CN119779170A - A method for measuring thickness distribution and refractive index dispersion curve of liquid film - Google Patents
A method for measuring thickness distribution and refractive index dispersion curve of liquid film Download PDFInfo
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Abstract
一种测量液膜的厚度分布与折射率色散曲线的方法，包括：将液膜覆盖在SPR传感模块上，将宽光谱线偏振平行光束照射至SPR传感模块上并发生全反射得到反射光，宽光谱线偏振平行光束通过全反射在SPR传感模块上激励SPR模式和/或PWR模式；反射光携带液膜的信息被高光谱成像仪接收得到高光谱图像，高光谱图像中的像素与液膜上的位置一一对应；根据高光谱图像，确定与目标像素对应的目标位置处的至少三个实测共振波长；根据目标位置处的至少三个实测共振波长得到目标位置处的液膜厚度和液膜的折射率色散曲线；根据目标位置处的液膜的折射率色散曲线以及每个其它位置处的实测共振波长得到其它位置处的液膜厚度；根据液膜在所有位置的厚度得到液膜的厚度分布。
A method for measuring the thickness distribution and refractive index dispersion curve of a liquid film comprises: covering a liquid film on an SPR sensor module, irradiating a wide-spectrum linearly polarized parallel light beam onto the SPR sensor module and causing total reflection to obtain reflected light, wherein the wide-spectrum linearly polarized parallel light beam excites an SPR mode and/or a PWR mode on the SPR sensor module through total reflection; the reflected light carries information of the liquid film and is received by a hyperspectral imager to obtain a hyperspectral image, wherein pixels in the hyperspectral image correspond to positions on the liquid film one by one; according to the hyperspectral image, determining at least three measured resonant wavelengths at a target position corresponding to the target pixel; obtaining the liquid film thickness at the target position and the refractive index dispersion curve of the liquid film according to the at least three measured resonant wavelengths at the target position; obtaining the liquid film thickness at other positions according to the refractive index dispersion curve of the liquid film at the target position and the measured resonant wavelength at each other position; and obtaining the thickness distribution of the liquid film according to the thickness of the liquid film at all positions.
Description
Technical Field
The invention relates to the field of precise detection, in particular to a method for measuring thickness distribution and refractive index dispersion curve of a liquid film.
Background
The liquid film (liquid film for short) has important application in the fields of environmental protection, petrochemical industry, chemical bionics, medicine and health, organic synthesis, analytical chemistry, gas separation and the like. The liquid film is widely used for mechanical sealing and bearing lubrication, can play roles of improving tightness, reducing friction and prolonging the service life of a mechanical device, is also commonly used for protecting the solid surface from oxidation, improving the optical and mechanical properties of the solid surface, is used for waterproofing, heat insulation and ultraviolet resistance, has high mass transfer rate and good molecular selectivity, is commonly used for selectively absorbing and separating gas molecules, has important roles in organisms, such as tear forming a uniform liquid film on the cornea surface, plays roles of reducing astigmatism and improving visual efficiency, has important application in the field of biochemical sensing, and has the advantages of simple film formation, easiness in updating, reusability of a substrate, capability of improving the selectivity of a sensor and the like by using the liquid film as a sensitive film. For example, specific detection of heavy metal mercury ions can be achieved by using an ionic liquid film as a sensor sensitive film. The liquid film is also an indispensable early state in the process of preparing the solid film by a chemical method, and is an important research object in the field of chemical film preparation technology. The thickness distribution and the refractive index dispersion curve are two important parameter indexes of the liquid film, accurate measurement of the thickness of the liquid film and two-dimensional distribution of the liquid film are helpful for establishing a controllable preparation method of the liquid film and optimizing the performance of the liquid film in different applications, and accurate measurement of the refractive index dispersion curve of the liquid film can effectively evaluate the change of the optical characteristics and chemical components of the liquid film in the use process. Synchronous measurement of the thickness distribution of the liquid film and the refractive index dispersion curve thereof can enable us to more comprehensively analyze and master the physical and chemical characteristics of the liquid film in the use process.
The optical measurement method has the advantages of accuracy, rapidness, no damage, easy implementation and the like, and is a main method for measuring the thickness of the liquid film and the refractive index thereof. Currently, optical instruments commonly used to measure the refractive index of liquids include ellipsometers, abbe refractometers, optical waveguide sensors, and SPR sensors. These optical instruments have high sensitivity and can accurately measure the thickness of a liquid film or the refractive index of the liquid film, but they have single functions, are not suitable for measuring the thickness and the refractive index of the liquid film at the same time, and are not suitable for measuring the two-dimensional distribution of the thickness of the liquid film and the refractive index dispersion curve of the liquid film at the same time. In real life, advanced methods and tools capable of synchronously measuring the thickness distribution of a liquid film and the refractive index dispersion curve are lacking.
Disclosure of Invention
In view of the above, a method for measuring the thickness distribution and refractive index dispersion curve of a liquid film has been proposed to solve the above problems.
As one aspect of the present invention, there is provided a method of measuring a liquid film thickness distribution and a refractive index dispersion curve of a liquid film, the method being implemented based on a hyperspectral SPR imaging apparatus including a SPR sensing module, the method comprising:
Covering the SPR sensing module with a liquid film;
The method comprises the steps of irradiating broad-spectrum linear polarization parallel light beams onto an SPR sensing module and generating total reflection to obtain reflected light, exciting an SPR mode and/or a PWR mode on the SPR sensing module through total reflection, and carrying information of a liquid film through interaction of the SPR mode and/or the PWR mode and the liquid film by the reflected light, wherein the reflected light is received by a hyperspectral imager to obtain a hyperspectral image, and pixels in the hyperspectral image are in one-to-one correspondence with positions on the liquid film;
Determining at least three actually measured resonance wavelengths at a target position corresponding to a target pixel according to the hyperspectral image, wherein the actually measured resonance wavelengths at the target position are resonance wavelengths of an SPR mode and/or a PWR mode;
obtaining the liquid film thickness at the target position and the refractive index dispersion curve of the liquid film according to at least three actually measured resonance wavelengths at the target position;
Obtaining the thickness of the liquid film at other positions according to the refractive index dispersion curve of the liquid film and the measured resonance wavelength at each other position, wherein the other positions are any position on the liquid film except the target position;
And obtaining the thickness distribution of the liquid film according to the liquid film thickness of the liquid film at all positions.
According to an embodiment of the invention, the SPR sensing module comprises a substrate and a metal film on the substrate, wherein the substrate is a prism, and the metal film is deposited on the bottom surface of the prism, or
The base is a combination of a prism and a transparent substrate closely contacted with the bottom surface of the prism, and the metal film is deposited on the surface of the transparent substrate far away from the prism;
The liquid film is arranged on the surface of the metal film;
the SPR mode is excited at an interface of the metal thin film and the substrate;
the PWR mode is excited within the liquid film.
According to the embodiment of the invention, a covering layer is also formed on the liquid film;
Obtaining a liquid film thickness at the target location and a refractive index dispersion curve of the liquid film according to at least three actually measured resonance wavelengths at the target location, comprising:
Bringing the refractive index of the substrate, the refractive index and the thickness of the metal film and the refractive index of the covering layer above the liquid film into a Fresnel reflection formula of a four-layer structure, and performing simulation fitting on at least three actually measured resonance wavelengths of the liquid film at the target position to obtain a first relation curve of each actually measured resonance wavelength at the target position, wherein the first relation curve is a relation curve of the refractive index of the liquid film and the thickness of the liquid film at the target position, and at least three actually measured resonance wavelengths correspond to at least three first curves;
and obtaining the liquid film thickness at the target position and the refractive index dispersion curve of the liquid film according to a Cauchy dispersion formula and at least three first relation curves of the liquid film at the target position.
According to an embodiment of the present invention, obtaining the thickness of the liquid film at each other location according to the refractive index dispersion curve of the liquid film and the measured resonance wavelength at the other location includes:
obtaining measured resonance wavelengths at the other locations using the hyperspectral image;
Determining the refractive index of the liquid film at the measured resonance wavelength at the other positions according to the refractive index dispersion curve of the liquid film;
and obtaining the thicknesses of the liquid films at other positions according to the refractive indexes of the liquid films at the other positions under the actual measurement resonance wavelengths and the Fresnel reflection formulas of the four-layer structure.
According to an embodiment of the invention, the Cauchy dispersion formula is expressed as follows:
Wherein, 、As a function of the parameters,Representing the refractive index of the liquid film at wavelength λ;
obtaining a liquid film thickness at the target position and a refractive index dispersion curve of the liquid film according to a Cauchy dispersion formula and at least three first relation curves of the liquid film at the target position, wherein the method comprises the following steps:
Obtaining at least two second relation curves at the target position according to a Cauchy dispersion formula and the at least three first relation curves, wherein the second relation curves are relation curves of the parameter b and the thickness of a liquid film at the target position, and all the second relation curves intersect at one point;
Obtaining the intersection point of at least two second relation curves to obtain the value of the parameter b and the thickness of the liquid film at the target position;
And according to the value of the parameter b and the thickness of the liquid film at the target position, combining any one of the at least three first relation curves to obtain the value of the parameter a, and carrying the values of the parameter a and the parameter b into the Cauchy dispersion formula to obtain the refractive index dispersion curve of the liquid film.
According to an embodiment of the present invention, the fresnel reflection formula of the four-layer structure is expressed as follows:
R= r1234·r1234 *
Wherein R represents the reflectivity of a four-layer structure consisting of the substrate, the metal film, the liquid film and the covering layer, the substrate, the metal film, the liquid film and the covering layer are respectively 1 st layer, 2 nd layer, 3 rd layer and 4 th layer from bottom to top, R 1234 represents the reflection coefficient of the four-layer structure, R 1234 * represents the complex conjugate of R 1234, D 2 is the thickness of the 2 nd layer, D 3 is the thickness of the 3 rd layer, k 2 and k 3 represent the vertical component of the propagation constant of the broad spectrum linear polarization parallel beam in the 2 nd layer and the 3 rd layer respectively, R 234 represents the reflection coefficient of light in the three-layer structure consisting of the 2 nd layer, the 3 rd layer and the 4 th layer, R ij represents the interface reflection coefficient of the i < th > layer and the j < th > layer, i=1, 2 or 3, j=2, 3 or 4, lambda is the wavelength of light in vacuum, and n i represents the refractive index of the i < th > layer at the wavelength lambda.
According to an embodiment of the invention, the broad spectral linear polarized parallel light beam is s-polarized light or p-polarized light or other linear polarized light which can be decomposed into s-polarized and p-polarized components.
According to an embodiment of the present invention, when the broad spectral linear polarized parallel beam is s polarized light, r ij is obtained by:
When the broad spectral linear polarized parallel beam is p polarized light, r ij is obtained by:
Wherein, θ i and θ j represent the corresponding incident angle and refraction angle when the broad spectrum linearly polarized light is emitted from the ith layer to the jth layer, respectively, the refractive index of the jth layer of n j, and k i and k j represent the vertical component of the propagation constants of the light in the ith layer and the jth layer, respectively.
According to the embodiment of the invention, the metal film does not fall off or change in physical and chemical characteristics after being covered by the liquid film, and the liquid film is stable in test time.
According to an embodiment of the invention, the at least three measured resonance wavelengths at the target location are obtained by one hyperspectral imaging measurement or by multiple hyperspectral imaging measurements under different conditions.
The basic methods for measuring the liquid film thickness and the liquid film refractive index in the embodiments of the present invention are a Surface Plasmon Resonance (SPR) sensing method and a Plasmon Waveguide Resonance (PWR) sensing method. SPR is a mature high-sensitivity biochemical sensing method. However, SPR sensors have a small detection depth, and can only detect 300nm thick liquid films at most in the visible light band. As the thickness of the liquid film increases (in the order of hundreds of nanometers to micrometers), PWR patterns are gradually generated in the liquid film. Therefore, a thicker (micrometer-scale thickness) liquid film can be measured by using the PWR mode, and a thinner (several nanometers to several tens of nanometers thickness) liquid film can be measured by using the SPR mode.
According to the embodiment of the invention, the thickness and refractive index dispersion curve of the liquid film comprises a plurality of unknowns, so that when the thickness distribution and refractive index dispersion curve of the liquid film are synchronously measured, the plurality of unknowns need to be determined, which requires that the resonance wavelengths of at least three SPR modes and/or PWR modes at the target position corresponding to the target pixel in the hyperspectral image are acquired in a test, and the three obtained measured resonance wavelengths can be used as known quantities to realize the measurement of the thickness and refractive index color line curve of the liquid film at the target position for the target pixel. The thickness of the liquid film changes with the change of the position, but the dispersion curve of the liquid film does not change with the change of the position, and the refractive index dispersion curve at the target position is the refractive index dispersion curve of the liquid film. Only one unknown, i.e. thickness, needs to be measured at each other location on the liquid film. Therefore, for other positions of the liquid film, the measured resonance wavelength and the refractive index dispersion curve at that position can be used to realize the thickness measurement of the liquid film at that position. Therefore, the embodiment of the invention can realize the simultaneous measurement of the thickness distribution of the liquid film and the refractive index dispersion curve of the liquid film.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following brief description of the drawings of the embodiments will make it apparent that the drawings in the following description relate only to some embodiments of the present invention and are not limiting of the present invention.
FIG. 1 illustrates a schematic diagram of a hyperspectral SPR imaging apparatus provided by an embodiment of the present invention;
FIG. 2 is a flow chart showing a method for measuring the thickness distribution and refractive index dispersion curve of a liquid film according to an embodiment of the present invention;
FIG. 3 is a flow chart showing a method for measuring the thickness distribution and refractive index dispersion curve of a liquid film according to another embodiment of the present invention.
FIG. 4A shows experimental and simulated spectra of a target pixel on a hyperspectral image of a silicon oil film provided in accordance with an embodiment of the present invention;
FIG. 4B shows two-dimensional profiles of measured resonant wavelengths for each of the five PWR modes obtained from FIG. 4A;
FIG. 4C shows three first curves obtained from FIG. 4A for three of the resonant wavelengths;
fig. 4D shows two second curves at the target position obtained from the three first curves of fig. 4C.
FIG. 5 shows the thickness distribution of a silicone oil film measured in accordance with the practice of the present invention;
FIG. 6 shows a comparison of four experimental spectra extracted from the other four pixels on a hyperspectral image of a measured silicon oil film and corresponding simulated spectra in accordance with an embodiment of the present invention;
FIG. 7 shows refractive index dispersion curves of a silicone oil film measured in accordance with the practice of the present invention;
FIG. 8A shows experimental and simulated spectra extracted from a target pixel on a hyperspectral image of a measured glycerol film in accordance with an embodiment of the present invention;
FIG. 8B shows a two-dimensional distribution of measured resonant wavelengths for each of the four PWR modes obtained from FIG. 8A;
FIG. 9A shows the refractive index dispersion curve of a glycerol film measured in accordance with the practice of the present invention;
Fig. 9B shows the thickness distribution of a measured dry oil liquid film performed in accordance with the present invention.
Reference numerals illustrate:
1-a linear polarizer;
A 2-SPR sensing module;
A 21-substrate;
211-prisms;
212—a glass substrate;
22-metal film;
3-liquid film;
4-a broadband light source;
5-an imaging lens;
6-hyperspectral imager;
7-cover layer.
Detailed Description
The present invention will be further described in detail below with reference to specific embodiments and with reference to the accompanying drawings, in order to make the objects, technical solutions and advantages of the present invention more apparent. This invention may, however, be embodied in different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art. In the drawings, the size of layers and regions, as well as the relative sizes, may be exaggerated for the same elements throughout.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The terms "comprises," "comprising," and/or the like, as used herein, specify the presence of stated features, steps, operations, and/or components, but do not preclude the presence or addition of one or more other features, steps, operations, or components.
Fig. 1 shows a schematic diagram of a hyperspectral SPR imaging apparatus.
As shown in figure 1, the hyperspectral SPR imaging device comprises an SPR sensing module 2, a liquid film 3 is positioned on the SPR sensing module 2, a broadband light source 4 and a hyperspectral imager 6 are respectively arranged on two sides of the SPR sensing module 2, a linear polarizer 1 is arranged between the broadband light source 4 and the SPR sensing module 2, and an imaging lens 5 is arranged between the SPR sensing module 2 and the hyperspectral imager 6. The hyperspectral SPR imaging device is used for realizing the synchronous measurement of the thickness distribution of the liquid film 2 and the refractive index dispersion curve of the liquid film 2.
FIG. 2 is a flow chart showing a method for measuring the thickness distribution and refractive index dispersion curve of a liquid film according to an embodiment of the present invention. Referring to fig. 1 and 2, the method for measuring the thickness distribution and refractive index dispersion curve of the liquid film 3 includes operations S1 to S6.
In operation S1, the liquid film 3 is coated on the SPR sensor module.
In operation S2, the broad spectrum linear polarization parallel beam is irradiated onto the SPR sensing module 2 and undergoes total reflection to obtain reflected light, and the broad spectrum linear polarization parallel beam excites the SPR mode and/or the PWR mode on the SPR sensing module 2 through total reflection, and the reflected light carries information of the liquid film 3 through interaction between the SPR mode and/or the PWR mode and the liquid film 3. The broad spectrum linear polarization parallel beam is obtained by passing through the linear polarizer 1 after being emitted by the broad band light source 4 of the hyperspectral SPR imaging apparatus. The reflected light is received by the hyperspectral imager 6 after passing through the imaging lens 5, so as to obtain a hyperspectral image, and pixels in the hyperspectral image are in one-to-one correspondence with positions on a liquid film.
And S3, determining at least three actual measurement resonance wavelengths at a target position corresponding to the target pixel according to the hyperspectral image, wherein the actual measurement resonance wavelengths at the target position are resonance wavelengths of an SPR mode and/or a PWR mode. The target pixel is, for example, a pixel at the center point of the field of view of the hyperspectral imager 6.
And S4, obtaining the liquid film thickness at the target position and the refractive index dispersion curve of the liquid film according to at least three actually measured resonance wavelengths at the target position.
And S5, obtaining the thickness of the liquid film at other positions according to the refractive index dispersion curve of the liquid film and the measured resonance wavelength of each other position, wherein the other positions are any position except the target position on the liquid film.
Operation S6 obtains the thickness distribution of the liquid film from the liquid film thicknesses at all positions on the liquid film 3.
The basic methods for measuring the liquid film thickness and the liquid film refractive index in the embodiments of the present invention are a Surface Plasmon Resonance (SPR) sensing method and a Plasmon Waveguide Resonance (PWR) sensing method. SPR is a mature high-sensitivity biochemical sensing method. However, SPR sensors have a small detection depth, and can only detect 300nm thick liquid films at most in the visible light band. As the thickness of the liquid film increases (in the order of hundreds of nanometers to micrometers), PWR patterns are gradually generated in the liquid film. Therefore, a thicker (micrometer-scale thickness) liquid film can be measured by using the PWR mode, and a thinner (several nanometers to several tens of nanometers thickness) liquid film can be measured by using the SPR mode. The embodiment of the invention can realize Surface Plasmon Resonance (SPR) and plasmon guided mode resonance (PWR), so that the embodiment of the invention can realize detection of thinner (hundreds of nanometers to tens of nanometers) liquid films and detection of thinner (hundreds of nanometers to micrometers) liquid films.
According to the embodiment of the invention, the thickness and refractive index dispersion curve of the liquid film comprises a plurality of unknowns, so that when the thickness distribution and refractive index dispersion curve of the liquid film are synchronously measured, the plurality of unknowns need to be determined, which requires that the resonance wavelengths of at least three SPR modes and/or PWR modes at the target position corresponding to the target pixel in the hyperspectral image are acquired in a test, and the three obtained measured resonance wavelengths can be used as known quantities to realize the measurement of the thickness and color line curve of the liquid film at the target position for the target pixel. The thickness of the liquid film changes with the change of the position, but the dispersion curve of the liquid film does not change with the change of the position, and the refractive index dispersion curve at the target position is the refractive index dispersion curve of the liquid film. Only one unknown, i.e. thickness, needs to be measured at each other location on the liquid film. Therefore, for other positions of the liquid film, the measured resonance wavelength and the refractive index dispersion curve at that position can be used to realize the thickness measurement of the liquid film at that position. Therefore, the embodiment of the invention can realize the simultaneous measurement of the liquid film thickness distribution and the liquid film refractive index dispersion curve.
According to an embodiment of the present invention, the liquid constituting the liquid film 3 must be a stable, uniform liquid. The liquid film 3 is a thin liquid film with a thickness ranging from 1 to 10 micrometers, and the specific thickness range is related to the hyperspectral SPR imaging device, so that the PWR mode can be generated, and at least three formants of the PWR mode can be formed in the measured spectrum range (400 to 10000 nm). The liquid film 3 can be prepared by natural diffusion method, spin coating method, or the like.
According to an embodiment of the present invention, SPR sensing module 2 includes a substrate 21 and a metal film 22 on substrate 21. In a first embodiment, a first Kretschmann prism coupling structure is used, wherein the substrate 21 is a prism, the material may be glass, and the metal film 22 is deposited on the bottom surface of the glass prism. In a second embodiment, i.e., as shown in fig. 2, a second Kretschmann prism coupling structure is employed, in which the base 21 is a combination of a prism 211 and a glass substrate 212 in close contact with the bottom surface of the prism 211. The metal film 21 is deposited on the surface of the glass substrate 212 away from the bottom surface of the prism 211, the glass substrate 212 is brought into close contact with the bottom surface of the prism 211 by the high refractive index coupling liquid, the liquid film is disposed on the surface of the metal film 22, and the liquid film 3 is exposed to the outermost side. The thickness of the metal film is between 10nm and 100nm, and when the metal film 22 is a gold film, the optimal thickness is 50 nm. The broad spectral linear polarization parallel beam passes through the substrate 21, is totally reflected at the glass-metal interface of the SPR sensing module 2, and after being emitted from the side of the prism 211, passes through the imaging lens 5 and is then received by the hyperspectral imager 6. The evanescent field accompanying the total reflection penetrates the metallic film 22 and excites the SPR mode at the interface of the metallic film 22 and the substrate 21 and/or excites the PWR mode within the liquid film. Either the SPR mode or the PWR mode may interact with the liquid film such that the reflected light carries information about the liquid film 3.
According to an embodiment of the present invention, when the SPR sensing module 2 in fig. 1 is combined in a Kretschmann prism coupling structure, broadband light emitted from the broadband light source 4, for example, a halogen tungsten lamp, is changed into an s-polarized or p-polarized parallel beam by the multimode quartz optical fiber, the prism 211 and the linear polarizer 1, and then is incident on the prism at an angle θ, where the angle θ can be adjusted by rotating the turntable of the device, and the broadband linear polarized parallel beam entering the prism 211 is totally reflected at the interface between the glass substrate 212 and the metal film 22 of the SPR sensing module 2, and the reflected light is incident on the hyperspectral imager 6 through the imaging prism 5. The evanescent field generated by total reflection may excite the PWR mode within the liquid film 3 or the SPR mode at the interface of the metallic film 22 and the liquid film 3. When the evanescent field generated by total reflection excites the PWR in the liquid film 3, the reflection spectrum will exhibit a plurality of wave troughs, so that the wavelength corresponding to the wave trough in each pixel spectrum in the hyperspectral image recorded by the hyperspectral imager 6 is the resonance wavelength λ R of the PWR mode. In addition to the Kretschmann prism, it should be clear to those skilled in the art that hyperspectral images of liquid films can also be obtained using an Otto prism coupling structure, and will not be described in detail here.
According to the embodiment of the present invention, when the liquid film 3 is very thin, the SPR mode is activated only at the interface of the metal thin film 22 and the liquid film 3, and the PWR mode is gradually activated as the thickness of the liquid film increases. When only the SPR mode is excited at the interface of the metal thin film 22 and the liquid film 3, the target pixel of each highlight image can obtain only one resonance wavelength at the target position. Or when the liquid film thickness is insufficient, each hyperspectral image can only be based on less than 3 resonance wavelengths of the target pixel, although the PWR mode can be excited.
A coating 7 is also formed on the liquid film 3. In order to obtain at least three actually measured resonant wavelengths at the target position corresponding to the target pixel, different hyperspectral images can be obtained by changing the test conditions, so that three resonant wavelengths at the target position are obtained. Changing the test conditions may for example comprise changing the material of the cover layer 7 or changing the polarization direction of a broad spectral linear polarized parallel beam.
For example, the reflected light may be hyperspectral imaged under different (at least three) cover layers 7, respectively, to obtain at least three hyperspectral images, and at least three measured resonance wavelengths at the target position may be obtained from the obtained at least three hyperspectral images. For example, when the cover layers 7 on the liquid film 3 are respectively air, water, a solid plate with a smooth surface, and the like, the reflected light is respectively subjected to hyperspectral imaging to obtain hyperspectral images corresponding to each cover layer 7, so that at least three actually measured resonance wavelengths at the target position are obtained according to the hyperspectral images corresponding to all the cover layers 7.
According to an embodiment of the present invention, three resonance wavelengths at the target position can also be obtained by changing the polarization direction of the broad spectral linear polarized parallel beam while changing the cover layer 7. Or three resonant wavelengths at the target location are obtained by simply changing the polarization direction of the broad spectral linear polarized parallel beam. For example, the material of the cover layer 7 is unchanged, and when the polarization directions of the broad-spectrum linearly polarized parallel light beams are different (S direction or P direction), the reflected light is subjected to hyperspectral imaging, respectively, to obtain hyperspectral images corresponding to each polarization direction. From the hyperspectral image corresponding to each polarization direction under the condition of the plurality of cover layers 7, at least three actually measured resonance wavelengths at the target position can be obtained.
The determination of the refractive index dispersion curve and the thickness distribution can be made as known amounts, regardless of the at least three resonance wavelengths obtained in either case.
According to the embodiment of the present invention, when the thickness of the liquid film 3 is large enough to support at least three PWR modes, at least three resonance wavelengths can be obtained at the target position by one hyperspectral imaging measurement, and thus, measurement of the liquid film can be achieved by using one hyperspectral image obtained by one imaging of reflected light.
In accordance with an embodiment of the present invention, the PWR mode generates multiple orders, one for each resonant wavelength, which is related to the thickness of the liquid film and the refractive index dispersion curve of the liquid film. In the PWR mode, the resonance wavelengths of a plurality of orders at the target position of the liquid film (PWR modes corresponding to different orders) can be used as a plurality of known amounts to calculate the refractive index dispersion curve of the liquid film and the thickness at that position at the same time. When the hyperspectral image is combined, the hyperspectral image can obtain the resonance spectrum of tens of thousands of pixels of the liquid film, and a large number of formants of tens of thousands of pixels can solve the thickness distribution of the liquid film of the refractive index dispersion curve.
According to the embodiment of the invention, operation S4, obtaining the liquid film thickness at the target position and the refractive index dispersion curve of the liquid film according to at least three actually measured resonance wavelengths at the target position, includes sub-operations S41-S42.
In sub-operation S41, the refractive index of the substrate, the refractive index and thickness of the metal film, and the refractive index of the cover layer 7 above the liquid film are brought into a fresnel reflection formula of a four-layer structure, and simulation fitting is performed on at least three measured resonance wavelengths of the liquid film at the target position to obtain a first relationship curve of each measured resonance wavelength at the target position, where the first relationship curve is a relationship curve of the refractive index of the liquid film and the thickness of the liquid film at the target position, and the at least three measured resonance wavelengths correspond to at least three first curves.
In sub-operation S42, a liquid film thickness at the target position and a refractive index dispersion curve of the liquid film are obtained according to the cauchy dispersion formula and at least three first relationship curves of the liquid film at the target position.
Cover layer 7 according to an embodiment of the present invention, the Cauchy dispersion curve is represented by formula (1).
(1)。
Wherein, As a function of the parameters,The refractive index of the liquid film at the wavelength λ is shown.
In sub-operation S42, according to the Cauchy dispersion formula and at least three first relation curves of the liquid film at the target position, the liquid film thickness at the target position and the refractive index dispersion curve of the liquid film are obtained, including sub-operations S421 to S423.
In the sub-operation S421, at least two second relationship curves at the target position are obtained according to the cauchy dispersion formula and at least three first relationship curves, where the second relationship curves are relationship curves of the parameter b and the thickness of the liquid film at the target position. Since both the parameter b and the liquid film thickness are independent of wavelength (i.e. both the parameter b and the liquid film thickness are independent of wavelength), all (at least two) second curves obtained at the target location tend to cross one point.
And a sub-operation S422 of obtaining the value of the parameter b and the thickness of the liquid film at the target position by obtaining the intersection point of at least two second relation curves.
In sub-operation S423, according to the value of the parameter b and the liquid film thickness at the target position, combining at least any one of the three first curves (the relation curve of the refractive index and the liquid film thickness at the target position) to obtain the value of the parameter a, and bringing the values of the parameter a and the parameter b into the Cauchy dispersion formula to obtain the refractive index dispersion curve of the liquid film 3. According to the embodiment of the present invention, when the refractive index dispersion curve of the liquid film 3 is determined using the cauchy dispersion formula, there are two unknown parameters, namely, parameter a and parameter b, at the target position of the liquid film 3, the thickness of the position needs to be measured in addition to the parameter a and the parameter b, and therefore, 3 unknowns need to be measured, and therefore, when the refractive index dispersion curve of the liquid film 3 is obtained using the cauchy dispersion formula, 3 resonance wavelengths of the target position need to be obtained. In order to improve the resolution of the parameters a and b and the liquid film thickness at the target location, at least three measured resonant wavelengths are selected on the basis of the principle that the wavelength interval is as large as possible when at least three measured resonant wavelengths are determined in a spectrum having three or more PWR formants.
The following describes the measurement principle of the distribution of the liquid film thickness and the refractive index dispersion curve in detail in combination with the Cauchy formula.
Taking the solution of the thickness and refractive index dispersion curves at the target location using the three measured resonance wavelengths of the target pixel as an example. The three measured resonance wavelengths of the target pixel are, for example, respectively、And. The refractive index of the substrate 21, the refractive index and thickness of the metal film 22 and the refractive index of the covering layer 7 above the liquid film are brought into a Fresnel reflection formula of a four-layer structure, and simulation fitting is carried out on each measured resonance wavelength of the liquid film 3 at the target position to obtain at least three first curves. I.e. the first curve isLower part(s)The relation with T is that the second curve isLower part(s)The relation with the T is that, the third curve isLower part(s)Relationship to T.Is thatThe refractive index is as follows,Is thatLower refractive index, andIs thatLower refractive index.
As can be obtained according to the formula (1),
(8)
(9)
(10)
According to (8) to (9), it is possible to obtain:
(11)
According to (9) to (10), it is possible to obtain:
(12)
Will be The relation with the T is that,The relation with the T is that,And (3) carrying out the relation with T into the relation (11) and the relation (12) respectively to obtain two curves of the relation between b and T, wherein the intersection point of the two curves of the relation between b and T is the value of b and T, and the a can be obtained according to the Cauchy formula. After determining a and b, the refractive index dispersion curve can be determined.
According to the embodiment of the present invention, in operation S5, the thickness of the liquid film at other positions is obtained according to the refractive index dispersion curve of the liquid film and the measured resonance wavelength at each other position, and may be divided into sub-operations S51 to S53.
The sub-operation S51 obtains other measured resonance wavelengths at other positions using the measured hyperspectral image.
In operation S52, the refractive index of the liquid film at the measured resonance wavelength at other positions is determined from the refractive index dispersion curve of the liquid film.
In the sub-operation S53, the thickness of the liquid film at other positions is obtained according to the refractive index of the liquid film at the measured resonance wavelength at other positions and the fresnel reflection formula of the four-layer structure.
According to the embodiment of the invention, a four-layer structured Fresnel formula is expressed as formula (2) to formula (5).
R= r1234·r1234 * (2)
(3)
(4)
(5)
Wherein R represents the reflectivity of a four-layer structure consisting of a substrate, a metal film, a liquid film and a cover layer, the substrate, the metal film, the liquid film and the cover layer are respectively 1 st layer, 2 nd layer, 3 rd layer and 4 th layer from bottom to top, R 1234 represents the reflection coefficient of the four-layer structure, R 1234 * represents the complex conjugate of R 1234, D 2 is the thickness of the 2 nd layer, D 3 is the thickness of the 3 rd layer, k 2 and k 3 respectively represent the vertical component of the propagation constant of a broad spectrum linear polarization parallel light beam in the 2 nd layer and the 3 rd layer, R 234 represents the reflection coefficient of light in the three-layer structure consisting of the 2 nd layer, the 3 rd layer and the 4 th layer, R ij represents the reflection coefficient of the interface of the i th layer and the j th layer, i=1, 2 or 3, j=2, 3 or 4, lambda is the wavelength of light, and n i represents the refractive index of the i th layer in vacuum.
The broad spectral linear polarized parallel beam may be s-polarized light or p-polarized light or other linear polarized light that may be decomposed into s-polarized and p-polarized components.
When the broad spectrum linear polarization parallel beam is s polarized light, r ij is obtained by the following formula, and r ij is obtained by the formula (6).
(6)
When the broad spectral linear polarization parallel beam is p-polarized light, r ij is obtained by the following formula.
(7)
For other linearly polarized light, it can be decomposed into s-polarized component and p-polarized component, which are calculated separately and then synthesized. θ i and θ j represent the corresponding incident and refraction angles of light from the i-th layer to the j-th layer, respectively, the single-wavelength refractive index of the j-th layer of n j, and k i and k j represent the vertical components of the propagation constants of light at the i-th and j-th layers, respectively.
According to an embodiment of the present invention, the metal film 22 needs to be capable of exciting SPR modes, typically gold, silver, aluminum or titanium, at its surface.
When the metal film 22 is covered with the liquid film, it is required that no falling off occurs and no change in physical and chemical characteristics occurs, and the liquid film is required to be stable for a test time.
The hyperspectral imager 6 may be, for example, a line scanning hyperspectral imager based on grating spectroscopy, or a hyperspectral imager based on light source wavelength scanning.
FIG. 3 is a flow chart showing a method for measuring the thickness distribution and refractive index dispersion curve of a liquid film according to another embodiment of the present invention.
The method of measuring the thickness distribution and refractive index dispersion curve of the liquid film according to the present invention will be described in detail with reference to fig. 1 and 3.
As shown in figure 1, the hyperspectral SPR imaging device comprises an SPR sensing module 2, a liquid film 3 is positioned on the SPR sensing module 2, a broadband light source 4 and a hyperspectral imager 6 are respectively arranged on two sides of the SPR sensing module 2, a linear polarizer 1 is arranged between the broadband light source 4 and the SPR sensing module 2, and an imaging lens 5 is arranged between the SPR sensing module 2 and the hyperspectral imager 6. The hyperspectral SPR imaging device is used for realizing the synchronous measurement of the thickness distribution of the liquid film 2 and the refractive index dispersion curve of the liquid film 2.
As shown in FIG. 3, the method for measuring the thickness distribution and the refractive index dispersion curve of the liquid film further comprises steps A to H. Step A, coating the SPR sensing module 2 with the liquid film 3.
And B, radiating the broad-spectrum linear polarization parallel light beam to the SPR sensing module 2 to generate total reflection to obtain reflected light, exciting an SPR mode and/or a PWR mode on the SPR sensing module 2 by the broad-spectrum linear polarization parallel light beam through total reflection, carrying information of the liquid film 3 through interaction of the SPR mode and/or the PWR mode and the liquid film 3, and receiving the reflected light by the hyperspectral imager 6 to obtain a hyperspectral image, wherein pixels in the hyperspectral image correspond to positions on the liquid film 3 one by one. The broad spectrum linear polarization parallel beam is obtained by passing through the linear polarizer 1 after being emitted by the broad band light source 4 of the hyperspectral SPR imaging apparatus.
And C, determining at least three actual measurement resonance wavelengths at a target position corresponding to the target pixel according to the hyperspectral image output by the hyperspectral imager 6, wherein the actual measurement resonance wavelengths at the target position are resonance wavelengths of an SPR mode and/or a PWR mode. The target pixel is, for example, a pixel at the center point of the field of view of the hyperspectral imager 6. At least three measured resonant wavelengths at the target location may be obtained by one hyperspectral imaging measurement or by multiple hyperspectral imaging measurements under different conditions.
And D, bringing the refractive index of the substrate, the refractive index and the thickness of the metal film and the refractive index of the covering layer above the liquid film into a Fresnel reflection formula of a four-layer structure, and performing simulation fitting on at least three actually measured resonance wavelengths of the liquid film at the target position to obtain at least three first relation curves at the target position, wherein the first relation curves are relation curves of the refractive index of the liquid film and the thickness of the liquid film at the target position, and each first curve corresponds to each actually measured resonance wavelength one by one.
And E, obtaining at least two second relation curves at the target position according to a Cauchy dispersion formula n (lambda) =a+blambda -2 and the obtained at least three first relation curves, wherein the second relation curves are relation curves of the parameter b and the liquid film thickness at the target position, and then obtaining the intersection point of the at least two second relation curves to obtain the value of the parameter b and the liquid film thickness at the target position. Since neither the parameter b nor the liquid film thickness is wavelength dependent, a plurality of second relationship curves obtained at the same location necessarily intersect at one point.
And F, according to the obtained value of the parameter b and the thickness of the liquid film at the target position, combining any one of the obtained at least three first relation curves to obtain the value of the parameter a, and carrying the values of the parameter a and the parameter b into a Cauchy dispersion formula to obtain a refractive index dispersion curve of the liquid film. Since the liquid film at the target position and the liquid film at other positions belong to the same material, the refractive index dispersion curve obtained by obtaining a plurality of first relationship curves and a plurality of second relationship curves at the target position is applicable to the entire liquid film 3.
And G, determining actual measurement resonance wavelengths at other positions according to the hyperspectral image output by the hyperspectral imager 6, determining the refractive index of the liquid film at the actual measurement resonance wavelengths at other positions according to the obtained refractive index dispersion curve of the liquid film, and obtaining the thickness of the liquid film at other positions according to the refractive index of the liquid film at the actual measurement resonance wavelengths at other positions and the Fresnel reflection formula of the four-layer structure.
And step H, obtaining the thickness distribution of the liquid film according to the obtained thickness of the liquid film at all positions. Here, all the positions include the target position and other positions than the target position.
The basic methods for measuring the thickness distribution of the liquid film 3 and the refractive index dispersion curve of the liquid film 3 in the embodiments of the present invention are a hyperspectral Surface Plasmon Resonance (SPR) imaging sensing method and a hyperspectral Plasmon Waveguide Resonance (PWR) imaging sensing method. SPR is a mature high-sensitivity biochemical sensing method. However, SPR sensors have a small detection depth, and can only detect 300nm thick liquid films at most in the visible light band. As the thickness of the liquid film increases (in the order of hundreds of nanometers to micrometers), PWR patterns are gradually generated in the liquid film. Therefore, a thicker (micrometer-scale thickness) liquid film can be measured by using the PWR mode, and a thinner (several nanometers to several tens of nanometers thickness) liquid film can be measured by using the SPR mode.
According to the embodiment of the present invention, the thickness and refractive index dispersion curve of the liquid film 3 includes a plurality of unknowns, so that when the thickness distribution and refractive index dispersion curve of the liquid film 3 are measured simultaneously, it is necessary to determine the plurality of unknowns, which requires an experiment to acquire resonance wavelengths of at least three SPR modes and/or PWR modes at a target position corresponding to a target pixel in a hyperspectral image, and for the target pixel, the three obtained measured resonance wavelengths can be used as known amounts to realize measurement of the thickness and color line curve at the target position. The thickness of the liquid film 3 changes with the change of the position, but the dispersion curve of the liquid film 3 does not change with the change of the position, and the refractive index dispersion curve at the target position is the refractive index dispersion curve of the liquid film 3. Only one unknown, i.e. thickness, needs to be measured at each other location on the liquid film 3. Therefore, for other positions of the liquid film 3, the liquid film thickness measurement at that position can be realized by using the measured resonance wavelength and the refractive index dispersion curve at that position. Therefore, the embodiment of the invention can realize the simultaneous measurement of the thickness distribution and the refractive index dispersion curve of the liquid film 3.
Thus far, the method for measuring the actual refractive index dispersion curve and the thickness of the liquid film in the embodiment is described. The present invention will be further described in detail below with reference to specific embodiments and with reference to the accompanying drawings, in order to make the objects, technical solutions and advantages of the present invention more apparent.
The actual measurement method for measuring the thickness distribution and refractive index dispersion curve of the liquid film will be described below by way of example one and example two. In both examples, the broadband light source 14 comprises a tungsten halogen lamp, a focusing lens and a linear polarizer 1. The metal film is also selected as a gold film, the thickness of the gold film is about 50 nm, and the hyperspectral SPR imaging sensor uses a Kretschmann prism coupling structure. In the first example, a silicone oil film was selected for the detailed description, and in the second example, a glycerol oil film was selected for the detailed description.
Example one
In the method for measuring the thickness distribution of the liquid film and the actual refractive index dispersion curve in this example, the liquid film 3 is a silicon oil film prepared on a glass substrate sputtered with a 50nm gold film using spin coating. The method for measuring the refractive index dispersion curve and the thickness distribution of the silicon oil film in the embodiment comprises the following steps:
A hyperspectral image of the silicon oil film was obtained using a hyperspectral SPR imaging apparatus.
First, the glass substrate is integrally fixed to a spin-coating stage, and a proper amount of silicone oil is dropped in the center of the substrate. Setting the rotating speed of the spin coating platform to 2000rpm, and spin-coating for 120s to obtain a spin-coated silicone oil film. Subsequently, the substrate spin-coated with silicone oil was fixed to the bottom surface of the glass prism, and the upper surface of the silicone oil was exposed to air, i.e., the corresponding cover layer was air at this time.
Next, the linear polarizer 1 was adjusted so that the incident broad-spectrum linear polarization parallel beam was p-polarized light, and hyperspectral images were recorded by using the hyperspectral imager 6 at an incidence angle of 50 ° of the reflected light of the p-polarized light on the SPR resonance module 2.
Fig. 4A shows an experimental spectrum and a simulation spectrum of a target pixel on a highlight image formed by a silicone oil film according to an embodiment of the present invention;
As shown in fig. 4A, the spectrum of the target pixel obtained when the incidence angle of the p-polarized light was 50 °, and the simulation result of the spectrum at the target pixel. The spectrum of the target pixel point comprises measured resonance wavelengths of a plurality of measured SPR modes and/or PWR modes, and the measured resonance wavelengths are the same as the simulated resonance wavelengths.
The measured resonance wavelengths (or simulated resonance wavelengths) of five of the measured SPR modes and/or PWR modes that are less affected by the broadband light source 14 spectrum are selected for fitting. The five resonance wavelengths are respectively a resonance wavelength No. 1, a resonance wavelength No. 2, a resonance wavelength No. 3, a resonance wavelength No. 4, and a resonance wavelength No. 5. From fig. 4A, it can be determined that the five more obvious resonant wavelengths (measured resonant wavelengths or simulated resonant wavelengths) lambda R of this pixel are 527.7 nm,563.9 nm,606.9nm,655.7 nm,714.0nm, respectively. After determining the five measured resonance wavelengths (or simulated resonance wavelengths) of the pixel, a two-dimensional distribution map of each of the measured resonance wavelengths of the five measured SPR modes and/or PWR modes may be drawn. FIG. 4B shows two-dimensional distribution graphs of measured resonance wavelengths for each of the five SPR modes and/or PWR modes obtained from FIG. 4A.
The thickness of the center position and the refractive index dispersion curve of the liquid film are obtained from the five measured resonance wavelengths of the target position (center position of the hyperspectral image). On the premise of knowing the resonance wavelength, the thickness is scanned, and a series of refractive indexes can be obtained through Fresnel formula fitting.
Fig. 4C shows three first curves obtained from fig. 4A for three of the resonant wavelengths.
As shown in fig. 4C, the refractive index-thickness simulation curves at the target positions plotted by the resonance wavelength No. 3, the resonance wavelength No.4, and the resonance wavelength No. 5 obtained in fig. 4A are shown. Since the resonance wavelength No. 3, the resonance wavelength No.4 and the resonance wavelength No. 5 are different, the refractive indexes corresponding to the three resonance peaks are not the same, and therefore, the three first curves have no intersection point. However, the refractive indexes corresponding to the three formants respectively accord with the Cauchy dispersion formula, and the refractive index of the liquid film can be converted into the parameter b of the Cauchy dispersion formula according to the formulas (11) and (12), so that a refractive index parameter b-thickness curve is drawn.
Fig. 4D shows two second curves at the target position obtained from the three first curves of fig. 4C.
As shown in fig. 4D, according to the formulas (11) to (12), two refractive index parameter-thickness curves (two second curves) obtained according to the refractive index-thickness simulation curves at the resonance wavelength No. 3, the resonance wavelength No. 4, and the resonance wavelength No. 5 in fig. 4C, under the experimental condition, since the liquid film thickness and the refractive index parameter at the target position are fixed, the intersection point of the two refractive index parameter-thickness curves intuitively depicts the method for solving the initial thickness of the pixel point at the target position. The initial thickness of the liquid film at the target position can be obtained from the position of the intersection pointnm。
Fig. 5 shows the thickness distribution of a silicone oil film provided in accordance with an embodiment of the present invention.
As shown in fig. 5, the thickness distribution of the silicone oil film is in the range of 3900-4100 nm.
Fig. 6 shows a comparison of simulated spectra obtained from the other four pixels on a hyperspectral image of a silicone oil film according to an embodiment of the present invention with experimental spectra.
As shown in fig. 6, the comparison between the simulated spectrum obtained by four pixels and the experimental spectrum is shown in fig. 5, where the simulated resonance wavelength obtained by simulating the spectrum of the other four pixels (except the target pixel) matches the actual resonance wavelength of the SPR mode and/or the PWR mode. The refractive index dispersion curve of the silica film is shown in FIG. 7, and the dispersion curve obtained in this example is。
Example two
Unlike the example one, the liquid film in this example was a glycerol film, and this example measured a hyperspectral SPR image of the glycerol film at an incidence angle of 52 ° for a broad spectral linear polarization parallel beam in the p-polarization direction. Because the glycerol film is thinner than the silicon film in example one, the PWR has fewer resonant orders, only four resonant wavelengths are selected for each pixel for fitting, and the resonant wavelength profile is plotted.
Fig. 8A shows an experimental spectrum and a simulation spectrum of a target pixel on a hyperspectral image formed by a glycerol film according to an embodiment of the present invention.
As shown in fig. 8A, the resonance wavelength of the center pixel (target pixel) is still preferentially fitted, and the preliminary fitting result is shown in fig. 8A. The four resonance wavelengths are 500.1 nm, 566.8 nm, 631.1nm and 729.7nm respectively. Preliminary fitting to obtain single-wavelength refractive index of the pixelThickness at target locationNm. FIG. 8B shows two-dimensional distribution plots of measured resonance wavelengths for each of the four SPR modes and/or PWR modes resulting from FIG. 8A.
The refractive index dispersion curve of the glycerin film is shown in FIG. 9A, the thickness distribution of the glycerin film is shown in FIG. 9B, and the dispersion curve in this example is。
According to the technical scheme, the method for measuring the refractive index dispersion curve and the thickness distribution of the liquid film has the advantages of low equipment cost, simplicity in operation, no complexity in theory involved in simulation fitting, capability of simultaneously obtaining the refractive index dispersion curve and the thickness distribution of the liquid film, and very important practical significance for rapidly and accurately obtaining a plurality of parameters of various liquid films simultaneously.
The foregoing description of the embodiments has been provided for the purpose of illustrating the general principles of the invention, and is not meant to limit the invention thereto, but to limit the invention thereto, and any modifications, equivalents, improvements and equivalents thereof may be made without departing from the spirit and principles of the invention.
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