CN108414444A - A kind of non-contact type superconducting thin-film material superconduction phase transformation and Photoinduced Electron local effect test device and its working method - Google Patents

A kind of non-contact type superconducting thin-film material superconduction phase transformation and Photoinduced Electron local effect test device and its working method Download PDF

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CN108414444A
CN108414444A CN201810195430.1A CN201810195430A CN108414444A CN 108414444 A CN108414444 A CN 108414444A CN 201810195430 A CN201810195430 A CN 201810195430A CN 108414444 A CN108414444 A CN 108414444A
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sample
temperature
light
reflectivity
light intensity
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张飒飒
陈霞
张衍敏
陈天弟
孙腾飞
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Shandong University
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    • 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
    • G01N21/01Arrangements or apparatus for facilitating the optical investigation
    • 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
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3563Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor

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Abstract

The present invention relates to a kind of non-contact type superconducting thin-film material superconduction phase transformations and Photoinduced Electron local effect test device and its working method.The present invention is measured the reflectivity of superconducting film material using the near-infrared optical reflectance spectrum technology of alternating temperature, then passes through the superconduction phase transformation of reflectivity, absorptivity, transmitance and photoconduction, the relationship analysis superconducting film material of D.C. resistance;Recycle whether the modified De Lude model analysis of Smith has occurred Photoinduced Electron local effect.

Description

A kind of non-contact type superconducting thin-film material superconduction phase transformation and Photoinduced Electron local effect Test device and its working method
Technical field
The present invention relates to a kind of non-contact type superconducting thin-film material superconduction phase transformations and Photoinduced Electron local effect test dress It sets and its working method, belongs to the technical field of superconducting film material optical research.
Background technology
Near-infrared reflection experiment is a kind of powerful optical technology, the non-contact characterization for superconductor material and research. Currently, the information such as the specific heat of superconducting film material, electronic transport, magnetic transport and tunnel frequency spectrum have been obtained for widely studying so It is and also fewer in optics aspect research to superconducting film material in the prior art, wherein superconduction phase transformation and Photoinduced Electron office Domain effect becomes research hotspot in recent years.
The research method of superconduction phase transformation and Photoinduced Electron local effect includes electricity means and optical instrument.Wherein, sharp Electricity consumption learns to do section measurement superconduction phase transformation and Photoinduced Electron local effect is complex, and the super of material is observed using AC resistance method Lead phase transformation has destructiveness to sample, and requirement of experiment is relatively high.Conventional optical instrument is typically using ellipsometer, sweeps Retouch electron microscope, XRD or transmission spectrum (bibliography:M.skiB.Kos′cielska, W.Sadowski.Structural and optical investigations of sol–gel derived lithium titanate thin films.Journal of Alloys and Compounds,Volume 536,2012,Pages 30- 32.);But above-mentioned optical instrument be to material it is simple characterization or compare, be unable to get material superconduction phase transition temperature or Electronic localization effect.
The superconducting thin film of fixed doping can be changed into superconducting phase with the variation of temperature by normal state, some superconductors are also There are counterfeit energy gap phases.For superconductor, the transition process and corresponding transition temperature (i.e. superconduction phase transition temperature) are to understand The pith of superconduction formation mechenism.
Electronic localization refers to that electronics is limited in some region, relatively large with electron mean free path, sample size It is small, free from admixture, unordered related;Impurity is more, unordered degree is bigger, and electronics is bigger by the possibility of local.Under light field, I Can detect superconductor electronic localization phenomenon, electronic localization is illustrated by parameter c in Drude-Smith models, and c is Negative value, numerical value is smaller, and electron backscattered degree is stronger, and electronic localization degree is bigger.The direction of motion after back scattering occurs for electronics With before on the contrary, cruising property be deteriorated.
In the prior art, since superconducting thin film sample preparation is difficult, contact type measurement is easy pollution even damage sample.Than It is needed in sample surfaces welding electrode as four probe method measures resistance characteristic, it is not only more demanding to experimental technique, it can also be to sample Product surface generates destructiveness, influences the use of other follow-up measurement means.
Invention content
In view of the deficiencies of the prior art, a kind of non-contact type superconducting thin-film material superconduction phase transformation of present invention offer and photoinduction Electronic localization effect test device.
The present invention provides a kind of working method of above-mentioned superconduction phase transformation and Photoinduced Electron local effect test device.
Summary of the invention:
The present invention is measured the reflectivity of superconducting film material using the near-infrared optical reflectance spectrum technology of alternating temperature, Then pass through reflectivity, absorptivity, transmitance and photoconduction, the superconducting phase of the relationship analysis superconducting film material of D.C. resistance Become;Recycle whether the modified De Lude model analysis of Smith has occurred Photoinduced Electron local effect.
The technical scheme is that:
A kind of non-contact type superconducting thin-film material superconduction phase transformation and Photoinduced Electron local effect test device, including press light Wide range infrared light supply that road is set gradually, the first beam-expanding collimation mirror, chopper, the second beam-expanding collimation mirror, low temperature sample room, third Beam-expanding collimation mirror, the 4th beam-expanding collimation mirror, monochromator and photodetector;The chopper passes sequentially through lock-in amplifier sum number It is connect with computer according to capture card;The lock-in amplifier is also connect with photodetector.
The wide range infrared light supply provides the light of a certain range of each wavelength.Beam-expanding collimation mirror ensures beam collimation, After focusing in normal incidence to sample and monochromator.Monochromator is used to extract the single wavelength in wide range infrared light;Photodetector Light intensity for measuring different wave length.The combination of the chopper and lock-in amplifier extracts small-signal from ambient noise Out.
According to currently preferred, the monochromator is connected with multiple photodetectors;Near infrared band corresponds to InGaAs Photodetector, it is seen that optical band corresponds to Si photodetectors, and far infrared band corresponds to TeCdHg detectors.
According to currently preferred, the low temperature sample room is no liquid helium closed loop device.The no liquid helium closed loop dress It is a kind of existing apparatus system to set, by cold head, cryostat, temperature controller, compressor, radiator (air-cooled or water cooling), The compositions such as vacuum pump.
According to currently preferred, the range of temperature of the low temperature sample room is 10mK~300K.
A kind of working method of superconduction phase transformation and Photoinduced Electron local effect test device, including steps are as follows:
1) light source switch is opened, the wide range infrared light supply sends out wide range infrared light, passes through the first beam-expanding collimation mirror, second Beam-expanding collimation mirror, third beam-expanding collimation mirror and the 4th beam-expanding collimation mirror debug light path, and hot spot convergent point is radiated at cryogenic sample The center of golden mirror, makes the slit of the vertical normal incidence monochromator of reflected light in room;
2) sample is fixed on to the hot spot irradiation position of Jin Jingshang;Open lock-in amplifier, chopper, monochromator and calculating Machine;Lock-in amplifier controls the noise in the chopper separation wide range infrared light, reduces influence of noise;
3) low temperature sample room is sealed, controls the vacuum degree of low temperature sample room to 10-3Torr or less;Change sample environment temperature To assigned temperature;
4) after sample environment temperature is down to assigned temperature, single wavelength is extracted from wide range infrared light by monochromator Exciting light detects corresponding reflective light intensity by photodetector;Change sample environment temperature to next temperature according to temperature interval M Degree point;Temperature interval M in the step 4) is variable, and the temperature interval setting of initial stage cooling is wider, attached close to transition temperature Closely, shorten temperature interval M, finely measured.
5) it repeats step 4) and obtains the correspondence of sample excitation wavelength and reflective light intensity at different ambient temperatures;
6) it is used as with reference to piece using gold or copper, when obtaining wide range infrared light supply and being irradiated on gold or copper, under different temperatures, is excited The correspondence of optical wavelength and reflective light intensity;The reflectivity of gold and copper is close to 1;
7) by step 5), 6) in data draw the temperature dependence curve of sample and reference plate;The temperature-independent is bent Line refers to one timing of temperature, the correspondence of excitation wavelength and reflective light intensity;It is infrared with the reflective light intensity divided by wide range of sample The light intensity of light obtains the reflectivity of sample;Finally obtain the curve that sample reflectivity changes with excitation wavelength;
8) observation of steps 7) obtain temperature dependence curve, draw under same excitation wavelength, sample reflectivity is with temperature Temperature at turning point is tentatively judged as superconduction phase transition temperature by the curve of variation;If the temperature at turning point is surveyed with electricity The superconducting transition temperature of amount then judges the temperature at break for superconduction transformation temperature within the M of temperature interval;
Significant change can occur for resistance at the superconducting transition temperature of electrical measurement, be reduced to 0 resistance.If surveyed using optics Amount, reflectivity intensity can change near the temperature, a turnover occur.
9) the sample reflectivity obtained according to step 7) uses Smith-Drude models with the curve of wavelength change:It is analyzed, works as cnIt is standard De Lude models when=0, does not consider electronics office Domain effect, then the reflectivity of light reduce with the increase of excitation wavelength;Work as cnWhen ≠ 0, the reflectivity of light is with excitation light wave Long increase and increase;If occurring reflectivity under same temperature with the increase of excitation wavelength to increase, judge occur Electronic localization phenomenon;
Preferably, after the step 9), the sample of different crystal orientations is analyzed, obtains the dc resistivity of different crystalline phase samples pxxAnd the relativeness of reflective light intensity, to obtain anisotropic properties;Detailed process is:
Utilize A+R+T=1, A (ω) ≈ σ1(ω)d/ε0Cn, Tinkham equationAnd σ (ω)∝1/ρxxRelationship, obtain reflective light intensity and dc resistivity ρxxRelational graph;Wherein, A is the absorptivity of sample, and T is The transmissivity of sample, n are the refractive index of sample, z0It is free space impedance, nsubIt is the refractive index of sample substrate, R is reflected light By force;σ is compound light conductivity, σ1It is the real part of compound light conductivity;D is the thickness of sample thin film, ε0It is permittivity of vacuum, ω is Frequency,C is the light velocity.It is opaque in surveyed wave band for specific sample, and resistance very little under superconducting state, resistance Rate is very big, and photoconductivity is also very big, so existing almost without transmission.According to above-mentioned formula, can be fitted to obtain D.C. resistance Rate with reflective light intensity relational graph.
According to currently preferred, the temperature dependence curve in the step 7) is drawn by Data Analysis Software origin It obtains;" curve that sample reflectivity varies with temperature " in the step 8) is drawn by Data Analysis Software origin It arrives.
Beneficial effects of the present invention are:
1. superconduction phase transformation of the present invention and Photoinduced Electron local effect test device, simple by non-contacting mode It is effectively obtained the superconduction phase transition temperature or electronic localization effect of material;It effectively avoids polluting and destroying caused by sample, more Duplicate measurements easy to implement.
Description of the drawings
Fig. 1 is the structural schematic diagram of superconduction phase transformation of the present invention and Photoinduced Electron local effect test device;
Wherein, 1, wide range infrared light supply;2, the first beam-expanding collimation mirror;3, the second beam-expanding collimation mirror;4, chopper;5, low temperature Sample room;6, third beam-expanding collimation mirror;7, the 4th beam-expanding collimation mirror;8, monochromator;9, photodetector;10, lock-in amplifier; 11, data collecting card;12, computer;13, sample.
Specific implementation mode
With reference to embodiment and Figure of description, the present invention will be further described, but not limited to this.
Embodiment 1
As shown in Figure 1.
A kind of non-contact type superconducting thin-film material superconduction phase transformation and Photoinduced Electron local effect test device, including press light Wide range infrared light supply 1 that road is set gradually, the first beam-expanding collimation mirror 2, chopper 4, the second beam-expanding collimation mirror 3, low temperature sample room 5, third beam-expanding collimation mirror 6, the 4th beam-expanding collimation mirror 7, monochromator 8 and photodetector 9;The chopper 4 passes sequentially through lock Phase amplifier 10 and data collecting card 11 are connect with computer 12;The lock-in amplifier 10 is also connect with photodetector 9.
The wide range infrared light supply 1 provides the light of a certain range of each wavelength.Beam-expanding collimation mirror ensures beam collimation, After focusing in normal incidence to sample and monochromator 8.Monochromator 8 is used to extract the single wavelength in wide range infrared light;Photodetection Device 9 is used to measure the light intensity of different wave length.The combination of the chopper 4 and lock-in amplifier 10 is by small-signal from ambient noise In extract.
The low temperature sample room 5 is the Cryofree series nothings of Oxford Instruments (Oxford Instrument) company production Liquid helium closed loop device.The range of temperature of the low temperature sample room 5 is 10mK~300K.
Embodiment 2
Non-contact type superconducting thin-film material superconduction phase transformation as described in Example 1 and Photoinduced Electron local effect test dress It sets, the difference is that the monochromator 8 is connected with multiple photodetectors 9;Near infrared band corresponds to InGaAs photodetections Device, it is seen that optical band corresponds to Si photodetectors, and far infrared band corresponds to TeCdHg detectors.
Embodiment 3
The working method of superconduction phase transformation and Photoinduced Electron local effect test device as described in embodiment 1 or 2, including Steps are as follows:
1) light source switch is opened, the wide range infrared light supply 1 sends out wide range infrared light, passes through the first beam-expanding collimation mirror 2, the Two beam-expanding collimation mirrors 3, third beam-expanding collimation mirror 6 and the 4th beam-expanding collimation mirror 7 debug light path, and hot spot convergent point is radiated at low temperature The center of golden mirror in sample room 5 makes the slit of the vertical normal incidence monochromator of reflected light 8;
2) sample is fixed on to the hot spot irradiation position of Jin Jingshang;Open lock-in amplifier 10, chopper 4,8 and of monochromator Computer 12;Lock-in amplifier 10 controls the noise in the separation wide range infrared light of the chopper 4, reduces influence of noise;
3) low temperature sample room 5 is sealed, controls the vacuum degree of low temperature sample room 5 to 10-3torr;Change sample environment temperature extremely Assigned temperature;
4) after sample environment temperature is down to assigned temperature, single wavelength is extracted from wide range infrared light by monochromator 8 Exciting light, corresponding reflective light intensity is detected by photodetector 9;Change sample environment temperature under according to temperature interval M One temperature spot;Temperature interval M in the step 4) is variable, and the temperature interval setting of initial stage cooling is wider, close to transformation temperature Near degree, shortens temperature interval M, finely measured.
5) it repeats step 4) and obtains the correspondence of sample excitation wavelength and reflective light intensity at different ambient temperatures;
6) Jin Shangshi is irradiated to as with reference to piece, obtaining wide range infrared light supply using gold, under different temperatures, excitation wavelength and The correspondence of reflective light intensity;
7) by step 5), 6) in data draw the temperature dependence curve of sample and reference plate;The temperature-independent is bent Line refers to one timing of temperature, the correspondence of excitation wavelength and reflective light intensity;It is infrared with the reflective light intensity divided by wide range of sample The light intensity of light obtains the reflectivity of sample;Finally obtain the curve that sample reflectivity changes with excitation wavelength;
8) observation of steps 7) obtain temperature dependence curve, draw under same excitation wavelength, sample reflectivity is with temperature Temperature at turning point is tentatively judged as superconduction phase transition temperature by the curve of variation;If the temperature at turning point is surveyed with electricity The superconducting transition temperature of amount then judges the temperature at break for superconduction transformation temperature within the M of temperature interval;
Significant change can occur for resistance at the superconducting transition temperature of electrical measurement, be reduced to 0 resistance.If surveyed using optics Amount, reflectivity intensity can change near the temperature, a turnover occur.
9) the sample reflectivity obtained according to step 7) uses Smith-Drude models with the curve of wavelength change:It is analyzed, works as cnIt is standard De Lude models when=0, does not consider electronic localization Change effect, then the reflectivity of light reduces with the increase of excitation wavelength;Work as cnWhen ≠ 0, the reflectivity of light is with excitation wavelength Increase and increase;If occurring reflectivity under same temperature with the increase of excitation wavelength to increase, it is judged that there is Electronic localization phenomenon;
Sample in the present embodiment is spinelle film sample;LiTi2O4Film thickness is 200nm, and substrate thickness is 25mm;Surface starts the cleaning processing;Using deuterium lamp as wide range infrared light supply;
Temperature dependence curve in the step 7) is drawn to obtain by Data Analysis Software origin;In the step 8) " curve that sample reflectivity varies with temperature " draw to obtain by Data Analysis Software origin.
Embodiment 4
The working method of superconduction phase transformation and Photoinduced Electron local effect test device as described in Example 3, further , after the step 9), the sample of different crystal orientations is analyzed, obtains the dc resistivity ρ of different crystalline phase samplesxxAnd reflected light Strong relativeness, to obtain anisotropic properties;Detailed process is:
Utilize A+R+T=1, A (ω) ≈ σ1(ω)d/ε0Cn, Tinkham equationAnd σ (ω)∝1/ρxxRelationship, obtain reflective light intensity and dc resistivity ρxxRelational graph;Wherein, A is the absorptivity of sample, and T is The transmissivity of sample, n are the refractive index of sample, z0It is free space impedance, nsubIt is the refractive index of sample substrate, R is reflected light By force;σ is compound light conductivity, σ1It is the real part of compound light conductivity;D is the thickness of sample thin film, ε0It is permittivity of vacuum, ω is Frequency,C is the light velocity.It is opaque in surveyed wave band for specific sample, and resistance very little under superconducting state, resistance Rate is very big, and photoconductivity is also very big, so existing almost without transmission.According to above-mentioned formula, can be fitted to obtain D.C. resistance Rate with reflective light intensity relational graph.

Claims (5)

1. a kind of non-contact type superconducting thin-film material superconduction phase transformation and Photoinduced Electron local effect test device, feature exist In including wide range infrared light supply, the first beam-expanding collimation mirror, chopper, the second beam-expanding collimation mirror, the low temperature set gradually by light path Sample room, third beam-expanding collimation mirror, the 4th beam-expanding collimation mirror, monochromator and photodetector;The chopper passes sequentially through lock Phase amplifier and data collecting card are connect with computer;The lock-in amplifier is also connect with photodetector.
2. non-contact type superconducting thin-film material superconduction phase transformation according to claim 1 and the test of Photoinduced Electron local effect Device, which is characterized in that the monochromator is connected with multiple photodetectors;Near infrared band corresponds to InGaAs photodetections Device, it is seen that optical band corresponds to Si photodetectors, and far infrared band corresponds to TeCdHg detectors.
3. non-contact type superconducting thin-film material superconduction phase transformation according to claim 1 and the test of Photoinduced Electron local effect Device, which is characterized in that the range of temperature of the low temperature sample room is 10mK~300K.
4. according to the work side of superconduction phase transformation and Photoinduced Electron local effect test device described in claim 1-3 any one Method, which is characterized in that including steps are as follows:
1) light source switch is opened, the wide range infrared light supply sends out wide range infrared light, expanded by the first beam-expanding collimation mirror, second Collimating mirror, third beam-expanding collimation mirror and the 4th beam-expanding collimation mirror debug light path, and hot spot convergent point is radiated in low temperature sample room The center of Jin Jing makes the slit of the vertical normal incidence monochromator of reflected light;
2) sample is fixed on to the hot spot irradiation position of Jin Jingshang;Open lock-in amplifier, chopper, monochromator and computer; Lock-in amplifier controls the noise in the chopper separation wide range infrared light, reduces influence of noise;
3) low temperature sample room is sealed, controls the vacuum degree of low temperature sample room to 10-3Torr or less;Change sample environment temperature extremely to refer to Constant temperature degree;
4) after sample environment temperature is down to assigned temperature, the excitation of single wavelength is extracted from wide range infrared light by monochromator Light detects corresponding reflective light intensity by photodetector;Change sample environment temperature to next temperature according to temperature interval M Point;
5) it repeats step 4) and obtains the correspondence of sample excitation wavelength and reflective light intensity at different ambient temperatures;
6) it is used as using gold or copper with reference to piece, when obtaining wide range infrared light supply and being irradiated on golden or copper, under different temperatures, excitation light wave The long correspondence with reflective light intensity;
7) by step 5), 6) in data draw the temperature dependence curve of sample and reference plate;The temperature dependence curve is Refer to one timing of temperature, the correspondence of excitation wavelength and reflective light intensity;With the reflective light intensity of sample divided by wide range infrared light Light intensity obtains the reflectivity of sample;Finally obtain the curve that sample reflectivity changes with excitation wavelength;
8) observation of steps 7) obtain temperature dependence curve, draw under same excitation wavelength, sample reflectivity varies with temperature Curve, the temperature at turning point is tentatively judged as superconduction phase transition temperature;If temperature and electrical measurement at turning point Superconducting transition temperature then judges the temperature at break for superconduction transformation temperature within the M of temperature interval;
9) the sample reflectivity obtained according to step 7) uses Smith-Drude models with the curve of wavelength change:It is analyzed, works as cnIt is standard De Lude models when=0, does not consider electronic localization Change effect, then the reflectivity of light reduces with the increase of excitation wavelength;Work as cnWhen ≠ 0, the reflectivity of light is with excitation wavelength Increase and increase;If occurring reflectivity under same temperature with the increase of excitation wavelength to increase, it is judged that there is Electronic localization phenomenon.
5. the working method of superconduction phase transformation according to claim 4 and Photoinduced Electron local effect test device, special Sign is, after the step 9), analyzes the sample of different crystal orientations, obtains the dc resistivity ρ of different crystalline phase samplesxxAnd it is anti- The relativeness for penetrating light intensity, to obtain anisotropic properties;Detailed process is:
Utilize A+R+T=1, A (ω) ≈ σ1(ω)d/ε0Cn, Tinkham equationAnd σ (ω) ∝1/ρxxRelationship, obtain reflective light intensity and dc resistivity ρxxRelational graph;Wherein, A is the absorptivity of sample, and T is sample Transmissivity, n is the refractive index of sample, z0It is free space impedance, nsubIt is the refractive index of sample substrate, R is reflective light intensity;σ It is compound light conductivity, σ1It is the real part of compound light conductivity;D is the thickness of sample thin film, ε0It is permittivity of vacuum, ω is frequency,C is the light velocity.
CN201810195430.1A 2018-03-09 2018-03-09 A kind of non-contact type superconducting thin-film material superconduction phase transformation and Photoinduced Electron local effect test device and its working method Pending CN108414444A (en)

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Application publication date: 20180817