CN115128002B - A system and method for measuring nonlinear optical properties of materials - Google Patents

A system and method for measuring nonlinear optical properties of materials Download PDF

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CN115128002B
CN115128002B CN202210698151.3A CN202210698151A CN115128002B CN 115128002 B CN115128002 B CN 115128002B CN 202210698151 A CN202210698151 A CN 202210698151A CN 115128002 B CN115128002 B CN 115128002B
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CN115128002A (en
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王俊
王梓鑫
陈晨端
董宁宁
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Shanghai Institute of Optics and Fine Mechanics of CAS
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    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract

The invention provides a system and a method for measuring nonlinear optical properties of a material, wherein the measuring method integrates a Z scanning technology and confocal microscopic imaging, adopts a microscopic objective lens to perform excitation light focusing, signal light collection, sample surface morphology imaging and spot synchronous imaging, and realizes real-time monitoring of the size of a spot; the three-dimensional precise translation stage is used for controlling the position of the sample, so that the nonlinear optical property of the micron-sized sample can be measured. The method can synchronously measure the nonlinear absorption and nonlinear refraction data of the material, is simultaneously suitable for measuring uniform and non-uniform, macroscopic and microscopic samples, solves the problem of nonlinear property test of non-uniform irregular small-size samples, and expands the application and test range of Z scanning technology.

Description

一种测量材料非线性光学性质的系统及方法A system and method for measuring nonlinear optical properties of materials

技术领域Technical Field

本发明涉及非线性光学测量技术领域,尤其涉及一种测量材料非线性光学性质的系统及方法。The present invention relates to the technical field of nonlinear optical measurement, and in particular to a system and method for measuring the nonlinear optical property of a material.

技术背景technical background

自1960年Maiman研制出世界上第一台红宝石激光器,激光科学与技术得到了飞速发展。在激光器问世的第二年(1961年),Franken等人发现光学二次谐波现象,标志着非线性光学作为一门新兴学科正式建立。Laser science and technology have developed rapidly since Maiman developed the world's first ruby laser in 1960. In 1961, the second year after the advent of the laser, Franken et al. discovered the optical second harmonic phenomenon, marking the formal establishment of nonlinear optics as an emerging discipline.

非线性吸收和非线性折射属于三阶非线性光学效应,是关于载流子在实际能级之间相互转换的非参量过程。尽管四波混频、干涉法和泵浦探测技术等可以实现三阶非线性吸收系数或非线性折射率的测量,但这些方法实验光路比较复杂,在实验过程和数据分析时需要克服许多困难。Z扫描技术是单光束测量材料非线性吸收和折射的最主要技术手段,该技术由Bahae等人于1990年率先提出,后来许多研究者加以改造,是目前测定光学非线性最简单、快捷、灵敏的实验方法。然而,传统Z扫描技术对样品要求较高,只适用于测试大尺寸均匀连续膜样品,对于小尺寸不规则样品很难实现定点测量。针对以上问题,Y.Li等人提出了显微非线性强度扫描系统,该系统对样品表面要求较低,可以测量不均匀样品,但该方法需要将样品放置在焦点位置,容易出现因焦点位置光斑面积测试不准确而造成较大系统误差,同时无法实现非线性折射信号的测试。Nonlinear absorption and nonlinear refraction belong to the third-order nonlinear optical effect, which is a nonparametric process about the mutual conversion of carriers between actual energy levels. Although four-wave mixing, interferometry and pump-probe technology can realize the measurement of third-order nonlinear absorption coefficient or nonlinear refractive index, the experimental optical path of these methods is relatively complex, and many difficulties need to be overcome in the experimental process and data analysis. Z scanning technology is the most important technical means for single-beam measurement of nonlinear absorption and refraction of materials. This technology was first proposed by Bahae et al. in 1990, and later many researchers have modified it. It is currently the simplest, fastest and most sensitive experimental method for measuring optical nonlinearity. However, the traditional Z scanning technology has high requirements for samples and is only suitable for testing large-sized uniform continuous film samples. It is difficult to achieve fixed-point measurement for small-sized irregular samples. In response to the above problems, Y. Li et al. proposed a microscopic nonlinear intensity scanning system. The system has low requirements for the sample surface and can measure non-uniform samples, but this method requires the sample to be placed at the focus position, which is prone to large system errors caused by inaccurate spot area testing at the focus position, and it is impossible to achieve the test of nonlinear refraction signals.

因此,现有技术还有待于改进和发展。Therefore, the prior art still needs to be improved and developed.

发明内容Summary of the invention

鉴于上述现有技术的不足,本发明的目的在于提供一种测量材料非线性光学性质的系统及方法,旨在解决现有技术难以实现对微米级样品的非线性光学性质进行测量的问题。In view of the above-mentioned deficiencies of the prior art, an object of the present invention is to provide a system and method for measuring the nonlinear optical properties of materials, aiming to solve the problem that the prior art is difficult to measure the nonlinear optical properties of micron-level samples.

本发明的技术方案如下:The technical solution of the present invention is as follows:

一种测量材料非线性光学性质的系统,其中,包括脉冲激光器、沿所述脉冲激光器的输出光束方向依次设置的第一镀膜全反镜、第二镀膜全反镜、圆形金属膜中性密度渐变滤光片、第一小孔光阑、第一分光平片、第二分光平片、聚焦物镜、待测样品、收集物镜、第二小孔光阑、第三分光平片、第二中型密度滤光片和第二探测器;沿所述第一分光平片的反射光方向依次设置有第一中性密度滤光片和第一探测器,沿所述第一分光平片的反射方向的另一侧设置有照明光源氙灯;沿所述第二分光平片的反射方向的另一侧设置有成像相机;沿所述第三分光平片的反射方向依次设置有第三小孔光阑、第三中性密度滤光片和第三探测器;还包括与所述第一探测器、第二探测器和第三探测器分别电连接的计算机;所述待测样品设置在三维精密平移台上,所述三维精密平移台通过控制器与所述计算机电连接;所述成像相机与所述计算机电连接。A system for measuring nonlinear optical properties of materials, comprising a pulse laser, a first film-coated total reflector, a second film-coated total reflector, a circular metal film neutral density gradient filter, a first pinhole diaphragm, a first beam splitter, a second beam splitter, a focusing objective lens, a sample to be measured, a collecting objective lens, a second pinhole diaphragm, a third beam splitter, a second medium density filter and a second detector; a first neutral density filter and a first detector are sequentially arranged along the direction of reflected light of the first beam splitter, and an illumination light source xenon lamp is arranged on the other side of the reflection direction of the first beam splitter; an imaging camera is arranged on the other side of the reflection direction of the second beam splitter; a third pinhole diaphragm, a third neutral density filter and a third detector are sequentially arranged along the reflection direction of the third beam splitter; a computer electrically connected to the first detector, the second detector and the third detector respectively is also included; the sample to be measured is arranged on a three-dimensional precision translation stage, and the three-dimensional precision translation stage is electrically connected to the computer through a controller; the imaging camera is electrically connected to the computer.

所述测量材料非线性光学性质的系统,其中,所述圆形金属膜中性密度渐变滤光片设置在电动旋转台上,所述电动旋转台通过控制器与所述计算机电连接。The system for measuring nonlinear optical properties of materials, wherein the circular metal film neutral density gradient filter is arranged on an electric rotating stage, and the electric rotating stage is electrically connected to the computer through a controller.

所述测量材料非线性光学性质的系统,其中,还包括与所述计算机电连接的能量计和光束质量分析仪。The system for measuring the nonlinear optical properties of a material further comprises an energy meter and a beam quality analyzer electrically connected to the computer.

所述测量材料非线性光学性质的系统,其中,所述第一镀膜全反镜、第二镀膜全反镜、第一分光平片、第二分光平片、第三分光平片与光轴夹角均为45°。The system for measuring the nonlinear optical properties of materials, wherein the angles between the first coated total reflector, the second coated total reflector, the first beam splitter, the second beam splitter, and the third beam splitter and the optical axis are all 45°.

所述测量材料非线性光学性质的系统,其中,所述第一分光平片对所述照明光源氙灯的分光比为50%。The system for measuring nonlinear optical properties of a material, wherein the splitting ratio of the first beam splitter to the illumination light source xenon lamp is 50%.

一种基于所述系统测量材料非线性光学性质的方法,其中,包括步骤:A method for measuring nonlinear optical properties of a material based on the system, comprising the steps of:

打开脉冲激光器,根据测量需要,选择激光波长、重复频率以及初始能量;Turn on the pulsed laser and select the laser wavelength, repetition frequency and initial energy according to the measurement requirements;

通过调整第一镀膜全反镜和第二镀膜全反镜使激光方向经过等高度第一小孔光阑和第二小孔光阑的中心;调整所述收集物镜使其焦点和聚焦物镜的焦点重合,同时保证所述聚焦物镜和收集物镜的中心与主光路重合;将能量计放置在聚焦物镜之后测量待测样品处激光能量;将所述光束质量分析仪放置在聚焦物镜焦点处测量激光束腰半径w0By adjusting the first coated total reflection mirror and the second coated total reflection mirror, the laser direction passes through the center of the first pinhole aperture and the second pinhole aperture of equal height; adjusting the collecting objective lens so that its focus coincides with the focus of the focusing objective lens, and at the same time ensuring that the centers of the focusing objective lens and the collecting objective lens coincide with the main light path; placing an energy meter behind the focusing objective lens to measure the laser energy at the sample to be tested; placing the beam quality analyzer at the focus of the focusing objective lens to measure the laser beam waist radius w 0 ;

将待测样品放置在样品架上,调节待测样品使其表面与主光路垂直,调节三维精密平移台z轴使待测样品在成像相机处形成清晰像,调节三维精密平移台x轴和y轴找到测试目标;Place the sample to be tested on the sample holder, adjust the sample to be tested so that its surface is perpendicular to the main light path, adjust the z-axis of the three-dimensional precision translation stage so that the sample to be tested forms a clear image at the imaging camera, and adjust the x-axis and y-axis of the three-dimensional precision translation stage to find the test target;

定义激光传播方向为z轴正方向,聚焦物镜焦点位置为z=0,沿负方向移动待测样品至光斑边缘与待测样品边缘重合,位置记为-z0,通过计算机设置所述电动旋转台的转动参数,包括初始角度θ0、终止角度θ和转动步长Δθ,所述电动旋转台每转动一个角度θi对应一个能量E1θi,其中,θi=θ0+i*Δθ,i=0,1,2,...,[(θ-θ0)/Δθ],E1θi随着θi的增大逐渐减小,利用公式和/>计算得到z1θi,所述第一探测器、第二探测器和第三探测器将探测到的能量信号输入到所述计算机中,测量完毕后电动旋转台的角度重新回到初始角度θ0Define the laser propagation direction as the positive direction of the z-axis, the focal position of the focusing lens as z=0, move the sample to be measured along the negative direction until the edge of the light spot coincides with the edge of the sample to be measured, and record the position as -z 0 . Set the rotation parameters of the electric rotating stage by a computer, including the initial angle θ 0 , the end angle θ and the rotation step Δθ. Each rotation of the electric rotating stage by an angle θ i corresponds to an energy E 1θi , wherein θ i0 +i*Δθ, i=0, 1, 2, ..., [(θ-θ 0 )/Δθ], and E 1θi gradually decreases as θ i increases. Use the formula and/> z 1θi is calculated, and the first detector, the second detector and the third detector input the detected energy signals into the computer. After the measurement is completed, the angle of the electric rotating stage returns to the initial angle θ 0 ;

通过计算机启动三维精密平移台,设置z轴移动参数,使待测样品移动范围在-z0到z0之间,所述精密平移台z轴每移动一定距离zi,zi=-z0+i*Δz,i=0,1,2,...,[2z0/Δz],所述第一探测器、第二探测器和第三探测器将探测到的能量信号输入到所述计算机中,测量完毕后所述精密平移台使样品移动到z0位置;The three-dimensional precision translation stage is started by a computer, and the z-axis movement parameters are set so that the movement range of the sample to be measured is between -z 0 and z 0. When the z-axis of the precision translation stage moves a certain distance z i , z i = -z 0 +i*Δz, i = 0, 1, 2, ..., [2z 0 /Δz], the first detector, the second detector and the third detector input the detected energy signals into the computer. After the measurement is completed, the precision translation stage moves the sample to the z 0 position;

通过计算机设置所述电动旋转台的转动参数,包括初始角度θ0、终止角度θ和转动步长Δθ,所述电动旋转台每转动一个角度θi对应一个能量E2θi,其中,θi=θ0+i*Δθ,i=0,1,2,...,[(θ-θ0)/Δθ],利用公式和/>计算得到E2θi,所述第一探测器、第二探测器和第三探测器将探测到的能量信号输入到所述计算机中;The rotation parameters of the electric rotating stage are set by a computer, including an initial angle θ 0 , an end angle θ and a rotation step Δθ. Each rotation of the electric rotating stage by an angle θ i corresponds to an energy E 2θi , wherein θ i0 +i*Δθ, i = 0, 1, 2, ..., [(θ-θ 0 )/Δθ], and the formula is used. and/> E 2θi is obtained by calculation, and the first detector, the second detector and the third detector input the detected energy signals into the computer;

第一探测器得到的能量信号为参考光信号,第二探测器与第一探测器的能量信号比值为透射开孔信号,第三探测器与透射开孔信号的比值为透射闭孔信号;以上述步骤中记录的z1θi、zi、z2θi为横坐标,以所述透射开孔信号为纵坐标,所绘曲线为待测样品的开孔非线性透过率曲线Topen(z),即非线性吸收信号;以移动距离zi为横坐标,以所述透射闭孔信号为纵坐标,所绘曲线为样品的闭孔非线性透过率曲线Tclosed(z),即非线性折射信号;The energy signal obtained by the first detector is the reference light signal, the ratio of the energy signal of the second detector to the first detector is the transmission open-pore signal, and the ratio of the energy signal of the third detector to the transmission open-pore signal is the transmission closed-pore signal; the z1θi , zi , z2θi recorded in the above steps are used as the horizontal coordinates, and the transmission open-pore signal is used as the vertical coordinate, and the plotted curve is the open-pore nonlinear transmittance curve T open (z) of the sample to be tested, that is, the nonlinear absorption signal; the moving distance z i is used as the horizontal coordinate, and the transmission closed-pore signal is used as the vertical coordinate, and the plotted curve is the closed-pore nonlinear transmittance curve T closed (z) of the sample, that is, the nonlinear refraction signal;

利用公式x=z/z0,/>对所述开孔非线性透过率曲线Topen(z)进行拟合,得到待测样品的非线性吸收系数β,其中k为波数,L为待测样品厚度,α0为线性吸收系数,z0为瑞利长度,I0为焦点处的轴上强度,w0为高斯光束的束腰半径;利用公式/>ΔΦ0=k·Δn(0,0)·Leff,/>对所述闭孔非线性透过率曲线Tclosed(z)进行拟合,得到待测样品的非线性折射率n2,其中n0为线性折射率。Using the formula x=z/z 0 ,/> The nonlinear transmittance curve T open (z) of the open hole is fitted to obtain the nonlinear absorption coefficient β of the sample to be tested, where k is the wave number, L is the thickness of the sample to be tested, α 0 is the linear absorption coefficient, z 0 is the Rayleigh length, I 0 is the axial intensity at the focus, and w 0 is the waist radius of the Gaussian beam; using the formula /> ΔΦ 0 = k·Δn(0,0)·L eff ,/> The closed-hole nonlinear transmittance curve T closed (z) is fitted to obtain the nonlinear refractive index n 2 of the sample to be tested, wherein n 0 is the linear refractive index.

有益效果:本发明基于Z扫描技术和共焦显微成像技术,突破了样品尺寸限制,实现了微区测量材料的非线性光学性质;该系统实现了自动化控制,具有集成度高、简单、灵敏、快速的特点;该系统采用显微物镜进行激发光聚焦、信号光收集、样品表面形貌成像以及光斑同步成像,可以实现光斑大小的实时监测;使用三维精密平移台控制样品位置,可以实现对微米级样品非线性光学性质的测量,解决了非均匀不规则小尺寸样品非线性性质测试难题,扩展了Z扫描技术的应用及测试范围。Beneficial effects: The present invention is based on Z scanning technology and confocal microscopy technology, which breaks through the sample size limitation and realizes the micro-area measurement of the nonlinear optical properties of materials; the system realizes automatic control and has the characteristics of high integration, simplicity, sensitivity and speed; the system uses a microscope objective to focus the excitation light, collect the signal light, image the sample surface morphology and synchronously image the light spot, which can realize real-time monitoring of the light spot size; the use of a three-dimensional precision translation stage to control the sample position can realize the measurement of the nonlinear optical properties of micron-level samples, solves the problem of testing the nonlinear properties of non-uniform and irregular small-sized samples, and expands the application and test scope of the Z scanning technology.

附图说明BRIEF DESCRIPTION OF THE DRAWINGS

图1为本发明一种测量材料非线性光学性质的系统结构示意图。FIG. 1 is a schematic diagram of the structure of a system for measuring nonlinear optical properties of a material according to the present invention.

具体实施方式Detailed ways

本发明提供了一种测量材料非线性光学性质的系统及方法,为使本发明的目的、技术方案及效果更加清楚、明确,以下对本发明进一步详细说明。应当理解,此处所描述的具体实施例仅用以解释本发明,并不用于限定本发明。The present invention provides a system and method for measuring the nonlinear optical properties of a material. To make the purpose, technical solution and effect of the present invention clearer and more specific, the present invention is further described in detail below. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

请参阅图1,图1为本发明提供的一种测量材料非线性光学性质的系统结构示意图,如图所示,其包括脉冲激光器10、沿所述脉冲激光器10的输出光束方向依次设置的第一镀膜全反镜20、第二镀膜全反镜30、圆形金属膜中性密度渐变滤光片40、第一小孔光阑50、第一分光平片60、第二分光平片70、聚焦物镜80、待测样品90、收集物镜100、第二小孔光阑110、第三分光平片120、第二中型密度滤光片130和第二探测器140;沿所述第一分光平片60的反射光方向依次设置有第一中性密度滤光片61和第一探测器62,沿所述第一分光平片60的反射方向的另一侧设置有照明光源氙灯63;沿所述第二分光平片70的反射方向的另一侧设置有成像相机71;沿所述第三分光平片120的反射方向依次设置有第三小孔光阑121、第三中性密度滤光片122和第三探测器123;还包括与所述第一探测器62、第二探测器140和第三探测器123分别电连接的计算机150;所述待测样品90设置在三维精密平移台91上,所述三维精密平移台91通过控制器与所述计算机150电连接;所述成像相机71与所述计算机150电连接。Please refer to FIG1 , which is a schematic diagram of the structure of a system for measuring the nonlinear optical properties of a material provided by the present invention. As shown in the figure, the system comprises a pulse laser 10, a first coated total reflector 20, a second coated total reflector 30, a circular metal film neutral density gradient filter 40, a first pinhole diaphragm 50, a first beam splitter plate 60, a second beam splitter plate 70, a focusing objective lens 80, a sample to be measured 90, a collecting objective lens 100, a second pinhole diaphragm 110, a third beam splitter plate 120, a second medium density filter 130, and a second detector 140; a first neutral density filter 61 and a second neutral density filter 62 are sequentially arranged along the direction of the reflected light of the first beam splitter plate 60; A detector 62 is provided, and a xenon lamp 63 is provided as an illumination light source along the other side of the reflection direction of the first spectroscopic plate 60; an imaging camera 71 is provided along the other side of the reflection direction of the second spectroscopic plate 70; a third pinhole diaphragm 121, a third neutral density filter 122 and a third detector 123 are provided in sequence along the reflection direction of the third spectroscopic plate 120; a computer 150 is also provided which is electrically connected to the first detector 62, the second detector 140 and the third detector 123 respectively; the sample to be tested 90 is provided on a three-dimensional precision translation stage 91, and the three-dimensional precision translation stage 91 is electrically connected to the computer 150 through a controller; the imaging camera 71 is electrically connected to the computer 150.

本实施例提供的系统还包括与所述计算机150电连接的能量计160和光束质量分析仪170。在本实施例中,所述圆形金属膜中性密度渐变滤光片40设置在电动旋转台41上,所述电动旋转台41通过控制器与所述计算机150电连接。在本实施例中,所述第一镀膜全反镜20、第二镀膜全反镜30、第一分光平片60、第二分光平片70、第三分光平片120与光轴夹角均为45°。所述第一分光平片60对所述照明光源氙灯63的分光比为50%。The system provided in this embodiment also includes an energy meter 160 and a beam quality analyzer 170 electrically connected to the computer 150. In this embodiment, the circular metal film neutral density gradient filter 40 is set on an electric rotating table 41, and the electric rotating table 41 is electrically connected to the computer 150 through a controller. In this embodiment, the angle between the first coated total reflector 20, the second coated total reflector 30, the first beam splitter plate 60, the second beam splitter plate 70, and the third beam splitter plate 120 and the optical axis is 45°. The first beam splitter plate 60 has a beam splitting ratio of 50% for the illumination light source xenon lamp 63.

本实施例通过对传统Z扫描技术进行改进,结合显微强度扫描系统的优点,提出了一种测量材料非线性光学性质的系统,该系统采用显微物镜进行激发光聚焦、信号光收集以及光斑同步成像,使用三维精密平移台控制待测样品位置,从而可以对微米级样品材料的非线性光学性质进行测量。基于该系统可在非线性光学性质测量前定位显微待测样品位置,测量过程中实时监测光斑大小,突破了待测样品尺寸的限制,对待测样品表面要求较低,可以测量显微小尺寸透明和半透明不规则样品的非线性光学性质。本实施例提供的系统还实现了自动化控制,具有集成度高、简单、灵敏、快速的特点。This embodiment improves the traditional Z scanning technology and combines the advantages of the microscopic intensity scanning system to propose a system for measuring the nonlinear optical properties of materials. The system uses a microscope objective to focus the excitation light, collect the signal light, and synchronously image the light spot. A three-dimensional precision translation stage is used to control the position of the sample to be tested, so that the nonlinear optical properties of micron-level sample materials can be measured. Based on this system, the position of the microscopic sample to be tested can be located before the nonlinear optical property measurement, and the size of the light spot can be monitored in real time during the measurement process, breaking through the limitation of the size of the sample to be tested. The surface requirements of the sample to be tested are relatively low, and the nonlinear optical properties of micro-sized transparent and translucent irregular samples can be measured. The system provided in this embodiment also realizes automatic control and has the characteristics of high integration, simplicity, sensitivity, and speed.

基于所述系统,本发明实施方式还提供了一种测量材料非线性光学性质的方法,主要是测得待测样品的非线性透过率数据和非线性折射率数据,然后对非线性透过率数据和非线性折射率数据分别进行拟合获得待测样品的非线性吸收系数β和非线性折射率n2,其包括以下步骤:Based on the system, the embodiment of the present invention also provides a method for measuring the nonlinear optical properties of a material, which mainly measures the nonlinear transmittance data and the nonlinear refractive index data of the sample to be measured, and then respectively fits the nonlinear transmittance data and the nonlinear refractive index data to obtain the nonlinear absorption coefficient β and the nonlinear refractive index n 2 of the sample to be measured, which includes the following steps:

打开脉冲激光器,根据测量需要,选择激光波长、重复频率以及初始能量;Turn on the pulsed laser and select the laser wavelength, repetition frequency and initial energy according to the measurement requirements;

通过调整第一镀膜全反镜和第二镀膜全反镜使激光方向经过等高度第一小孔光阑和第二小孔光阑的中心;调整所述收集物镜使其焦点和聚焦物镜的焦点重合,同时保证所述聚焦物镜和收集物镜的中心与主光路重合;将能量计放置在聚焦物镜之后测量待测样品处激光能量;将所述光束质量分析仪放置在聚焦物镜焦点处测量激光束腰半径w0By adjusting the first coated total reflection mirror and the second coated total reflection mirror, the laser direction passes through the center of the first pinhole aperture and the second pinhole aperture of equal height; adjusting the collecting objective lens so that its focus coincides with the focus of the focusing objective lens, and at the same time ensuring that the centers of the focusing objective lens and the collecting objective lens coincide with the main light path; placing an energy meter behind the focusing objective lens to measure the laser energy at the sample to be tested; placing the beam quality analyzer at the focus of the focusing objective lens to measure the laser beam waist radius w 0 ;

将待测样品放置在样品架上,调节待测样品使其表面与主光路垂直,调节三维精密平移台z轴使待测样品在成像相机处形成清晰像,调节三维精密平移台x轴和y轴找到测试目标;Place the sample to be tested on the sample holder, adjust the sample to be tested so that its surface is perpendicular to the main light path, adjust the z-axis of the three-dimensional precision translation stage so that the sample to be tested forms a clear image at the imaging camera, and adjust the x-axis and y-axis of the three-dimensional precision translation stage to find the test target;

定义激光传播方向为z轴正方向,聚焦物镜焦点位置为z=0,沿负方向移动待测样品至光斑边缘与待测样品边缘重合,位置记为-z0,通过计算机设置所述电动旋转台的转动参数,包括初始角度θ0、终止角度θ和转动步长Δθ,所述电动旋转台每转动一个角度θi对应一个能量E1θi,其中,θi=θ0+i*Δθ,i=0,1,2,...,[(θ-θ0)/Δθ],E1θi随着θi的增大逐渐减小,利用公式和/>十算得到z1θi,所述第一探测器、第二探测器和第三探测器将探测到的能量信号输入到所述计算机中,测量完毕后电动旋转台的角度重新回到初始角度θ0Define the laser propagation direction as the positive direction of the z-axis, the focal position of the focusing lens as z=0, move the sample to be measured along the negative direction until the edge of the light spot coincides with the edge of the sample to be measured, and record the position as -z 0 . Set the rotation parameters of the electric rotating stage by a computer, including the initial angle θ 0 , the end angle θ and the rotation step Δθ. Each rotation of the electric rotating stage by an angle θ i corresponds to an energy E 1θi , wherein θ i0 +i*Δθ, i=0, 1, 2, ..., [(θ-θ 0 )/Δθ], and E 1θi gradually decreases as θ i increases. Use the formula and/> The first detector, the second detector and the third detector input the detected energy signals into the computer. After the measurement is completed, the angle of the electric rotating stage returns to the initial angle θ 0 ;

通过计算机启动三维精密平移台,设置z轴移动参数,使待测样品移动范围在-z0到z0之间,所述精密平移台z轴每移动一定距离zi,zi=-z0+i*Δz,i=0,1,2,...,[2z0/Δz],所述第一探测器、第二探测器和第三探测器将探测到的能量信号输入到所述计算机中,测量完毕后所述精密平移台使样品移动到z0位置;The three-dimensional precision translation stage is started by a computer, and the z-axis movement parameters are set so that the movement range of the sample to be measured is between -z 0 and z 0. When the z-axis of the precision translation stage moves a certain distance z i , z i = -z 0 +i*Δz, i = 0, 1, 2, ..., [2z 0 /Δz], the first detector, the second detector and the third detector input the detected energy signals into the computer. After the measurement is completed, the precision translation stage moves the sample to the z 0 position;

通过计算机设置所述电动旋转台的转动参数,包括初始角度θ0、终止角度θ和转动步长Δθ,所述电动旋转台每转动一个角度θi对应一个能量E2θi,其中,θi=θ0+i*Δθ,i=0,1,2,...,[(θ-θ0)/Δθ],利用公式和/>计算得到E2θi,所述第一探测器、第二探测器和第三探测器将探测到的能量信号输入到所述计算机中;The rotation parameters of the electric rotating stage are set by a computer, including an initial angle θ 0 , an end angle θ and a rotation step Δθ. Each rotation of the electric rotating stage by an angle θ i corresponds to an energy E 2θi , wherein θ i0 +i*Δθ, i = 0, 1, 2, ..., [(θ-θ 0 )/Δθ], and the formula is used. and/> E 2θi is obtained by calculation, and the first detector, the second detector and the third detector input the detected energy signals into the computer;

第一探测器得到的能量信号为参考光信号,第二探测器与第一探测器的能量信号比值为透射开孔信号,第三探测器的能量信号与透射开孔信号的比值为透射闭孔信号;以上述步骤中记录的z1θi、zi、z2θi为横坐标,以所述透射开孔信号为纵坐标,所绘曲线为待测样品的开孔非线性透过率曲线Topen(z),即非线性吸收信号;以移动距离zi为横坐标,以所述透射闭孔信号为纵坐标,所绘曲线为样品的闭孔非线性透过率曲线Tc1osed(z),即非线性折射信号;The energy signal obtained by the first detector is the reference light signal, the ratio of the energy signal of the second detector to the first detector is the transmission open-pore signal, and the ratio of the energy signal of the third detector to the transmission open-pore signal is the transmission closed-pore signal; the z1θi , zi , z2θi recorded in the above steps are used as the horizontal coordinates, and the transmission open-pore signal is used as the vertical coordinate, and the plotted curve is the open-pore nonlinear transmittance curve T open (z) of the sample to be tested, that is, the nonlinear absorption signal; the moving distance z i is used as the horizontal coordinate, and the transmission closed-pore signal is used as the vertical coordinate, and the plotted curve is the closed-pore nonlinear transmittance curve T c1osed (z) of the sample, that is, the nonlinear refraction signal;

利用公式x=z/z0,/>对所述开孔非线性透过率曲线Topen(z)进行拟合,得到待测样品的非线性吸收系数β,其中k为波数,L为待测样品厚度,α0为线性吸收系数,z0为瑞利长度,I0为焦点处的轴上强度,w0为高斯光束的束腰半径,q0和q00的引入是在计算过程中为了让公式更简化,没有具体物理含义;利用公式/>ΔΦ0=k·Δn(0,0)·Leff对所述闭孔非线性透过率曲线Tclosed(z)进行拟合,得到待测样品的非线性折射率n2,其中n0为线性折射率。Using the formula x=z/z 0 ,/> The nonlinear transmittance curve T open (z) of the open hole is fitted to obtain the nonlinear absorption coefficient β of the sample to be tested, where k is the wave number, L is the thickness of the sample to be tested, α 0 is the linear absorption coefficient, z 0 is the Rayleigh length, I 0 is the axial intensity at the focus, w 0 is the waist radius of the Gaussian beam, and q 0 and q 00 are introduced in the calculation process to simplify the formula and have no specific physical meaning; using the formula /> ΔΦ 0 = k·Δn(0,0)·L eff , The closed-hole nonlinear transmittance curve T closed (z) is fitted to obtain the nonlinear refractive index n 2 of the sample to be tested, wherein n 0 is the linear refractive index.

本实施例提供的方法结合了传统Z扫描技术和显微强度扫描技术,利用显微物镜进行激发光聚集、信号光收集、样品表面形貌成像以及光斑同步成像,实现了光斑大小的实时监测;同时使用三维精密平移台控制待测样品位置,实现了对微米级样品的非线性光学性质的测量(包括非线性透过率数据和非线性折射率数据),解决了非均匀不规则微米级小尺寸样品非线性性质测试难题,扩展了Z扫描技术的应用及测试范围。The method provided in this embodiment combines the traditional Z scanning technology and the microscopic intensity scanning technology, and utilizes the microscope objective to focus the excitation light, collect the signal light, image the sample surface morphology, and synchronously image the light spot, thereby realizing the real-time monitoring of the light spot size. At the same time, a three-dimensional precision translation stage is used to control the position of the sample to be tested, thereby realizing the measurement of the nonlinear optical properties of micron-level samples (including nonlinear transmittance data and nonlinear refractive index data), solving the problem of testing the nonlinear properties of non-uniform and irregular micron-level small-size samples, and expanding the application and test scope of the Z scanning technology.

应当理解的是,本发明的应用不限于上述的举例,对本领域普通技术人员来说,可以根据上述说明加以改进或变换,所有这些改进和变换都应属于本发明所附权利要求的保护范围。It should be understood that the application of the present invention is not limited to the above examples. For ordinary technicians in this field, improvements or changes can be made based on the above description. All these improvements and changes should fall within the scope of protection of the claims attached to the present invention.

Claims (6)

1. The system for measuring the nonlinear optical property of the material is characterized by comprising a pulse laser, a first film plating total reflection mirror, a second film plating total reflection mirror, a circular metal film neutral density gradient filter, a first aperture diaphragm, a first beam splitting flat plate, a second beam splitting flat plate, a focusing objective lens, a sample to be measured, a collecting objective lens, a second aperture diaphragm, a third beam splitting flat plate, a second medium-sized density filter and a second detector which are sequentially arranged along the direction of an output beam of the pulse laser; a first neutral density filter and a first detector are sequentially arranged along the reflecting light direction of the first light splitting flat sheet, and an illumination light source xenon lamp is arranged along the other side of the reflecting direction of the first light splitting flat sheet; an imaging camera is arranged along the other side of the reflection direction of the second beam splitting flat sheet; a third aperture diaphragm, a third neutral density filter and a third detector are sequentially arranged along the reflection direction of the third light splitting flat sheet; the computer is electrically connected with the first detector, the second detector and the third detector respectively; the sample to be measured is arranged on a three-dimensional precise translation stage, and the three-dimensional precise translation stage is electrically connected with the computer through a controller; the imaging camera is electrically connected with the computer.
2. The system for measuring nonlinear optical properties of a material according to claim 1, wherein the circular metal film neutral density graded filter is disposed on an motorized rotary stage, the motorized rotary stage being electrically connected to the motorized rotary stage by a controller.
3. The system for measuring a nonlinear optical property of a material in accordance with claim 1, further comprising an energy meter and a beam quality analyzer electrically connected to said electrode.
4. The system for measuring nonlinear optical properties of a material according to claim 1, wherein the first coated total reflection mirror, the second coated total reflection mirror, the first beam splitting plate, the second beam splitting plate, and the third beam splitting plate are all at an angle of 45 ° to the optical axis.
5. The system for measuring nonlinear optical properties of a material according to claim 1, wherein the first light splitting plane has a 50% split ratio to the illumination source xenon lamp.
6. A method of measuring nonlinear optical properties of a material based on the system of any one of claims 1-5, comprising the steps of:
turning on a pulse laser, and selecting laser wavelength, repetition frequency and initial energy according to measurement requirements;
the laser direction passes through the centers of the first aperture diaphragm and the second aperture diaphragm with equal heights by adjusting the first film plating total reflection mirror and the second film plating total reflection mirror; adjusting the collecting objective lens to enable the focus of the collecting objective lens to coincide with the focus of the focusing objective lens, and simultaneously ensuring that the centers of the focusing objective lens and the collecting objective lens coincide with a main light path; placing an energy meter behind a focusing objective lens to measure laser energy at a sample to be measured; the beam quality analyzer is placed at the focus of the focusing objective lens to measure the laser beam waist radius w 0
Placing a sample to be tested on a sample frame, adjusting the sample to be tested to enable the surface of the sample to be tested to be perpendicular to a main light path, adjusting the z axis of a three-dimensional precise translation stage to enable the sample to be tested to form a clear image at an imaging camera, and adjusting the x axis and the y axis of the three-dimensional precise translation stage to find a test target;
defining the laser propagation direction as the positive direction of the z axis, the focal position of the focusing objective lens as z=0, moving the sample to be detected along the negative direction until the light spot edge coincides with the edge of the sample to be detected, and recording the position as-z 0 Setting rotation parameters of the electric rotating table through a computer, wherein the rotation parameters comprise an initial angle theta 0 A termination angle theta and a rotation step delta theta, wherein each rotation of the electric rotating table is one angle theta i Corresponding to one energy E 1θi Wherein θ i =θ 0 +i*Δθ,i=0,1,2,…,[(θ-θ 0 )/Δθ],E 1θi With theta i Gradually decreasing in increase of (c) using the formulaAnd->Calculating to obtain z 1θi The first detector, the second detector and the third detector input the detected energy signals into the computer, and the angle of the electric rotating table returns to the initial angle theta after the measurement is finished 0
Starting a three-dimensional precise translation stage through a computer, setting a z-axis movement parameter to enable the movement range of a sample to be measured to be-z 0 To z 0 Each time the z axis of the precise translation stage moves a certain distance z i ,z i =-z 0 +i*Δz,i=0,1,2,…,[2z 0 /Δz]The first detector, the second detector and the third detector input detected energy signals into the computer, and the precise translation stage moves the sample to z after the measurement is finished 0 A location;
setting rotation parameters of the electric rotating table through a computer, wherein the rotation parameters comprise an initial angle theta 0 A termination angle theta and a rotation step delta theta, wherein each rotation of the electric rotating table is one angle theta i Corresponding to one energy E 2θi Wherein θ i =θ 0 +i*Δθ,i=0,1,2,…,[(θ-θ 0 )/Δθ]Using the formulaAnd->E is calculated to obtain 2θi The first detector, the second detector and the third detector input detected energy signals into the computer;
the energy signal obtained by the first detector is a reference light signal, the ratio of the energy signal of the second detector to that of the first detector is a transmission open hole signal, and the ratio of the energy signal of the third detector to that of the transmission open hole signal is transmissionA closed cell signal; z recorded in the above step 1θi 、z i 、z 2θi Taking the transmission open pore signal as an ordinate and the plotted curve as an open pore nonlinear transmittance curve T of a sample to be measured open (z), i.e. nonlinear absorption signals; at a moving distance z i On the abscissa, the transmission closed cell signal is taken as the ordinate, and the plotted curve is a closed cell nonlinear transmittance curve T of a sample closed (z), i.e. a nonlinear refractive signal;
using the formulax=z/z 0Nonlinear transmittance curve T for the aperture open (z) fitting to obtain nonlinear absorption coefficient beta of the sample to be measured, wherein k is wave number, L is thickness of the sample to be measured, and alpha 0 Is a linear absorption coefficient, z 0 For Rayleigh length, I 0 Is the on-axis intensity at the focus, w 0 Is the beam waist radius of the Gaussian beam; using the formula->ΔΦ 0 =k·Δn(0,0)·L eff ,/>A nonlinear transmittance curve T for the closed cells closed (z) fitting to obtain nonlinear refractive index n of the sample to be measured 2 Wherein n is 0 Is a linear refractive index.
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