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CN108593563A - Optical material test method and optic analytical instrument used - Google Patents

Optical material test method and optic analytical instrument used Download PDF

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Publication number
CN108593563A
CN108593563A CN201810460434.8A CN201810460434A CN108593563A CN 108593563 A CN108593563 A CN 108593563A CN 201810460434 A CN201810460434 A CN 201810460434A CN 108593563 A CN108593563 A CN 108593563A
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optical
sample
laser light
path
analysis instrument
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黄凌雄
张戈
陈瑞平
李丙轩
廖文斌
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Fujian Institute of Research on the Structure of Matter of CAS
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Fujian Institute of Research on the Structure of Matter of CAS
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/21Polarisation-affecting properties
    • G01N21/23Bi-refringence
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/41Refractivity; Phase-affecting properties, e.g. optical path length
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/47Scattering, i.e. diffuse reflection
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/47Scattering, i.e. diffuse reflection
    • G01N2021/4735Solid samples, e.g. paper, glass

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

The invention discloses a kind of optical material test method and optic analytical instrument used, the method for this method optical material test includes the following steps:Step S100:Outfield is loaded to the optical sample;Step S200:Optical sample described in laser irradiation obtains the optical information of the optical sample light-emitting surface;Step S300:Adjust the outfield, the optical information is analyzed by optical detecting method, obtain the optical crystal two-fold exit point and/or refractive index with the outfield variation, analyze it is described change obtain the corresponding optical sample in each outfield phase transformation or domain structure variation.Refractive index parameter and second nonlinear signal by measuring optical sample can be achieved to study phase transformation or the domain structure variation in optical material.Another aspect of the present invention additionally provides analytical instrument used in a kind of this method.

Description

光学材料测试方法及所用光学分析仪器Optical material testing methods and optical analysis instruments used

技术领域technical field

本发明涉及一种光学材料测试方法及所用光学分析仪器,属于材料性能测试领域。The invention relates to an optical material testing method and the used optical analysis instrument, belonging to the field of material performance testing.

背景技术Background technique

光学材料的门类众多,应用广泛,如光学玻璃、光学晶体、光学薄膜等等。随着人类社会的进步,对各种先进光学材料的需求也在不断增长,例如铁电光学材料,其在光信息处理、先进光学器件等领域表现出极大的应用潜力,无论是国防还是民用方面,市场前景巨大。而探索具有优异性能的铁电光学材料,不仅有赖于新材料的合成,还需要能检测材料性能的测试手段进行辅助,才能实现对材料的有效分析和评价。There are many types of optical materials and are widely used, such as optical glass, optical crystal, optical film and so on. With the progress of human society, the demand for various advanced optical materials is also increasing, such as ferroelectric optical materials, which show great application potential in the fields of optical information processing and advanced optical devices, whether for national defense or civilian use On the one hand, the market prospect is huge. The exploration of ferroelectric optical materials with excellent properties not only depends on the synthesis of new materials, but also requires the assistance of testing methods that can detect the properties of materials, so as to achieve effective analysis and evaluation of materials.

现有研究中经常涉及对材料相变的研究,材料的应用领域常由其相变特性决定。材料的相变情况,是评价材料性能优劣的重要指标。由于材料内部结构的改变可能伴随相变发生变化,对于光学材料来说,内部结构的改变会对该材料的光学参数产生显著影响,如从有心结构转变为无心结构、从各向异性转变为各向同性等。同样,存在于部分光学材料中的畴结构,其畴的分布取向,同样会对光学材料的光学性能产生极大的影响,而且还存在有序度的问题。The existing research often involves the study of the phase transition of materials, and the application fields of materials are often determined by their phase transition characteristics. The phase transition of materials is an important index to evaluate the performance of materials. Since the change of the internal structure of the material may be accompanied by a phase change, for optical materials, the change of the internal structure will have a significant impact on the optical parameters of the material, such as the change from a centered structure to a centerless structure, from anisotropic to anisotropic. same-sex etc. Similarly, the distribution and orientation of the domain structure existing in some optical materials will also have a great impact on the optical properties of the optical material, and there is also a problem of order degree.

发明内容Contents of the invention

根据本发明的一个方面,提供了一种操作简便,结果准确性高的光学材料测试的方法。该方法为光学材料的研究,提供了简便的检测方法。According to one aspect of the present invention, a method for testing optical materials with simple operation and high result accuracy is provided. This method provides a simple detection method for the research of optical materials.

所述光学材料测试的方法,包括以下步骤:The method for said optical material test comprises the following steps:

步骤S100:向所述光学样品加载外场;Step S100: applying an external field to the optical sample;

步骤S200:激光照射所述光学样品,获取所述光学样品出光面的光学信息;Step S200: irradiating the optical sample with laser light to obtain optical information on the light-emitting surface of the optical sample;

步骤S300:调节所述外场,按光学检测方法对所述光学信息进行分析,得到所述光学晶体的双折射点和/或折射率随所述外场的变化,分析所述变化得到各所述外场对应的所述光学样品的相变或畴结构变化;Step S300: Adjust the external field, analyze the optical information according to the optical detection method, obtain the change of the birefringence point and/or refractive index of the optical crystal with the external field, and analyze the change to obtain each of the external fields a corresponding phase transition or domain structure change of said optical sample;

所述外场为温度场和/或电场。The external field is a temperature field and/or an electric field.

可选的,光学信息为双折射率,所述光学检测方法为偏振光学检测。Optionally, the optical information is birefringence, and the optical detection method is polarization optical detection.

可选的,所述光学信息为双折射率和折射率,所述光学检测方法为折射率检测。Optionally, the optical information is birefringence and refractive index, and the optical detection method is refractive index detection.

可选的,所述光学信息为散射信息,所述光学检测方法为光学散射。Optionally, the optical information is scattering information, and the optical detection method is optical scattering.

可选的,所述光学检测方法为二阶非线性效应,所述光学信息为相变和微观结构。Optionally, the optical detection method is a second-order nonlinear effect, and the optical information is phase change and microstructure.

本发明的又一方面提供了一种所述光学材料用光学分析仪器,包括:激光光源、样品平台和主探测器,光学样品设置于所述样品平台上,所述激光光源与所述光学样品的入光面光路连接;所述主探测器与所述光学样品的出光面光路连接,所述样品平台包括加载装置,所述加载装置向所述光学样品加载至少一种外场。Another aspect of the present invention provides an optical analysis instrument for the optical material, including: a laser light source, a sample platform and a main detector, the optical sample is arranged on the sample platform, the laser light source and the optical sample The optical path of the light incident surface of the optical sample is connected; the main detector is connected with the optical path of the light outgoing surface of the optical sample, and the sample platform includes a loading device, and the loading device loads at least one external field to the optical sample.

优选地,光学材料用光学分析仪器还包括:系统光路,所述系统光路设置于所述激光光源和所述光学样品的入光面的连接光路中,所述系统光路包括:第一偏振光学器件、光阑和平行光管,所述激光光源与所述第一偏振光学器件光路连接;所述第一偏振光学器件与所述光阑光路连接;所述光阑与所述平行光管光路连接;所述平行光管与所述光学样品的入光面光路连接。Preferably, the optical analysis instrument for optical materials further includes: a system optical path, the system optical path is set in the connecting optical path between the laser light source and the light incident surface of the optical sample, and the system optical path includes: a first polarizing optical device , an aperture and a collimator, the laser light source is connected to the optical path of the first polarizing optical device; the first polarizing optical device is connected to the optical path of the aperture; the optical diaphragm is connected to the optical path of the collimator ; The collimator is connected with the optical path of the light incident surface of the optical sample.

优选地,系统光路还包括:半透/半反射镜和辅助探测器,所述半透/半反射镜与所述平行光管光路连接;入射和/或反射进入所述半透/半反射镜的激光与所述辅助探测器光路连接;透射所述半透/半反射镜的激光与所述光学样品光路连接。Preferably, the optical path of the system further includes: a half-transparent/half-reflective mirror and an auxiliary detector, the half-transparent/half-reflective mirror is connected to the optical path of the collimator; the incident and/or reflection enters the half-transparent/half-reflective mirror The laser light is connected to the optical path of the auxiliary detector; the laser light transmitted through the half-transparent/half-reflective mirror is connected to the optical path of the optical sample.

优选地,激光光源的能量强度>0;所述激光光源为紫外激光、可见波长激光或近红外激光中的至少一种。Preferably, the energy intensity of the laser light source is >0; the laser light source is at least one of ultraviolet laser, visible wavelength laser or near-infrared laser.

优选地,所述光学材料用光学分析仪器用于如上述的光学材料测试的方法。Preferably, the optical analysis instrument for the optical material is used in the above optical material testing method.

优选地,样品平台绕所述样品平台中心轴旋转,并能读取转动角度的度数。Preferably, the sample platform rotates around the central axis of the sample platform, and the rotation angle can be read in degrees.

优选地,外场为温度场和/或电压场。Preferably, the external field is a temperature field and/or a voltage field.

优选地,加载装置包括:温场装置和供电装置,所述温场装置设置于所述样品平台上,并调节所述光学样品的温度;所述供电装置设置于所述样品平台上,并向所述光学样品供电。Preferably, the loading device includes: a temperature field device and a power supply device, the temperature field device is arranged on the sample platform, and adjusts the temperature of the optical sample; the power supply device is arranged on the sample platform, and provides The optical sample is powered.

优选地,温场装置为电阻加热元件,所述电阻加热元件提供的温场为室温~500℃;或所述温场装置为半导体元件,所述半导体元件提供的温场为-20~100℃;或所述温场装置为液氮,所述液氮提供的温场为-100℃~室温。Preferably, the temperature field device is a resistance heating element, and the temperature field provided by the resistance heating element is from room temperature to 500°C; or the temperature field device is a semiconductor element, and the temperature field provided by the semiconductor element is -20 to 100°C ; or the temperature field device is liquid nitrogen, and the temperature field provided by the liquid nitrogen is -100° C. to room temperature.

优选地,所述供电装置提供的电场为0~10000V。Preferably, the electric field provided by the power supply device is 0-10000V.

优选地,光学材料用光学分析仪器还包括:主探测器平台和第二偏振光学器件,所述第二偏振光学器件设置于所述主探测器与所述光学样品出光面相连的光路上;所述第二偏振光学器件与所述主探测器设置于所述主探测器平台上;所述主探测器平台以所述光学样品为圆心绕所述光学样品旋转。Preferably, the optical analysis instrument for optical materials further includes: a main detector platform and a second polarizing optical device, and the second polarizing optical device is arranged on the optical path where the main detector is connected to the light-emitting surface of the optical sample; The second polarization optical device and the main detector are arranged on the main detector platform; the main detector platform rotates around the optical sample with the optical sample as the center.

本发明的有益效果包括但不限于:The beneficial effects of the present invention include but are not limited to:

(1)本发明所提供的光学材料测试方法,操作简便,结果准确性高。(1) The optical material testing method provided by the present invention is easy to operate and has high accuracy of results.

(2)本发明所提供的光学材料用光学分析仪器,通过将光学材料制成样品器件后,置于样品平台上,施加外场,并以激光光源照射测量样品。再通过光学探测仪器采集激光信号,主要通过测量光学样品的折射率参数和二阶非线性信号来研究光学材料中的相变或者畴结构变化。通过对光学材料的折射率参数和二阶非线性光学信号的测量,能够精确反应光学材料内部结构的变化。精密测定光学材料的折射率参数和非线性信号,实现实时观察分析光学材料的相变过程或畴结构的变化。(2) In the optical analysis instrument for optical materials provided by the present invention, the optical material is made into a sample device, placed on a sample platform, an external field is applied, and a laser light source is used to irradiate the sample for measurement. Then the laser signal is collected by the optical detection instrument, and the phase transition or domain structure change in the optical material is mainly studied by measuring the refractive index parameter and the second-order nonlinear signal of the optical sample. By measuring the refractive index parameters and second-order nonlinear optical signals of optical materials, it can accurately reflect the changes in the internal structure of optical materials. Precisely measure the refractive index parameters and nonlinear signals of optical materials, and realize real-time observation and analysis of phase transition process or domain structure changes of optical materials.

(3)本发明所提供的光学材料用光学分析仪器,通过在光学材料上施加可调的外场,以激光照射测量样品,使用光学探测仪器采集光学材料出射的激光信号,得到测量光学样品的折射率和二阶非线性信号,并以此来研究光学材料中的相变或者畴结构变化。为光学材料的研究,提供了简便的检测仪器。(3) The optical analysis instrument for optical material provided by the present invention, by applying an adjustable external field on the optical material, irradiates the measurement sample with laser light, uses the optical detection instrument to collect the laser signal emitted by the optical material, and obtains the refraction of the optical sample. Ratio and second-order nonlinear signals, and use it to study phase transitions or domain structure changes in optical materials. For the study of optical materials, a simple detection instrument is provided.

附图说明Description of drawings

图1是本发明提供的第一优选实施例中光学材料用光学分析仪器的结构示意图;Fig. 1 is a schematic structural view of an optical analysis instrument for optical materials in a first preferred embodiment provided by the present invention;

图2是本发明提供的第二优选实施例中光学材料用光学分析仪器的结构示意图;Fig. 2 is a schematic structural view of an optical analysis instrument for optical materials in a second preferred embodiment provided by the present invention;

图3是本发明提供的第三优选实施例中光学材料用光学分析仪器的结构示意图。Fig. 3 is a schematic structural view of an optical analysis instrument for optical materials in a third preferred embodiment provided by the present invention.

部件和附图标记列表:List of parts and reference numbers:

部件名称Part Name 附图标记reference sign 激光光源Laser light source 1010 第一偏振光学器件first polarizing optics 21twenty one 光阑aperture 22twenty two 平行光管collimator 23twenty three 半透/半反射镜Half-transparent/half-reflecting mirror 24twenty four 辅助探测器auxiliary detector 2525 主探测器轨迹main detector track 3131 样品平台sample platform 3333 光学样品optical sample 4040 主探测器平台main detector platform 5151 第二偏振光学器件second polarizing optics 5252 主探测器main detector 5353

具体实施方式Detailed ways

下面结合实施例详述本发明,但本发明并不局限于这些实施例。The present invention is described in detail below in conjunction with examples, but the present invention is not limited to these examples.

本发明的一方面提供了一种采用上述光学材料用光学分析仪器的光学材料测试方法,包括以下步骤:One aspect of the present invention provides a method for testing optical materials using the above-mentioned optical analysis instrument for optical materials, comprising the following steps:

步骤S100:向所述光学样品加载外场;Step S100: applying an external field to the optical sample;

步骤S200:激光照射所述光学样品,获取所述光学样品出光面的光学信息;Step S200: irradiating the optical sample with laser light to obtain optical information on the light-emitting surface of the optical sample;

步骤S300:调节所述外场,按光学检测方法对所述光学信息进行分析,得到所述光学晶体的双折射点和/或折射率随所述外场的变化,分析所述变化得到各所述外场对应的所述光学样品的相变或畴结构变化;Step S300: Adjust the external field, analyze the optical information according to the optical detection method, obtain the change of the birefringence point and/or refractive index of the optical crystal with the external field, and analyze the change to obtain each of the external fields a corresponding phase transition or domain structure change of said optical sample;

所述外场为温度场和/或电场。The external field is a temperature field and/or an electric field.

通过该操作方法,便于对肉眼不可见的光学样品的相变和畴结构进行研究,通过调节所施加的外场的变化,获得外场与光学样品内部结构变化的关系,为进一步研究光学样品提供依据。此处的调节外场包括对外场的升高或降低。光学检测方法包括但不限于:偏振光学检测、光学散射检测、折射率测量、二阶非线性效应检测。Through this operation method, it is convenient to study the phase transition and domain structure of optical samples that are invisible to the naked eye. By adjusting the change of the applied external field, the relationship between the external field and the internal structure change of the optical sample is obtained, which provides a basis for further research on optical samples. Adjusting the outer field here includes raising or lowering the outer field. Optical detection methods include, but are not limited to: polarized optical detection, optical scattering detection, refractive index measurement, second order nonlinear effect detection.

可选的,光学信息为双折射率,所述光学检测方法为偏振光学检测。作为一种可选的光学检测方法,当按该方法进行光学器件的偏振光学检测时,可检测到的相变过程包括双折射现象。Optionally, the optical information is birefringence, and the optical detection method is polarization optical detection. As an optional optical detection method, when the polarized optical detection of the optical device is carried out according to this method, the detectable phase transition process includes birefringence.

可选的,所述光学信息为双折射率和折射率,所述光学检测方法为折射率检测。该方法用于测量折射率时,双折射和折射率均可检测到对应发生的改变。Optionally, the optical information is birefringence and refractive index, and the optical detection method is refractive index detection. When this method is used to measure the refractive index, both birefringence and refractive index can detect corresponding changes.

可选的,所述光学信息为散射信息,所述光学检测方法为光学散射。该方法用于测量光学散射时,可检测到散射现象的改变。Optionally, the optical information is scattering information, and the optical detection method is optical scattering. When this method is used to measure optical scattering, changes in the scattering phenomenon can be detected.

可选的,所述光学检测方法为二阶非线性效应,所述光学信息为相变和微观结构。该方法用于测量二阶非线性效应时,可检测到相变和微观结构的改变。此处的微观结构是指畴的微观结构。Optionally, the optical detection method is a second-order nonlinear effect, and the optical information is phase change and microstructure. When this method is used to measure second-order nonlinear effects, phase transitions and microstructural changes can be detected. The microstructure here refers to the microstructure of domains.

在一具体实施例中,改变加载在光学样品40上的温度和电场强度,即温度和电场强度作为一对变量,测量对应的折射率和二阶非线性信号,以此对光学样品40进行分析。由于此处光学样品40具有一对平行的光学通光面,所以利用M-Z干涉法或测量激光光束的平移量可测量出光学样品40的折射率;在主探测器53前设置截止滤光片或使用光栅,对二阶非线性信号进行分析。假设待测量的光学材料在温度T时产生相变,相变过程中由各向异性(低温态)转变为各向同性(高温态),本发明设计的光学分析仪器中,激光光源10作用于最初处于低温态的光学样品40,可以测量到双折射现象,随着光学样品40上的温度升高到达温度T,双折射现象消失;假定待测量的光学材料在温度T时产生相变,相变过程中由无心结构(低温态)转变为有心结构(高温态),该材料为无心结构是具有二阶非线性光学效应,即处于无心结构时,激光光源作用其上能够产生二阶非线性光学信号,随着光学样品40上的温度升高到达温度T,光学材料转变为有心结构,此时二阶非线性光学信号消失。对于畴结构的研究也是类似的,对于各向异性的光学材料,若其间的畴结构取向处于无序状态,那么双折射现象将消失,二阶非线性信号与光学样品40的方向关联不大,在光学样品40上升高温度、加强电场强度,在此动态过程中,双折射率逐步增大直至一定数值,二阶非线性光学信号与光学样品40的方向关联也不断加强,辅以光学质量分析,还能够对光学样品40的畴结构生长进行间接观测。In a specific embodiment, the temperature and the electric field strength loaded on the optical sample 40 are changed, that is, the temperature and the electric field strength are used as a pair of variables, and the corresponding refractive index and second-order nonlinear signal are measured, so as to analyze the optical sample 40 . Since the optical sample 40 has a pair of parallel optical light-passing surfaces here, the refractive index of the optical sample 40 can be measured by using the M-Z interferometry or measuring the translation of the laser beam; Using gratings, second-order nonlinear signals are analyzed. Assuming that the optical material to be measured undergoes a phase transition at temperature T, during the phase transition, it changes from anisotropic (low temperature state) to isotropic (high temperature state), in the optical analysis instrument designed in the present invention, the laser light source 10 acts on The optical sample 40 that is initially in a low-temperature state can measure the birefringence phenomenon. As the temperature on the optical sample 40 increases to reach the temperature T, the birefringence phenomenon disappears; assuming that the optical material to be measured produces a phase change at the temperature T, the phase In the process of transformation, it changes from a centerless structure (low temperature state) to a centered structure (high temperature state). The material has a centerless structure and has a second-order nonlinear optical effect. For the optical signal, as the temperature on the optical sample 40 increases to reach the temperature T, the optical material transforms into a centered structure, and the second-order nonlinear optical signal disappears at this time. The research on the domain structure is also similar. For anisotropic optical materials, if the orientation of the domain structure is in a disordered state, then the birefringence phenomenon will disappear, and the second-order nonlinear signal has little correlation with the direction of the optical sample 40. Raise the temperature on the optical sample 40 and strengthen the electric field intensity. During this dynamic process, the birefringence gradually increases to a certain value, and the direction correlation between the second-order nonlinear optical signal and the optical sample 40 is also continuously strengthened, supplemented by optical quality analysis. , also enabling indirect observation of the domain structure growth of the optical sample 40 .

在一个具体实施例中,以升温和/或施加电场为例,按上述方法分析,所得光学信息变化过程,及其对应的光学样品的相变和踌结构变化过程列于表1。In a specific embodiment, taking heating and/or applying an electric field as an example, and analyzing according to the above method, the obtained optical information change process, and the corresponding phase change and phase change process of the optical sample are listed in Table 1.

表1升温和/或施加电场后光学材料测试方法分析结果表Table 1 Analysis result table of optical material test method after heating up and/or applying electric field

由表1可知,本发明提供的该检测方法可以用于研究光学材料内部,肉眼不可见结构的变化情况。研究过程简单便捷,结果准确可靠。It can be seen from Table 1 that the detection method provided by the present invention can be used to study the changes of the invisible structure inside the optical material. The research process is simple and convenient, and the results are accurate and reliable.

参见图1,本发明提供的光学材料用光学分析仪器,包括:激光光源10、样品平台33和主探测器53。光学样品40设置于所述样品平台33上,所述激光光源10与所述光学样品40的入光面光路连接;所述主探测器53与所述光学样品40的出光面光路连接,所述样品平台33包括加载装置,所述加载装置向所述光学样品40加载至少一种外场。Referring to FIG. 1 , the optical analysis instrument for optical materials provided by the present invention includes: a laser light source 10 , a sample platform 33 and a main detector 53 . The optical sample 40 is arranged on the sample platform 33, the laser light source 10 is connected to the light path of the light incident surface of the optical sample 40; the main detector 53 is connected to the light path of the light exit surface of the optical sample 40, and the The sample platform 33 includes a loading device that loads the optical sample 40 with at least one external field.

本文中加载外场是指向光学样品40上负载可负载的外场。外场包括但不限于电场、热场、光场、压力场、磁场等物理量场。加载装置可以为各类施加物理量时常用的装置,例如温场装置。加载装置可以安装于光学样品40的任何位置,仅需能实现对光学样品40的加载即可。本发明提供的光学材料用光学分析仪器尤其适用于检测光学材料的相变及畴结构变化情况。光学材料用光学分析仪器通过向待检测光学样品40射出激光。激光入射光学样品40后,一方面可以通过主探测器53获取光学样品40的折射率等参数。同时通过在样品平台33上设置的加载装置对光学样品40施加各种条件的变化,例如温度、电压、电流强度。从而测得光学样品40在不同的环境参数条件下,光学样品40的折射率参数和二阶非线性信号,并借此来研究光学材料的相变或者畴结构变化。可根据光学分析的需要在激光光源10与样品平台33连接的光路上设置偏振器、光阑、平行光管及相关的光学器件。线性或非线性信号可以为从光学样品40透射,或光学样品40反射进入主探测器53的激光。Herein, loading an external field refers to an external field that can be loaded on the optical sample 40 . External fields include, but are not limited to, physical quantity fields such as electric fields, thermal fields, light fields, pressure fields, and magnetic fields. The loading device can be various commonly used devices for applying physical quantities, such as a temperature field device. The loading device can be installed at any position of the optical sample 40 , it only needs to be able to load the optical sample 40 . The optical analysis instrument for optical materials provided by the invention is especially suitable for detecting phase transition and domain structure changes of optical materials. The optical analysis instrument for optical materials emits laser light to the optical sample 40 to be inspected. After the laser light is incident on the optical sample 40 , parameters such as the refractive index of the optical sample 40 can be obtained through the main detector 53 on the one hand. At the same time, changes in various conditions, such as temperature, voltage, and current intensity, are applied to the optical sample 40 through the loading device provided on the sample platform 33 . Therefore, the refractive index parameters and second-order nonlinear signals of the optical sample 40 under different environmental parameter conditions are measured, and the phase transition or domain structure change of the optical material is studied by this. Polarizers, diaphragms, collimators and related optical devices can be arranged on the optical path connecting the laser light source 10 and the sample platform 33 according to the needs of optical analysis. The linear or non-linear signal can be laser light transmitted from the optical sample 40 or reflected from the optical sample 40 into the main detector 53 .

光学材料用光学分析仪器的分析测试对象为光学材料的相变过程或畴结构变化。光学材料的相变过程中可能的内部结构变化会改变其物理特性,通过主探测器53观测到相关的物理量变化,如从各向同性结构转变为各向异性结构,光学材料会从光学均质体转变为具有双折射特性,以本发明设计的光学分析仪器,能够精确测量相变过程中光学折射率的变化,从而准确把握光学材料在不同外场参数下,对应的内部结构变化情况。例如,光学材料在从有心结构转变为无心结构时,以激光光源10照射光学样品40,产生的二阶非线性信号也会发生相应的变化,二阶非线性信号能够为主探测器53捕捉。对于光学材料中的畴结构,其折射率信息和二阶非线性信号也与畴的大小、分布取向密切相关,畴的变化也会带来二者的改变。从而可以通过光学材料用光学分析仪器来研究光学材料的相变和畴的变化。The analysis and test object of the optical analysis instrument for optical materials is the phase transition process or domain structure change of optical materials. The possible internal structure changes in the phase transition process of the optical material will change its physical properties. The relevant physical quantity changes are observed through the main detector 53, such as changing from an isotropic structure to an anisotropic structure, and the optical material will change from an optical homogeneity to an anisotropic structure. The bulk transition has birefringence characteristics, and the optical analysis instrument designed by the present invention can accurately measure the change of the optical refractive index during the phase transition, so as to accurately grasp the corresponding internal structure changes of the optical material under different external field parameters. For example, when the optical material changes from a centered structure to a centerless structure, the laser light source 10 irradiates the optical sample 40 , and the generated second-order nonlinear signal will change accordingly, and the second-order nonlinear signal can be captured by the main detector 53 . For the domain structure in optical materials, its refractive index information and second-order nonlinear signals are also closely related to the size and distribution orientation of domains, and changes in domains will also bring about changes in both. Therefore, the phase transition and domain change of optical materials can be studied by using optical analysis instruments for optical materials.

此处所用的主探测器53为能采集激光信号的光学探测仪器。主探测仪器包括光学图像采集系统、光能量计或示波器,工作过程中可由其中任意一种或多种仪器组合分析采集光信号。The main detector 53 used here is an optical detection instrument capable of collecting laser signals. The main detection instrument includes an optical image acquisition system, an optical energy meter or an oscilloscope, and any one or a combination of these instruments can be used to analyze and collect optical signals during the work process.

参见图2,为了满足光学分析仪器的测量要求,在激光光源10照射光学样品40前需要对激光进行适当的处理,如以平行光管对激光光束进行整形以控制激光的光束质量。通过设置偏振器以使激光光束产生单一偏振态激光。优选的,光学材料用光学分析仪器还包括:系统光路,所述系统光路设置于所述激光光源10和所述光学样品40连接的光路中,所述系统光路包括:第一偏振光学器件21、光阑22和平行光管23,所述激光光源10与所述第一偏振光学器件21光路连接;所述第一偏振光学器件21与所述光阑22光路连接;所述光阑22与所述平行光管23光路连接;所述平行光管23与所述光学样品40的入光面光路连接。第一偏振光学器件21能够控制射入光学样品40中激光的偏振方向。光阑22为可调节圆形光阑或狭缝光阑,以控制入射光学样品40激光的光学质量。平行光管23对入射光学样品40的激光进行整形以控制激光的发散角。Referring to FIG. 2 , in order to meet the measurement requirements of the optical analysis instrument, before the laser light source 10 irradiates the optical sample 40 , the laser needs to be properly processed, such as using a collimator to shape the laser beam to control the beam quality of the laser. By setting the polarizer so that the laser beam produces a single polarization state laser. Preferably, the optical analysis instrument for optical materials further includes: a system optical path, which is arranged in the optical path connecting the laser light source 10 and the optical sample 40, and the system optical path includes: a first polarizing optical device 21, Diaphragm 22 and collimator 23, the laser light source 10 is connected with the optical path of the first polarized optical device 21; the first polarized optical device 21 is connected with the optical path of the diaphragm 22; the diaphragm 22 is connected with the optical path of the The optical path of the collimator 23 is connected; the optical path of the collimator 23 is connected with the light incident surface of the optical sample 40 . The first polarization optical device 21 can control the polarization direction of the laser light incident into the optical sample 40 . The aperture 22 is an adjustable circular aperture or a slit aperture to control the optical quality of the laser light incident on the optical sample 40 . The collimator 23 shapes the laser beam incident on the optical sample 40 to control the divergence angle of the laser beam.

在一具体实施例中,以激光光源10与光学样品40所连光路作为本发明设计的光学分析仪器的工作主轴(l);沿工作主轴(l)设置依序光路连接的第一偏振光学器件21、光阑22和平行光管23,第一偏振光学器件21能够绕工作主轴(l)自旋转。光阑22为可调节圆形光阑或狭缝光阑。In a specific embodiment, the optical path connected by the laser light source 10 and the optical sample 40 is used as the working main axis (1) of the optical analysis instrument designed by the present invention; the first polarization optical device connected to the optical path in sequence is arranged along the working main axis (1) 21. A diaphragm 22 and a collimator 23. The first polarizing optical device 21 can rotate around the main axis of work (1). The diaphragm 22 is an adjustable circular diaphragm or a slit diaphragm.

参见图3,优选的,所述系统光路还包括:半透/半反射镜24和辅助探测器25,所述半透/半反射镜24与所述平行光管23光路连接;入射和/或反射进入所述半透/半反射镜24的激光和所述辅助探测器25光路连接;透射所述半透/半反射镜24的激光与所述光学样品40光路连接。此处的反射是指光学样品40入光面上反射产生的光。Referring to Fig. 3, preferably, the optical path of the system further includes: a semi-transparent/half-reflective mirror 24 and an auxiliary detector 25, the semi-transparent/half-reflective mirror 24 is connected to the optical path of the collimator 23; the incident and/or The laser light reflected into the half-transparent/half-reflective mirror 24 is connected with the optical path of the auxiliary detector 25 ; the laser light transmitted through the half-transparent/half-reflective mirror 24 is connected with the optical path of the optical sample 40 . The reflection here refers to the light generated by reflection on the light incident surface of the optical sample 40 .

半透/半反射镜24能够旋转90°,能将入射光学样品40前的激光及由光学样品40反射回的激光分别进行采样,并将所得光学样品40的反射激光和入射激光的激光信号反射到辅助探测器25进行分析。从而准确测量得到光学样品40的折射率。The semi-transparent/half-reflecting mirror 24 can be rotated by 90°, and can sample the laser light before the incident optical sample 40 and the laser light reflected back by the optical sample 40, and reflect the reflected laser light of the obtained optical sample 40 and the laser signal of the incident laser light To the auxiliary detector 25 for analysis. Thus, the refractive index of the optical sample 40 can be accurately measured.

参见图3,在一具体实施例中,以激光光源10与光学样品40所连光路作为本发明提供的光学分析仪器的工作主轴(l);沿工作主轴(l)设置依序光路连接的第一偏振光学器件21、光阑22、平行光管23和半透/半反射镜24。第一偏振光学器件21能够绕工作主轴(l)自旋转。光阑22为可调节圆形光阑或狭缝光阑。(l2)为辅助探测器25的中心对称轴,半透/半反射镜24设置于(l2)和(l)的垂直相交点处。辅助探测器25设置于(l2)上,并与半透/半反射镜24光路连接。Referring to Fig. 3, in a specific embodiment, the optical path connected with laser light source 10 and optical sample 40 is used as the working main axis (1) of the optical analysis instrument provided by the present invention; A polarizing optical device 21 , an aperture 22 , a collimator 23 and a half-transparent/half-reflecting mirror 24 . The first polarization optics 21 are capable of self-rotation about the main axis of work (1). The diaphragm 22 is an adjustable circular diaphragm or a slit diaphragm. (12) is the central symmetry axis of the auxiliary detector 25, and the half-transparent/half-reflecting mirror 24 is arranged at the vertical intersection of (12) and (1). The auxiliary detector 25 is arranged on (12), and is connected with the half-transparent/half-reflecting mirror 24 in an optical path.

优选的,所述样品平台33绕所述样品平台33中心轴旋转,并能读取转动角度的度数。Preferably, the sample platform 33 rotates around the central axis of the sample platform 33, and the degree of the rotation angle can be read.

优选的,该光学材料用光学分析仪器可以用于实现上述光学材料测试的方法。Preferably, the optical analysis instrument for optical materials can be used to realize the above-mentioned optical material testing method.

本发明中样品平台33具备水平方向360°旋转功能,而且还能准确读取平台转动角度,便于实现通过光学材料用光学分析仪器准确测量光学样品40的折射率。现有光学材料折射率的测量方法有几何法和干涉法,根据方法的不同,它们对测量样品的要求有所区别,如最小偏转角法,需要将待测量的光学材料加工成满足一定要求的棱镜,而干涉法中待测量的光学材料可以为平片或楔形样品,无论哪种测量方法,通过获取测量样品的精确角度值,能提高对折射率的测量精度。与此相似,激光在光学材料中产生的二阶非线性信号更是与角度密切相关,样品平台33的旋转和测角功能有助于实现光学材料相关参数测量准确。In the present invention, the sample platform 33 has the function of rotating 360° in the horizontal direction, and can also accurately read the rotation angle of the platform, which facilitates the accurate measurement of the refractive index of the optical sample 40 by using an optical analysis instrument for optical materials. The existing measurement methods for the refractive index of optical materials include geometric method and interferometry. According to different methods, they have different requirements for the measurement sample. For example, the minimum deflection angle method needs to process the optical material to be measured into a shape that meets certain requirements. Prisms, and the optical material to be measured in the interferometry can be a flat sheet or a wedge-shaped sample. No matter which measurement method is used, the measurement accuracy of the refractive index can be improved by obtaining the precise angle value of the measurement sample. Similar to this, the second-order nonlinear signal generated by the laser in the optical material is closely related to the angle, and the rotation and angle measurement functions of the sample platform 33 help to achieve accurate measurement of related parameters of the optical material.

优选的,所述激光光源10的能量强度>0。更优选的,激光光源10的能量强度为0.5~107W/cm-2。具体能量强度可根据所进行的测试要求选择。例如在线性光学测试时,可以采用较低的激光能量密度;在进行二阶非线性光学测试时,则采用较高的激光能量密度。Preferably, the energy intensity of the laser light source 10 is >0. More preferably, the energy intensity of the laser light source 10 is 0.5-10 7 W/cm -2 . The specific energy intensity can be selected according to the test requirements. For example, in linear optical testing, lower laser energy density can be used; in second-order nonlinear optical testing, higher laser energy density can be used.

采用该强度的激光光源10能实现以光学分析的方式精确分析光学材料的相变过程和畴结构变化。首先,激光光源10的单色性和方向性能够确保精准测量折射率上的微小变化,其次,激光的能量特性是在光学材料中产生足够强度二阶非线性信号的保障。考虑到光学材料的特性和光的波长密切相关,优选的激光光源10的波长为可更换的。以便实现对各种不同光学材料的准确测量。Using the laser light source 10 with this intensity can realize the precise analysis of the phase transition process and the domain structure change of the optical material in the way of optical analysis. Firstly, the monochromaticity and directivity of the laser light source 10 can ensure accurate measurement of small changes in the refractive index, and secondly, the energy characteristics of the laser are the guarantee for generating sufficient intensity second-order nonlinear signals in optical materials. Considering that the properties of optical materials are closely related to the wavelength of light, the preferred wavelength of the laser light source 10 is replaceable. In order to achieve accurate measurement of various optical materials.

优选地,所述激光光源10为紫外激光、可见波长激光或近红外激光中的至少一种。可根据需要,选择单一波长激光或多个不同波长的激光同时照射光学样品40。Preferably, the laser light source 10 is at least one of ultraviolet laser, visible wavelength laser or near-infrared laser. According to needs, a single wavelength laser or multiple lasers with different wavelengths can be selected to irradiate the optical sample 40 simultaneously.

优选的,所述外场为温度场和/或电压场。优选的,所述加载装置包括温场装置和供电装置,所述温场装置设置于所述样品平台33上,并调节所述光学样品40的温度;所述供电装置设置于所述样品平台33上,并向所述光学样品40供电。Preferably, the external field is a temperature field and/or a voltage field. Preferably, the loading device includes a temperature field device and a power supply device, the temperature field device is arranged on the sample platform 33, and adjusts the temperature of the optical sample 40; the power supply device is arranged on the sample platform 33 , and supply power to the optical sample 40 .

从而实现,样品平台33能够为光学样品40施加可调节强度的温场和电场。温度是导致材料相变和畴结构变化的重要因素之一,因此本发明提供的样品平台33需要对测量样品的温度进行有效控制。同时根据需要在测量样品上引入电场,以满足研究中的特殊要求。Thereby, the sample platform 33 can apply a temperature field and an electric field with adjustable intensity to the optical sample 40 . Temperature is one of the important factors leading to material phase transition and domain structure change, so the sample platform 33 provided by the present invention needs to effectively control the temperature of the measurement sample. At the same time, an electric field is introduced on the measurement sample as needed to meet the special requirements in the research.

优选地,所述温场装置为电阻加热元件,所述电阻加热元件提供的温场为室温~500℃。该温场可作用于光学样品40。Preferably, the temperature field device is a resistance heating element, and the temperature field provided by the resistance heating element is from room temperature to 500°C. This temperature field can act on the optical sample 40 .

优选地,所述温场装置为半导体元件,所述半导体元件提供的温场为-20~100℃。从而调节所述光学样品40的温度范围为-20~100℃。Preferably, the temperature field device is a semiconductor element, and the temperature field provided by the semiconductor element is -20-100°C. Therefore, the temperature range of the optical sample 40 is adjusted to be -20-100°C.

优选地,所述温场装置为液氮,所述液氮提供的温场为-100℃~室温。对光学样品40进行冷却,能调节所述光学样品40的温度范围为-100℃~室温。Preferably, the temperature field device is liquid nitrogen, and the temperature field provided by the liquid nitrogen is from -100°C to room temperature. Cooling the optical sample 40 can adjust the temperature range of the optical sample 40 to be -100° C. to room temperature.

优选地,所述供电装置提供的电场为0~10000V。调节所述光学样品40的电压范围为0~10000V。此处的供电装置产生的电流可以为直流或交流。Preferably, the electric field provided by the power supply device is 0-10000V. The voltage range for adjusting the optical sample 40 is 0-10000V. The current generated by the power supply device here can be direct current or alternating current.

优选的,所述主探测器53以所述光学样品40为圆心绕所述光学样品40旋转。Preferably, the main detector 53 rotates around the optical sample 40 with the optical sample 40 as the center.

主探测仪器围绕测试样品旋转以采集光学信号,根据测量的要求可选择不同的光学探测仪器以采集光学信号的强度、波长、偏振特性、图像等。从而可以获取光学样品40不同角度的光学参数。The main detection instrument rotates around the test sample to collect optical signals. According to the measurement requirements, different optical detection instruments can be selected to collect the intensity, wavelength, polarization characteristics, images, etc. of optical signals. Thus, optical parameters of the optical sample 40 at different angles can be acquired.

为了满足本发明提供的光学分析仪器的测量要求,在主探测器53前需要设置合适的光学元器件以满足信号采集的要求。主探测仪器前可放置光学偏振器、光阑及相关光学器件。In order to meet the measurement requirements of the optical analysis instrument provided by the present invention, suitable optical components need to be arranged in front of the main detector 53 to meet the requirements of signal collection. Optical polarizers, diaphragms and related optical devices can be placed in front of the main detection instrument.

参见图2和3,优选的,所述光学材料用光学分析仪器还包括:主探测器平台51和第二偏振光学器件52,所述第二偏振光学器件52设置于所述主探测器53与所述光学样品40出光面相连的光路上;所述第二偏振光学器件52与所述主探测器53设置于所述主探测器平台51上;所述主探测器平台51以所述光学样品40为圆心绕所述光学样品40旋转。2 and 3, preferably, the optical analysis instrument for optical materials further includes: a main detector platform 51 and a second polarization optical device 52, the second polarization optical device 52 is arranged between the main detector 53 and The optical path where the light-emitting surface of the optical sample 40 is connected; the second polarization optical device 52 and the main detector 53 are arranged on the main detector platform 51; 40 is the center of a circle rotating around the optical sample 40 .

优选的,所述光学样品40为光学材料加工而成的一楔角棱镜,棱镜的各项参数满足测量要求,将其置于样品平台33的中心,使用最小偏转角法或者自准直法可以精确测量该样品的折射率,以主探测器53围绕样品平台33旋转,在合适的位置探测从光学样品40产生的二阶非线性信号。Preferably, the optical sample 40 is a wedge prism processed from optical materials, and the parameters of the prism meet the measurement requirements. It is placed in the center of the sample platform 33, and the minimum deflection angle method or the self-collimation method can be used. The refractive index of the sample is precisely measured, and the main detector 53 rotates around the sample platform 33 to detect the second-order nonlinear signal generated from the optical sample 40 at a suitable position.

作为一个具体的实施方式,在图3中给出了本发明提供的用于光学材料相变及畴结构研究的光学分析仪器一种典型工作形式,可大致分为:光源部分a,系统光路部分b,样品平台部分c,探测器部分d。其中包括:激光光源10、第一偏振光学器件21、光阑22、平行光管23、半透/半反射镜24、辅助探测器25、样品平台33和光学样品40。第二偏振光学器件52在一具体实施方式中为光学信号检偏的偏振光学器件。31表示主探测器53的旋转轨迹。在一具体实施例中,主探测器平台51可以沿主探测器轨迹31围绕光学样品旋转,(l)为本发明设计的光学分析仪器的工作主轴,(l1)为通过样品平台33中心且与工作主轴(l)垂直的轴线,(l2)为辅助探测器25的中心对称轴。As a specific implementation mode, a typical working form of the optical analysis instrument for optical material phase transition and domain structure research provided by the present invention is shown in Fig. 3, which can be roughly divided into: light source part a, system optical path part b, Sample platform part c, detector part d. It includes: a laser light source 10 , a first polarizing optical device 21 , an aperture 22 , a collimator 23 , a half-transparent/half-reflecting mirror 24 , an auxiliary detector 25 , a sample platform 33 and an optical sample 40 . In a specific embodiment, the second polarization optics 52 are polarization optics for optical signal analysis. 31 denotes the rotation locus of the main probe 53 . In a specific embodiment, the main detector platform 51 can rotate around the optical sample along the main detector track 31, (1) is the working axis of the optical analysis instrument designed in the present invention, (11) passes through the center of the sample platform 33 and is connected with The working axis (l) is the vertical axis, and (l2) is the central symmetry axis of the auxiliary detector 25.

激光光源10根据测量分析的要求选择激光的辐射波长,并使激光通过所述样品平台33的旋转中心,以激光光源10与光学样品40所连光路作为本发明提供的光学分析仪器的工作主轴(l);沿工作主轴(l)设置第一偏振光学器件21、光阑22、平行光管23和半透/半反射镜24,第一偏振光学器件21能够绕工作主轴(l)旋转以控制入射光学样品40激光的偏振方向,光阑22为可调节圆形光阑或狭缝光阑,以控制入射光学样品40的激光的光学质量,平行光管23对入射光学样品40的激光进行整形以控制激光的发散角,半透/半反射镜24能够旋转90°,分别对入射光学样品40前的激光及由光学样品40反射回的激光进行采样,将激光信号反射到辅助探测器25进行分析。为光学样品40由光学材料加工而成,为具有一对平行通光面的光学平片,其放置于样品平台33的旋转中心,在光学样品40上施加一定范围内电压可调的电场,电场方向垂直或平行于工作主轴(l),根据测量分析的要求,选择不同的附件控制光学样品40的温场。The laser light source 10 selects the radiation wavelength of the laser according to the requirements of measurement and analysis, and makes the laser pass through the center of rotation of the sample platform 33, and the optical path connected by the laser light source 10 and the optical sample 40 is used as the working axis of the optical analysis instrument provided by the present invention ( l); along the main axis of work (1) the first polarizing optics 21, aperture 22, collimator 23 and half-transparent/half-reflecting mirror 24 are set, the first polarizing optics 21 can rotate around the main axis of work (1) to control The polarization direction of the incident optical sample 40 laser light, the diaphragm 22 is an adjustable circular diaphragm or slit diaphragm to control the optical quality of the incident optical sample 40 laser light, and the collimator 23 shapes the incident optical sample 40 laser light To control the divergence angle of the laser light, the semi-transparent/half-reflective mirror 24 can be rotated 90° to sample the laser light before the incident optical sample 40 and the laser light reflected back by the optical sample 40, and reflect the laser signal to the auxiliary detector 25 for further processing. analyze. The optical sample 40 is processed from optical materials, and is an optical flat plate with a pair of parallel light-transmitting surfaces. It is placed on the rotation center of the sample platform 33, and an electric field with an adjustable voltage within a certain range is applied to the optical sample 40. The direction is vertical or parallel to the main axis of work (1), and different accessories are selected to control the temperature field of the optical sample 40 according to the requirements of measurement and analysis.

光学探测器平台51沿主探测器轨迹31围绕样品平台33的旋转中心转动,该平台上放置有主探测器53及相关的光学元器件,主探测器53用于接收激光光源10作用在光学样品40后的线性及非线性信号,信号可以是从光学样品40透射,或光学样品40反射,第二偏振光学器件52即为主探测器53前最为常用的光学元器件,用来辅助主探测器53对激光信号的偏振特性进行分析,根据应用需求,在主探测器53前较为常用的光学元器件还有滤光片、衰减片、光阑等。The optical detector platform 51 rotates around the rotation center of the sample platform 33 along the main detector track 31. The main detector 53 and related optical components are placed on the platform. The main detector 53 is used to receive the laser light source 10 and act on the optical sample. The linear and nonlinear signals after 40, the signal can be transmitted from the optical sample 40, or reflected by the optical sample 40, the second polarization optical device 52 is the most commonly used optical component before the main detector 53, used to assist the main detector 53 analyzes the polarization characteristics of the laser signal. According to application requirements, optical components commonly used in front of the main detector 53 include optical filters, attenuators, and apertures.

为了更清楚地描述本申请的光学材料测试方法及所用光学分析仪器,以下将以不同的实施例对本申请的光学材料测试方法及所用光学分析仪器进行进一步的说明。In order to describe the optical material testing method and the optical analysis instrument used in the present application more clearly, the optical material testing method and the optical analysis instrument used in the present application will be further described in different embodiments below.

如无特别说明,本发明的实施例中的原料均通过商业途径购买。Unless otherwise specified, the raw materials in the examples of the present invention were purchased through commercial channels.

实施例1采用上述光学材料用光学分析仪器测试测量样品的折射率及双折射现象相关结构变化Example 1 Using the above-mentioned optical material to test and measure the refractive index and birefringence related structural changes of the sample with an optical analysis instrument

根据本发明的一种具体实施方式,如图3所示,研究钛酸钡铁电晶体的相变过程。钛酸钡铁电晶体加工成具有一对平行的光学通光面的光学样品40,样品厚度2~10mm,将其置于样品平台33的旋转中心,通过更换温场附件的方式为光学样品40提供-100~200℃的温度调节范围。激光光源10使用632.8nm氦氖激光,可旋转地第一偏振光学器件21控制激光的偏振方向为45°,直接照射光学样品40;主探测器53使用CCD线阵探测器,固定于工作主轴(l)方向,该探测器前放置准直放大镜组。通过测量激光光束相对工作主轴(l)的平移量,结合光学样品40光学通光面的法线与工作主轴(l)的夹角,计算出光学样品40的折射率。光学样品40的温度从-100℃上升到120℃的过程中,可以观察到双折射现象,在-80℃和0℃位置,双折射点有较为明显的变动,在120℃时,双折射现象消失,这三个温度点分别对应三方晶系→正交晶系、正交晶系→四方晶系、四方晶系→立方晶系的相变点。According to a specific embodiment of the present invention, as shown in FIG. 3 , the phase transition process of barium titanate ferroelectric crystal is studied. The barium titanate ferroelectric crystal is processed into an optical sample 40 with a pair of parallel optical transparent surfaces, the thickness of the sample is 2-10 mm, it is placed on the rotation center of the sample platform 33, and the optical sample 40 is heated by replacing the temperature field attachment. Provide a temperature adjustment range of -100 ~ 200 ℃. The laser light source 10 uses a 632.8nm helium-neon laser, and the rotatable first polarization optical device 21 controls the polarization direction of the laser to be 45°, directly irradiating the optical sample 40; the main detector 53 uses a CCD linear array detector, fixed on the working spindle ( l) direction, a collimating magnifying glass group is placed in front of the detector. The refractive index of the optical sample 40 is calculated by measuring the translation of the laser beam relative to the working axis (l) and combining the angle between the normal of the optical surface of the optical sample 40 and the working axis (l). When the temperature of the optical sample 40 rises from -100°C to 120°C, birefringence can be observed. At -80°C and 0°C, the birefringence point changes significantly. At 120°C, the birefringence These three temperature points correspond to the phase transition points of trigonal crystal system→orthorhombic system, orthorhombic system→tetragonal system, tetragonal system→cubic system.

实施例2采用上述光学材料用光学分析仪器测试测量样品的折射率及双折射现象相关结构变化Example 2 Using the above-mentioned optical material to test and measure the refractive index and birefringence related structural changes of the sample with an optical analysis instrument

根据本发明的一种具体实施方式,如图3所示,研究钛酸钡铁电晶体的相变过程。钛酸钡铁电晶体加工成直角棱镜形状的光学样品40,其中棱镜的直角面为a切向,将其置于样品平台33的旋转中心,选择合适的温场附件为光学样品40提供室温至200℃的温度调节范围。激光光源10使用高光学质量的合束激光,激光波长包含有473nm、532nm、632.8nm和1064nm,激光依次通过第一偏振光学器件21、光阑22、平行光管23、半透/半反射镜24后照射光学样品40;辅助探测器25使用高灵敏度光电型能量计,光电型能量计装有光阑以精确控制入射光线光路。使用自准直法,由辅助探测器25精确测量棱镜的顶角和折射光束的反射角度,能够精确测量出光学样品40的折射率。光学样品40的温度从室温上升到200℃,光学样品40的温度从室温开始上升,在到达120℃之前,可以观察到双折射现象,并精确测量各波长下不同偏振态所对应的折射率,折射率随温度轻微变化;当光学样品40的温度越过120℃,即晶体内部结构由四方晶系转变为立方晶系,此时双折射现象消失,折射率产生变化。According to a specific embodiment of the present invention, as shown in FIG. 3 , the phase transition process of barium titanate ferroelectric crystal is studied. The barium titanate ferroelectric crystal is processed into an optical sample 40 in the shape of a right-angle prism, wherein the right-angle surface of the prism is a tangential direction, and it is placed on the rotation center of the sample platform 33, and a suitable temperature field accessory is selected to provide the optical sample 40 from room temperature to 200°C temperature adjustment range. The laser light source 10 uses high optical quality combined beam lasers. The laser wavelengths include 473nm, 532nm, 632.8nm and 1064nm. The laser light passes through the first polarizing optical device 21, the diaphragm 22, the collimator 23, and the half-transparent/half-reflecting mirror in turn. After 24, the optical sample 40 is irradiated; the auxiliary detector 25 uses a high-sensitivity photoelectric energy meter, and the photoelectric energy meter is equipped with an aperture to precisely control the optical path of the incident light. Using the self-collimation method, the auxiliary detector 25 accurately measures the vertex angle of the prism and the reflection angle of the refracted light beam, so that the refractive index of the optical sample 40 can be accurately measured. The temperature of the optical sample 40 rises from room temperature to 200°C, and the temperature of the optical sample 40 starts to rise from room temperature. Before reaching 120°C, birefringence can be observed, and the refractive index corresponding to different polarization states at each wavelength can be accurately measured. The refractive index changes slightly with temperature; when the temperature of the optical sample 40 exceeds 120°C, that is, the internal structure of the crystal changes from a tetragonal crystal system to a cubic crystal system, the birefringence disappears and the refractive index changes.

实施例3采用上述光学材料用光学分析仪器测试测量样品的折射率及双折射现象相关结构变化Example 3 Using the above-mentioned optical material to test and measure the refractive index and birefringence related structural changes of the sample with an optical analysis instrument

根据本发明的一种具体实施方式,如图3所示,研究钛酸铅铁电晶体的相变过程。钛酸铅铁电晶体加工成直角棱镜形状的光学样品40,其中棱镜的直角面为a切向,将其置于样品平台33的旋转中心,选择合适的温场附件为光学样品40提供室温至500℃的温度调节范围,并在光学样品40上施加一个可调直流电场,电场电压从0~10000V,电场方向垂直于工作主轴(l)。激光光源10使用高光束质量的1064nm电光调制脉冲激光,激光依次通过第一偏振光学器件21、光阑22、半透/半反射镜24后照射光学样品40;主探测器53使用硅光电型能量计,硅光电型能量计前放置有截止滤光片,能够完全滤除1064nm光信号,辅助探测器25使用高灵敏度光电型能量计,光电型能量计装有光阑以精确控制入射光线光路。使用自准直法,由辅助探测器25精确测量棱镜的顶角和折射光束的反射角度,能够精确测量出光学样品40的折射率。光学样品40在室温及任意电场强度条件下,由于内部存在的畴结构取向任意,所以无法表现出双折射现象,存在明显散射;当测量样品上所通电场强度达到一定值,施加其上的电场开始体现出作用,可以开始观察到双折射现象,并且双折射率随着电场强度的提高而逐步变大,双折射率达到一定值后不再变化,同时晶体内部的散射现象也较最初减弱。在测量折射率的同时,使用主探测器53采集二阶非线性信号,在室温时,二阶非线性信号与晶体方向性联系不大,随着光学样品40上温度的升高和作用电场的加强,二阶非线性信号与晶体的方向性关联缓慢提升,温度和电场超过一定范围后,激光沿晶体绝大部分方向产生的二阶非线性信号较室温要微弱,只有在特定方向上,二阶非线性信号明显加强。可通过对光学样品40外加加热装置实现对光学样品40上温度的控制。According to a specific embodiment of the present invention, as shown in FIG. 3 , the phase transition process of lead titanate ferroelectric crystal is studied. The lead titanate ferroelectric crystal is processed into an optical sample 40 in the shape of a right-angle prism, wherein the right-angle surface of the prism is a tangential direction, and it is placed on the rotation center of the sample platform 33, and an appropriate temperature field accessory is selected to provide the optical sample 40 with room temperature to The temperature adjustment range is 500°C, and an adjustable DC electric field is applied on the optical sample 40, the electric field voltage is from 0 to 10000V, and the electric field direction is perpendicular to the working axis (l). The laser light source 10 uses a 1064nm electro-optic modulated pulsed laser with high beam quality, and the laser light sequentially passes through the first polarizing optical device 21, the diaphragm 22, and the half-transparent/half-reflecting mirror 24 to irradiate the optical sample 40; the main detector 53 uses silicon photoelectric energy A cut-off filter is placed in front of the silicon photoelectric energy meter, which can completely filter out the 1064nm optical signal. The auxiliary detector 25 uses a high-sensitivity photoelectric energy meter. The photoelectric energy meter is equipped with a diaphragm to precisely control the optical path of the incident light. Using the self-collimation method, the auxiliary detector 25 accurately measures the vertex angle of the prism and the reflection angle of the refracted light beam, so that the refractive index of the optical sample 40 can be accurately measured. Under the conditions of room temperature and arbitrary electric field strength, the optical sample 40 cannot show birefringence and has obvious scattering due to the arbitrary orientation of the domain structure existing inside; when the electric field strength applied to the measured sample reaches a certain value, the electric field It begins to show its effect, and the birefringence phenomenon can be observed, and the birefringence index gradually increases with the increase of the electric field intensity. After the birefringence index reaches a certain value, it will not change. At the same time, the scattering phenomenon inside the crystal is also weaker than the initial one. While measuring the refractive index, the main detector 53 is used to collect the second-order nonlinear signal. At room temperature, the second-order nonlinear signal has little connection with the crystal directionality. As the temperature on the optical sample 40 increases and the applied electric field Strengthening, the correlation between the second-order nonlinear signal and the directionality of the crystal slowly increases. When the temperature and electric field exceed a certain range, the second-order nonlinear signal generated by the laser along most directions of the crystal is weaker than that at room temperature. Only in a specific direction, the second-order nonlinear signal The order nonlinear signal is obviously strengthened. The temperature on the optical sample 40 can be controlled by adding a heating device to the optical sample 40 .

以上所述,仅是本发明的几个实施例,并非对本发明做任何形式的限制,虽然本发明以较佳实施例揭示如上,然而并非用以限制本发明,任何熟悉本专业的技术人员,在不脱离本发明技术方案的范围内,利用上述揭示的技术内容做出些许的变动或修饰均等同于等效实施案例,均属于技术方案范围内。The above are only a few embodiments of the present invention, and do not limit the present invention in any form. Although the present invention is disclosed above with preferred embodiments, it is not intended to limit the present invention. Any skilled person familiar with this field, Without departing from the scope of the technical solution of the present invention, some changes or modifications made using the technical content disclosed above are equivalent to equivalent implementation cases, and all belong to the scope of the technical solution.

Claims (10)

1.一种光学材料测试的方法,其特征在于,包括以下步骤:1. A method for optical material testing, is characterized in that, comprises the following steps: 步骤S100:向所述光学样品加载外场;Step S100: applying an external field to the optical sample; 步骤S200:激光照射所述光学样品,获取所述光学样品出光面的光学信息;Step S200: irradiating the optical sample with laser light to obtain optical information on the light-emitting surface of the optical sample; 步骤S300:调节所述外场,按光学检测方法对所述光学信息进行分析,得到所述光学晶体的双折射点和/或折射率随所述外场的变化,分析所述变化得到各所述外场对应的所述光学样品的相变或畴结构变化;Step S300: Adjust the external field, analyze the optical information according to the optical detection method, obtain the change of the birefringence point and/or refractive index of the optical crystal with the external field, and analyze the change to obtain each of the external fields a corresponding phase transition or domain structure change of said optical sample; 所述外场为温度场和/或电场。The external field is a temperature field and/or an electric field. 2.根据权利要求1所述的光学材料测试的方法,其特征在于,所述光学信息为双折射率,所述光学检测方法为偏振光学检测。2. The method for testing optical materials according to claim 1, wherein the optical information is birefringence, and the optical detection method is polarization optical detection. 3.根据权利要求1所述的光学材料测试的方法,其特征在于,所述光学信息为双折射率和折射率,所述光学检测方法为折射率检测。3. The method for testing optical materials according to claim 1, wherein the optical information is birefringence and refractive index, and the optical detection method is refractive index detection. 4.根据权利要求1所述的光学材料测试的方法,其特征在于,所述光学信息为散射信息,所述光学检测方法为光学散射。4. The method for testing optical materials according to claim 1, wherein the optical information is scattering information, and the optical detection method is optical scattering. 5.根据权利要求1所述的光学材料测试的方法,其特征在于,所述光学检测方法为二阶非线性效应,所述光学信息为相变和微观结构。5. The method for testing optical materials according to claim 1, wherein the optical detection method is a second-order nonlinear effect, and the optical information is phase change and microstructure. 6.一种光学材料用光学分析仪器,其特征在于,包括:激光光源、样品平台和主探测器,光学样品设置于所述样品平台上,所述激光光源与所述光学样品的入光面光路连接;6. An optical analysis instrument for optical materials, comprising: a laser light source, a sample platform and a main detector, the optical sample is arranged on the sample platform, the light incident surface of the laser light source and the optical sample Optical connection; 所述主探测器与所述光学样品的出光面光路连接,所述样品平台包括加载装置,所述加载装置向所述光学样品加载至少一种外场。The main detector is connected to the optical path of the light exit surface of the optical sample, and the sample platform includes a loading device, and the loading device loads at least one external field to the optical sample. 7.根据权利要求6所述的光学材料用光学分析仪器,其特征在于,所述光学材料用光学分析仪器还包括:系统光路,所述系统光路设置于所述激光光源和所述光学样品的入光面的连接光路中,所述系统光路包括:第一偏振光学器件、光阑和平行光管,所述激光光源与所述第一偏振光学器件光路连接;7. The optical analysis instrument for optical materials according to claim 6, characterized in that, the optical analysis instrument for optical materials further comprises: a system optical path, the system optical path is arranged between the laser light source and the optical sample In the connecting optical path of the light incident surface, the optical path of the system includes: a first polarizing optical device, a diaphragm and a collimator, and the laser light source is connected to the optical path of the first polarizing optical device; 所述第一偏振光学器件与所述光阑光路连接;所述光阑与所述平行光管光路连接;所述平行光管与所述光学样品的入光面光路连接。The first polarizing optical device is connected to the optical path of the aperture; the aperture is connected to the optical path of the collimator; and the collimator is connected to the optical path of the light incident surface of the optical sample. 8.根据权利要求7所述的光学材料用光学分析仪器,其特征在于,所述系统光路还包括:半透/半反射镜和辅助探测器,所述半透/半反射镜与所述平行光管光路连接;8. The optical analysis instrument for optical materials according to claim 7, wherein the optical path of the system further comprises: a semi-transparent/half-reflecting mirror and an auxiliary detector, the semi-transparent/half-reflecting mirror is parallel to the Light pipe light path connection; 入射和/或反射进入所述半透/半反射镜的激光与所述辅助探测器光路连接;透射所述半透/半反射镜的激光与所述光学样品光路连接。The laser light incident and/or reflected into the semi-transparent/half-reflecting mirror is connected to the optical path of the auxiliary detector; the laser light transmitted through the semi-transparent/half-reflecting mirror is connected to the optical path of the optical sample. 9.根据权利要求6所述的光学材料用光学分析仪器,其特征在于,所述激光光源的能量强度>0;9. The optical analysis instrument for optical materials according to claim 6, wherein the energy intensity of the laser light source is >0; 所述激光光源为紫外激光、可见波长激光或近红外激光中的至少一种。The laser light source is at least one of ultraviolet laser, visible wavelength laser or near-infrared laser. 10.根据权利要求6所述的光学材料用光学分析仪器,其特征在于,所述光学材料用光学分析仪器用于如权利要求1~5中任一项所述的光学材料测试的方法。10 . The optical analysis instrument for optical materials according to claim 6 , wherein the optical analysis instrument for optical materials is used for the optical material testing method according to any one of claims 1 to 5 . 11 .
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