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CN115078279A - A differential reflection detection method and device suitable for variable temperature environment - Google Patents

A differential reflection detection method and device suitable for variable temperature environment Download PDF

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CN115078279A
CN115078279A CN202210722008.3A CN202210722008A CN115078279A CN 115078279 A CN115078279 A CN 115078279A CN 202210722008 A CN202210722008 A CN 202210722008A CN 115078279 A CN115078279 A CN 115078279A
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temperature
split
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王译那
郭迎庆
张雷
徐赵东
隋青美
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Nanjing Forestry University
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Abstract

The invention relates to a differential reflection detection method suitable for a variable-temperature environment, which is characterized in that a first light split and a second light split which have the same wavelength and the same intensity and are obtained based on light split of light emitted by a light source (1) are switched and controlled according to a first substrate (4) in a temperature-controllable environment, the first light split and the second light split are sequentially reflected by the first substrate (4) and reflected by a two-dimensional sample to be detected arranged on the surface of a second substrate (5) in a sample chamber (3), and structural feature detection of the two-dimensional sample to be detected is realized according to an absorption feature spectrum of a standard product corresponding to the two-dimensional sample to be detected through differential operation between the obtained first detection light reflection light intensity information and the second detection light reflection light intensity information; the design method has the advantages of strong temperature interference resistance and good environmental adaptability; and the device for realizing the method is further designed, and the working efficiency of the structural characteristic detection of the sample to be detected can be further improved through the modular light path layout structure design.

Description

一种适用于变温环境的差分反射检测方法及装置A differential reflection detection method and device suitable for variable temperature environment

技术领域technical field

本发明涉及一种适用于变温环境的差分反射检测方法及装置,属于光学表征及检测仪器技术领域。The invention relates to a differential reflection detection method and device suitable for a variable temperature environment, belonging to the technical field of optical characterization and detection instruments.

背景技术Background technique

光学检测仪器及其技术在材料特性表征、材料生长原位监测等方面,具有举足轻重的作用,它的发展有利于探究材料的性质,制备高质量材料。差分反射检测是利用不同状态下样品反射光的变化,得到被测对象的光谱信息,通过分析光子能量与反射光变化量之间的关系,从而判断被测对象结构特征和所处状态的光学检测技术。它具有快速、无损、灵敏度高、非接触等特点,特别适合材料生长原位监测。Optical detection instruments and their technologies play a pivotal role in the characterization of material properties and in-situ monitoring of material growth. Its development is conducive to exploring the properties of materials and preparing high-quality materials. Differential reflection detection is an optical detection method that uses the changes of the reflected light of the sample under different states to obtain the spectral information of the measured object, and analyzes the relationship between the photon energy and the amount of reflected light change to judge the structural characteristics and state of the measured object. technology. It has the characteristics of fast, non-destructive, high sensitivity and non-contact, and is especially suitable for in-situ monitoring of material growth.

目前常见的材料特性光学检测仪器,包括光学显微镜、原子力显微镜、透射电子显微镜、扫描电子显微镜、拉曼光谱仪等,但它们在不同程度上存在一定的缺陷。光学显微镜检测简单快速,但检测精度低、检测空间有限;原子力显微镜检测精度高,但检测范围有限;透射电子显微镜分辨率高,但对检测环境要求极高;扫描电子显微镜的检测分辨率高、直观,但会破坏样品结构;拉曼光谱仪检测速度快、检测方法简单,但检测结构复杂。At present, common optical testing instruments for material properties, including optical microscopes, atomic force microscopes, transmission electron microscopes, scanning electron microscopes, Raman spectrometers, etc., have certain defects to varying degrees. Optical microscope detection is simple and fast, but the detection accuracy is low and the detection space is limited; atomic force microscopy has high detection accuracy, but the detection range is limited; transmission electron microscope has high resolution, but requires extremely high detection environment; scanning electron microscope has high detection resolution, Intuitive, but it will destroy the sample structure; Raman spectrometer has fast detection speed and simple detection method, but the detection structure is complex.

综述所述,以上检测仪器和技术存在明显的不足,很难应用在材料原位监测;另外,在许多试验条件,试验温度并不是一成不变的,变温的环境会对材料基底的性质产生影响,从而对检测结果产生误差。由于现有检测装置存在的不足,开发一种适用于变温环境的检测装置及其试验方法具有重要意义。As mentioned in the review, the above detection instruments and technologies have obvious shortcomings, and it is difficult to apply them to in-situ monitoring of materials; in addition, in many test conditions, the test temperature is not static, and the changing temperature environment will have an impact on the properties of the material substrate, thus error in the test results. Due to the shortcomings of the existing detection devices, it is of great significance to develop a detection device and a test method suitable for the variable temperature environment.

发明内容SUMMARY OF THE INVENTION

本发明所要解决的技术问题是提供一种适用于变温环境的差分反射检测方法,基于光源下的分光操作,结合温度可控环境下的第一基底,针对样品室内第二基底表面所设的二维待测样品进行结构特征检测。The technical problem to be solved by the present invention is to provide a differential reflection detection method suitable for a variable temperature environment. Based on the spectroscopic operation under the light source, combined with the first substrate in a temperature-controlled environment, for the second substrate set on the surface of the second substrate in the sample chamber Structural feature detection of the sample to be tested.

本发明为了解决上述技术问题采用以下技术方案:本发明设计了一种适用于变温环境的差分反射检测方法,基于光源与光谱仪,根据温度可控环境下的第一基底,按如下步骤A至步骤F,针对样品室内第二基底表面所设的二维待测样品进行结构特征检测;In order to solve the above technical problems, the present invention adopts the following technical solutions: The present invention designs a differential reflection detection method suitable for a variable temperature environment, based on a light source and a spectrometer, and according to the first substrate in a temperature-controlled environment, according to the following steps A to steps F, performing structural feature detection on the two-dimensional sample to be tested set on the surface of the second substrate in the sample chamber;

步骤A.针对光源的出射光进行分光,获得彼此波长相同、强度相同的第一分光与第二分光,并进入步骤B;Step A. Splitting the light emitted from the light source, obtaining a first splitting light and a second splitting light with the same wavelength and the same intensity, and entering step B;

步骤B.基于样品室内温度恒定的时长t,阻挡第一分光,同时控制第二分光射向第二基底表面所设的二维待测样品表面,通过反射产生第二检测光,由光谱仪接收端接收该第二检测光,并保持此状态持续时长t,以及获得此状态下样品室内的温度T,然后进入步骤C;Step B. Based on the constant time duration t of the temperature in the sample chamber, block the first light split, while controlling the second light split to be directed to the surface of the two-dimensional sample to be tested set on the surface of the second substrate, and generate the second detection light through reflection, which is transmitted by the receiving end of the spectrometer. Receive the second detection light, keep this state for a duration t, and obtain the temperature T in the sample chamber in this state, and then enter step C;

步骤C.控制第一基底所处环境的温度为温度T,并阻挡第二分光,同时控制第一分光射向第一基底表面,通过反射产生第一检测光,由光谱仪接收端接收该第一检测光,并保持此状态持续时长t,然后进入步骤D;Step C. Control the temperature of the environment where the first substrate is located to be temperature T, and block the second light splitting, while controlling the first splitting light to be directed to the surface of the first substrate, generating the first detection light by reflection, and receiving the first light by the spectrometer receiving end. Detect light, keep this state for a duration of t, and then enter step D;

步骤D.光谱仪针对接收到的第二检测光、第一检测光,分别检测获得第二检测光所对应的反射光强信息R2、第一检测光所对应的反射光强信息R1,并进入步骤E;Step D. The spectrometer respectively detects and obtains the reflected light intensity information R 2 corresponding to the second detection light and the reflected light intensity information R 1 corresponding to the first detection light for the received second detection light and the first detection light, and obtains the reflected light intensity information R 1 corresponding to the first detection light. Enter step E;

步骤E.根据如下公式进行差分运算;Step E. carry out differential operation according to the following formula;

Figure BDA0003699866710000021
Figure BDA0003699866710000021

获得二维待测样品所对应的吸收光谱Δ,即样品光吸收特性与波长的关系,并进入步骤F;Obtain the absorption spectrum Δ corresponding to the two-dimensional sample to be tested, that is, the relationship between the light absorption characteristics of the sample and the wavelength, and enter step F;

步骤F.根据二维待测样品所对应标准品的吸收特征光谱,针对二维待测样品所对应的光吸收特性与波长光谱进行分析,即实现对二维待测样品的结构特征检测。Step F. According to the absorption characteristic spectrum of the standard corresponding to the two-dimensional test sample, analyze the light absorption characteristics and wavelength spectrum corresponding to the two-dimensional test sample, that is, realize the structural feature detection of the two-dimensional test sample.

作为本发明的一种优选技术方案:所述步骤A中,首先针对光源的出射光进行处理,获得平行光,然后针对该平行光进行分光,获得彼此波长相同、强度相同的第一分光与第二分光。As a preferred technical solution of the present invention: in the step A, firstly, the output light of the light source is processed to obtain parallel light, and then the parallel light is split to obtain the first split light and the second light beam with the same wavelength and the same intensity. Divided light.

作为本发明的一种优选技术方案:所述步骤E中,针对差分运算结果,经SG平滑算法处理更新,获得二维待测样品所对应的吸收光谱,即光吸收特性与波长的关系。As a preferred technical solution of the present invention: in the step E, the difference operation result is processed and updated by the SG smoothing algorithm to obtain the absorption spectrum corresponding to the two-dimensional sample to be tested, that is, the relationship between the light absorption characteristics and the wavelength.

本发明所要解决的技术问题是提供一种适用于变温环境的差分反射检测方法的装置,采用全新模块布局结构设计,能够高效实现所设计方法,提高待测样品结构特征检测的工作效率。The technical problem to be solved by the present invention is to provide a device for a differential reflection detection method suitable for a variable temperature environment, which adopts a new module layout structure design, which can efficiently implement the designed method and improve the work efficiency of the structural feature detection of the sample to be tested.

本发明为了解决上述技术问题采用以下技术方案:本发明设计了一种适用于变温环境的差分反射检测方法的装置,基于所述光源与所述光谱仪,包括第一离轴抛物面镜、分光镜、第二离轴抛物面镜、电控挡板、上位机;其中,第一离轴抛物面镜的内弧面面向光源的出射端,光源的出射光射向第一离轴抛物面镜的内弧面产生平行光;分光镜设于第一离轴抛物面镜射出平行光的光路上,由分光镜针对平行光通过反射、透射方式,产生彼此波长相同、强度相同的第一分光与第二分光;所述二维待测样品表面面向第二分光方向,第二分光经二维待测样品表面产生第二反射光;所述第一基底表面面向第一分光方向,第一分光经第一基底表面产生第一反射光;第二离轴抛物面镜的内弧面面向第一反射光、第二反射光,第一反射光、第二反射光分别经第二离轴抛物面镜的内弧面产生第一检测光、第二检测光;光谱仪的接收端面向并接收第一检测光、第二检测光;上位机分别与光谱仪、电控挡板连接,电控挡板在上位机的控制下,切换择一针对第一分光或第二分光进行遮挡。In order to solve the above technical problems, the present invention adopts the following technical solutions: the present invention designs a device for a differential reflection detection method suitable for a variable temperature environment, based on the light source and the spectrometer, including a first off-axis parabolic mirror, a beam splitter, The second off-axis parabolic mirror, the electronically controlled baffle, and the upper computer; wherein, the inner arc surface of the first off-axis parabolic mirror faces the exit end of the light source, and the outgoing light of the light source is directed to the inner arc surface of the first off-axis parabolic mirror to generate parallel light; the beam splitter is arranged on the optical path of the parallel light emitted by the first off-axis parabolic mirror, and the beam splitter generates the first beam splitting and the second beam splitting with the same wavelength and the same intensity for the parallel light through reflection and transmission; the The surface of the two-dimensional sample to be tested faces the second light splitting direction, and the second light splitting generates the second reflected light through the surface of the two-dimensional sample to be tested; the surface of the first substrate faces the first light splitting direction, and the first light splitting generates the second light beam through the surface of the first substrate. a reflected light; the inner arc surface of the second off-axis parabolic mirror faces the first reflected light and the second reflected light, and the first reflected light and the second reflected light respectively pass through the inner arc surface of the second off-axis parabolic mirror to generate the first detection light and second detection light; the receiving end of the spectrometer faces and receives the first detection light and the second detection light; the upper computer is respectively connected with the spectrometer and the electric control baffle, and the electric control baffle is switched under the control of the upper computer to select one Blocking is performed for the first split light or the second split light.

作为本发明的一种优选技术方案:还包括入射光纤、准直镜、出射光纤,所述光源的出射端对接入射光纤的其中一端,入射光纤的另一端指向第一离轴抛物面镜的内弧面,光源的出射光经入射光纤射向第一离轴抛物面镜的内弧面产生平行光;准直镜的输入端面向并接收第一检测光、第二检测光,准直镜的输出端对接出射光纤的其中一端,出射光纤的另一端对接光谱仪的接收端,由光谱仪经出射光纤接收第一检测光、第二检测光。As a preferred technical solution of the present invention: it also includes an incident optical fiber, a collimating mirror, and an outgoing optical fiber. The outgoing end of the light source is connected to one end of the incident optical fiber, and the other end of the incident optical fiber points to the inner arc of the first off-axis parabolic mirror. The output light of the light source is directed to the inner arc surface of the first off-axis parabolic mirror through the incident optical fiber to generate parallel light; the input end of the collimating mirror faces and receives the first detection light and the second detection light, and the output end of the collimating mirror faces and receives the first detection light and the second detection light. One end of the outgoing optical fiber is docked, and the other end of the outgoing optical fiber is docked with the receiving end of the spectrometer, and the spectrometer receives the first detection light and the second detection light through the outgoing optical fiber.

作为本发明的一种优选技术方案:所述电控挡板包括相互连接的挡板控制器与光学挡板,所述上位机与挡板控制器连接,光学挡板在上位机经挡板控制器的控制下,切换择一针对第一分光或第二分光进行遮挡。As a preferred technical solution of the present invention: the electronically controlled baffle includes a baffle controller and an optical baffle that are connected to each other, the upper computer is connected to the baffle controller, and the optical baffle is controlled by the upper computer through the baffle. Under the control of the controller, switch to choose one to block the first split light or the second split light.

作为本发明的一种优选技术方案:所述光学挡板表面覆有黑色表面。As a preferred technical solution of the present invention, the surface of the optical baffle is covered with a black surface.

作为本发明的一种优选技术方案:所述入射光纤为SMA905连接头的圆形光纤束多模光纤,所述准直镜为镜片直径为5毫米或者10毫米的SMA连接头的准直镜,所述出射光纤为直径1.3毫米或2.0毫米的SMA905连接头的圆形光纤束多模光纤。As a preferred technical solution of the present invention: the incident optical fiber is a circular fiber bundle multimode fiber of an SMA905 connector, and the collimating lens is a collimating lens of an SMA connector with a lens diameter of 5 mm or 10 mm, The outgoing optical fiber is a circular fiber bundle multimode fiber with a diameter of 1.3 mm or 2.0 mm and an SMA905 connector.

作为本发明的一种优选技术方案:还包括变温台,所述第一基底设置于变温台上,由变温台构成温度可控环境,实现第一基底位于温度可控环境中。As a preferred technical solution of the present invention, it further includes a temperature-changing table, the first substrate is disposed on the temperature-changing table, and the temperature-changing table constitutes a temperature-controlled environment, so that the first substrate is located in the temperature-controlled environment.

作为本发明的一种优选技术方案:所述第一离轴抛物面镜为反射焦距为1英寸或2英寸、镀紫外增强铝模的离轴抛物面镜,所述第二离轴抛物面镜为反射焦距为2英寸或3英寸、镀紫外增强铝模的90度离轴抛物面镜,所述分光镜为边长为10毫米的非偏振50:50分束立方体,由分光镜针对经第一离轴抛物面镜内弧面产生的平行光,平分为彼此波长相同、强度相同、强度相同的第一分光与第二分光。As a preferred technical solution of the present invention: the first off-axis parabolic mirror is an off-axis parabolic mirror with a reflective focal length of 1 inch or 2 inches and is coated with UV-enhanced aluminum mold, and the second off-axis parabolic mirror is a reflective focal length It is a 2-inch or 3-inch 90-degree off-axis parabolic mirror with UV-enhanced aluminum mold, and the beam splitter is a non-polarized 50:50 beam splitting cube with a side length of 10 mm. The parallel light generated by the inner arc surface of the mirror is equally divided into the first split light and the second split light with the same wavelength, the same intensity and the same intensity.

本发明所述一种适用于变温环境的差分反射检测方法及装置,采用以上技术方案与现有技术相比,具有以下技术效果:A differential reflection detection method and device suitable for a variable temperature environment according to the present invention, using the above technical solution compared with the prior art, has the following technical effects:

本发明所设计一种适用于变温环境的差分反射检测方法,基于光源出射光分光所获彼此波长相同、强度相同的第一分光与第二分光,以温度可控环境下的第一基底为依据,切换控制第一分光与第二分光依次经第一基底反射、以及样品室内第二基底表面所设二维待测样品反射,并通过分别所获第一检测光反射光强信息、第二检测光反射光强信息之间的差分运算,依据二维待测样品所对应标准品的吸收特征光谱,实现对二维待测样品的结构特征检测;设计方法具有抗温度干扰能力强、环境适应性好的优点;并进一步设计实现该方法的装置,通过模块化光路布局结构设计,能够进一步提高待测样品结构特征检测的工作效率。The present invention designs a differential reflection detection method suitable for a temperature-variable environment. The first and second light splits with the same wavelength and the same intensity are obtained based on the light splitting of the light emitted by the light source, and the first substrate in a temperature-controlled environment is used as the basis. , switch and control the first split light and the second split light to be reflected by the first substrate and the two-dimensional sample to be tested set on the surface of the second substrate in the sample chamber, and the reflected light intensity information of the first detection light and the second detection light are obtained respectively. The differential operation between the light reflected light intensity information, based on the absorption characteristic spectrum of the standard corresponding to the two-dimensional sample to be tested, realizes the structural feature detection of the two-dimensional sample to be tested; the design method has strong resistance to temperature interference and environmental adaptability and further design a device for realizing the method, through the modular optical path layout structure design, the work efficiency of the structural feature detection of the sample to be tested can be further improved.

附图说明Description of drawings

图1是本发明设计适用于变温环境的差分反射检测方法的装置的模块示意图。FIG. 1 is a schematic block diagram of an apparatus for designing a differential reflection detection method suitable for a variable temperature environment according to the present invention.

其中,1.光源,2.光谱仪,3.样品室,4.第一基底,5.第二基底,6.第一离轴抛物面镜,7.分光镜,8.第二离轴抛物面镜,9.上位机,10.入射光纤,11.准直镜,12.出射光纤,13.挡板控制器,14.光学挡板,15.变温台,16.光源控制器。Among them, 1. light source, 2. spectrometer, 3. sample chamber, 4. first substrate, 5. second substrate, 6. first off-axis parabolic mirror, 7. beam splitter, 8. second off-axis parabolic mirror, 9. Host computer, 10. Incident fiber, 11. Collimating mirror, 12. Outgoing fiber, 13. Baffle controller, 14. Optical baffle, 15. Variable temperature stage, 16. Light source controller.

具体实施方式Detailed ways

下面结合说明书附图对本发明的具体实施方式作进一步详细的说明。The specific embodiments of the present invention will be described in further detail below with reference to the accompanying drawings.

本发明设计了一种适用于变温环境的差分反射检测方法,实际应用当中,基于光源1与光谱仪2,根据温度可控环境下的第一基底4,按如下步骤A至步骤F,针对样品室3内第二基底5表面所设的二维待测样品进行结构特征检测。The present invention designs a differential reflection detection method suitable for a variable temperature environment. In practical applications, based on the light source 1 and the spectrometer 2, and according to the first substrate 4 in a temperature-controlled environment, the following steps A to F are performed for the sample chamber. The two-dimensional sample to be tested set on the surface of the second substrate 5 in 3 is subjected to structural feature detection.

步骤A.首先针对光源1的出射光进行处理,获得平行光,然后针对该平行光进行分光,获得彼此波长相同、强度相同的第一分光与第二分光,并进入步骤B。Step A. First, process the outgoing light of the light source 1 to obtain parallel light, and then split the parallel light to obtain the first and second light splits with the same wavelength and the same intensity, and proceed to step B.

步骤B.基于样品室3内温度恒定的时长t,阻挡第一分光,同时控制第二分光射向第二基底5表面所设的二维待测样品表面,通过反射产生第二检测光,由光谱仪2接收端接收该第二检测光,并保持此状态持续时长t,以及获得此状态下样品室3内的温度T,然后进入步骤C。Step B. Based on the constant time duration t of the temperature in the sample chamber 3, block the first light split, and simultaneously control the second light split to be directed to the surface of the two-dimensional sample to be measured set on the surface of the second substrate 5, and generate the second detection light by reflection, which is composed of The receiving end of the spectrometer 2 receives the second detection light, maintains this state for a duration t, and obtains the temperature T in the sample chamber 3 in this state, and then proceeds to step C.

步骤C.控制第一基底4所处环境的温度为温度T,并阻挡第二分光,同时控制第一分光射向第一基底4表面,通过反射产生第一检测光,由光谱仪2接收端接收该第一检测光,并保持此状态持续时长t,然后进入步骤D。Step C. Control the temperature of the environment where the first substrate 4 is located to be the temperature T, and block the second light splitting, while controlling the first splitting light to be directed to the surface of the first substrate 4, generating the first detection light by reflection, which is received by the receiving end of the spectrometer 2 The first detection light is kept in this state for a duration of t, and then the process proceeds to step D.

步骤D.光谱仪2针对接收到的第二检测光、第一检测光,分别检测获得第二检测光所对应的反射光强信息R2、第一检测光所对应的反射光强信息R1,并进入步骤E。Step D. The spectrometer 2 respectively detects and obtains the reflected light intensity information R 2 corresponding to the second detection light and the reflected light intensity information R 1 corresponding to the first detection light for the received second detection light and the first detection light, and go to step E.

步骤E.根据如下公式进行差分运算;Step E. carry out differential operation according to the following formula;

Figure BDA0003699866710000041
Figure BDA0003699866710000041

获得二维待测样品所对应的吸收光谱Δ,进一步针对二维待测样品所对应的吸收光谱Δ,经SG平滑算法处理更新,获得二维待测样品所对应的吸收光谱,即光吸收特性与波长的关系,并进入步骤F。The absorption spectrum Δ corresponding to the two-dimensional sample to be tested is obtained, and the absorption spectrum Δ corresponding to the two-dimensional sample to be tested is further processed and updated by the SG smoothing algorithm to obtain the absorption spectrum corresponding to the two-dimensional sample to be tested, that is, the light absorption characteristics vs wavelength, and proceed to step F.

步骤F.根据二维待测样品所对应标准品的吸收特征光谱,针对二维待测样品所对应的光吸收特性与波长光谱进行分析,即实现对二维待测样品的结构特征检测。Step F. According to the absorption characteristic spectrum of the standard corresponding to the two-dimensional test sample, analyze the light absorption characteristics and wavelength spectrum corresponding to the two-dimensional test sample, that is, realize the structural feature detection of the two-dimensional test sample.

关于上述所设计适用于变温环境的差分反射检测方法,进一步设计了实现该方法的装置,如图1所示,基于所述光源1与所述光谱仪2,包括第一离轴抛物面镜6、分光镜7、第二离轴抛物面镜8、电控挡板、上位机9;其中,第一离轴抛物面镜6的内弧面面向光源1的出射端,光源1的出射光射向第一离轴抛物面镜6的内弧面产生平行光;分光镜7设于第一离轴抛物面镜6射出平行光的光路上,由分光镜7针对平行光通过反射、透射方式,产生彼此波长相同、强度相同的第一分光与第二分光;所述二维待测样品表面面向第二分光方向,第二分光经二维待测样品表面产生第二反射光;所述第一基底4表面面向第一分光方向,第一分光经第一基底4表面产生第一反射光;第二离轴抛物面镜8的内弧面面向第一反射光、第二反射光,第一反射光、第二反射光分别经第二离轴抛物面镜8的内弧面产生第一检测光、第二检测光;光谱仪2的接收端面向并接收第一检测光、第二检测光;上位机9分别与光谱仪2、电控挡板连接,电控挡板在上位机9的控制下,切换择一针对第一分光或第二分光进行遮挡。Regarding the above-designed differential reflection detection method suitable for variable temperature environments, a device for implementing the method is further designed. As shown in FIG. 1 , based on the light source 1 and the spectrometer 2 , the light source 1 and the spectrometer 2 include a first off-axis parabolic mirror 6 , a beam splitter Mirror 7, second off-axis parabolic mirror 8, electronically controlled baffle, and host computer 9; wherein, the inner arc surface of the first off-axis parabolic mirror 6 faces the exit end of the light source 1, and the outgoing light of the light source 1 is directed to the first off-axis parabolic mirror 6. The inner arc surface of the axial parabolic mirror 6 generates parallel light; the beam splitter 7 is arranged on the optical path of the first off-axis parabolic mirror 6 to emit parallel light, and the beam splitter 7 produces parallel light through reflection and transmission to produce the same wavelength and intensity. The same first split and second split; the surface of the two-dimensional sample to be tested faces the second split direction, and the second split generates second reflected light through the surface of the two-dimensional sample to be tested; the surface of the first substrate 4 faces the first In the beam splitting direction, the first beam passes through the surface of the first substrate 4 to generate the first reflected light; the inner arc surface of the second off-axis parabolic mirror 8 faces the first reflected light and the second reflected light, and the first reflected light and the second reflected light are respectively The first detection light and the second detection light are generated through the inner arc surface of the second off-axis parabolic mirror 8; the receiving end of the spectrometer 2 faces and receives the first detection light and the second detection light; The control baffles are connected, and under the control of the host computer 9, the electronic control baffles switch to select one to block the first light splitting or the second light splitting.

其中,光源1有宽光谱光源和模拟光源控制器16组成;宽光谱光源主要由钨灯或氙灯组成;模拟光源控制器可以控制光源的发光状态亮/灭以及光源亮度;宽光谱光源和模拟光源控制器之间通过传输线进行连接。Among them, the light source 1 is composed of a wide-spectrum light source and an analog light source controller 16; the wide-spectrum light source is mainly composed of a tungsten lamp or a xenon lamp; the analog light source controller can control the light-emitting state of the light source on/off and the brightness of the light source; the wide-spectrum light source and the analog light source The controllers are connected by transmission lines.

关于第一基底4位于温度可控环境的设计,具体设计采用变温台15,所述第一基底4设置于变温台15上,由变温台15构成温度可控环境,实现第一基底4位于温度可控环境中。Regarding the design that the first substrate 4 is located in a temperature-controlled environment, the specific design adopts a temperature-changing table 15, the first substrate 4 is arranged on the temperature-changing table 15, and the temperature-changing table 15 constitutes a temperature-controlled environment, so that the first substrate 4 is located in a temperature-controlled environment. in a controlled environment.

实际应用当中,基于上述所设计装置的方案,进一步设计引入入射光纤10、准直镜11、出射光纤12,所述光源1的出射端对接入射光纤10的其中一端,入射光纤10的另一端指向第一离轴抛物面镜6的内弧面,光源1的出射光经入射光纤10射向第一离轴抛物面镜6的内弧面产生平行光;准直镜11的输入端面向并接收第一检测光、第二检测光,准直镜11的输出端对接出射光纤12的其中一端,出射光纤12的另一端对接光谱仪2的接收端,由光谱仪2经出射光纤12接收第一检测光、第二检测光。In practical application, based on the scheme of the above designed device, an incident optical fiber 10, a collimating mirror 11, and an outgoing optical fiber 12 are further designed. The outgoing end of the light source 1 is connected to one end of the incident optical fiber 10, and the other end of the incident optical fiber 10 points to On the inner arc surface of the first off-axis parabolic mirror 6, the outgoing light of the light source 1 is directed to the inner arc surface of the first off-axis parabolic mirror 6 through the incident optical fiber 10 to generate parallel light; the input end of the collimating mirror 11 faces and receives the first off-axis parabolic mirror 6. For the detection light and the second detection light, the output end of the collimating mirror 11 is docked with one end of the outgoing optical fiber 12, and the other end of the outgoing optical fiber 12 is docked with the receiving end of the spectrometer 2, and the spectrometer 2 receives the first detection light and the second detection light through the outgoing optical fiber 12. 2. Detection light.

实际应用当中,关于电控挡板,进一步设计电控挡板包括相互连接的挡板控制器13与光学挡板14,所述上位机9与挡板控制器13连接,光学挡板14在上位机9经挡板控制器13的控制下,切换择一针对第一分光或第二分光进行遮挡;并且在应用中,进一步设计光学挡板14表面覆有黑色表面。In practical applications, regarding the electronically controlled baffles, the electronically controlled baffles are further designed to include the interconnected baffle controller 13 and the optical baffle 14 , the upper computer 9 is connected to the baffle controller 13 , and the optical baffle 14 is in the upper position. Under the control of the baffle controller 13, the machine 9 switches to choose one to block the first split light or the second split light; and in the application, the surface of the optical baffle 14 is further designed to be covered with a black surface.

将上述所设计装置应用于实际当中,入射光纤10采用SMA905连接头的圆形光纤束多模光纤,所述准直镜11采用镜片直径为5毫米或者10毫米的SMA连接头的准直镜,所述出射光纤12采用直径1.3毫米或2.0毫米的SMA905连接头的圆形光纤束多模光纤;所述第一离轴抛物面镜6为反射焦距为1英寸或2英寸、镀紫外增强铝模的离轴抛物面镜,所述第二离轴抛物面镜8为反射焦距为2英寸或3英寸、镀紫外增强铝模的90度离轴抛物面镜,所述分光镜7为边长为10毫米的非偏振50:50分束立方体,由分光镜7针对经第一离轴抛物面镜6内弧面产生的平行光,平分为彼此波长相同、强度相同、强度相同的第一分光与第二分光。Applying the above-designed device to practice, the incident optical fiber 10 adopts a circular fiber bundle multimode fiber with an SMA905 connector, and the collimating mirror 11 adopts a collimating mirror with an SMA connector with a lens diameter of 5 millimeters or 10 millimeters, The outgoing optical fiber 12 adopts a circular fiber bundle multimode fiber with a diameter of 1.3 mm or 2.0 mm SMA905 connector; the first off-axis parabolic mirror 6 is a reflection focal length of 1 inch or 2 inches, and is coated with UV-enhanced aluminum mode. Off-axis parabolic mirror, the second off-axis parabolic mirror 8 is a 90-degree off-axis parabolic mirror with a reflective focal length of 2 inches or 3 inches and a UV-enhanced aluminum mold, and the beam splitter 7 is a non-parabolic mirror with a side length of 10 mm. For the beam splitting cube with polarization of 50:50, the parallel light generated by the inner arc surface of the first off-axis parabolic mirror 6 is equally divided by the beam splitter 7 into the first beam splitting and the second beam splitting with the same wavelength, the same intensity and the same intensity.

实际应用当中,基于上述所设计装置下适用于变温环境的差分反射检测方法,执行如下步骤A至步骤F。In practical applications, the following steps A to F are performed based on the differential reflection detection method suitable for a variable temperature environment under the above designed device.

步骤A.启动光源控制器,选择合适的光源1亮度,使光源1发出出射光,光源1的出射光经入射光纤10射向第一离轴抛物面镜6的内弧面产生平行光,并由分光镜7针对平行光通过反射、透射方式,产生彼此波长相同、强度相同的第一分光与第二分光,然后进入步骤B。Step A. Start the light source controller, select the appropriate brightness of the light source 1, so that the light source 1 emits outgoing light, and the outgoing light of the light source 1 is directed to the inner arc surface of the first off-axis parabolic mirror 6 through the incident optical fiber 10 to generate parallel light, and is generated by The beam splitter 7 generates a first split beam and a second split beam with the same wavelength and the same intensity with respect to the parallel light through reflection and transmission, and then proceeds to step B.

步骤B.基于样品室3内温度恒定的时长t,电控挡板在上位机9的控制下,切换对第一分光进行遮挡,同时第二分光射向第二基底5表面所设的二维待测样品表面,通过反射产生第二反射光,第二反射光经第二离轴抛物面镜8的内弧面产生第二检测光,准直镜11接收第二检测光,并经出射光纤12输向光谱仪2,由光谱仪2接收第二检测光,并保持此状态持续时长t,以及获得此状态下样品室3内的温度T,然后进入步骤C。Step B. Based on the time length t of the constant temperature in the sample chamber 3, the electronically controlled baffle is switched to block the first beam under the control of the host computer 9, while the second beam is directed to the two-dimensional set on the surface of the second substrate 5. The surface of the sample to be tested generates a second reflected light through reflection, and the second reflected light passes through the inner arc surface of the second off-axis parabolic mirror 8 to generate a second detection light. Send to the spectrometer 2, receive the second detection light by the spectrometer 2, maintain this state for a duration t, and obtain the temperature T in the sample chamber 3 in this state, and then proceed to step C.

步骤C.控制变温台15,使得第一基底4所处环境的温度为温度T,并且基于电控挡板在上位机9的控制下,切换对第二分光进行遮挡,同时控制第一分光射向第一基底4表面,通过反射产生第一反射光,第一反射光经第二离轴抛物面镜8的内弧面产生第一检测光,并经出射光纤12输向光谱仪2,由光谱仪2接收第一检测光,并保持此状态持续时长t,然后进入步骤D。Step C. Control the temperature changing stage 15, so that the temperature of the environment where the first substrate 4 is located is the temperature T, and based on the electronically controlled baffle, under the control of the host computer 9, the second split light is switched to block the second beam, and the first beam is controlled simultaneously. To the surface of the first substrate 4, the first reflected light is generated by reflection. The first reflected light generates the first detection light through the inner arc surface of the second off-axis parabolic mirror 8, and is sent to the spectrometer 2 through the exit fiber 12, and the spectrometer 2 The first detection light is received, and this state is maintained for a duration of t, and then step D is entered.

步骤D.光谱仪2针对接收到的第二检测光、第一检测光,分别检测获得第二检测光所对应的反射光强信息R2、第一检测光所对应的反射光强信息R1,并进入步骤E。Step D. The spectrometer 2 respectively detects and obtains the reflected light intensity information R 2 corresponding to the second detection light and the reflected light intensity information R 1 corresponding to the first detection light for the received second detection light and the first detection light, and go to step E.

步骤E.上位机9接收第二检测光所对应的反射光强信息R2、第一检测光所对应的反射光强信息R1,并根据如下公式进行差分运算;Step E. The host computer 9 receives the reflected light intensity information R 2 corresponding to the second detection light and the reflected light intensity information R 1 corresponding to the first detection light, and performs a differential operation according to the following formula;

Figure BDA0003699866710000071
Figure BDA0003699866710000071

获得二维待测样品所对应的吸收光谱Δ,进一步针对二维待测样品所对应的吸收光谱Δ,经SG平滑算法处理更新,获得二维待测样品所对应的吸收光谱,即光吸收特性与波长的关系,并进入步骤F。The absorption spectrum Δ corresponding to the two-dimensional sample to be tested is obtained, and the absorption spectrum Δ corresponding to the two-dimensional sample to be tested is further processed and updated by the SG smoothing algorithm to obtain the absorption spectrum corresponding to the two-dimensional sample to be tested, that is, the light absorption characteristics vs wavelength, and proceed to step F.

步骤F.上位机9根据二维待测样品所对应标准品的吸收特征光谱,针对二维待测样品所对应的光吸收特性与波长光谱进行分析,即实现对二维待测样品的结构特征检测。Step F. The upper computer 9 analyzes the light absorption characteristics and wavelength spectrum corresponding to the two-dimensional sample to be tested according to the absorption characteristic spectrum of the standard product corresponding to the two-dimensional sample to be tested, that is, to realize the structural characteristics of the two-dimensional sample to be tested. detection.

上述技术方案所设计适用于变温环境的差分反射检测方法,基于光源1出射光分光所获彼此波长相同、强度相同的第一分光与第二分光,以温度可控环境下的第一基底4为依据,切换控制第一分光与第二分光依次经第一基底4反射、以及样品室3内第二基底5表面所设二维待测样品反射,并通过分别所获第一检测光反射光强信息、第二检测光反射光强信息之间的差分运算,依据二维待测样品所对应标准品的吸收特征光谱,实现对二维待测样品的结构特征检测;设计方法具有抗温度干扰能力强、环境适应性好的优点;并进一步设计实现该方法的装置,通过模块化光路布局结构设计,能够进一步提高待测样品结构特征检测的工作效率。The differential reflection detection method designed by the above technical solution is suitable for a variable temperature environment. Based on the light splitting of the light emitted by the light source 1, the first and second light splits with the same wavelength and the same intensity are obtained. The first substrate 4 in a temperature-controlled environment is According to the switching control, the first split light and the second split light are sequentially reflected by the first substrate 4 and the two-dimensional sample to be tested set on the surface of the second substrate 5 in the sample chamber 3, and the reflected light intensity of the first detected light is obtained by respectively The differential operation between the information and the reflected light intensity information of the second detection light, based on the absorption characteristic spectrum of the standard corresponding to the two-dimensional sample to be tested, realizes the structural feature detection of the two-dimensional sample to be tested; the design method has the ability to resist temperature interference The advantages of strong and good environmental adaptability; and a device for realizing the method is further designed, and the work efficiency of the structural feature detection of the sample to be tested can be further improved through the modular optical path layout structure design.

上面结合附图对本发明的实施方式作了详细说明,但是本发明并不限于上述实施方式,在本领域普通技术人员所具备的知识范围内,还可以在不脱离本发明宗旨的前提下做出各种变化。The embodiments of the present invention have been described in detail above in conjunction with the accompanying drawings, but the present invention is not limited to the above-mentioned embodiments, and can also be made within the scope of knowledge possessed by those of ordinary skill in the art without departing from the purpose of the present invention. Various changes.

Claims (10)

1. A differential reflection detection method suitable for a temperature-varying environment is characterized by comprising the following steps: based on the light source (1) and the spectrometer (2), according to the first substrate (4) in the temperature-controllable environment, carrying out structural feature detection on a two-dimensional sample to be detected arranged on the surface of the second substrate (5) in the sample chamber (3) according to the following steps A to F;
step A, splitting light of emergent light of a light source (1) to obtain first split light and second split light which have the same wavelength and the same intensity, and entering step B;
b, blocking the first light split based on the time T of constant temperature in the sample chamber (3), controlling the second light split to be directed to the surface of a two-dimensional sample to be detected arranged on the surface of a second substrate (5), generating second detection light through reflection, receiving the second detection light by a receiving end of a spectrometer (2), keeping the state for the time T, obtaining the temperature T in the sample chamber (3) in the state, and entering the step C;
c, controlling the temperature of the environment where the first substrate (4) is located to be the temperature T, blocking the second light split, controlling the first light split to be emitted to the surface of the first substrate (4), generating first detection light through reflection, receiving the first detection light by a receiving end of the spectrometer (2), keeping the state for a duration T, and then entering the step D;
step D, the spectrometer (2) respectively detects and obtains the reflected light intensity information R corresponding to the second detection light aiming at the received second detection light and the first detection light 2 The reflected light intensity information R corresponding to the first detection light 1 And entering step E;
step E, carrying out differential operation according to the following formula;
Figure FDA0003699866700000011
obtaining an absorption spectrum delta corresponding to a two-dimensional sample to be detected, namely the relation between the light absorption characteristic of the sample and the wavelength, and entering the step F;
and F, analyzing the light absorption characteristics and the wavelength spectrum corresponding to the two-dimensional sample to be detected according to the absorption characteristic spectrum of the standard substance corresponding to the two-dimensional sample to be detected, namely realizing the detection of the structural characteristics of the two-dimensional sample to be detected.
2. The differential reflection detection method suitable for use in a variable temperature environment according to claim 1, wherein: in the step A, the emergent light of the light source (1) is processed to obtain parallel light, and then the parallel light is split to obtain first split light and second split light which have the same wavelength and the same intensity.
3. The differential reflection detection method suitable for use in a variable temperature environment according to claim 1, wherein: and in the step E, aiming at the difference operation result, the difference operation result is processed and updated by an SG smoothing algorithm, and the absorption spectrum corresponding to the two-dimensional sample to be detected, namely the relation between the light absorption characteristic and the wavelength, is obtained.
4. An apparatus for implementing the differential reflection detection method suitable for use in a temperature-varying environment according to any one of claims 1 to 3, wherein: based on the light source (1) and the spectrometer (2), the spectrometer comprises a first off-axis parabolic mirror (6), a spectroscope (7), a second off-axis parabolic mirror (8), an electric control baffle plate and an upper computer (9); the inner cambered surface of the first off-axis parabolic mirror (6) faces the emergent end of the light source (1), and emergent light of the light source (1) emits to the inner cambered surface of the first off-axis parabolic mirror (6) to generate parallel light; the spectroscope (7) is arranged on a light path of parallel light emitted by the first off-axis parabolic mirror (6), and the spectroscope (7) generates first light split and second light split which have the same wavelength and the same intensity aiming at the parallel light in a reflection and transmission mode; the surface of the two-dimensional sample to be detected faces a second light splitting direction, and second reflected light is generated by the second light splitting through the surface of the two-dimensional sample to be detected; the surface of the first substrate (4) faces a first light splitting direction, and first reflected light is generated by the first light splitting through the surface of the first substrate (4); the inner arc surface of the second off-axis parabolic mirror (8) faces the first reflected light and the second reflected light, and the first reflected light and the second reflected light respectively generate first detection light and second detection light through the inner arc surface of the second off-axis parabolic mirror (8); the receiving end of the spectrometer (2) faces and receives the first detection light and the second detection light; the upper computer (9) is respectively connected with the spectrometer (2) and the electric control baffle, and the electric control baffle switches to select one light splitting device to shield the first light splitting device or the second light splitting device under the control of the upper computer (9).
5. The apparatus of claim 4, wherein the apparatus is adapted for use in a differential reflection detection method in a temperature-varying environment, and comprises: the light source device is characterized by further comprising an incident optical fiber (10), a collimating mirror (11) and an emergent optical fiber (12), wherein the emergent end of the light source (1) is in butt joint with one end of the incident optical fiber (10), the other end of the incident optical fiber (10) points to the inner arc surface of the first off-axis parabolic mirror (6), and emergent light of the light source (1) is emitted to the inner arc surface of the first off-axis parabolic mirror (6) through the incident optical fiber (10) to generate parallel light; the input end of the collimating mirror (11) faces and receives the first detection light and the second detection light, the output end of the collimating mirror (11) is in butt joint with one end of the emergent optical fiber (12), the other end of the emergent optical fiber (12) is in butt joint with the receiving end of the spectrometer (2), and the spectrometer (2) receives the first detection light and the second detection light through the emergent optical fiber (12).
6. The apparatus of claim 4, wherein the apparatus is adapted for use in a differential reflection detection method in a temperature-varying environment, and comprises: the electronic control baffle comprises a baffle controller (13) and an optical baffle (14) which are connected with each other, the upper computer (9) is connected with the baffle controller (13), and the optical baffle (14) is switched to be selected to shield the first light splitting or the second light splitting under the control of the upper computer (9) through the baffle controller (13).
7. The apparatus of claim 6, wherein the apparatus is adapted for use in a differential reflection detection method in a variable temperature environment, and comprises: the surface of the optical baffle plate (14) is covered with a black surface.
8. The apparatus of claim 5, wherein the apparatus is adapted for use in a differential reflection detection method in a variable temperature environment, and comprises: incident fiber (10) are the round fiber bundle multimode fiber of SMA905 connector, collimating mirror (11) are the collimating mirror of the SMA connector that the lens diameter is 5 millimeters or 10 millimeters, emergent fiber (12) are the round fiber bundle multimode fiber of the SMA905 connector of diameter 1.3 millimeters or 2.0 millimeters.
9. The apparatus of the differential reflection detection method for use in temperature-varying environments according to any one of claims 4 to 6, wherein: the temperature-changing table (15) is further included, the first substrate (4) is arranged on the temperature-changing table (15), the temperature-changing table (15) forms a temperature-controllable environment, and the first substrate (4) is located in the temperature-controllable environment.
10. The apparatus for differential reflection detection method suitable for use in temperature-varying environments according to claim 9, wherein: the first off-axis parabolic mirror (6) is an off-axis parabolic mirror with a reflection focal length of 1 inch or 2 inches and plated with an ultraviolet enhanced aluminum mold, the second off-axis parabolic mirror (8) is a 90-degree off-axis parabolic mirror with a reflection focal length of 2 inches or 3 inches and plated with an ultraviolet enhanced aluminum mold, the spectroscope (7) is a non-polarized 50:50 beam splitting cube with the side length of 10 millimeters, and parallel light generated by the beam splitter (7) through the inner arc surface of the first off-axis parabolic mirror (6) is divided into a first beam splitter and a second beam splitter which are identical in wavelength, intensity and intensity.
CN202210722008.3A 2022-06-17 2022-06-17 A differential reflection detection method and device suitable for variable temperature environment Pending CN115078279A (en)

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