CN110455745B - A method for measuring liquid refractive index dispersion and its application - Google Patents
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Abstract
本发明公开一种测量液体折射率色散的方法及其应用。本发明通过将一束单色光入射到棱镜的磨砂侧面,经其散射后进入棱镜并射到棱镜底面与样品的交界面,经交界面反射的光通过该棱镜另一侧面出射,检测出射光经棱镜底面与样品的交界面全反射形成半荫视场对应的出射角;对标准样品和待测样品下的出射角分别进行检测,代入公式A计算待测样品折射率。该方法在棱镜折射率未知的情况下实现液体折射率色散的测量;不但可以测量透明液体的折射率色散,而且可以测量弱吸收或散射液体的折射率色散;同时适用于测量固体、较厚薄膜及气体的折射率色散;测量精度高,达0.0001~0.0003。
The invention discloses a method for measuring liquid refractive index dispersion and its application. In the present invention, a beam of monochromatic light is incident on the frosted side of the prism, after being scattered, it enters the prism and hits the interface between the bottom surface of the prism and the sample, and the light reflected by the interface exits through the other side of the prism to detect the outgoing light. The exit angle corresponding to the semi-shade field of view is formed by total reflection at the interface between the bottom surface of the prism and the sample; the exit angles under the standard sample and the sample to be tested are detected respectively, and the refractive index of the sample to be tested is calculated by substituting formula A. The method realizes the measurement of the refractive index dispersion of liquids when the refractive index of the prism is unknown; it can not only measure the refractive index dispersion of transparent liquids, but also measure the refractive index dispersion of weakly absorbing or scattering liquids; it is also suitable for measuring solids and thick films. And the refractive index dispersion of the gas; the measurement accuracy is high, reaching 0.0001 to 0.0003.
Description
技术领域technical field
本发明属于光电精密测量技术领域,尤其涉及一种测量液体折射率色散的方法及其应用。The invention belongs to the technical field of photoelectric precision measurement, and in particular relates to a method for measuring liquid refractive index dispersion and its application.
背景技术Background technique
折射率色散或光谱是指一种介质对不同波长具有不同折射率的现象。液体的折射率色散或光谱测量具有重要应用意义,通过液体折射率色散的测量,可以了解到液体的折射率与波长的关系、浓度及组成等特性,测量液体的折射率方法主要包括:激光全反射法、光纤法、最小偏向角法、棱镜法、阿贝折光仪法、衍射法、椭圆偏振法等。理论上,这些方法都可以用于液体折射率色散或光谱的测量,但实际实验测量还存在不少困难,如光源的选择、待测液体放置及信号的检测方式等。最小偏向角法是在空心棱镜中装入不同液体,通过不同波长光的偏转来测量相应波长的折射率,该方法需要专门的空心棱镜,测量液体量较多;阿贝折光仪法是利用临界角来确定不同波长光的折射率,此方法目前只能测量波长为589nm的液体折射率,不适合于测量折射率色散;棱镜法是在两个等边三棱镜之间加入液体膜,在利用全反射原理的基础上,增加了一个棱镜用于产生色散,该方法需要三个棱镜,实验系统搭建较为繁琐,且待测液体膜会产生干涉条纹,导致测量误差较大,测量折射率精度只能达到小数点后三位。椭圆偏振法主要用于固体或薄膜的折射率测量,可以用于液体折射率光谱的测量,但所使用的光谱椭偏仪价格昂贵,数据处理复杂,直接测量液体色散时,液面噪声较大,使用棱镜配合测量也会带来样品调节过程繁琐及误差大等问题。因此,急需一种操作简单、方便、测量精度高的折射率色散测量方法。Refractive index dispersion or spectroscopy refers to the phenomenon that a medium has different refractive indices for different wavelengths. The refractive index dispersion or spectrum measurement of liquids has important application significance. Through the measurement of liquid refractive index dispersion, the relationship between the refractive index and wavelength, concentration and composition of liquids can be known. The methods of measuring the refractive index of liquids mainly include: laser full Reflection method, optical fiber method, minimum deflection angle method, prism method, Abbe refractometer method, diffraction method, ellipsometry method, etc. In theory, these methods can be used for the measurement of liquid refractive index dispersion or spectrum, but there are still many difficulties in actual experimental measurement, such as the choice of light source, the placement of the liquid to be measured, and the detection method of the signal. The minimum deflection angle method is to put different liquids in a hollow prism, and measure the refractive index of the corresponding wavelength through the deflection of light of different wavelengths. This method requires a special hollow prism and measures a large amount of liquid; the Abbe refractometer method uses a critical At present, this method can only measure the refractive index of liquid with a wavelength of 589 nm, and is not suitable for measuring refractive index dispersion; the prism method is to add a liquid film between two equilateral triangular prisms. On the basis of the reflection principle, a prism is added to generate dispersion. This method requires three prisms. The experimental system is complicated to build, and the liquid film to be measured will produce interference fringes, resulting in a large measurement error, and the measurement accuracy of the refractive index can only be to three decimal places. Ellipsometry is mainly used for the measurement of the refractive index of solids or thin films, and can be used to measure the refractive index spectrum of liquids, but the spectroscopic ellipsometer used is expensive and complicated in data processing. When the liquid dispersion is directly measured, the liquid surface noise is relatively large. , the use of prisms to cooperate with the measurement will also bring problems such as cumbersome sample adjustment process and large errors. Therefore, there is an urgent need for a refractive index dispersion measurement method with simple operation, convenience and high measurement accuracy.
发明内容SUMMARY OF THE INVENTION
本发明的首要目的在于克服现有技术的缺点与不足,提供一种测量液体折射率色散的方法。The primary purpose of the present invention is to overcome the shortcomings and deficiencies of the prior art, and to provide a method for measuring liquid refractive index dispersion.
本发明的另一目的在于提供上述测量液体折射率色散的方法的应用。Another object of the present invention is to provide an application of the above method for measuring the refractive index dispersion of a liquid.
为实现上述目的,本发明通过下述技术方案实现:To achieve the above object, the present invention is achieved through the following technical solutions:
一种测量液体折射率色散的方法,包括如下步骤:A method for measuring liquid refractive index dispersion, comprising the steps of:
(1)一束单色光入射到棱镜的磨砂侧面,经其散射后进入棱镜并射到棱镜底面与样品的交界面,经交界面反射的光通过该棱镜另一侧面出射,检测出射光经棱镜底面与样品的交界面全反射形成半荫视场对应的出射角;(1) A beam of monochromatic light is incident on the frosted side of the prism, and after being scattered, it enters the prism and hits the interface between the bottom surface of the prism and the sample. The light reflected by the interface exits through the other side of the prism, and the outgoing light is detected by The total reflection at the interface between the bottom surface of the prism and the sample forms the output angle corresponding to the semi-shadow field of view;
(2)通过步骤(1)对标准样品和待测样品下的出射角分别进行检测,代入公式A计算待测样品折射率;(2) by step (1), the exit angles under the standard sample and the sample to be tested are respectively detected, and the refractive index of the sample to be tested is calculated by substituting formula A;
(3)通过步骤(1)和步骤(2)获得待测样品在不同波长的单色光的折射率及其色散;(3) obtaining the refractive index and dispersion of the monochromatic light of the sample to be tested at different wavelengths through steps (1) and (2);
所述的公式A为:The formula A is:
其中,n2d(λ)为待测样品折射率、n2(λ)为标准样品折射率、α为棱镜底角、Φ(λ)、Φd(λ)分别为测量标准样品、待测样品时出射光经棱镜底面与样品的交界面全反射形成半荫视场对应的出射角。Among them, n 2d (λ) is the refractive index of the sample to be measured, n 2 (λ) is the refractive index of the standard sample, α is the bottom angle of the prism, Φ(λ), Φ d (λ) are the measurement standard sample and the sample to be measured, respectively. When the outgoing light is totally reflected by the interface between the bottom surface of the prism and the sample, the outgoing angle corresponding to the semi-shadow field of view is formed.
步骤(1)中所述的棱镜的进光面(工作面)为磨砂面。The light entrance surface (working surface) of the prism described in step (1) is a frosted surface.
步骤(1)中所述的棱镜优选为等腰棱镜;更优选为底角为45°或60°的等腰棱镜;最优选为折射率n1=1.7450或1.5100、底角为45°或60°的等腰棱镜。The prism described in the step (1) is preferably an isosceles prism; more preferably an isosceles prism with a base angle of 45° or 60°; most preferably a refractive index n 1 =1.7450 or 1.5100, and a base angle of 45° or 60° ° isosceles prism.
步骤(1)中所述的样品优选为液体、固体或薄膜。The sample described in step (1) is preferably liquid, solid or thin film.
步骤(2)中所述的标准样品优选为标准液体或已知折射率的液体。The standard sample described in step (2) is preferably a standard liquid or a liquid with a known refractive index.
步骤(2)中所述的待测样品优选为液体、固体或薄膜。The sample to be tested in step (2) is preferably a liquid, a solid or a thin film.
本发明测量液体折射率色散的流程如图1所示,具体如下:The process of measuring the liquid refractive index dispersion of the present invention is shown in Figure 1, and the details are as follows:
一束复色光源通过单色仪,依次选择不同波长的单色光经棱镜磨砂侧面入射到棱镜与样品的交界面,在棱镜的另一侧面检测出射光半荫视场对应的出射角;分别通过对标准样品出射角和待测样品出射角的测量,按公式A计算得到待测样品在不同波长的单色光下的折射率及其色散。A beam of polychromatic light source passes through a monochromator, and sequentially selects monochromatic light of different wavelengths to enter the interface between the prism and the sample through the frosted side of the prism, and detects the exit angle corresponding to the semi-shade field of view of the outgoing light on the other side of the prism; respectively; By measuring the exit angle of the standard sample and the exit angle of the sample to be tested, the refractive index and dispersion of the sample to be tested under different wavelengths of monochromatic light are calculated according to formula A.
本发明方法原理分析如下:The principle analysis of the method of the present invention is as follows:
如图2所示,设λ为入射光束的波长,no、n1(λ)、n2(λ)分别为空气、棱镜、标准液体折射率,且满足n2(λ)小于n1(λ),θ1(λ)、θ2(λ)、Φ(λ)分别为测量标准液体时棱镜底面与标准液体交界面的入射角、折射角、该棱镜另一侧面与空气交界面的出射角,α为棱镜的底角,空气折射率n0=1,根据光的折射定律,有:As shown in Figure 2, let λ be the wavelength of the incident beam, n o , n 1 (λ), and n 2 (λ) are the refractive indices of air, prism, and standard liquid, respectively, and n 2 (λ) is less than n 1 ( λ), θ 1 (λ), θ 2 (λ), Φ(λ) are the incident angle and refraction angle of the interface between the bottom surface of the prism and the standard liquid when measuring the standard liquid, and the exit angle of the interface between the other side of the prism and the air. angle, α is the base angle of the prism, and the refractive index of air is n 0 =1. According to the law of refraction of light, there are:
n1(λ)sinθ1(λ)=n2(λ)sinθ2(λ) (1)n 1 (λ) sinθ 1 (λ)=n 2 (λ) sinθ 2 (λ) (1)
当入射角逐渐增大时,发生全反射,有θ2(λ)=90°:When the incident angle gradually increases, total reflection occurs, with θ 2 (λ)=90°:
由图2中的三角关系及折射定律,发生全反射时,容易得到:From the triangular relationship and the law of refraction in Figure 2, when total reflection occurs, it is easy to obtain:
θ3(λ)=|α-θ1(λ)| (3)θ 3 (λ)=|α-θ 1 (λ)| (3)
n1(λ)sinθ3(λ)=n0 sinφ(λ) (4)n 1 (λ) sinθ 3 (λ)=n 0 sinφ(λ) (4)
其中θ3(λ)为发生全反射时光线在AC面的入射角。where θ 3 (λ) is the incident angle of light on the AC surface when total reflection occurs.
根据三角公式,将(3)、(4)带入(2)中可得:According to the trigonometric formula, (3), (4) into (2) can be obtained:
同理,当测量待测液体时,设n2d(λ)为待测液体的折射率,且n2d(λ)小于n1(λ),θ1d(λ)、θ2d(λ)、Φd(λ)分别为测量待测液体时棱镜底面与待测液体交界面的入射角、折射角、该棱镜另一侧面与空气交界面的出射角,根据光的折射定律,有:Similarly, when measuring the liquid to be tested, let n 2d (λ) be the refractive index of the liquid to be tested, and n 2d (λ) is less than n 1 (λ), θ 1d (λ), θ 2d (λ), Φ d (λ) are the incident angle and refraction angle of the interface between the bottom surface of the prism and the liquid to be measured, and the exit angle of the interface between the other side of the prism and the air when measuring the liquid to be measured. According to the law of refraction of light, there are:
n1(λ)sinθ1d(λ)=n2d(λ)sinθ2d(λ) (6)n 1 (λ) sinθ 1d (λ)=n 2d (λ) sinθ 2d (λ) (6)
当入射角逐渐增大时,发生全反射,有θ2d(λ)=90°:When the incident angle gradually increases, total reflection occurs, with θ 2d (λ)=90°:
n2d(λ)=n1(λ)sinθ1d(λ) (7)n 2d (λ)=n 1 (λ) sinθ 1d (λ) (7)
同理,对于待测液体可得:In the same way, for the liquid to be tested, we can get:
θ3d(λ)=|α-θ1d(λ)| (8)θ 3d (λ)=|α-θ 1d (λ)| (8)
n1(λ)sinθ3d(λ)=n0 sinφd(λ) (9)n 1 (λ) sinθ 3d (λ)=n 0 sinφ d (λ) (9)
其中θ3d(λ)为发生全反射时光线在AC面的入射角。where θ 3d (λ) is the incident angle of light on the AC surface when total reflection occurs.
根据三角关系,将式(5)、(8)、(9)代入式(7)中可得,According to the trigonometric relationship, substituting equations (5), (8), and (9) into equation (7) can be obtained,
由式(10)可知,待测液体折射率n2d(λ)与棱镜折射率无关。如果已知标准液体的色散n2(λ)及棱镜底角α,只要分别测量得到相应波长的标准液体及待测液体的出射角,就可以计算得到待测液体的折射率色散或光谱。It can be known from formula (10) that the refractive index n 2d (λ) of the liquid to be measured has nothing to do with the refractive index of the prism. If the dispersion n 2 (λ) of the standard liquid and the base angle α of the prism are known, the refractive index dispersion or spectrum of the liquid to be measured can be calculated as long as the corresponding wavelengths of the standard liquid and the liquid to be measured are measured respectively.
在利用本发明方法测量折射率色散过程中,实验系统调节好以后,测量一次标准样品的一系列不同波长的出射角作为已知数据备用。测量未知待测样品折射率色散时,直接可以调用该数据代入式(10)计算待测样品折射率色散。In the process of measuring refractive index dispersion by the method of the present invention, after the experimental system is adjusted, the emission angles of a series of different wavelengths of a standard sample are measured once as known data for use. When measuring the refractive index dispersion of the unknown sample to be tested, the data can be directly called and substituted into formula (10) to calculate the refractive index dispersion of the sample to be tested.
所述的测量液体折射率色散的方法在测量样品折射率色散中的应用。The application of the method for measuring the refractive index dispersion of liquid in measuring the refractive index dispersion of a sample.
所述的样品包括液体、固体及薄膜。The samples include liquids, solids and films.
所述标准样品为其已知折射率色散的液体或标准液体。The standard sample is a liquid or standard liquid with known refractive index dispersion.
一种测量折射率色散的装置,是通过上述方法设计得到的,包括光源、第一凸透镜、单色仪、第二凸透镜、小孔光阑、棱镜、样品载体、旋转载物台、外转盘、望远镜;沿着光束前进的方向,光源、第一凸透镜、单色仪、第二凸透镜、小孔光阑和旋转载物台依次排列,旋转载物台设置在外转盘的中心区域,棱镜位于旋转载物台的转轴中心,棱镜底面连接有样品载体,用于装载样品;外转盘与望远镜连接一体并同步旋转,用于出射光束半荫视场观察与测量,外转盘可以读出望远镜所处位置的角度值,望远镜还具有自准直的功能,可以标定自己的角度位置。A device for measuring refractive index dispersion is designed and obtained by the above method, comprising a light source, a first convex lens, a monochromator, a second convex lens, an aperture diaphragm, a prism, a sample carrier, a rotating stage, an outer turntable, Telescope; along the direction of the light beam, the light source, the first convex lens, the monochromator, the second convex lens, the aperture diaphragm and the rotating stage are arranged in sequence, the rotating stage is arranged in the central area of the outer turntable, and the prism is located in the rotating stage. At the center of the rotation axis of the stage, the bottom surface of the prism is connected with a sample carrier for loading samples; the outer turntable is connected with the telescope and rotates synchronously, which is used for the observation and measurement of the semi-shade field of view of the outgoing beam. The outer turntable can read the position of the telescope. The telescope also has the function of self-collimation, which can calibrate its own angular position.
所述的光源为复色光源,优选为氙灯、卤钨灯、汞灯、钠灯及各种激光器等连续光谱或分立光谱的光源。The light source is a polychromatic light source, preferably a continuous spectrum or discrete spectrum light source such as a xenon lamp, a tungsten halogen lamp, a mercury lamp, a sodium lamp and various lasers.
所述的第一凸透镜及第二凸透镜优选为石英玻璃单透镜。The first convex lens and the second convex lens are preferably quartz glass single lenses.
所述的单色仪优选为光栅或棱镜单色仪,可以通过手动或自动的方式选择输出不同波长的单色光。The monochromator is preferably a grating or prism monochromator, which can be selected to output monochromatic light of different wavelengths manually or automatically.
所述的波长分辨率优选为2~10nm。The wavelength resolution is preferably 2-10 nm.
所述的小孔光阑优选为可调光阑,可以通过手动调节光阑大小增加半荫视场对比度。The aperture diaphragm is preferably an adjustable diaphragm, and the semi-shade field of view contrast can be increased by manually adjusting the diaphragm size.
所述的棱镜优选为等腰棱镜;更优选为底角为45°或60°的等腰棱镜;最优选为折射率n1=1.7450或1.5100、底角为45°或60°的等腰棱镜。The prism is preferably an isosceles prism; more preferably an isosceles prism with a base angle of 45° or 60°; most preferably an isosceles prism with a refractive index n 1 =1.7450 or 1.5100 and a base angle of 45° or 60° .
所述的样品载体优选为U型槽、贴上黑色胶带的玻璃片、黑色毛玻璃、黑色胶带、贴上黑色胶带的玻璃衬底中的一种。The sample carrier is preferably one of U-shaped groove, glass sheet with black tape, black frosted glass, black tape, and glass substrate with black tape.
所述的外转盘的读数圆盘有0°~360°的刻度盘,其转角精度为0.5°。The reading disc of the outer turntable has a dial with a range of 0° to 360°, and the accuracy of its rotation angle is 0.5°.
所述的外转盘相隔180°处有两个对称的角游标,最小分度为1′。The outer turntable has two symmetrical angular verniers at a distance of 180°, and the minimum division is 1'.
所述的外转盘的中心区域设置有内转盘。The central area of the outer turntable is provided with an inner turntable.
所述的内转盘与旋转载物台优选为固定连接。The inner turntable and the rotating stage are preferably fixedly connected.
所述的望远镜与外转盘优选为固定连接,当内转盘固定时,望远镜转过一定的角度,就可以从游标读出该转角的值;记录数据时,读取两个游标所示的数值,取其平均值。The telescope and the outer turntable are preferably fixedly connected. When the inner turntable is fixed, the telescope rotates through a certain angle, and the value of the rotation angle can be read from the cursor; when recording data, read the values shown by the two cursors, Take its average.
所述的望远镜由物镜、阿贝目镜、分划板组成,通过自准直法调节载物平台的中心轴与望远镜光轴垂直,与外转盘固连可以标定自己的位置,读出角度值。The telescope is composed of an objective lens, an Abbe eyepiece, and a reticle. The central axis of the object platform is adjusted to be perpendicular to the optical axis of the telescope by the self-collimation method, and its position can be calibrated and the angle value can be read by being fixed with the outer turntable.
上述装置的光路调整过程如下:The optical path adjustment process of the above device is as follows:
把光源、第一凸透镜、单色仪、第二凸透镜及小孔光阑放一直线上使它们共轴,使棱镜的底面位于旋转载物台的转轴中心,使光源出射的光经第一凸透镜聚焦到单色仪入射狭缝,从单色仪出射狭缝出来波长为λ的单色光经第二凸透镜及小孔光阑入射到棱镜的磨砂侧面,同时调整旋转载物台及外转盘的角度,使望远镜中由透明小十字线经物镜发出的平行绿光经棱镜出射面反射后的小十字像与目镜内的上十字叉丝重合,固定旋转载物台。Place the light source, the first convex lens, the monochromator, the second convex lens and the aperture diaphragm on a straight line to make them coaxial, so that the bottom surface of the prism is located in the center of the rotation axis of the rotating stage, so that the light emitted by the light source passes through the first convex lens. Focus on the entrance slit of the monochromator, and the monochromatic light with a wavelength of λ emerges from the exit slit of the monochromator and enters the frosted side of the prism through the second convex lens and the aperture diaphragm. Angle, so that the parallel green light emitted by the small transparent cross line in the telescope through the objective lens is reflected by the exit surface of the prism and the small cross image coincides with the upper cross line in the eyepiece, and the rotating stage is fixed.
上述装置的具体测量步骤如下:The specific measurement steps of the above device are as follows:
(1)通过单色仪波长选择旋钮选定出射波长,记下该波长值;(1) Select the outgoing wavelength through the wavelength selection knob of the monochromator, and record the wavelength value;
(2)标准样品出射角的测量:把标准样品置于样品载体,调整望远镜观察棱镜出射侧面,在望远镜视场中看到由棱镜底面与样品交界面的全反射形成的半荫视场,把半荫视场的分界线调至望远镜目镜中垂直准线处,此时在外转盘上读出两个游标所示数值,求平均得到其位置角度值a,转动望远镜对准棱镜的出射侧面,使由透明小十字线经物镜发出的平行绿光经棱镜出射侧面反射后的小十字像与目镜内的上十字叉丝重合,记下此时在外转盘上的两个游标所示数值,求平均得到其位置角度值b,两个位置角度值相减a-b绝对值为标准样品的出射角。(2) Measurement of the exit angle of the standard sample: place the standard sample on the sample carrier, adjust the telescope to observe the exit side of the prism, and see the half-shadow field of view formed by the total reflection of the interface between the bottom surface of the prism and the sample in the field of view of the telescope. The dividing line of the semi-shadow field of view is adjusted to the vertical alignment line in the eyepiece of the telescope. At this time, the values indicated by the two cursors are read out on the outer turntable, and the average position angle value a is obtained. Turn the telescope to align the exit side of the prism, so that The small cross image after the parallel green light emitted by the transparent small cross line through the objective lens and reflected by the prism exit side coincides with the upper cross wire in the eyepiece, record the value indicated by the two cursors on the outer turntable at this time, and average it to get Its position angle value b, the absolute value of the subtraction a-b of the two position angle values is the exit angle of the standard sample.
(3)待测样品出射角的测量:把待测样品置于样品载体,调整望远镜观察棱镜出射侧面,在望远镜视场中看到由棱镜底面与样品交界面的全反射形成的半荫视场,把半荫视场的分界线调至望远镜目镜中垂直准线处,此时在外转盘上读出两个游标所示数值,求平均得到其位置角度值c,转动望远镜对准棱镜的出射侧面,使由透明小十字线经物镜发出的平行绿光经棱镜出射侧面反射后的小十字像与目镜内的上十字叉丝重合,记下此时在外转盘上的两个游标所示数值,求平均得到其位置角度值d,两个位置角度值相减c-d绝对值为待测样品的出射角。(3) Measurement of the exit angle of the sample to be tested: place the sample to be tested on the sample carrier, adjust the telescope to observe the exit side of the prism, and see the semi-shadow field of view formed by the total reflection of the interface between the bottom surface of the prism and the sample in the field of view of the telescope , adjust the dividing line of the semi-shade field of view to the vertical alignment line in the eyepiece of the telescope. At this time, read the values indicated by the two cursors on the outer turntable, and average them to obtain the position angle value c. Turn the telescope to align the exit side of the prism. , so that the small cross image of the parallel green light emitted by the transparent small cross line through the objective lens and reflected by the prism exit side coincides with the upper cross line in the eyepiece, and record the value indicated by the two cursors on the outer turntable at this time, and find The average position angle value d is obtained, and the absolute value of the subtraction c-d of the two position angle values is the exit angle of the sample to be tested.
(4)待测样品折射率计算:把测量得到的角度值代入公式(10),得到待测样品在波长λ处的折射率,通过单色仪改变入射光波长,重复以上步骤,得到待测样品折射率色散或光谱。(4) Calculation of the refractive index of the sample to be tested: Substitute the measured angle value into formula (10) to obtain the refractive index of the sample to be tested at the wavelength λ, change the wavelength of the incident light by a monochromator, and repeat the above steps to obtain the sample to be tested. Sample refractive index dispersion or spectrum.
本发明相对于现有技术具有如下的优点及效果:Compared with the prior art, the present invention has the following advantages and effects:
1、本发明在棱镜折射率未知的情况下可以实现液体折射率色散的测量;1. The present invention can realize the measurement of liquid refractive index dispersion under the condition that the refractive index of the prism is unknown;
2、本发明不但可以测量透明液体的折射率色散,而且可以测量弱吸收或散射液体的折射率色散;2. The present invention can measure not only the refractive index dispersion of transparent liquids, but also the refractive index dispersions of weakly absorbing or scattering liquids;
3、本发明也适用于测量固体、较厚(大于1微米)薄膜及气体的折射率色散;3. The present invention is also suitable for measuring the refractive index dispersion of solids, thicker (greater than 1 micron) films and gases;
4、本发明测量精度高,其中测量液体折射率精度达0.0001~0.0003;4. The measurement accuracy of the present invention is high, and the measurement accuracy of the refractive index of the liquid is 0.0001-0.0003;
5、本发明测量装置简单,操作及测量过程方便。5. The measuring device of the present invention is simple, and the operation and measuring process are convenient.
附图说明Description of drawings
图1为本发明的测量方法流程图。FIG. 1 is a flow chart of the measurement method of the present invention.
图2为本发明的测量原理光路图。FIG. 2 is an optical path diagram of the measurement principle of the present invention.
图3为本发明实施例1提供的测量装置及光路示意图。FIG. 3 is a schematic diagram of a measuring device and an optical path according to Embodiment 1 of the present invention.
图4为本发明实施例2提供的测量装置及光路示意图。FIG. 4 is a schematic diagram of a measurement device and an optical path according to
图5为本发明实施例3提供的测量装置及光路示意图。FIG. 5 is a schematic diagram of a measurement device and an optical path according to
图6为本发明实施例4提供的测量装置及光路示意图。FIG. 6 is a schematic diagram of a measurement device and an optical path according to
图7为本发明实施例2中60%葡萄糖溶液折射率色散曲线图。7 is a graph of the refractive index dispersion curve of a 60% glucose solution in Example 2 of the present invention.
图8为本发明实施例3中盖玻片折射率色散曲线图。FIG. 8 is a graph of the refractive index dispersion curve of the cover glass in Example 3 of the present invention.
图9为本发明实施例4中明胶薄膜折射率色散曲线图。9 is a graph of the refractive index dispersion curve of the gelatin film in Example 4 of the present invention.
图3~6中,1-复色光源、2-第一凸透镜、3-单色仪、4-第二凸透镜、5-小孔光阑、6-棱镜、7-液体样品、8-U型槽、9-旋转载物台、10-外转盘、11-望远镜、12-黑色胶带、13-玻璃片、14-匹配液、15-待测固体样品、16-薄膜样品、17-玻璃衬底。In Figures 3-6, 1- polychromatic light source, 2- first convex lens, 3- monochromator, 4- second convex lens, 5- pinhole diaphragm, 6- prism, 7- liquid sample, 8- U-shape Tank, 9-rotating stage, 10-outer turntable, 11-telescope, 12-black tape, 13-glass sheet, 14-matching liquid, 15-solid sample to be tested, 16-film sample, 17-glass substrate .
具体实施方式Detailed ways
下面结合实施例及附图对本发明作进一步详细的描述,但本发明的实施方式不限于此。The present invention will be described in further detail below with reference to the embodiments and the accompanying drawings, but the embodiments of the present invention are not limited thereto.
实施例1Example 1
一种测量液体折射率色散的装置,如图3所示,包括复色光源1、第一凸透镜2、单色仪3、第二凸透镜4、小孔光阑5、棱镜6、液体样品7、U型槽8、旋转载物台9、外转盘10、望远镜11。其中,沿着光束前进的方向,复色光源1、第一凸透镜2、单色仪3、第二凸透镜4、小孔光阑5和旋转载物台9依次排列,旋转载物台9设置在外转盘10的中心区域,棱镜6位于旋转载物台9的转轴中心,棱镜6底面连接有U型槽8,用于装载液体;外转盘10与望远镜11连接一体并同步旋转,用于出射光束半荫视场观察与测量。外转盘10可以读出望远镜11所处位置的角度值。望远镜11还具有自准直的功能,可以标定自己的角度位置。A device for measuring liquid refractive index dispersion, as shown in Figure 3, includes a polychromatic light source 1, a first
复色光源1为氙灯、卤钨灯、汞灯、钠灯及各种激光器等连续光谱或分立光谱的光源;第一凸透镜2及第二凸透镜4为石英玻璃单透镜;单色仪3为光栅或棱镜单色仪,通过手动或自动的方式选择输出不同波长的单色光,其波长分辨率2~10nm;棱镜6为等腰棱镜或等边棱镜,首选底角为60或45°的常见棱镜,如棱镜折射n1=1.7450或1.5100;小孔光阑5为可调光阑,可以通过手动调节光阑大小增加半荫视场对比度;U型槽8为防渗水槽;外转盘10的读数圆盘有0°~360°的刻度盘,其转角精度为0.5°,外转盘10带有内转盘,内转盘设置在外转盘10的中心区域,外转盘和内转盘相隔180°处有两个对称的角游标,最小分度为1′,内转盘与旋转载物台9固定连接;望远镜11与外转盘10固连。当内转盘固定时,若望远镜转过一定的角度,就可以从游标读出该转角的值。记录数据时,读取两个游标所示的数值,取其平均值;望远镜11是由物镜、阿贝目镜、分划板组成,通过自准直法调节载物平台的中心轴与望远镜光轴垂直,与外转盘10固定连接可以标定自己的位置,读出角度值。The polychromatic light source 1 is a continuous spectrum or discrete spectrum light source such as xenon lamp, tungsten halogen lamp, mercury lamp, sodium lamp and various lasers; the first
上述装置的光路调整过程如下:The optical path adjustment process of the above device is as follows:
把复色光源1、凸透镜2、单色仪3、凸透镜4及小孔光阑5放一直线上使它们共轴,使棱镜6的底面位于旋转载物台9的转轴中心,使复色光源1出射的光经凸透镜2聚焦到单色仪3入射狭缝,从单色仪3出射狭缝出来波长为λ的单色光经凸透镜4及小孔光阑5入射到棱镜的磨砂侧面,同时调整旋转载物台9及外转盘10的角度,使望远镜11中由透明小十字线经物镜发出的平行绿光经棱镜出射面反射后的小十字像与目镜内的上十字叉丝重合,固定旋转载物台9。Put the polychromatic light source 1, the
上述装置的具体测量步骤如下:The specific measurement steps of the above device are as follows:
(1)通过单色仪3波长选择旋钮选定出射波长,记下该波长值;(1) Select the outgoing wavelength through the
(2)标准液体出射角的测量:将标准液体倒进U型槽8,调整望远镜11观察棱镜出射侧面,在望远镜视场中看到由棱镜底面与液体交界面的全反射形成的半荫视场,把半荫视场的分界线调至望远镜目镜中垂直准线处,此时在外转盘10上读出两个游标所示数值,求平均得到其位置角度值a,转动望远镜11对准棱镜6的出射侧面,使由透明小十字线经物镜发出的平行绿光经棱镜出射侧面反射后的小十字像与目镜内的上十字叉丝重合,记下此时在外转盘10上的两个游标所示数值,求平均得到其位置角度值b,两个位置角度值相减a-b绝对值为标准液体的出射角。(2) Measurement of the exit angle of the standard liquid: pour the standard liquid into the
(3)待测液体出射角的测量:将待测液体倒进U型槽8,调整望远镜11观察棱镜出射侧面,在望远镜视场中看到由棱镜底面与液体交界面的全反射形成的半荫视场,把半荫视场的分界线调至望远镜目镜中垂直准线处,此时在外转盘10上读出两个游标所示数值,求平均得到其位置角度值c,转动望远镜11对准棱镜6的出射侧面,使由透明小十字线经物镜发出的平行绿光经棱镜出射侧面反射后的小十字像与目镜内的上十字叉丝重合,记下此时在外转盘10上的两个游标所示数值,求平均得到其位置角度值d,两个位置角度值相减c-d绝对值为待测液体的出射角。(3) Measurement of the exit angle of the liquid to be measured: pour the liquid to be measured into the
(4)待测液体折射率计算:将测量得到的角度值代入(10)式,得到待测液体在波长λ处的折射率,通过单色仪改变入射光波长,重复以上步骤,得到待测液体折射率色散或光谱。(4) Calculation of the refractive index of the liquid to be measured: Substitute the measured angle value into the formula (10) to obtain the refractive index of the liquid to be measured at the wavelength λ, change the wavelength of the incident light by a monochromator, and repeat the above steps to obtain the liquid to be measured. Liquid Refractive Index Dispersion or Spectroscopy.
实施例2Example 2
一种测量液体折射率色散的装置,如图4所示,包括复色光源1、第一凸透镜2、单色仪3、第二凸透镜4、小孔光阑5、棱镜6、液体样品7、旋转载物台9、外转盘10、望远镜11、黑色胶带12、玻璃片13。A device for measuring liquid refractive index dispersion, as shown in Figure 4, includes a polychromatic light source 1, a first
本实施例提供的装置与实施例1的区别在于:液体样品的载体不同,即将贴有黑色胶带12的玻璃片13取代U型槽8。玻璃片13一侧贴上黑色胶带12防止背反,取少量液体样品7置于黑色胶带上并紧贴棱镜底面,与棱镜一起置于旋转载物台9上。本实施例中也可将黑色的毛玻璃或者将毛玻璃涂黑后作为液体样品的载体,实现少量液体样品色散的测量。The difference between the device provided in this embodiment and the embodiment 1 is that the carrier of the liquid sample is different, that is, the
分别采用本实施例提供的装置及方法、双棱镜法测量60%葡萄糖溶液折射率色散,其中,棱镜折射率n1=1.7450,底角α=60°,以纯水为标准液体,结果如图7所示:表明采用本实施例提供的装置及方法与常见的双棱镜法得到的结果非常接近。The device and method provided in this embodiment and the double prism method are used to measure the refractive index dispersion of 60% glucose solution, wherein the prism refractive index n 1 =1.7450, the base angle α = 60°, and pure water is used as the standard liquid, the results are shown in the figure 7: It shows that the results obtained by the device and method provided in this embodiment are very close to the results obtained by the common double prism method.
实施例3Example 3
一种测量固体折射率色散的装置,如图5所示,包括复色光源1、第一凸透镜2、单色仪3、第二凸透镜4、小孔光阑5、棱镜6、旋转载物台9、外转盘10、望远镜11、黑色胶带12、匹配液14、待测固体样品15。A device for measuring solid refractive index dispersion, as shown in Figure 5, includes a polychromatic light source 1, a first
本实施例提供的装置与实施例1的区别在于:待测样品及其载体不同,即将待测固体样品15取代液体样品7,将黑色胶带12取代U型槽8,同时添加匹配液14。待测固体样品15一面贴上黑色胶带12防止背部反射光,另一面滴少许与棱镜折射率相同的匹配液14后紧贴棱镜底面,保证棱镜与固体样品之间没有气泡;样品与棱镜一起置于旋转载物台9上。The difference between the device provided in this embodiment and Embodiment 1 is that the sample to be tested and its carrier are different, that is, the
采用本实施例提供的装置及方法测量普通盖玻片折射率色散,其中,棱镜折射率n1=1.7450,底角α=60°,以纯水为标准液体,结果如图8所示。The device and method provided in this embodiment are used to measure the refractive index dispersion of a common cover glass, wherein the prism refractive index n 1 =1.7450, the base angle α = 60°, and pure water is used as the standard liquid. The results are shown in FIG. 8 .
实施例4Example 4
一种测量薄膜折射率色散的装置,如图6所示,包括复色光源1、第一凸透镜2、单色仪3、第二凸透镜4、小孔光阑5、棱镜6、旋转载物台9、外转盘10、望远镜11、黑色胶带12、匹配液14、薄膜样品16、玻璃衬底17。A device for measuring the refractive index dispersion of thin films, as shown in Figure 6, includes a polychromatic light source 1, a first
本实施例提供的装置与实施例1的区别在于:待测样品及其载体不同,即将薄膜样品15取代液体样品7,将贴有黑色胶带12的玻璃衬底17取代U型槽8,同时添加匹配液14。待测薄膜样品16涂镀于玻璃衬底17一面上,玻璃衬底17的另一面贴上黑色胶带12防止背反,薄膜面滴少许与棱镜折射率相同的匹配液14后紧贴棱镜底面,保证棱镜与固体样品之间没有气泡;样品与棱镜一起置于旋转载物台9上。The difference between the device provided in this embodiment and Embodiment 1 is that the sample to be tested and its carrier are different, that is, the
采用本实施例提供的装置及方法测量玻璃表面明胶薄膜样品折射率色散,其中,棱镜折射率n1=1.7450,底角α=60°,以纯水为标准液体,结果如图9所示。The device and method provided in this embodiment are used to measure the refractive index dispersion of the gelatin film sample on the glass surface, wherein the prism refractive index n 1 =1.7450, the base angle α = 60°, and pure water is used as the standard liquid. The results are shown in FIG. 9 .
对比实施例1Comparative Example 1
为了比较测量精确度,分别采用经典阿贝折射仪与实施例2提供的装置及方法测量蒸馏水及5%葡萄糖溶液在波长589nm处的折射率,测量结果如表1所示。结果表明:本发明方法测量液体折射率的精度到达0.0001。In order to compare the measurement accuracy, a classical Abbe refractometer and the device and method provided in Example 2 were used to measure the refractive indices of distilled water and 5% glucose solution at a wavelength of 589 nm. The measurement results are shown in Table 1. The results show that the method of the present invention can measure the refractive index of liquid with an accuracy of 0.0001.
表1阿贝折射仪与本方法测量蒸馏水及5%葡萄糖溶液折射率结果Table 1 Abbe refractometer and this method measure the refractive index results of distilled water and 5% glucose solution
总之,本发明的具体结构多种多样,只要是采用一束单色光入射到棱镜的磨砂侧面,经检测出射光经棱镜底面与标准样品(待测样品)的交界面全反射形成半荫视场对应的出射角,来测量待测样品折射率及其色散的装置,都属于本申请的保护范围。In a word, the specific structure of the present invention is various, as long as a beam of monochromatic light is incident on the frosted side of the prism, the detected outgoing light is totally reflected by the interface between the bottom surface of the prism and the standard sample (sample to be tested) to form a semi-shadow view The device for measuring the refractive index of the sample to be measured and its dispersion according to the exit angle corresponding to the field all belong to the protection scope of the present application.
上述实施例为本发明较佳的实施方式,但本发明的实施方式并不受上述实施例的限制,其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化,均应为等效的置换方式,都包含在本发明的保护范围之内。The above-mentioned embodiments are preferred embodiments of the present invention, but the embodiments of the present invention are not limited by the above-mentioned embodiments, and any other changes, modifications, substitutions, combinations, The simplification should be equivalent replacement manners, which are all included in the protection scope of the present invention.
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