CN113109282A - Wide-wavelength-coverage photo-thermal deflection spectrum testing device - Google Patents

Wide-wavelength-coverage photo-thermal deflection spectrum testing device Download PDF

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Publication number
CN113109282A
CN113109282A CN202110529166.2A CN202110529166A CN113109282A CN 113109282 A CN113109282 A CN 113109282A CN 202110529166 A CN202110529166 A CN 202110529166A CN 113109282 A CN113109282 A CN 113109282A
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beam splitter
wavelength
wide
absorption cell
light source
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金一政
金王骁
刘杨
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Zhejiang University ZJU
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Zhejiang University ZJU
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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
    • G01N21/25Colour; 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
    • 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

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  • Spectroscopy & Molecular Physics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Investigating Or Analysing Materials By Optical Means (AREA)

Abstract

The invention discloses a wide-wavelength-coverage photo-thermal deflection spectrum testing device, which comprises a pump light source, a monochromator, an optical chopper and a beam splitter which are sequentially arranged along a light path; a photoelectric detector is arranged on a reflection light path of the beam splitter, and an absorption cell is arranged on a transmission light path of the beam splitter; the signal output end of the photoelectric detector is connected with a computer; the absorption cell is respectively provided with a detection light source and a position sensitive detector on two side surfaces which are vertical to the transmission light path of the beam splitter; the signal output end of the position sensitive detector is sequentially connected with the phase-locked amplifier and the computer; the absorption tank is used for accommodating a heat-conducting medium, the bottom of the absorption tank is fixedly provided with a sample table, and the sample table is used for fixing a film to be detected; a focusing lens is arranged between the absorption cell and the beam splitter, and the pump light transmitted through the beam splitter enters the absorption cell through the focusing lens; the pumping light source adopts laser to drive a broadband light source and is used for emitting pumping light with the wavelength of 170nm to 2100 nm. With the present invention, the testing requirements from narrow bandgap materials to wide bandgap materials can be met simultaneously.

Description

Wide-wavelength-coverage photo-thermal deflection spectrum testing device
Technical Field
The invention belongs to the technical field of spectrum detection, and particularly relates to a wide-wavelength-coverage photo-thermal deflection spectrum testing device.
Background
The film is the basis of the photoelectric device, and directly determines the performance of the photoelectric device. The existing general thin film characterization means is often applicable to limited objects and low in sensitivity. Therefore, it is necessary to develop a thin film characterization method with wide application range and high sensitivity to guide the development and application of the optoelectronic device.
At present, there are many thin film characterization methods based on light absorption. For example, chinese patent publication No. CN106546536A discloses a high-precision weak absorption testing device and method for thin films, and chinese patent publication No. CN105021627A discloses a high-sensitivity rapid online detection method for laser damage on the surface of optical thin films and elements.
After the film absorbs light, light energy or heat energy can be released. The phenomenon of the material absorbing light energy and converting it into heat energy is called photothermal effect. A beam of pumping light irradiates on the film, and the film absorbs light to generate heat. In the region of the medium near the membrane, a temperature gradient is produced due to thermal diffusion. The refractive index of the medium is temperature dependent, thereby forming a refractive index gradient. The probe light sweeps over a region of significant refractive index gradient above the film, deflecting in the direction of travel. There is a quantitative relationship between the amount of deflection of the probe light and the absorbance of the film. The above characterization means based on the photothermal effect is called photothermal deflection spectroscopy.
The reported photothermal deflection spectroscopy test device cannot meet the high sensitivity test requirements of narrow-bandgap materials and wide-bandgap materials due to the low power output of common pump light sources (such as xenon lamps) in the ultraviolet region and the near infrared region and the structure of the whole test device.
Disclosure of Invention
In order to solve the defects in the prior art, the invention provides a wide-wavelength-coverage photo-thermal deflection spectrum testing device which can simultaneously meet the testing requirements from a narrow-bandgap material to a wide-bandgap material.
The technical scheme of the invention is as follows:
a wide-wavelength-coverage photo-thermal deflection spectrum testing device comprises a pump light source, a monochromator, an optical chopper and a beam splitter which are sequentially arranged along a light path; a photoelectric detector is arranged on a reflection light path of the beam splitter, and an absorption cell is arranged on a transmission light path of the beam splitter; the signal output end of the photoelectric detector is connected with a computer;
the absorption cell is respectively provided with a detection light source and a position sensitive detector on two side surfaces which are vertical to the transmission light path of the beam splitter; the signal output end of the position sensitive detector is sequentially connected with the phase-locked amplifier and the computer;
the absorption tank is used for accommodating a heat-conducting medium, and a sample table is fixed on the inner bottom surface of the absorption tank and used for fixing a film to be detected; a focusing lens is arranged between the absorption cell and the beam splitter, and the pump light transmitted by the beam splitter enters the absorption cell through the focusing lens;
the pump light source adopts laser to drive a broadband light source and is used for emitting pump light with the wavelength of 170-2100 nm.
When the invention is tested, the emergent light of the pump light source is led into a monochrometer controlled by a computer, and monochromatic light of a specific wave band is led out; the monochromatic light is modulated in light intensity by an optical chopper arranged behind the monochromator, and the modulation frequency is introduced into the phase-locked amplifier to be used as a reference signal; the beam splitter divides the light into two beams, the photoelectric detector monitors the light intensity of one beam of the light intensity, the signal is transmitted into a computer, and the other beam of the light is guided into an absorption cell; the film to be measured and the substrate are fixed in the sample stage, the position of the film in the light path is fixed, and the absorption pool is filled with a heat-conducting medium; the pump light irradiates on the film, and the detection light emitted by the detection light source sweeps above the film; the position sensitive detector is arranged on an emergent light path of the absorption cell, and a detection signal is transmitted into the phase-locked amplifier for demodulation; the signal demodulated by the phase-locked amplifier is transmitted to a computer.
The pumping light source adopts laser to drive the broadband light source, the pumping light has stronger power distribution from an ultraviolet region (170 nm) to an infrared region (2100 nm), the testing requirements from narrow band gap materials (such as lead selenide, lead telluride and the like) to wide band gap materials (such as zinc oxide, nickel oxide and the like) are met, and the application range of the photo-thermal deflection spectrum technology is greatly expanded.
The heat-conducting medium filled in the absorption cell needs to be fluid which has no absorption to pump light and probe light, low heat conductivity, small refractive index and large refractive index change along with temperature, thereby being beneficial to forming larger refractive index gradient, increasing the deflection amount of the probe light and improving the testing sensitivity. Preferably, the heat-conducting medium is perfluoroalkane.
Preferably, the sample platform be equipped with two sets of steps of symmetry from top to bottom along vertical direction, two sets of steps constitute the indent structure, the sample platform is equipped with the light trap in the bottom of indent structure, is equipped with the fixed part that is used for fixed basement on two sets of steps, the basement be used for placing the film that awaits measuring.
Optionally, the fixing portion includes two sets of mounting holes symmetrically disposed on the two sets of steps and clips disposed on the mounting holes for clamping the substrate.
In order to fix and disassemble the sample table in the absorption tank, a groove matched with the lower end of the sample table in an embedded mode is formed in the inner bottom surface of the absorption tank.
Preferably, the detection light emitted by the detection light source passes through the front part of the outer surface of the film to be detected, and the distance between the detection light and the outer surface of the film to be detected is less than 50 microns, so that the detection light passes through a region with a larger refractive index gradient to generate larger deflection, and the test sensitivity is improved.
Preferably, the diameter of a light spot irradiated by the pumping light emitted by the pumping light source on the film to be detected is larger than 3 μm, and the diameter of the light spot can be adjusted through the front and rear positions of the focusing lens, so that the detection light passes through a sufficiently long region with a refractive index gradient to generate larger deflection and improve the signal-to-noise ratio.
Preferably, the photothermal deflection spectrum testing device is built on a shock insulation platform, so that the disturbance of ground vibration to a light path is reduced, the interference signal intensity is reduced, and the signal to noise ratio is improved.
Preferably, the optical chopper is connected with a phase-locked amplifier, and a signal of the optical chopper is input to a reference signal end of the phase-locked amplifier.
Furthermore, during testing, the whole light path system is covered by a light-tight cover, so that the intensity of interference signals formed by outside stray light and air disturbance is reduced, and the signal-to-noise ratio is increased.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention adopts a laser-driven broadband light source as a pumping light source, the spectrum detection range covers a part of far ultraviolet region to a majority of near infrared region, and simultaneously, the high-sensitivity detection requirements from narrow band gap materials (such as lead selenide, lead telluride and the like) to wide band gap materials (such as zinc oxide, nickel oxide and the like) are met.
2. The device has the advantages of simple structure, convenient installation and operation and higher detection sensitivity.
Drawings
FIG. 1 is a schematic diagram of an optical path of a wide-wavelength-coverage photothermal deflection spectroscopy test apparatus according to the present invention;
FIG. 2 is a schematic top view of an absorption cell in an embodiment of the present invention;
FIG. 3 is a schematic structural diagram of a sample stage according to an embodiment of the present invention;
FIG. 4 is a prior art deuterium lamp emission spectrum;
FIG. 5 is a diagram of an EQ-99X emission spectrum of a laser-driven broad spectrum light source according to an embodiment of the present invention;
figure 6 is an ultraviolet-visible absorption spectrum of a wide bandgap material in accordance with an embodiment of the present invention, wherein (a) is a zinc oxide nanocrystal ultraviolet-visible absorption spectrum; (b) is the ultraviolet-visible absorption spectrum of the nickel oxide nanocrystal.
In the figure: 1-a pump light source; 2-monochromator; 3-an optical chopper; 4-a beam splitter; 5-a photodetector; 6-a detection light source; 7-an absorption tank; 71-a film to be tested; 72-a substrate; 73-a heat conducting medium; 74-sample stage; 741-a concave structure; 742-a light hole; 743-mounting hole; an 8-position sensitive detector; 9-a phase-locked amplifier; 10-a computer; 11-focusing lens.
Detailed Description
The invention will be described in further detail below with reference to the drawings and examples, which are intended to facilitate the understanding of the invention without limiting it in any way.
As shown in FIG. 1, the wide-wavelength-coverage photothermal deflection spectrum testing device comprises a pump light source 1, a monochromator 2, an optical chopper 3, a beam splitter 4, a detection light source 6, an absorption cell 7, a position sensitive detector 8, a photoelectric detector 5, a lock-in amplifier 9, a computer 10 and the like. The whole photo-thermal deflection spectrum testing device is built on a shock insulation platform.
Wherein, the pump light source 1, the monochromator 2, the optical chopper 3 and the beam splitter 4 are arranged in sequence along the light path; a photoelectric detector 5 is arranged on a reflection light path of the beam splitter 4, and an absorption cell 7 is arranged on a transmission light path of the beam splitter 4; the signal output end of the photoelectric detector 5 is connected with a computer 10.
The absorption cell 7 is respectively provided with a detection light source 6 and a position sensitive detector 8 on two side surfaces which are vertical to a transmission light path of the beam splitter 4; the signal output end of the position sensitive detector 8 is connected with a phase-locked amplifier 9 and a computer 10 in sequence.
The pump light source 1 emits pump light PP, which is guided into the monochromator 2 controlled by the computer 10 through an optical fiber, and the pump light PP of a specific waveband is guided out. In order to meet the requirements of universality and high sensitivity of the test, the device selects a laser-driven broadband light source, such as EQ-99X (an emission spectrum is shown in figure 5), as the pump light source 1. Meanwhile, the light splitting range of the monochromator 2 is matched with the pumping light source 1.
Compared with the emission spectrum of a common deuterium lamp (as shown in figure 4), the spectrum detection range of the laser-driven broadband light source adopted by the invention covers a part of far ultraviolet region to a majority of near infrared region, and simultaneously meets the high-sensitivity detection requirements from narrow-bandgap materials (such as lead selenide, lead telluride and the like) to wide-bandgap materials (such as zinc oxide, nickel oxide and the like).
The pump light PP passes through an optical chopper 3 arranged behind the monochromator 2, and the light intensity of the pump light PP is modulated; the signal of the optical chopper 3 is input to the reference signal terminal of the lock-in amplifier 9.
The beam splitter 4 splits the pump light PP into two beams, wherein one beam of reflected light is received by the photodetector 5 to eliminate the test error caused by the power variation of the pump light source 1. The signal of the photoelectric detector 5 is processed and then input into a computer 10. Another beam of transmitted light is injected into the absorption cell 7.
As shown in fig. 2, the absorption cell 7 is filled with a heat conducting medium 73, a sample stage 74 is fixed at the bottom, and a base 72 for fixing the film 71 to be measured is arranged on the sample stage 74. A focusing lens 11 is further arranged between the absorption cell 7 and the beam splitter 4, and the pump light transmitted through the beam splitter 4 enters the absorption cell 7 through the focusing lens 11.
After the transposing is completed, the film 71 to be measured and the base 72 are fixed in the sample stage 74, the sample stage 74 is fixed in the absorption cell 7, and the position of the absorption cell 7 is fixed, so that the position of the film 71 to be measured in the optical path is fixed.
As shown in fig. 3, two sets of steps are vertically and symmetrically arranged on the sample stage 74, the two sets of steps form an inner concave structure 741, a light-transmitting hole 742 is arranged at the bottom of the inner concave structure 741 in the sample stage 74, two sets of mounting holes 743 are symmetrically arranged on the two sets of steps, the number of the mounting holes 743 in each set is three, and clamping pieces (not shown in the figure) for clamping the substrate 72 are arranged on the mounting holes 743.
In order to facilitate the fixing and the dismounting of the sample table 74 in the absorption cell 7, a groove which is matched with the lower end of the sample table 74 in an embedding manner is arranged on the inner bottom surface of the absorption cell 7.
In this embodiment, the absorption cell 7 is filled with a heat-conducting medium, namely perfluoroalkane, which has low thermal conductivity, small refractive index, large change of refractive index with temperature, and no absorption for the pumping light PP and the probe light PB. The pump light PP is focused and then irradiates on the film 71 to be measured to form a light spot with the diameter larger than 3 mm; the film 71 to be measured absorbs light to generate heat; in the area of the heat transfer medium 73 near the film 71 to be measured, a temperature gradient is generated due to heat diffusion, and the temperature is higher closer to the film surface. The higher the temperature of the heat transfer medium 73, the smaller the refractive index, thereby forming a refractive index gradient, the closer to the film surface the smaller the refractive index.
The detection light PB emitted by the detection light source 6 is emitted into the absorption cell 7 and sweeps through a high-refractive-index gradient region with the distance less than 50 mu m from the surface of the film; the probe light PB is deflected away from the film by the refractive index gradient. The position sensitive detector 9 is arranged on an emergent light path of the absorption cell 7, and a detection signal is transmitted into the phase-locked amplifier 9 for demodulation; the signal demodulated by the lock-in amplifier 9 is transmitted to a computer 10 for data analysis.
As shown in fig. 6, the uv-vis absorption spectrum of the wide band gap material in this example is shown, wherein (a) is the uv-vis absorption spectrum of the zinc oxide nanocrystals; (b) is the ultraviolet-visible absorption spectrum of the nickel oxide nanocrystal. It can be seen that the absorption peaks of the two wide band gap oxide nanocrystals are both in the ultraviolet band below 350 nm. The radiation spectrum of the common xenon lamp cannot cover the wave band, and the laser driving broadband light source adopted by the invention has stronger distribution in the wave band, so that the accurate test with high sensitivity can be carried out.
The embodiments described above are intended to illustrate the technical solutions and advantages of the present invention, and it should be understood that the above-mentioned embodiments are only specific embodiments of the present invention, and are not intended to limit the present invention, and any modifications, additions and equivalents made within the scope of the principles of the present invention should be included in the scope of the present invention.

Claims (8)

1. The wide-wavelength-coverage photothermal deflection spectrum testing device is characterized by comprising a pump light source (1), a monochromator (2), an optical chopper (3) and a beam splitter (4) which are sequentially arranged along a light path; a photoelectric detector (5) is arranged on a reflection light path of the beam splitter (4), and an absorption cell (7) is arranged on a transmission light path of the beam splitter (4); the signal output end of the photoelectric detector (5) is connected with a computer (10);
the absorption cell (7) is respectively provided with a detection light source (6) and a position sensitive detector (8) on two side surfaces which are vertical to a transmission light path of the beam splitter (4); the signal output end of the position sensitive detector (8) is sequentially connected with a phase-locked amplifier (9) and a computer (10);
the absorption cell (7) is used for accommodating a heat-conducting medium (73), a sample table (74) is fixed on the inner bottom surface of the absorption cell (7), and the sample table (74) is used for fixing a film (71) to be detected; a focusing lens (11) is arranged between the absorption cell (7) and the beam splitter (4), and the pump light transmitted through the beam splitter (4) enters the absorption cell (7) through the focusing lens (11);
the pump light source (1) adopts laser to drive a broadband light source and is used for emitting pump light with the wavelength of 170-2100 nm.
2. The wide-wavelength-coverage photothermal deflection spectroscopy device of claim 1, wherein said heat conducting medium (73) is a perfluoroalkane.
3. The wide-wavelength-coverage photothermal deflection spectroscopy test device according to claim 1, wherein the sample stage (74) is provided with two sets of steps which are vertically symmetrical, the two sets of steps form the concave structure (741), the sample stage (74) is provided with a light hole (742) at the bottom of the concave structure (741), the two sets of steps are provided with fixing portions for fixing the substrate (72), and the substrate (72) is used for placing the film (71) to be tested.
4. The wide-wavelength-coverage photothermal deflection spectroscopy apparatus of claim 3, wherein said fixing portion comprises two sets of mounting holes (743) symmetrically disposed on two sets of steps and a clip disposed on the mounting holes (743) for clipping the substrate (72).
5. The wide-wavelength-coverage photothermal deflection spectroscopy test device according to claim 1, wherein the inner bottom surface of the absorption cell (7) is provided with a groove for fitting with the lower end of the sample stage (74).
6. The wide-wavelength-coverage photothermal deflection spectroscopy apparatus according to claim 1, wherein the probe light emitted from the probe light source (6) passes through the front of the outer surface of the film under test (71) and is less than 50 μm away from the outer surface of the film under test (71).
7. The wide-wavelength-coverage photothermal deflection spectroscopy test device of claim 1, wherein the photothermal deflection spectroscopy test device is built on a vibration-isolated platform.
8. The wide-wavelength-coverage photothermal deflection spectroscopy test device according to claim 1, wherein the optical chopper (3) is connected to a lock-in amplifier (9), and a signal of the optical chopper (3) is inputted to a reference signal terminal of the lock-in amplifier (9).
CN202110529166.2A 2021-05-14 2021-05-14 Wide-wavelength-coverage photo-thermal deflection spectrum testing device Pending CN113109282A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113237639A (en) * 2021-06-29 2021-08-10 苏州大学 Testing device for light diode

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JPH09229883A (en) * 1996-02-20 1997-09-05 Bunshi Bio Photonics Kenkyusho:Kk Dark field type photothermal transduction spectrometer
US20040085540A1 (en) * 2000-12-28 2004-05-06 Lapotko Dmitri Olegovich Method and device for photothermal examination of microinhomogeneities
US20050062971A1 (en) * 2003-09-24 2005-03-24 Alex Salnik Photothermal system with spectroscopic pump and probe
US20050128570A1 (en) * 2002-03-11 2005-06-16 Jung-Hoon Shin Top-pumped optical device
CN104596996A (en) * 2015-01-06 2015-05-06 香港理工大学深圳研究院 Gas detection method and gas detection system based on hollow-core optical fiber photothermal effect
CN105737982A (en) * 2016-03-02 2016-07-06 南京先进激光技术研究院 Photo-thermal deflection spectrum detection device and detection method
CN112611746A (en) * 2020-12-16 2021-04-06 合肥利弗莫尔仪器科技有限公司 Absorption spectrum detection device and detection method for material micro-area
CN215066133U (en) * 2021-05-14 2021-12-07 浙江大学 Wide-wavelength-coverage photo-thermal deflection spectrum testing device

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09229883A (en) * 1996-02-20 1997-09-05 Bunshi Bio Photonics Kenkyusho:Kk Dark field type photothermal transduction spectrometer
US20040085540A1 (en) * 2000-12-28 2004-05-06 Lapotko Dmitri Olegovich Method and device for photothermal examination of microinhomogeneities
US20050128570A1 (en) * 2002-03-11 2005-06-16 Jung-Hoon Shin Top-pumped optical device
US20050062971A1 (en) * 2003-09-24 2005-03-24 Alex Salnik Photothermal system with spectroscopic pump and probe
CN104596996A (en) * 2015-01-06 2015-05-06 香港理工大学深圳研究院 Gas detection method and gas detection system based on hollow-core optical fiber photothermal effect
CN105737982A (en) * 2016-03-02 2016-07-06 南京先进激光技术研究院 Photo-thermal deflection spectrum detection device and detection method
CN112611746A (en) * 2020-12-16 2021-04-06 合肥利弗莫尔仪器科技有限公司 Absorption spectrum detection device and detection method for material micro-area
CN215066133U (en) * 2021-05-14 2021-12-07 浙江大学 Wide-wavelength-coverage photo-thermal deflection spectrum testing device

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113237639A (en) * 2021-06-29 2021-08-10 苏州大学 Testing device for light diode

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