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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Prior art keywords
optical
sample
laser
light path
optical material
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CN201810460434.8A
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Inventor
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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Priority to CN201810460434.8A priority Critical patent/CN108593563A/en
Publication of CN108593563A publication Critical patent/CN108593563A/en
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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

Optical material test method and optic analytical instrument used
Technical field
The present invention relates to a kind of optical material test method and optic analytical instruments used, belong to material properties test neck Domain.
Background technology
The class of optical material is numerous, is widely used, such as optical glass, optical crystal, optical thin film.With the mankind Social progress, the demand to various advanced optical materials is also constantly increasing, such as ferroelectric optical material, at optical information The fields such as reason, advanced optical device show great application potential, and either national defence or civilian aspect, market prospects is huge Greatly.And the ferroelectric optical material with excellent properties is explored, not only depend on the synthesis of new material, it is also necessary to material can be detected The means of testing of energy is assisted, and could realize effective analysis and evaluation to material.
The research to material phase transformation is frequently involved in existing research, the application field of material is often determined by its phase-change characteristic. The phase transformation situation of material is the important indicator for evaluating material property quality.Since the change of material internal structure may be with phase Change changes, and for optical material, the change of internal structure can make a significant impact the optical parameter of the material, such as It is changed into no core structure from there is core structure, is changed into isotropism from anisotropy etc..It similarly there are in partial optical material Domain structure, the distribution on farmland is orientated, and can equally generate strong influence to the optical property of optical material, but also there are The problem of sequence is spent.
Invention content
According to an aspect of the invention, there is provided it is a kind of easy to operate, the as a result high optical material test of accuracy Method.This method is the research of optical material, provides easy detection method.
The method of the 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:The outfield is adjusted, the optical information is analyzed by optical detecting method, obtains the light For the two-fold exit point and/or refractive index of crystal with the variation in the outfield, it is corresponding that the analysis variation obtains each outfield The phase transformation or domain structure of the optical sample change;
The outfield is temperature field and/or electric field.
Optionally, optical information is birefringence, and the optical detecting method detects for polarization optics.
Optionally, the optical information is birefringence and refractive index, and the optical detecting method detects for refractive index.
Optionally, the optical information is scattered information, and the optical detecting method is optical scattering.
Optionally, the optical detecting method is second order nonlinear effect, and the optical information is phase transformation and microstructure.
It is yet another aspect of the present invention to provide a kind of optical material optic analytical instruments, including:Laser light source, sample Product platform and main detector, optical sample are set on the example platform, and the laser light source enters with the optical sample Smooth surface light path connects;The main detector is connect with the light-emitting surface light path of the optical sample, and the example platform includes load Device, the loading device load at least one outfield to the optical sample.
Preferably, optical material further includes with optic analytical instrument:System light path, the system light path are set to described sharp In the connection light path of the incidence surface of radiant and the optical sample, the system light path includes:First polarization optics, light Door screen and parallel light tube, the laser light source are connect with the first polarization optics light path;First polarization optics It is connect with the diaphragm light path;The diaphragm is connect with the parallel light tube light path;The parallel light tube and the optical sample Incidence surface light path connection.
Preferably, system light path further includes:Semi-transparent/half-reflecting mirror and auxiliary detector, the semi-transparent/half-reflecting mirror and institute State the connection of parallel light tube light path;Laser that is incident and/or being reflected into the semi-transparent/half-reflecting mirror and the auxiliary detector light Road connects;The laser for transmiting the semi-transparent/half-reflecting mirror is connect with the optical sample light path.
Preferably, the energy intensity > 0 of laser light source;The laser light source is ultraviolet laser, visible wavelength lasers or close At least one of infrared laser.
Preferably, the method that the optical material is used to test such as above-mentioned optical material with optic analytical instrument.
Preferably, example platform is around the example platform center axis rotation, and can read the number of degrees of rotational angle.
Preferably, outfield is temperature field and/or voltage field.
Preferably, loading device includes:Thermal field device and for electric installation, the thermal field device is set to the example platform On, and adjust the temperature of the optical sample;It is described to be set on the example platform for electric installation, and to the optical sample Power supply.
Preferably, thermal field device is stratie, and the thermal field that the stratie provides is room temperature~500 ℃;Or the thermal field device is semiconductor element, the thermal field that the semiconductor element provides is -20~100 DEG C;Or the thermal field Device is liquid nitrogen, and the thermal field that the liquid nitrogen provides is -100 DEG C~room temperature.
Preferably, the electric field provided for electric installation is 0~10000V.
Preferably, optical material further includes with optic analytical instrument:Main detector platform and the second polarization optics, institute The second polarization optics are stated to be set in the light path that the main detector is connected with the optical sample light-emitting surface;Described second Polarization optics are set to the main detector on the main detector platform;The main detector platform is with the optics Sample is that the center of circle is rotated around the optical sample.
Beneficial effects of the present invention include but not limited to:
(1) optical material test method provided by the present invention, easy to operate, as a result accuracy is high.
(2) optical material optic analytical instrument provided by the present invention, after samples devices are made in optical material, It is placed on example platform, applies outfield, and irradiated with laser light source and measure sample.Laser letter is acquired by optical detection instrument again Number, mainly by measure refractive index parameter and the second nonlinear signal of optical sample study phase transformation in optical material or Domain structure changes.By the measurement of refractive index parameter and second nonlinear optic signal to optical material, can accurately react The variation of optical material internal structure.The refractive index parameter and nonlinear properties of micrometric measurement optical material realize observation in real time Analyze the phase transition process of optical material or the variation of domain structure.
(3) optical material optic analytical instrument provided by the present invention, it is adjustable outer by applying on optical material , sample is measured with laser irradiation, using the laser signal of optical detection instrument acquisition optical material outgoing, obtains measuring optics The refractive index and second nonlinear signal of sample, and changed to study phase transformation in optical material or domain structure with this.For light The research for learning material provides easy detecting instrument.
Description of the drawings
Fig. 1 is the structural schematic diagram of optical material optic analytical instrument in first preferred embodiment provided by the invention;
Fig. 2 is the structural schematic diagram of optical material optic analytical instrument in the second preferred embodiment provided by the invention;
Fig. 3 is the structural schematic diagram of optical material optic analytical instrument in third preferred embodiment provided by the invention.
Component and reference numerals list:
Component names Reference numeral
Laser light source 10
First polarization optics 21
Diaphragm 22
Parallel light tube 23
Semi-transparent/half-reflecting mirror 24
Auxiliary detector 25
Main detector track 31
Example platform 33
Optical sample 40
Main detector platform 51
Second polarization optics 52
Main detector 53
Specific implementation mode
The present invention is described in detail with reference to embodiment, but the invention is not limited in these embodiments.
An aspect of of the present present invention provides a kind of optical material test using above-mentioned optical material optic analytical instrument Method 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:The outfield is adjusted, the optical information is analyzed by optical detecting method, obtains the light For the two-fold exit point and/or refractive index of crystal with the variation in the outfield, it is corresponding that the analysis variation obtains each outfield The phase transformation or domain structure of the optical sample change;
The outfield is temperature field and/or electric field.
Passed through convenient for studying the phase transformation and domain structure of visually sightless optical sample by the operating method The variation in applied outfield is adjusted, the relationship in outfield and optical sample internal structure change is obtained, for further research optics Sample provides foundation.Adjusting outfield herein includes that outfield is raised and lowered.Optical detecting method includes but not limited to:Partially Shake optical detection, optical scattering detection, refractometry, second order nonlinear effect detection.
Optionally, optical information is birefringence, and the optical detecting method detects for polarization optics.As a kind of optional Optical detecting method, when in this way carry out optical device polarization optics detection when, detectable phase transition process includes Birefringent phenomenon.
Optionally, the optical information is birefringence and refractive index, and the optical detecting method detects for refractive index.It should Method is for when measuring refractive index, birefringence and refractive index to can detect the corresponding change occurred.
Optionally, the optical information is scattered information, and the optical detecting method is optical scattering.This method is for surveying When measuring optical scattering, the change of scattering phenomenon can detect.
Optionally, the optical detecting method is second order nonlinear effect, and the optical information is phase transformation and microstructure. This method is for when measuring second order nonlinear effect, can detect the change of phase transformation and microstructure.Microstructure herein is Refer to the microstructure on farmland.
In one embodiment, change temperature and electric field strength of the load on optical sample 40, i.e. temperature and electric field Intensity is measured corresponding refractive index and second nonlinear signal, is analyzed optical sample 40 with this as a pair of of variable.By There is a pair of parallel optics light pass surface in optical sample 40 herein, so utilizing the flat of M-Z interferometries or measuring laser beam Shifting amount can measure out the refractive index of optical sample 40;Edge filter is set before main detector 53 or uses grating, to second order Nonlinear properties are analyzed.Assuming that optical material to be measured generates phase transformation in temperature T, by anisotropy in phase transition process (cold state) is changed into isotropism (high temperature state), and in the optic analytical instrument that the present invention designs, laser light source 10 acts on most It is just in the optical sample 40 of cold state, birefringent phenomenon can be measured, is reached as the temperature on optical sample 40 increases Temperature T, birefringent phenomenon disappear;It is assumed that optical material to be measured generates phase transformation in temperature T, by no hearty cord in phase transition process Structure (cold state), which is changed into, core structure (high temperature state), with second order nonlinear optical effect, i.e., which is for no core structure When in no core structure, laser light source effect can generate second nonlinear optic signal thereon, on optical sample 40 Temperature, which increases, reaches temperature T, and optical material, which is changed into, core structure, at this time second nonlinear optic blackout.Farmland is tied The research of structure is also similar, for anisotropic optical material, if domain structure therebetween is oriented in disordered state, then Birefringent phenomenon will disappear, and second nonlinear signal and the directional correlation of optical sample 40 are little, are increased on optical sample 40 Temperature reinforces electric field strength, and in this dynamic process, birefringence incrementally increases until certain numerical value, second nonlinear optic The directional correlation of signal and optical sample 40 is also constantly reinforced, and is aided with optical quality analysis, additionally it is possible to the farmland of optical sample 40 Structure growth carries out indirect operation.
In a specific embodiment, it for heating up and/or apply electric field, analyzes as stated above, gained optics letter The phase transformation of breath change procedure and its corresponding optical sample and structure change process of hesitating are listed in table 1.
Optical material analysis of test methods result table after the heating of table 1 and/or application electric field
As shown in Table 1, the detection method provided by the invention can be used for studying inside optical material, the invisible knot of naked eyes The situation of change of structure.Research process is simple and convenient, as a result accurately and reliably.
Referring to Fig. 1, optical material optic analytical instrument provided by the invention, including:Laser light source 10, example platform 33 With main detector 53.Optical sample 40 is set on the example platform 33, the laser light source 10 and the optical sample 40 Incidence surface light path connection;The main detector 53 is connect with the light-emitting surface light path of the optical sample 40, the example platform 33 include loading device, and the loading device loads at least one outfield to the optical sample 40.
Load outfield is directed to load the outfield that can be loaded on optical sample 40 herein.Outfield includes but not limited to electricity The Physical Quantity Fields such as field, thermal field, light field, pressure field, magnetic field.Loading device common device when can be all kinds of application physical quantitys, Such as thermal field device.Loading device can be installed on any position of optical sample 40, it is only necessary to can realize to optical sample 40 Load.Optical material provided by the invention is particularly suitable for the phase transformation of detection optical material with optic analytical instrument and farmland is tied Structure situation of change.Optical material optic analytical instrument to optical sample 40 to be detected by projecting laser.Laser beam incident optical After sample 40, the parameters such as the refractive index of optical sample 40 on the one hand can be obtained by main detector 53.Simultaneously by sample The loading device being arranged on platform 33 applies optical sample 40 variation of various conditions, such as temperature, voltage, current strength. To measure optical sample 40 under the conditions of different environmental parameters, the refractive index parameter and second nonlinear of optical sample 40 are believed Number, and the phase transformation or domain structure to study optical material change whereby.It can be according to the needs of optical analysis in laser light source 10 Polarizer, diaphragm, parallel light tube and relevant optical device are set in the light path being connect with example platform 33.Linearly or nonlinearly Signal can be the laser that main detector 53 is reflected into from the transmission of optical sample 40 or optical sample 40.
The analysis test object of optical material optic analytical instrument is phase transition process or the domain structure variation of optical material. Possible internal structure change can change its physical characteristic in the phase transition process of optical material, and phase is observed by main detector 53 The physical quantity variation of pass, is such as changed into anisotropic structure from isotropic structure, and optical material can change from optics isotropic body Can accurately to measure light refractive index in phase transition process with birefringent characteristic with the optic analytical instrument that the present invention designs Variation, to accurately hold optical material outside difference under field parameters, corresponding internal structure change situation.For example, optics Material irradiates optical sample 40, the second nonlinear of generation when from there is core structure to be changed into no core structure, with laser light source 10 Signal can also occur to change accordingly, and second nonlinear signal can be that main detector 53 captures.For the farmland in optical material Structure, refractive index information and second nonlinear signal are also closely related with the size on farmland, distribution orientation, and the variation on farmland also can band Carry out the change of the two.So as to study the phase transformation of optical material and the change on farmland with optic analytical instrument by optical material Change.
Main detector 53 used herein is the optical detection instrument that can acquire laser signal.Main detection instrument includes optics Image capturing system, luminous energy or oscillograph can be adopted by any of which or the analysis of a variety of instrument combinations in the course of work Collect optical signal.
Referring to Fig. 2, in order to meet the measurement request of optic analytical instrument, needed before laser light source 10 irradiates optical sample 40 Processing appropriate is carried out to laser, shaping is such as carried out to control the beam quality of laser to laser beam with parallel light tube.It is logical Setting polarizer is crossed so that laser beam generates single polarization state laser.Preferably, optical material is also wrapped with optic analytical instrument It includes:System light path, the system light path is set in the light path that the laser light source 10 and the optical sample 40 connect, described System light path includes:First polarization optics 21, diaphragm 22 and parallel light tube 23, the laser light source 10 are inclined with described first 21 light path of optical device of shaking connects;First polarization optics 21 are connect with 22 light path of the diaphragm;The diaphragm 22 with 23 light path of the parallel light tube connects;The parallel light tube 23 is connect with the incidence surface light path of the optical sample 40.First partially The optical device 21 that shakes can control the polarization direction for injecting laser in optical sample 40.Diaphragm 22 is adjustable circular iris or narrow Diaphragm is stitched, to control the optical quality of 40 laser of beam incident optical sample.Parallel light tube 23 to the laser of beam incident optical sample 40 into Row shaping is to control the angle of divergence of laser.
In one embodiment, the optics designed using laser light source 10 and 40 connected light path of optical sample as the present invention The working-spindle (l) of analytical instrument;Along the first polarization optics 21, the diaphragm of working-spindle (l) setting sequentially light path connection 22 and parallel light tube 23, the first polarization optics 21 can be around working-spindle (l) spinning.Diaphragm 22 is adjustable circular light Door screen or slit diaphragm.
Referring to Fig. 3, it is preferred that the system light path further includes:Semi-transparent/half-reflecting mirror 24 and auxiliary detector 25, it is described Semi-transparent/half-reflecting mirror 24 is connect with 23 light path of the parallel light tube;It is incident and/or be reflected into the semi-transparent/half-reflecting mirror 24 Laser connected with 25 light path of the auxiliary detector;Transmit the laser of the semi-transparent/half-reflecting mirror 24 and the optical sample 40 light paths connect.Reflection herein refers to that the light of generation is reflected on 40 incidence surface of optical sample.
Semi-transparent/half-reflecting mirror 24 can be rotated by 90 °, can by before beam incident optical sample 40 laser and by optical sample 40 it is anti- The laser being emitted back towards is sampled respectively, and the laser signal of the reflection laser of gained optical sample 40 and incident laser is reflected into Auxiliary detector 25 is analyzed.The refractive index of optical sample 40 is obtained to accurately measure.
Referring to Fig. 3, in one embodiment, carried using laser light source 10 and 40 connected light path of optical sample as the present invention The working-spindle (l) of the optic analytical instrument of confession;Along the first polarization optics of working-spindle (l) setting sequentially light path connection 21, diaphragm 22, parallel light tube 23 and semi-transparent/half-reflecting mirror 24.First polarization optics 21 can spin around working-spindle (l) Turn.Diaphragm 22 is adjustable circular iris or slit diaphragm.(l2) it is the central symmetry axis of auxiliary detector 25, it is semi-transparent/partly anti- Mirror 24 is penetrated to be set at (l2) and intersecting vertically (l).Auxiliary detector 25 is set on (l2), and with semi-transparent/half reflection 24 light path of mirror connects.
Preferably, the example platform 33 is around 33 center axis rotation of the example platform, and can read the degree of rotational angle Number.
Preferably, the method which can be used to implement above-mentioned optical material test with optic analytical instrument.
Example platform 33 has 360 ° of rotation functions of horizontal direction in the present invention, and can also accurate reading platform angle of rotation Degree, is easy to implement the refractive index for accurately measuring optical sample 40 with optic analytical instrument by optical material.Existing optical material The measurement method of refractive index has geometric method and interferometry, according to the difference of method, they to measuring the requirement different from of sample, Such as minimum deflection horn cupping, need optical material to be measured being processed into the prism to meet certain requirements, and it is to be measured in interferometry The optical material of amount can be plain film or wedge shaped sample, no matter which kind of measurement method, pass through acquisition measure sample accurate angle Value, can improve the measurement accuracy of refractive index.Similarly, the second nonlinear signal that laser generates in optical material is even more Closely related with angle, the rotation of example platform 33 and angle measurement function help to realize optical material relevant parameter and measure accurately.
Preferably, the energy intensity > 0 of the laser light source 10.It is furthermore preferred that the energy intensity of laser light source 10 is 0.5 ~107W/cm-2.Specific energy intensity can be selected according to the test request carried out.Such as in linear optic test, it can adopt With lower laser energy density;When carrying out second-order nonlinear optical test, then higher laser energy density is used.
Use the laser light source 10 of the intensity that can realize the phase transformation of the Accurate Analysis optical material in a manner of optical analysis Journey and domain structure variation.First, the monochromaticjty and directionality of laser light source 10 can ensure to accurately measure small in refractive index Variation, secondly, the energy response of laser are that the guarantee of sufficient intensity second nonlinear signal is generated in optical material.It considers The characteristic of optical material and the wavelength of light are closely related, and the wavelength of preferred laser light source 10 is replaceable.To realize pair The accurate measurement of various difference optical materials.
Preferably, the laser light source 10 is at least one of ultraviolet laser, visible wavelength lasers or near-infrared laser. Can be as needed, select the laser of single wavelength laser or multiple and different wavelength to irradiate optical sample 40 simultaneously.
Preferably, the outfield is temperature field and/or voltage field.Preferably, the loading device include thermal field device and For electric installation, the thermal field device is set on the example platform 33, and adjusts the temperature of the optical sample 40;The confession Electric installation is set on the example platform 33, and is powered to the optical sample 40.
Hereby, it is achieved that example platform 33, which can be optical sample 40, applies the thermal field and electric field that intensity is adjusted.Temperature is One of an important factor for causing material phase transformation and domain structure to change, therefore example platform provided by the invention 33 is needed to measuring sample The temperature of product control effectively.Electric field is introduced on measuring sample as needed simultaneously, to meet the particular/special requirement in studying.
Preferably, the thermal field device is stratie, the thermal field that the stratie provides be room temperature~ 500℃.The thermal field may act on optical sample 40.
Preferably, the thermal field device is semiconductor element, and the thermal field that the semiconductor element provides is -20~100 DEG C. Temperature range to adjust the optical sample 40 is -20~100 DEG C.
Preferably, the thermal field device is liquid nitrogen, and the thermal field that the liquid nitrogen provides is -100 DEG C~room temperature.To optical sample 40 are cooled down, and the temperature range that can adjust the optical sample 40 is -100 DEG C~room temperature.
Preferably, the electric field provided for electric installation is 0~10000V.Adjust the voltage range of the optical sample 40 For 0~10000V.The electric current generated for electric installation herein can be direct current or exchange.
Preferably, the main detector 53 is that the center of circle is rotated around the optical sample 40 with the optical sample 40.
Main detection instrument is rotated around test sample to acquire optical signalling, and different light may be selected according to the requirement of measurement Learn intensity, wavelength, polarization characteristic, image etc. of the detection instrument to acquire optical signalling.So as to obtain optical sample 40 not With the optical parameter of angle.
In order to meet the measurement request of optic analytical instrument provided by the invention, need setting suitable before main detector 53 Optical component to meet the requirement of signal acquisition.Optical polarizator, diaphragm and related optical can be placed before main detection instrument Device.
Referring to Fig. 2 and 3, it is preferred that the optical material further includes with optic analytical instrument:Main detector platform 51 and Two polarization optics 52, second polarization optics 52 are set to the main detector 53 and go out with the optical sample 40 In the connected light path of smooth surface;Second polarization optics 52 are set to the main detector platform with the main detector 53 On 51;The main detector platform 51 is that the center of circle is rotated around the optical sample 40 with the optical sample 40.
Preferably, the optical sample 40 is the angle of wedge prism that optical material is process, and the parameters of prism are full Sufficient measurement request places it in the center of example platform 33, can accurately be measured using minimum deflection horn cupping or autocollimation method The refractive index of the sample is rotated with main detector 53 around example platform 33, detects produced from optical sample 40 in place Raw second nonlinear signal.
As a specific embodiment, it has been presented in Fig. 3 provided by the present invention for optical material phase transformation and farmland A kind of exemplary operation form of optic analytical instrument of structural research, can be roughly divided into:Light source part a, system light path part b, sample Product terrace part c, explorer portion d.Including:Laser light source 10, the first polarization optics 21, diaphragm 22, directional light Pipe 23, semi-transparent/half-reflecting mirror 24, auxiliary detector 25, example platform 33 and optical sample 40.Second polarization optics 52 exist It is the polarization optics of optical signalling analyzing in one specific implementation mode.31 indicate the rotational trajectory of main detector 53.One In specific embodiment, main detector platform 51 can be rotated along main detector track 31 around optical sample, (l) be set for the present invention The working-spindle of the optic analytical instrument of meter, (l1) be by 33 center of example platform and the axis vertical with working-spindle (l), (l2) it is the central symmetry axis of auxiliary detector 25.
Laser light source 10 selects the radiation wavelength of laser according to the requirement for measuring analysis, and it is flat so that laser is passed through the sample The rotation center of platform 33, using laser light source 10 and 40 connected light path of optical sample as optic analytical instrument provided by the invention Working-spindle (l);It is anti-that the first polarization optics 21, diaphragm 22, parallel light tube 23 and semi-transparent/half are set along working-spindle (l) Mirror 24 is penetrated, the first polarization optics 21 can be rotated around working-spindle (l) to control the polarization of 40 laser of beam incident optical sample Direction, diaphragm 22 is adjustable circular iris or slit diaphragm, to control the optical quality of the laser of beam incident optical sample 40, is put down Row light pipe 23 carries out shaping to control the angle of divergence of laser to the laser of beam incident optical sample 40, and semi-transparent/half-reflecting mirror 24 can Be rotated by 90 °, respectively to before beam incident optical sample 40 laser and the laser that is reflected back by optical sample 40 sample, by laser Signal reflex is analyzed to auxiliary detector 25.It is process by optical material for optical sample 40, for a pair of parallel The optical plate of light pass surface is positioned over the rotation center of example platform 33, applies electricity in a certain range on optical sample 40 Press adjustable electric field, direction of an electric field is perpendicular or parallel to working-spindle (l), according to the requirement for measuring analysis, selects different attached Part controls the thermal field of optical sample 40.
Rotation center of the optical detector platform 51 along main detector track 31 around example platform 33 rotates, on the platform It is placed with main detector 53 and relevant optical component, main detector 53 acts on optical sample for receiving laser light source 10 Linear and nonlinear properties after 40, signal can be reflected from the transmission of optical sample 40 or optical sample 40, the second polarised light The most commonly used optical component before device 52 as main detector 53, for assisting main detector 53 to the inclined of laser signal Characteristic of shaking is analyzed, and according to application demand, more common optical component also has optical filter, decaying before main detector 53 Piece, diaphragm etc..
It, below will be with not for the optical material test method for more clearly describing the application and optic analytical instrument used The optical material test method of the application and optic analytical instrument used is further detailed in same embodiment.
Unless otherwise instructed, the raw material in the embodiment of the present invention is bought by commercial sources.
Embodiment 1 tests the refractive index and birefringent phenomenon for measuring sample using above-mentioned optical material with optic analytical instrument Dependency structure changes
A kind of specific implementation mode according to the present invention, as shown in figure 3, the phase transition process of research barium titanate ferroelectric crystal. Barium titanate ferroelectric crystal is processed into the optical sample 40 with a pair of parallel optics light pass surface, 2~10mm of thickness of sample, by it It is placed in the rotation center of example platform 33, -100~200 DEG C are provided for optical sample 40 by way of replacing thermal field attachment Temperature regulating range.Laser light source 10 uses 632.8nm He-Ne Lasers, and rotatably the first polarization optics 21 control laser Polarization direction be 45 °, direct irradiation optical sample 40;Main detector 53 uses CCD linear array detectors, is fixed on working-spindle (l) collimation amplification microscope group is placed in direction before the detector.Translational movement by measuring laser beam with respect to working-spindle (l), knot The angle for closing the normal and working-spindle (l) of 40 optics light pass surface of optical sample, calculates the refractive index of optical sample 40.Optics The temperature of sample 40 is from during -100 DEG C rise to 120 DEG C, it is observed that birefringent phenomenon, in -80 DEG C and 0 DEG C of position It sets, two-fold exit point has more apparent variation, and at 120 DEG C, birefringent phenomenon disappears, these three temperature spots correspond to tripartite respectively The transformation temperature of crystallographic system → rhombic system, rhombic system → tetragonal crystal system, tetragonal crystal system → cubic system.
Embodiment 2 tests the refractive index and birefringent phenomenon for measuring sample using above-mentioned optical material with optic analytical instrument Dependency structure changes
A kind of specific implementation mode according to the present invention, as shown in figure 3, the phase transition process of research barium titanate ferroelectric crystal. Barium titanate ferroelectric crystal is processed into the optical sample 40 of right-angle prism shape, and the wherein right-angle surface of prism is that a is tangential, is placed it in The rotation center of example platform 33 selects the temperature that suitable thermal field attachment provides room temperature to 200 DEG C for optical sample 40 to adjust Range.Laser light source 10 using high optical quality conjunction Shu Jiguang, optical maser wavelength include 473nm, 532nm, 632.8nm and 1064nm, laser irradiate after passing sequentially through the first polarization optics 21, diaphragm 22, parallel light tube 23, semi-transparent/half-reflecting mirror 24 Optical sample 40;Auxiliary detector 25 is using highly sensitive photoelectric type energy meter, and photoelectric type energy meter is equipped with diaphragm accurately to control Incident ray light path processed.Using autocollimation method, by the reflection of the apex angle and deflecting light beams of 25 accurate measuring prism of auxiliary detector Angle can accurately measure the refractive index of optical sample 40.The temperature of optical sample 40 rises to 200 DEG C from room temperature, optics The temperature of sample 40 is begun to ramp up from room temperature, before reaching 120 DEG C, it is observed that birefringent phenomenon, and accurately measure each Refractive index under wavelength corresponding to different polarization states, refractive index is with temperature slight change;When the temperature of optical sample 40 crosses 120 DEG C, i.e., internal crystal structure is changed into cubic system by tetragonal crystal system, and birefringent phenomenon disappears at this time, and refractive index generates variation.
Embodiment 3 tests the refractive index and birefringent phenomenon for measuring sample using above-mentioned optical material with optic analytical instrument Dependency structure changes
A kind of specific implementation mode according to the present invention, as shown in figure 3, the phase transition process of research lead titanates ferroelectric crystal. Lead titanates ferroelectric crystal is processed into the optical sample 40 of right-angle prism shape, and the wherein right-angle surface of prism is that a is tangential, is placed it in The rotation center of example platform 33 selects the temperature that suitable thermal field attachment provides room temperature to 500 DEG C for optical sample 40 to adjust Range, and apply an adjustable DC electric field on optical sample 40, voltage of electric field from 0~10000V, direction of an electric field perpendicular to Working-spindle (l).Laser light source 10 uses the 1064nm electro-optic modulation pulse lasers of high light beam quality, laser to pass sequentially through first Optical sample 40 is irradiated after polarization optics 21, diaphragm 22, semi-transparent/half-reflecting mirror 24;Main detector 53 uses silicon photoelectric type Energy meter is placed with edge filter before silicon photoelectric type energy meter, can filter out 1064nm optical signals, auxiliary detector 25 completely Using highly sensitive photoelectric type energy meter, photoelectric type energy meter is equipped with diaphragm to accurately control incident ray light path.Use autocollimatic Straight method can accurately measure optics by the reflection angle of the apex angle and deflecting light beams of 25 accurate measuring prism of auxiliary detector The refractive index of sample 40.Optical sample 40 is under the conditions of room temperature and arbitrary electric field strength, since domain structure existing for inside is orientated Arbitrarily, so birefringent phenomenon can not be shown, there are apparent scatterings;Reach certain when measuring institute's energization field intensity on sample Value, the electric field applied thereon start to embody effect, can be initially observed birefringent phenomenon, and birefringence is with electric field The raising of intensity and gradually become larger, birefringence no longer changes after reaching certain value, at the same the scattering phenomenon of crystals also compared with Initially weaken.While measuring refractive index, second nonlinear signal is acquired using main detector 53, in room temperature, second order is non- Linear signal contacts less with crystallographic direction, with the reinforcement of the raising and effect electric field of temperature on optical sample 40, second order Nonlinear properties are associated with slow promotion, temperature and electric field with the directionality of crystal more than after a certain range, and laser is big absolutely along crystal The second nonlinear signal that part direction generates is faint compared with room temperature, and only in particular directions, second nonlinear signal is apparent Reinforce.It can be by realizing the control to temperature on optical sample 40 to 40 additional heating device of optical sample.
The above is only several embodiments of the present invention, not any type of limitation is done to the present invention, although this hair It is bright to be disclosed as above with preferred embodiment, however not to limit the present invention, any person skilled in the art is not taking off In the range of technical solution of the present invention, makes a little variation using the technology contents of the disclosure above or modification is equal to Case study on implementation is imitated, is belonged in technical proposal scope.

Claims (10)

1. a kind of method of optical material test, which is characterized in that include 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:The outfield is adjusted, the optical information is analyzed by optical detecting method, it is brilliant to obtain the optics For the two-fold exit point and/or refractive index of body with the variation in the outfield, it is corresponding described that the analysis variation obtains each outfield The phase transformation or domain structure of optical sample change;
The outfield is temperature field and/or electric field.
2. the method for optical material test according to claim 1, which is characterized in that the optical information is birefringence Rate, the optical detecting method detect for polarization optics.
3. the method for optical material test according to claim 1, which is characterized in that the optical information is birefringence And refractive index, the optical detecting method detect for refractive index.
4. the method for optical material test according to claim 1, which is characterized in that the optical information is that scattering is believed Breath, the optical detecting method are optical scattering.
5. the method for optical material test according to claim 1, which is characterized in that the optical detecting method is second order Nonlinear effect, the optical information are phase transformation and microstructure.
6. a kind of optical material optic analytical instrument, which is characterized in that including:Laser light source, example platform and main detector, Optical sample is set on the example platform, and the laser light source is connect with the incidence surface light path of the optical sample;
The main detector is connect with the light-emitting surface light path of the optical sample, and the example platform includes loading device, described Loading device loads at least one outfield to the optical sample.
7. optical material optic analytical instrument according to claim 6, which is characterized in that the optical material optics Analytical instrument further includes:System light path, the system light path are set to the incidence surface of the laser light source and the optical sample Connection light path in, the system light path includes:First polarization optics, diaphragm and parallel light tube, the laser light source with The first polarization optics light path connection;
First polarization optics are connect with the diaphragm light path;The diaphragm is connect with the parallel light tube light path;Institute Parallel light tube is stated to connect with the incidence surface light path of the optical sample.
8. optical material optic analytical instrument according to claim 7, which is characterized in that the system light path also wraps It includes:Semi-transparent/half-reflecting mirror and auxiliary detector, the semi-transparent/half-reflecting mirror are connect with the parallel light tube light path;
Laser that is incident and/or being reflected into the semi-transparent/half-reflecting mirror is connect with the auxiliary detector light path;Described in transmission The laser of semi-transparent/half-reflecting mirror is connect with the optical sample light path.
9. optical material optic analytical instrument according to claim 6, which is characterized in that the energy of the laser light source Intensity > 0;
The laser light source is at least one of ultraviolet laser, visible wavelength lasers or near-infrared laser.
10. optical material optic analytical instrument according to claim 6, which is characterized in that the optical material is used up It learns analytical instrument and is used for the method such as optical material according to any one of claims 1 to 5 test.
CN201810460434.8A 2018-05-15 2018-05-15 Optical material test method and optic analytical instrument used Pending CN108593563A (en)

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