, the parameters of the nuclear magnetic resonance imager can be adjusted at this time, so as to be perpendicular to the liquid-gas interface and pass through the liquid-gas interface from at least one direction. In the plane of the center point (that is, the plane passing through the central axis of the liquid), NMR imaging is performed on the liquid in the solid-liquid system sample, and the images are compared and analyzed to obtain a cross-sectional view of the liquid passing through the central axis suitable for further analysis .

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。 Afterwards, in step S4, accurate axis profile curves of the solid-liquid and liquid-gas interfaces can be obtained according to the obtained profile.

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。 Finally, in step S5, the axial section curve is fitted, and the solid-liquid contact angle is obtained through measurement or calculation.

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。 In the following specific examples, the inventor takes the wettability research of water and dodecane in glass nuclear magnetic tubes, polytetrafluoroethylene tubes and polyamide tubes as examples to illustrate the measurement of solid-liquid contact angles in solid-liquid systems, that is, liquid wettability The principle of representation.

仪器与材料Instruments and materials

采用苏州纽迈电子科技有限公司生产的NMI20-Analyst磁共振成像分析仪对液体进行成像。 The liquid was imaged by NMI20-Analyst magnetic resonance imaging analyzer produced by Suzhou Numai Electronic Technology Co., Ltd.

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。 The contact angle measurement software SCA20 (Dataphysics, Germany) was used to fit the solid-liquid interface curve in the NMR images.

固体:聚四氟乙烯管(Φ12,长度为约3.5 cm);聚酰胺管(Φ12,长度为约3.5 cm);玻璃核磁管(Φ5和Φ15)。 Solid: polytetrafluoroethylene tube ( Φ 12, about 3.5 cm in length); polyamide tube ( Φ 12, about 3.5 cm in length); glass NMR tube ( Φ 5 and Φ 15).

液体:二次去离子水;十二烷。 Liquids: Secondary deionized water; dodecane.

实施例1Example 1

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。 Solid-liquid system preparation: Use acetone, ethanol and secondary deionized water to ultrasonically wash the PTFE tube for 15 minutes, dry it for later use; inject the secondary deionized water into the PTFE tube, calculate according to the diameter of the tube Inject the amount of water, and control the amount of water so that the height of the water column in the pipe is not greater than 2 cm.

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。 The control of the height of the liquid is to meet the requirements of the equipment used in this experiment for the height of the sample. It should be understood that this parameter can be adjusted appropriately when using other solid-liquid systems, spaces with different shapes, or measuring on other nuclear magnetic resonance imagers. without affecting the scope of the present invention.

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轴或x轴为成像方向,磁场强度为0.5 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。 Nuclear magnetic resonance imaging: Put the water-polytetrafluoroethylene tube system vertically into the nuclear magnetic resonance imager, select the z-axis or x-axis as the imaging direction, and the magnetic field strength is 0.5 T. The multi-layer spin echo sequence is used as the imaging sequence. The waiting time of repeated sampling was 1000 ms, and the accumulation times were 32 times, and the water in the Teflon tube was imaged.

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。 Liquid axis profile curve: adjust the brightness and contrast of the image, and obtain the water-PTFE and air-water phase interface curves from the figure.

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 ± 1.1°。 Fitting and measurement calculation: The water-polytetrafluoroethylene and air-water phase interface was fitted by the contact angle measurement software SCA20 (Dataphysics, Germany), and the contact angle was measured, and the contact angle of water in the pipeline was obtained as 107.5 ±1.1°.

实施例2Example 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1类似。 The procedure is similar to Example 1 except that a polyamide tube is used instead of a polytetrafluoroethylene tube.

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°。 The water-polyamide and air-water phase interfaces were fitted by the contact angle measurement software SCA20 (Dataphysics, Germany), and the contact angle was measured, and the contact angle of water in the pipeline was obtained to be 69.4 ± 1.9°.

实施例3Example 3

除了使用十二烷代替二次去离子水以外,步骤与实施例1类似。其中核磁共振成像过程中,重复采用等待时间为500 ms。 The procedure was similar to Example 1 except that dodecane was used instead of secondary deionized water. During the MRI process, the waiting time for repeated use was 500 ms.

通过接触角测量软件SCA20(Dataphysics, Germany)对十二烷-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°。 The contact angle measurement software SCA20 (Dataphysics, Germany) was used to fit the dodecane-polytetrafluoroethylene and air-dodecane phase interface, and the contact angle was measured, and the contact angle of dodecane in the pipeline was 45.7 ±2.0°.

实施例4Example 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。其中核磁共振成像过程中,重复采用等待时间为500 ms。 The procedure was similar to Example 2 except that dodecane was used instead of secondary deionized water. During the MRI process, the waiting time for repeated use was 500 ms.

通过接触角测量软件SCA20(Dataphysics, Germany)对十二烷-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°。 The contact angle measurement software SCA20 (Dataphysics, Germany) was used to fit the dodecane-polyamide and air-dodecane phase interface, and the contact angle was measured, and the contact angle of dodecane in the pipeline was 41.3 ± 3.6 °.

实施例5Example 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1类似。 Except using Φ 5 NMR tubes instead of polytetrafluoroethylene tubes, the steps are similar to Example 1.

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°。 The contact angle measurement software SCA20 (Dataphysics, Germany) was used to fit the water-glass and air-water phase interfaces, and the contact angle was measured, and the contact angle of water in the pipeline was obtained to be 24.3 ± 2.7°.

实施例6Example 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。其中核磁共振成像过程中,重复采用等待时间为500 ms。 The procedure was similar to Example 5 except that dodecane was used instead of secondary deionized water. During the MRI process, the waiting time for repeated use was 500 ms.

通过接触角测量软件SCA20(Dataphysics, Germany)对十二烷-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°。 The contact angle measurement software SCA20 (Dataphysics, Germany) was used to fit the dodecane-glass and air-dodecane phase interface, and the contact angle was measured, and the contact angle of dodecane in the pipeline was 24.5 ± 2.8° .

实施例7Example 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 using Φ 15 nuclear magnetic tubes instead of Φ 5 nuclear magnetic tubes, the steps are similar to embodiment 5.

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29.1 ± 5.6°。 The contact angle measurement software SCA20 (Dataphysics, Germany) was used to fit the water-glass and air-water phase interfaces, and the contact angle was measured, and the contact angle of water in the pipeline was obtained to be 29.1 ± 5.6°.

实施例8Example 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。 The procedure was similar to Example 7 except that dodecane was used instead of secondary deionized water.

通过接触角测量软件SCA20(Dataphysics, Germany)对十二烷-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°。 The contact angle measurement software SCA20 (Dataphysics, Germany) was used to fit the dodecane-glass and air-dodecane phase interfaces, and the contact angle was measured, and the contact angle of dodecane in the pipeline was obtained to be 33.7 ± 6.3° .

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。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。 Embodiment 1-4 is to the measurement of solid-liquid contact angle under opaque condition; Embodiment 5-8 is to the measurement of solid-liquid contact angle under transparent condition. It can be seen that the contact angle measurement method based on nuclear magnetic resonance imaging of the present invention does not require any transparency of solids, which greatly broadens the research scope of liquid wettability.

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。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。 In order to illustrate the superiority of the solid-liquid contact angle measurement method based on nuclear magnetic resonance imaging in the present invention compared with the existing optical imaging method, the inventors carried out optical imaging and nuclear magnetic resonance imaging respectively on the water in the polytetrafluoroethylene tube . The obtained images are shown in Fig. 2, where a) is an optical imaging image; b) is an MRI image.

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。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。 It can be clearly seen from the figure that due to the opacity of the PTFE tube, it is difficult to understand the wetting behavior of water in the PTFE tube by traditional optical methods, but it can be clearly observed by magnetic resonance imaging that the wetting behavior of water in the PTFE tube Wetting state in vinyl tubing. Therefore, the method of the present invention can effectively overcome the defect that the optical imaging method cannot be imaged in an opaque space, and is especially suitable for measuring the solid-liquid contact angle in an opaque space, thereby helping to understand the wettability of a liquid to a solid in an opaque space.

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。 Figure 3 shows the images obtained by using nuclear magnetic resonance imaging to image water in a Φ 5 cylindrical glass nuclear magnetic tube (a) and a conical glass container (b).

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。图中的图像清楚地反映出玻璃的亲水特性。 It can be seen that the method of the present invention has no limitation on the shape of the space, which can be cylindrical, conical, or any other shape. The image in the figure clearly reflects the hydrophilic nature of the glass.

图4举例说明了通过采用圆形拟合测量接触角θ的示意图。 Figure 4 illustrates a schematic diagram of the measurement of the contact angle θ by employing a circle fit.

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。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。 Above, we have successfully realized the imaging of liquids in opaque polytetrafluoroethylene and polyamide pipes and transparent glass nuclear magnetic tubes by taking advantage of the advantages of magnetic resonance imaging technology in opaque conditions, and by analyzing the The interface curve is analyzed and measured to obtain the contact angle value which is difficult to obtain by optical methods. Therefore, the method of the present invention has no requirements on whether the space is transparent or the shape of the space is regular, which greatly expands the application range of solid-liquid contact angle measurement and liquid wettability characterization.

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。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。 The specific embodiments of the present invention described above do not constitute a limitation to the protection scope of the present invention. Any other corresponding changes and modifications made according to the technical concept of the present invention shall be included in the protection scope of the claims 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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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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