CN108226040A - A kind of assay method and device of two-dimensional material photo-thermal effect - Google Patents

A kind of assay method and device of two-dimensional material photo-thermal effect Download PDF

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Publication number
CN108226040A
CN108226040A CN201810044280.4A CN201810044280A CN108226040A CN 108226040 A CN108226040 A CN 108226040A CN 201810044280 A CN201810044280 A CN 201810044280A CN 108226040 A CN108226040 A CN 108226040A
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light
dimensional material
polarization
prism
photo
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刘智波
高晓光
田建国
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Nankai University
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Nankai University
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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
    • G01N21/01Arrangements 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
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • 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
    • G01N21/84Systems specially adapted for particular applications

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  • Health & Medical Sciences (AREA)
  • Physics & Mathematics (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)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Investigating Or Analyzing Materials Using Thermal Means (AREA)

Abstract

A kind of method of highly sensitive detection two-dimensional material photo-thermal effect, polarization absorption effect based on pump probe technology and two-dimensional material under total internal reflection structure, two-dimensional material is irradiated using pump light, two-dimensional material generates heat after absorbing light, and be transmitted in surrounding medium, since temperature change causes surrounding medium refraction index changing during heat propagation.It will detect light using convex lens and focus on and irradiated in two-dimensional material by prism total internal reflection mode, reflected light is separated the light of s polarizations and p-polarization using polarization spectro, the electric signal difference of s polarizations and p-polarization is measured by balanced detector, and then obtains the variations in refractive index caused by photo-thermal effect.Pump light is modulated in the measurements, and modulation intelligence is fed back in lock-in amplifier, while differential detector electric signal is input to lock-in amplifier, measurement to Photothermal Signals is realized using phase enlarging function is locked.The present invention is suitable for the photo-thermal effect of the different two-dimensional materials such as research graphene, molybdenum disulfide, black phosphorus, rhenium disulfide.

Description

A kind of assay method and device of two-dimensional material photo-thermal effect
Technical field
The invention belongs to two-dimensional materials and Opto-thertnal detection technical field, are related to a kind of using pump probe technology and complete interior anti- Penetrate two-dimensional material photo-thermal effect assay method and device that structure is combined.
Background technology
After photo-thermal effect refers to the irradiation of material light, photon energy interacts with lattice, vibration aggravation, temperature raising, by The electrology characteristic of substance is caused, and as heat propagation causes the variation of surrounding medium refractive index in the variation of temperature.Utilize light The detector of fuel factor:Thermistor, thermocouple, thermoelectric pile and pyroelectric detector etc..Photo-thermal effect is also used as a kind of optics The Measurement for Biotechnique of dependence has the advantages such as high-resolution, high contrast, can realize photothermal imaging, with other bio-imagings Good complementation is formd with detection method.Pump light research object is absorbed in photo-thermal effect, followed by releases heat Cause the variation of local indexes of refraction.Photothermal imaging technology provides very sensitive hand to measure the non-fluorescent molecules in solution Section.Research gold nano grain is already used to, directly intracellular mitochondria is imaged or even is realized sensitive unimolecule examines It surveys.At present, photothermal imaging is mainly the scattering of detection light to be caused to measure using thermotropic variations in refractive index, it is desirable that photo-thermal into As experimental provision is often extremely complex.
The two-dimensional materials such as graphene, transient metal sulfide (TDMCs), hexagonal boron nitride (hBN), black phosphorus are due to its uniqueness Two-dimensional structure and excellent photoelectron performance and obtain extensive research.In these two-dimensional materials, graphene, curing Molybdenum, hexagonal boron nitride etc. have isotropic electricity, optics, calorifics and mechanical property in plane, the tools such as black phosphorus, rhenium disulfide There are electricity, optics, calorifics and the mechanical property of anisotropic.For the photo-thermal effect of these two-dimensional materials, bio-imaging, Biological detection etc. has potential application value, however how to measure the photo-thermal effect of these two-dimensional materials, does not have also at present There is ripe method, especially to the monocrystal thin films of high quality, due to the limitation of its dimensional structure, traditional Opto-thertnal detection technology It can not realize the photothermal measurement of two-dimensional material.
Invention content
The object of the present invention is to provide a kind of methods and dress of measurement two-dimensional material photo-thermal effect that can be highly sensitive It puts, so as to the more accurately photo-thermal property of study two-dimensional material and its application in bio-sensing etc..
To achieve the above object, the step of the method for the invention is as follows:
The first step, the preparation of two-dimensional material are made on prism on a quartz substrate or directly with the method for mechanical stripping It is standby, obtain the sample of mechanical stripping;
Second step does a sink around two-dimensional material with PDMS, has added liquid medium and has used coverslip again later Encapsulation, in order to avoid generate bubble;
Third walks, and detection light part is incident using circularly polarized light or non-polarized light, is converged to by 50 times of object lens with mesh The prism of two-dimensional material and the interface of base material are marked, total reflection light is divided into the two of s polarizations and p-polarization using polarization spectro Shu Guang uses balanced detector detection s polarizations and the electric signal of p-polarization after being focused on respectively with object lens mirror.Adjust height and prism Angle makes focal beam spot beat on the base material contacted with graphene, and is totally reflected at the interface, is moved with translation stage Dynamic base material overlaps two-dimensional material and detection hot spot;
After 4th step, two-dimensional material sample and detection hot spot overlap, the attenuator before adjustment detector makes s inclined It shakes as the intensity of p-polarization light;
5th step introduces the linear polarization pump light by acousto-optic modulator modulation, and the pump light that will have been focused on, detection light is also There is sample three coincidence;
Acousto-optic modulator feeds back to the modulating frequency of pump light lock-in amplifier, while will detect flash ranging by the 6th step The s polarizations of amount and the electric signal of p-polarization are input to lock-in amplifier and carry out signal measurement, by the angle of polarization for changing pump light Degree, to record the variation of Photothermal Signals.
Description of the drawings
The light path schematic diagram of Fig. 1 Photothermal Signals detection;
The optics picture and Photothermal Signals of Fig. 2 graphene samples are by force with the datagram that pump light polarization angle changes;
The optics picture and Photothermal Signals of Fig. 3 black phosphorus samples are by force with the datagram that pump light polarization angle changes;
The optics picture and Photothermal Signals of Fig. 4 rhenium disulfide samples are by force with the data that pump light polarization angle changes Figure.
Specific embodiment
In order to further illustrate the present invention, below in a manner of attached drawing and with reference to example to two-dimensional material provided by the invention Photo-thermal effect measuring method and device are described in detail, but cannot be understood as limiting the scope of the present invention.With Material and instrument employed in lower embodiment are commercially available.In addition, any method similar or impartial to described content and Material is all applied in the method for the present invention.
Embodiment 1
The detection of graphene Photothermal Signals
As shown in Figure 2 a, few layer graphene is prepared on a quartz substrate with the method for mechanical stripping first, in few layer of graphite PDMS sinks are made around alkene, alcohol is added dropwise as photo-thermal medium, is finally encapsulated with coverslip.The pump light that will have been focused on is visited It surveys light and sample overlaps and generates Photothermal Signals later.Graphene Photothermal Signals are observed by changing the polarization angle of pump light Variation.Because of isotropism in graphene face, significant change does not occur for the size of Photothermal Signals in figure 2b.
Embodiment 2
Fig. 3 a are shown prepares few layer of black phosphorus sample on a quartz substrate with the method for mechanical stripping.Black phosphorus is in face Anisotropic material.With the thickness of atomic force microscope (AFM) test sample, obtaining the thickness of different zones sample is respectively 5nm, 8nm and 13nm, the Photothermal Signals of test different zones black phosphorus sample have obtained Fig. 3 b.Wherein Photothermal Signals maximum when pair Black phosphorus crystal orientation AC directions are answered, minimum value corresponds to black phosphorus ZZ directions, and by testing the reflectance spectrum of black phosphorus, the above results, which are obtained for, to be tested Card.The pumping light power 300 μ W, detection of optical power 3mW used in test.
Embodiment 3
Fig. 4 a show rhenium disulfide micro-image, and rhenium disulfide equally has intra-face anisotropy, with AFM test samples Thickness.And in different-thickness region, the Photothermal Signals of the polarization angle test sample by changing pump light.Obtained data Figure such as Fig. 4 b.The pumping light power 300 μ W, detection of optical power 5mW used in test.

Claims (9)

1. a kind of assay method of two-dimensional material photo-thermal effect, it is characterised in that the light of various two-dimensional materials can be measured in real time Thermal signal, the method include:Two-dimensional material is attached to prism surface first, and one layer is covered thoroughly above two-dimensional material Bright medium will be irradiated to by medium in two-dimensional material by the pump light that acousto-optic modulator is modulated, and two-dimensional material absorbs pumping Heat is generated after light, and is transmitted in the medium around covered, medium causes the change of refractive index due to temperature change.Using convex Lens, which will detect light and focus on, to be irradiated by prism total internal reflection mode in two-dimensional material, and reflected light is polarized s using polarization spectro It is separated with the light of p-polarization, the electric signal difference of s polarizations and p-polarization is measured by balanced detector, and then obtain imitating due to photo-thermal It should caused variations in refractive index.Pump light is modulated in the measurements, and modulation intelligence is fed back in lock-in amplifier, together When differential detector electric signal is input to lock-in amplifier, realize measurement to Photothermal Signals using phase enlarging function is locked.
2. according to the method described in claim 1, it is characterized in that, measured two-dimensional material includes:Isotropic two dimension Material, such as graphene, molybdenum disulfide;Anisotropic two-dimensional material, such as black phosphorus, rhenium disulfide.
3. according to the method described in claim 1, it is characterized in that, the combination of two-dimensional material and prism can be directly by graphite Alkene, which attaches to, to be attached on prism or first by two-dimensional material on transparent sheet, is then mutually tied with prism by index-matching fluid It closes.
4. according to the method described in claim 1, it is characterized in that, the medium covered above two-dimensional material includes:Solid dielectric, Such as PMMA, PDMS, silica;Liquid medium, such as water, alcohol, chloroform.
5. a kind of measurement device of two-dimensional material photo-thermal effect, which is characterized in that including:Light unit is detected, while there is S-polarization It can be circularly polarized light, 45 degree of linearly polarized lights or non-polarized light with two kinds of polarised lights of P polarization, emergent light is divided into s polarizations and p Two-beam is polarized, measures the opposite variation of two kinds of polarised lights;Light unit is pumped, certain frequency is modulated into using modulator, For the absorption of two-dimensional material;Prism total reflection structural unit with two-dimensional material, dependent on Jie contacted with two-dimensional material Matter generates different absorptions with variations in refractive index caused by temperature to s polarizations and p-polarization;;Phase amplifying unit is locked, using locking phase Amplifier obtains the detectable signal with pumping light modulation frequency, realizes the measurement of photo-thermal effect.
6. device according to claim 5, which is characterized in that detection light unit includes:With s polarizations and p-polarization component Detection light;Detection light, which will be reflected, using polarization spectro is divided into s polarizations and p-polarization light;Two kinds are polarized using balanced detector Light measure simultaneously, obtain as the electric signal caused by polarization variations.
7. device according to claim 5, which is characterized in that pumping light unit includes:Pump light with linear polarization;It can The acousto-optic modulator or electrooptic modulator of intensity modulation are realized to pump light;For control the polarizer of pump light polarization variations and Wave plate.
8. device according to claim 5, which is characterized in that the prism total reflection structural unit packet with two-dimensional material It includes:The combination of two-dimensional material and prism can directly attach to two-dimensional material to attach on prism or first by two-dimensional material On transparent sheet, then it is combined by index-matching fluid and prism;Solid dielectric or liquid medium are covered in two-dimentional material Expect surface.
9. device according to claim 5, which is characterized in that lock phase amplifying unit includes:Lock phase enlarging function can be achieved Lock-in amplifier;Pumping light modulation frequency is fed back into lock-in amplifier, using lock-in amplifier to the spy comprising the frequency Light signal measures.
CN201810044280.4A 2018-01-12 2018-01-12 A kind of assay method and device of two-dimensional material photo-thermal effect Pending CN108226040A (en)

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CN109238968A (en) * 2018-10-23 2019-01-18 哈尔滨工业大学 A kind of photo-thermal heterodyne micro-imaging detection system and method
CN109342325A (en) * 2018-10-30 2019-02-15 南开大学 A kind of imaging method and device that low-dimensional materials anisotropy is micro-
CN112763421A (en) * 2021-01-18 2021-05-07 太原理工大学 Graphene GH displacement and photothermal effect-based solution detection device and method
CN112763726A (en) * 2021-01-18 2021-05-07 太原理工大学 Graphene photothermal sensing-based lung cancer marker miRNA quantitative detection method
CN114384018A (en) * 2021-12-27 2022-04-22 中国科学院福建物质结构研究所 Measuring device for measuring weak anisotropy in large-size isotropic transparent medium, measuring method and application

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Publication number Priority date Publication date Assignee Title
CN109238968A (en) * 2018-10-23 2019-01-18 哈尔滨工业大学 A kind of photo-thermal heterodyne micro-imaging detection system and method
CN109342325A (en) * 2018-10-30 2019-02-15 南开大学 A kind of imaging method and device that low-dimensional materials anisotropy is micro-
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CN112763421A (en) * 2021-01-18 2021-05-07 太原理工大学 Graphene GH displacement and photothermal effect-based solution detection device and method
CN112763726A (en) * 2021-01-18 2021-05-07 太原理工大学 Graphene photothermal sensing-based lung cancer marker miRNA quantitative detection method
CN112763421B (en) * 2021-01-18 2021-09-28 太原理工大学 Graphene GH displacement and photothermal effect-based solution detection device and method
CN112763726B (en) * 2021-01-18 2021-12-28 太原理工大学 Graphene photothermal sensing-based lung cancer marker miRNA quantitative detection method
CN114384018A (en) * 2021-12-27 2022-04-22 中国科学院福建物质结构研究所 Measuring device for measuring weak anisotropy in large-size isotropic transparent medium, measuring method and application

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