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CN107219191B - Oblique incidence light reflection difference device based on Fourier transform - Google Patents

Oblique incidence light reflection difference device based on Fourier transform Download PDF

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CN107219191B
CN107219191B CN201710243338.3A CN201710243338A CN107219191B CN 107219191 B CN107219191 B CN 107219191B CN 201710243338 A CN201710243338 A CN 201710243338A CN 107219191 B CN107219191 B CN 107219191B
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CN107219191A (en
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费义艳
陈儒
朱成钢
葛碧临
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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
    • G01N21/17Systems 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
    • G01BMEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B11/00Measuring arrangements characterised by the use of optical techniques
    • G01B11/02Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness
    • G01B11/06Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness for measuring thickness ; e.g. of sheet material
    • 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
    • G01N2021/4126Index of thin films

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Abstract

The invention relates to a Fourier transform-based oblique incidence light reflection difference device, which comprises: and the equipment management unit is used for periodically modulating the incident light path of the incident light polarization state, detecting the reflection light path of the reflection light polarization state and carrying out data acquisition, processing and system control. The device management unit of the device adopts a Fourier transform method to analyze signals, effectively replaces two phase-locked amplifiers, has the advantages of miniaturization, simplification, low cost, high precision and the like, is the premise of preparing the portable oblique incidence light reflection difference device, and further widens the wide application of the device in the fields of in-situ real-time detection of film growth, high-flux characterization of biomolecular interaction and the like.

Description

Oblique incidence light reflection difference device based on Fourier transform
Technical Field
The invention belongs to the technical field of optical instruments, and particularly relates to a detection device for detecting thickness change of a thin film in situ in real time by using an optical method.
Background
The oblique incidence light reflection difference technology is a high-sensitivity optical detection method developed in recent years, has the outstanding characteristics of high sensitivity, no damage, in-situ real-time measurement and the like, and has been widely applied in the fields of in-situ real-time monitoring of film growth, high-flux detection of biomolecular interaction and the like. The inventor and the collaborators develop the oblique incidence light reflection difference technology for in-situ real-time monitoring of the film growth, and have obtained two patents (patent numbers: ZL03153938.6 and Z103276452.9) of the granted invention and the utility model. The inventor and the collaborators develop a full-automatic control oblique incidence light reflection difference imaging technology to realize the rapid high-flux detection of the biochip, and have applied for the invention patent (patent application number: CN 201510211220.3). The oblique incidence light reflection difference device periodically modulates the polarization state of incidence light and obtains information such as film thickness, refractive index and the like by measuring the amplitude of a fundamental frequency signal and the amplitude of a frequency doubling signal of polarization modulation frequency. To date, oblique incidence optical reflectance difference devices typically use two phase-locked amplifiers to measure the amplitude of the fundamental frequency signal and the amplitude of the multiplied frequency signal. The lock-in amplifier is not only bulky, but also expensive, which hinders the miniaturization, simplification and high efficiency of the oblique incidence light reflection difference device, and is a technical bottleneck for developing portable oblique incidence light reflection difference devices.
Disclosure of Invention
The invention aims to provide a small, efficient and low-cost oblique incidence light reflection difference device.
The oblique incidence light reflection difference device provided by the invention adopts Fourier transform to replace an alternating current signal measuring instrument such as a phase-locked amplifier and the like, and specifically comprises the following components: an equipment management unit for periodically modulating the incident light path of the incident light polarization state, detecting the reflected light path of the reflected light polarization state, and performing data acquisition, processing and system control; wherein:
the incident light path for periodically modulating the polarization state of incident light comprises a monochromatic light generator and a polarization modulator.
The monochromatic light generator comprises a continuous spectrum light source and a light splitting device or a monochromatic light emitting device.
The light splitting device is a spectrometer or an optical filter, and the monochromatic light emitting device is a laser or a light emitting diode.
The polarization modulator is a photoelastic modulator, an electro-optic phase modulator, a rotating wave plate, a rotating polarizer or a rotating reflecting surface.
The incident light path for periodically modulating the polarization state of incident light further comprises a polarizer for generating a determined polarization state.
The polarizer is a polarizing prism, a scattering polarizer or a dichroic linear polarizer.
The incident light path for periodically modulating the polarization state of incident light further comprises a phase shifter for introducing adjustable phase change.
The phase shifter is a Pockels cell, a Kerr cell, a liquid crystal phase retarder, a wave plate, a Babinet compensator, a Soley compensator or a Berek compensator.
The monochromatic light generator, the beam expander, the polarizer, the polarization modulator and the phase shifter are sequentially arranged, wherein reflectors are respectively arranged between the monochromatic light generator and the beam expander and between the beam expander and the polarizer; and the incident light path for periodically modulating the polarization state of the incident light is formed.
The reflection light path for detecting the polarization state of the reflection light comprises an analyzer and a photoelectric detector.
The analyzer is a polarizing prism, a scattering polarizer or a dichroic linear polarizer.
The photoelectric detector is a linear photoelectric diode, a photoelectric diode array, a charge-coupled device image sensor or a complementary metal oxide semiconductor image sensor.
A lens is arranged in front of the analyzer, and a slit is arranged between the analyzer and the photodiode to form a reflection light path for detecting the polarization state of the reflected light.
The equipment management unit for data acquisition, processing and system control comprises an amplifying circuit, a data acquisition unit and a system control unit.
The data acquisition unit comprises a data acquisition card and a data acquisition unit.
The system control unit may be a microcomputer in which the oblique incidence light reflection difference signal is measured using a fourier transform method.
The fourier transform is a discrete fourier transform.
The discrete fourier transform is a fast fourier transform.
The fourier transform analyzes the signal that varies over a period of time and obtains the amplitude of the signal at a particular frequency.
Fourier transform analysis is carried out on the time domain discrete signal of the oblique incidence light reflection difference device to obtain a frequency domain discrete signal, and fundamental frequency and frequency doubling amplitude on a frequency spectrum are obtained.
The Fourier transform analysis includes: the output signal of the photoelectric detector in the oblique incidence light reflection difference device comprises a direct current component, a fundamental frequency signal and a frequency doubling signal of polarization modulation frequency and a higher order harmonic signal:
Figure 100002_DEST_PATH_IMAGE002
wherein,
Figure 100002_DEST_PATH_IMAGE004
is the photodetector output signal, A0、A1、A2Respectively, the amplitude of the DC signal, the amplitude of the fundamental frequency signal and the amplitude of the frequency-doubled signal, fMIs the modulation frequency of the polarization modulator,
Figure 100002_DEST_PATH_IMAGE006
and
Figure DEST_PATH_IMAGE008
the initial phases of the fundamental and multiplied frequency signals, respectively, and t is time.
The working principle of the oblique incidence light reflection difference device is as follows:
when the film thickness d is much smaller than the wavelength λ of the incident light, the amplitude A of the fundamental frequency signal1And the frequency-doubled signal amplitude A2The relationship between the ratio of (A) to (B) and the film properties is:
Figure DEST_PATH_IMAGE010
where, theta is the angle of incidence,
Figure DEST_PATH_IMAGE012
is the dielectric constant of the substrate and is,
Figure DEST_PATH_IMAGE014
is the dielectric constant of the environment and is,
Figure DEST_PATH_IMAGE016
is the film dielectric constant. Therefore, the information such as the thickness or the refractive index of the film can be obtained by measuring the amplitudes of the fundamental frequency signal and the frequency doubling signal, so that the OI-RD can be widely applied to the fields of in-situ real-time monitoring of the film growth, high-flux detection of the interaction of biomolecules and the like.
Compared with the prior art, the invention has the following advantages:
the device of the invention adopts Fourier transform to replace two phase-locked amplifiers to measure the corresponding amplitudes of two frequencies, and has the following outstanding advantages:
(1) the space is saved: the oblique incidence light reflection difference device generally adopts two phase-locked amplifiers to respectively measure the amplitude of a fundamental frequency signal and the amplitude of a frequency doubling signal of a polarization modulation frequency. The lock-in amplifier is bulky in size and occupies a large amount of space. The device adopts Fourier transform to replace a phase-locked amplifier, greatly saves space, and makes it possible to develop a miniaturized, simplified and portable oblique incidence light reflection difference device;
(2) the cost is reduced: the two phase-locked amplifiers have high cost (30% of the cost of the oblique incidence light reflection difference device); the device does not use a phase-locked amplifier, so that the cost of the oblique incidence light reflection difference device is greatly reduced;
(3) and (3) enhancing flexibility: the phase-locked amplifier can only measure the amplitude of a fundamental frequency signal and the amplitude of a frequency multiplication signal of the polarization modulation frequency, and the Fourier transform method can analyze the amplitudes of all harmonic signals of the polarization modulation frequency, so that the measurement flexibility of the oblique incidence light reflection difference device is greatly enhanced;
(4) performance is improved; compared with a phase-locked amplifier, the sampling rate of Fourier transform is faster, and the signal-to-noise ratio is higher. The device of the invention adopts Fourier transform, greatly improves the performance of the oblique incidence light reflection difference device, and realizes faster and more accurate measurement of the device.
Drawings
FIG. 1 is a schematic diagram of a Fourier transform-based oblique incidence light reflection difference device according to the present invention.
Fig. 2 is a comparison graph of the standard deviation of the fundamental frequency signal of the device for simultaneously measuring the reflection difference of oblique incidence light by using the fast fourier transform and the lock-in amplifier.
FIG. 3 is a comparison graph of biochip reaction difference image and real-time reaction curve for simultaneously measuring the fundamental frequency signal of the oblique incidence light reflection difference device by using fast Fourier transform and a phase-locked amplifier.
Reference numbers in the figures: the device comprises a monochromatic light generator 1, a reflector 2 and a reflector 4, a beam expander 3, a polarizer 5, a photoelastic modulator 6, a phase shifter 7, a lens 8, a lens 9, an analyzer 10, a slit 11, a photodiode 12, an amplifying circuit 13, a data acquisition unit (data acquisition board) 14, a system control unit (microcomputer) 15 and a sample 16.
Detailed Description
The invention is further described below with reference to the following figures and examples:
example 1:
as shown in fig. 1, a fourier transform-based oblique incidence light reflectance difference device according to the present invention was fabricated. The monochromatic light generator 1 adopts a helium-neon laser with the output wavelength of 632.8 nm; the output light of the laser is expanded into collimated light through the beam expander 3; the beam expanding collimated light passes through a polarizer 5 which is arranged at an angle of 45 degrees between a light transmission shaft and the horizontal direction and then becomes linearly polarized light, and the vibration direction of the polarizer and the horizontal direction form an angle of 45 degrees; the polarization modulator 6 adopts a photoelastic modulator which is horizontally arranged to periodically modulate the polarization state at 50 kHz; emergent light passes through a phase shifter 7, the phase shifter 7 adopts a zero-order half-wave plate, the fast axis of the zero-order half-wave plate is along the p-polarization direction, and adjustable phase difference can be introduced between the p-polarization component and the s-polarization component by rotating the half-wave plate by taking the fast axis as a rotating axis; emergent light is focused by the lens 8, the lens 8 is realized by the scanning field lens and the galvanometer, the focal length of the scanning field lens is 7.5cm, incident light is focused on the lower surface of the sample 16 at an incident angle of 65 degrees (the incident angle on the interface between the air and the sample 16), and the scanning field lens is combined with the galvanometer to realize rapid line scanning of the incident light in the vertical direction; the reflected light passes through an imaging lens 9, and the imaging lens 9 is formed by a single objective lens and focuses the reflected light to a slit 11; the focused light passes through an analyzer 10 with a transmission axis forming an angle of-45 degrees with the horizontal direction to detect the polarization state, and the slit 11 selects the reflected light passing through the lower surface of the sample 16; the photodiode 12 receives the light reflected by the lower surface of the sample 16, and the photodetector 12 adopts a linear photodetector which converts an optical signal into an electrical signal; the electrical signal is then filtered by the amplification circuit 13 for a dc signal and an ac time domain signal is amplified; the data acquisition card 14 acquires data and discretizes the time domain signal to obtain a discrete periodic signal; the sampling frequency is 625kHz and the number of sampling points is 500. And obtaining the discrete signal of the frequency domain by fast Fourier transform of the discrete signal of the time domain, and finally obtaining the amplitudes of the fundamental frequency signal and the frequency doubling signal of the photoelastic modulation frequency on the frequency spectrum. The output signal of the photodiode 12 in the oblique incidence reflection difference device comprises a direct current component, a fundamental frequency signal and a frequency multiplication signal of the modulation frequency of the photoelastic modulator 6 and a higher order harmonic signal:
Figure DEST_PATH_IMAGE018
(1)
wherein A is0、A1、A2The device for measuring the oblique incidence light reflection difference respectively adopts two phase-locked amplifiers to accurately measure A1And A2Thereby performing characterization of physical quantities such as film thickness or refractive index. F in formula (1)MIs the modulation frequency of the photoelastic modulator,
Figure DEST_PATH_IMAGE020
and
Figure DEST_PATH_IMAGE022
the initial phases of the fundamental frequency signal and the frequency multiplication signal, respectively.
By fundamental frequency components
Figure DEST_PATH_IMAGE024
Illustrating the measurement of the amplitude A of the frequency signal by using Fourier transform instead of a lock-in amplifier1The principle and process of (a). First, the data acquisition board 14 samples at a frequency fs(sampling period is T)s) The periodic signal in the time domain is sampled and discretized, and the nth (integer) discrete point of the signal can be represented as:
Figure DEST_PATH_IMAGE026
(2)
the fourier transform is performed on a time-domain discrete signal containing N discrete points (N is the number of sampling points) to obtain:
Figure DEST_PATH_IMAGE028
(3)
wherein,
Figure DEST_PATH_IMAGE030
is the sampling interval and k is the frequency domain channel. When in use
Figure DEST_PATH_IMAGE032
When, each term of the formula (3) is zero, so X1(k) And = 0. When in use
Figure DEST_PATH_IMAGE034
In time, the two terms of the formula (3) are not zero, and the final expression is as follows:
Figure DEST_PATH_IMAGE036
(4)
Figure DEST_PATH_IMAGE038
(5)
the above analysis shows that the amplitude of the fundamental frequency signal to be measured by the oblique incidence light reflection difference device can be obtained from the discrete frequency domain signal by performing Fourier transform on the time domain discrete periodic signal
Figure DEST_PATH_IMAGE040
The channel is obtained corresponding to the amplitude of the frequency, as shown in equation (5). The frequency multiplied signal amplitude can be measured according to similar principles.
Fig. 2 is a comparison graph of the standard deviation of the fundamental frequency signal of the device for simultaneously measuring the reflection difference of oblique incidence light by using the fast fourier transform and the lock-in amplifier. The abscissa of fig. 2 represents the number of sampling points for the fast fourier transform, and represents the number of sampling points used for the fourier transform. The larger the number of sampling points, the longer the sampling time. The ordinate of FIG. 2 is the standard deviation of the OI-RD signal. The larger the standard deviation, the more noisy the OI-RD signal. The black filled squares in the figure represent the standard deviation of the lock-in amplifier measurement signal and the open circles represent the standard deviation of the fast fourier transform measurement signal. Fig. 2 shows that when the number of sampling points is less than 600, the standard deviation of the oblique incidence light reflection difference signal measured by fourier transform is less than that of the signal measured by the lock-in amplifier, so that the signal-to-noise ratio of fourier transform is better than that of the measurement result of the lock-in amplifier. When the number of samples is greater than 2000, the standard deviation of the fourier transform measurement signal is close to the standard deviation of the lock-in amplifier measurement. This shows that the fast fourier transform can obtain the same signal to noise ratio measurement faster than the lock-in amplifier, which will greatly improve the scan speed of the oblique incidence light reflectance difference device.
FIG. 3 is a real-time response curve and difference image of the oblique incidence light reflection difference device using fast Fourier transform and lock-in amplifier to simultaneously measure the interaction between biochip and protein. The biochip contains 20 biological sample spots. The reaction difference image in fig. 3 shows that the brighter the sample spot, the greater the magnitude of the reaction between the sample spot and the protein. In the real-time response curve of fig. 3, the abscissa represents time, and the ordinate represents the amplitude of the fundamental frequency signal of the oblique incident light reflection difference. Each curve represents the real-time change in the interaction between the sample spot and the protein at the position corresponding to the image over time. Fig. 3 shows that the use of fast fourier transform can replace lock-in amplifiers for high-throughput label-free measurement of biochips.
Example 2:
implemented as embodiment 1, the transmission axis of the polarizer 5 is along the horizontal direction, the polarization modulator 6 is placed at an angle of 45 degrees with the horizontal direction, and the phase shifter 7 is placed behind the imaging lens 9; the lens 8 uses a cylindrical lens to replace a scanning field lens and a galvanometer, and the focal length of the lens is 5 cm; a photodetector 12 using a diode array comprising 152 photodiodes instead of linear photodiodes; and analyzing the time domain periodic signals by adopting a discrete Fourier transform method, wherein the sampling frequency is 625kHz, and the number of sampling points is 1000.

Claims (9)

1. A fourier transform-based oblique incidence light reflectance difference device, comprising: an equipment management unit for periodically modulating the incident light path of the incident light polarization state, detecting the reflected light path of the reflected light polarization state, and performing data acquisition, processing and system control; the incident light route for periodically modulating the polarization state of the incident light is formed by sequentially arranging a monochromatic light generator, a beam expander, a polarizer, a polarization modulator and a phase shifter, wherein reflectors are respectively arranged between the monochromatic light generator and the beam expander and between the beam expander and the polarizer; the reflected light path for detecting the polarization state of the reflected light consists of an analyzer and a photoelectric detector, a lens is arranged in front of the analyzer, and a slit is arranged between the analyzer and the photoelectric detector; the equipment management unit for data acquisition, processing and system control is formed by sequentially connecting an amplifying circuit, a data acquisition unit and a system control unit, and the system control unit measures oblique incidence light reflection difference signals by adopting a Fourier transform method;
the Fourier transform is a discrete fast Fourier transform, a time domain discrete signal of the oblique incidence light reflection difference device is analyzed through the Fourier transform to obtain a frequency domain discrete signal, and the amplitude of fundamental frequency and frequency doubling on a frequency spectrum is obtained, which is specifically as follows:
the output signal of the photoelectric detector in the oblique incidence light reflection difference device comprises a direct current component, a fundamental frequency signal and a frequency doubling signal of polarization modulation frequency and a higher order harmonic signal:
Figure DEST_PATH_IMAGE002
where x (t) is the photodetector output signal, A0、A1、A2Respectively, the amplitude of the DC signal, the amplitude of the fundamental frequency signal and the amplitude of the frequency-doubled signal, fMIs the modulation frequency of the polarization modulator,
Figure DEST_PATH_IMAGE004
and
Figure DEST_PATH_IMAGE006
the initial phases of the fundamental and multiplied frequency signals, respectively, and t is time.
2. The device according to claim 1, wherein the monochromatic light generator comprises a continuous spectrum light source and a light splitting device or a monochromatic light emitting device.
3. The fourier transform-based oblique-incidence light reflectance difference device according to claim 2, wherein the light splitting device is a spectrometer or a filter, and the monochromatic light emitting device is a laser or a light emitting diode.
4. The fourier transform-based oblique-incidence light reflectance difference device according to claim 1, wherein the polarization modulator is a photoelastic modulator, an electro-optic phase modulator, a rotating wave plate, a rotating polarizer, or a rotating reflective surface.
5. The fourier transform-based oblique-incidence light reflectance difference device according to claim 1, wherein the polarizer is a polarizing prism, a scattering polarizer, or a dichroic linear polarizer.
6. The fourier transform-based oblique-incidence light reflectance difference device according to claim 1, wherein the phase shifter is a pockels cell, a kerr cell, a liquid crystal phase retarder, a wave plate, a babinet compensator, a sorel compensator or a berek compensator.
7. The fourier transform-based oblique-incidence light reflectance difference device according to claim 1, wherein the analyzer is a polarizing prism, a scattering polarizer, or a dichroic linear polarizer.
8. The fourier transform-based oblique-incidence light reflectance difference device according to claim 1, wherein the photodetector is a linear photodiode, a photodiode array, a charge-coupled device image sensor, or a cmos image sensor.
9. The oblique incidence light reflection difference device based on the Fourier transform as claimed in claim 1, wherein the data acquisition unit is a data acquisition card and a data collector.
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