CN107860945B - Scanning probe-elliptical polarization multifunctional coupling in-situ measurement method - Google Patents
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Abstract
The invention discloses a scanning probe-elliptical polarization multifunctional coupling in-situ measurement method, which comprises the steps of selecting a measured area by using an XYZ coarse motion scanner, enabling a scanning probe to be close to the surface of a sample and arranging the scanning probe at the central position of an incident light spot of an elliptical polarization light measurement mechanism; taking the central position as a measurement origin, controlling an XY scanner to move a certain relative XY coordinate to perform scanning measurement on the microscopic morphology of the sample to be measured, and recording a scanning track to obtain the serial number of a scanning point in an XY plane; moving the scanning probe out of the range of an incident light spot of the elliptical polarized light measuring mechanism along the Z-axis direction, and simultaneously restoring the XY micro-motion scanner to the position of a measurement origin according to the scanning track; performing elliptical polarized light measurement according to the scanning track to obtain point-by-point optical and material characteristics of the sample; optical and surface topography information in the scanned area is acquired. The invention has the beneficial effects that: the macroscopic optical property, the thickness and the microscopic information of the sample can be measured in situ, synchronously and in real time. Convenient operation, accurate test and high efficiency.
Description
Technical Field
The invention relates to the technical field of in-situ test of macroscopic properties and microstructures of thin film materials, in particular to a scanning probe-elliptical polarization multifunctional coupling in-situ measurement method.
Background
As an important branch of thin film material research in advanced manufacturing technology, characterization and detection methods of characteristic parameters of thin film materials are the key bases. Scanning Probe Microscopy (SPM) is an analytical method for measuring the microstructure and properties of a material surface. The microscopic method has a series of advantages of high resolution, low cost, low consumption, wide working range and the like; the three-dimensional appearance of the surface of the high-resolution object can be obtained; continuous dynamic analysis can be performed; the disadvantage is that only microscopic local analysis can be performed; an Ellipsometer (elipsometer) is an optical measurement method for obtaining information on a sample to be measured by measuring changes (amplitude ratio and phase difference) in polarization states before and after incident light and reflected light on a surface of the sample. With the complexity of the device structure, the unknown quantity to be measured is increased continuously, so that the traditional elliptical polarized light measuring instrument has certain limitations on film thickness measurement, appearance characteristics and the like of the thin film.
In recent years, with the continuous development of thin film materials, simple atomic force microscopic measurement and elliptical polarized light measurement cannot meet the requirements of in-situ, microscopic, macroscopic and multifunctional coupling simultaneous measurement. In order to meet the requirements of macroscopic performance and microscopic test of in-situ photoelectric multifunctional coupling, the invention provides a measuring method combining scanning probe microscopic measurement and elliptical polarized light measurement, expands the measurement characterization function and application range of the existing measurement, improves the efficiency of detection and characterization, and plays a good role in promoting the research and development of thin film materials.
Disclosure of Invention
The invention aims to solve the technical problem of providing a multifunctional coupling detection method based on in-situ detection scanning probe micro-measurement-ellipsometry, which can meet the requirements of scientific research personnel on the combination of in-situ, synchronous and real-time macroscopic performance test and microstructure characterization on a sample.
In order to solve the technical problems, the invention adopts the technical scheme that: a scanning probe-elliptical polarization multifunctional coupling in-situ measurement method comprises the following steps:
the method comprises the following steps: a coaxial illumination observation mechanism and an imaging CCD detector of the scanning probe micro-measuring mechanism are used for enabling a probe of the scanning probe micro-measuring mechanism to be close to the surface of a sample and to be arranged at the center position of a laser spot on an incident sample of the elliptical polarized light measuring mechanism through Z-axis off-plane coarse scanning of an XYZ coarse scanning device and micro feeding of a Z-axis piezoelectric micro-scanning device; step two: controlling an XY micro-scanner to move a certain relative XY coordinate, namely a scanning area, in a horizontal plane by taking the central position of a light spot as a measurement origin, performing scanning probe micro-measurement on the micro-topography of the sample to be measured, and recording a scanning track to obtain (X, Y, Z) ij, wherein i and j are the serial numbers of scanning points in an XY plane; step three: roughly adjusting the probe of the scanning probe micro-measuring mechanism along the Z axis by a screw micrometer of the coaxial illumination observation mechanism along the Z axis direction to move out of the incident light spot range of the elliptical polarized light measuring mechanism, and simultaneously restoring the XY micro-scanner to the measurement origin position according to the scanning track; step four: performing elliptical polarized light measurement according to the scanning track to obtain point-by-point optical and material characteristics (psi, delta) ij of the sample; step five: the scanning process is ended, and each scanning point in the scanning area contains (Ψ, Δ, X, Y, Z) ij, where: (Ψ, Δ) ij is the optical information and (X, Y, Z) ij is the surface topography information.
And the scanning point coordinates and the scanning track of the scanning probe micro-measuring mechanism and the elliptical polarized light measuring mechanism in the first step are the same, so that in-situ measurement is formed.
The scanning probe micro-measuring mechanism is used for measuring, and the scanning probe is arranged at the center of an incident light spot of the elliptical polarized light measuring mechanism and is in contact with or not in contact with a measured surface.
And the distance between the scanning probe and the measured surface of the sample in the non-contact measurement is less than 20 nm.
The probe was moved away from the spot area of the spectroscopic ellipsometer along the Z-axis, and then the ellipsometer was measured.
The invention has the beneficial effects that: the method for the ellipsometry and the scanning probe microscopic measurement is organically combined with the functions, and the macroscopic optical performance (such as refractive index, extinction coefficient and the like) and the thickness and microscopic information (such as surface morphology, roughness and the like) of the sample can be measured in situ, synchronously and in real time. Compared with other off-line testing methods, the scanning probe-elliptic polarization multifunctional coupling in-situ measurement method is convenient to operate, the test result is more accurate, the macroscopic performance and microstructure information of a sample can be measured in situ, synchronously and in real time, the problem that two instruments cannot guarantee that the two instruments are in a unified measurement area in non-situ measurement is solved, the measurement time which needs hours and days is shortened to a few minutes, and the measurement characterization efficiency is improved.
Drawings
FIG. 1 is a schematic diagram of an overall front view of a scanning probe-ellipsometric multifunctional coupling in-situ measurement device according to the present invention;
figure 2 is a side logic block diagram schematic of the scanning probe micro-measurement mechanism of figure 1,
FIG. 3 is a schematic diagram showing the relative positions of the scanning probe and the mechanism of each part of the multifunctional coupling device for ellipsometry in situ according to the present invention;
FIG. 4 is a flow chart of a scanning probe-ellipsometric multifunctional coupling in-situ measurement method.
Wherein:
101: CCD detector
102: coaxial lighting observation mechanism
1021: light collimator 1022: mirror 1023: semi-transparent semi-reflecting mirror
103: z-axis piezoelectric micro-motion scanner
104: scanning probe and holder
105: micro-motion scanner driver
106: scanning probe driving controller
107: probe signal preamplifier
108: screw micrometer
109: external lighting source
201: elliptical polarized light source
202: polarizer
203: polarization analyzer
204: photoelectric detector
205: XYZ coarse movement scanner
1: scanning probe micro-measuring mechanism
2: elliptical polarized light measuring mechanism
3: sample support
4: XY micro-motion scanner
5: base seat
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments. It is to be understood that the specific embodiments described herein are merely illustrative of the invention and are not to be construed as limiting the invention. It should be further noted that, for the convenience of description, only some of the structures related to the present invention are shown in the drawings, not all of the structures.
The invention provides a technical scheme of a multifunctional coupling detection device for scanning probe microscopic measurement-elliptical polarized light measurement for in-situ detection. As shown in fig. 1, fig. 2 and fig. 3, the detecting apparatus for in-situ, synchronous and real-time measuring macro optical information, such as refractive index and extinction coefficient, and thickness and micro geometric information, such as surface morphology and roughness, of a working sample includes: the scanning probe microscopic measuring mechanism 1 is used for acquiring the microscopic appearance of a sample to be measured, namely (Z) ij; an XY micro-motion scanning mechanism 4, which is used for obtaining the position information of the scanning point in the XY plane, namely (X, Y) ij, and jointly forms (X, Y, Z) ij, wherein i and j are the serial numbers of the scanning points in the XY plane; an elliptical polarized light measuring mechanism 2 for obtaining point-by-point optical and material properties (Ψ, Δ) ij of the sample.
The sample support 3 to be tested, the XY micro-motion scanner 4 and the XYZ coarse-motion scanner 205 are connected in series along the Z axis, the sample support 3 to be tested is connected with the XY micro-motion scanner 4 through magnetic force or air negative pressure, and the XY micro-motion scanner 4 is connected and fixed with the XYZ coarse-motion scanner 205 through screws; the XY micro-motion scanner 4 is a two-dimensional piezoelectric ceramic mechanism; the XYZ coarse movement scanner 205 is a stepping motor screw nut mechanism, and not only provides large-scale scanning of an elliptically polarized measurement spot in a horizontal plane and coarse movement scanning of a measurement area shared with the scanning probe measurement mechanism 1, but also provides coarse movement position adjustment of a distance between a probe and a sample in an off-plane Z-axis direction; the Z-axis piezoelectric scanner 103 completes micro-motion scanning tracking in the Z-axis direction; the elliptical polarized light measuring mechanism 2, the XYZ coarse motion scanner 205 and the scanning probe measuring mechanism 1 are rigidly connected to a base 5 of the detecting device through a mechanical structure; the tip of the probe is located at the intersection of the incident light and the reflected light of the elliptical polarization measuring unit 2, and the YZ plane formed by the probe and the Z axis is perpendicular to the XZ plane where the incident light and the reflected light of the elliptical polarization measuring unit are located.
The scanning probe micro-measuring mechanism 1 includes: a micrometer screw 108, a Z-axis piezoelectric micro-motion scanner 103, a micro-motion scanner driver 105, a scanning probe and holder 104, a scanning probe driving controller 106 and a probe signal preamplifier 107; the Z-axis piezoelectric coarse motion scanning mechanism of the XYZ coarse motion scanner 205 and the screw micrometer 108 are respectively used for adjusting the distance between the probe of the scanning probe micro-measuring mechanism 1 and the surface of the sample in an electric mode and a manual mode, and the probe is arranged at the center position of a laser spot of the elliptical polarized light measuring mechanism 2 incident on the sample; the micrometer caliper 108 is also used for moving the probe out of the laser spot along the Z axis after completing the scanning probe microscopic measurement, and the elliptical polarized light measuring mechanism 2 is used for measuring the optical parameters and the film thickness; the Z-axis piezoelectric micro-motion scanner 103 is respectively connected with the micrometer screw 108 and the scanning probe holder 104, and the scanning probe driving controller 106 and the probe signal preamplifier 107 are respectively used for providing the excitation signal of the probe and the detection and pre-amplification of the excitation signal modulated by the surface topography of the sample.
And the coaxial illumination observation mechanism 102 is used for observing the relative position of the probe of the scanning probe micro-measurement mechanism 1 and a sample to be measured and providing field illumination. A beam of white light emitted by the external light source 109 is collimated by the light collimating mirror 1021, reflected by the reflecting mirror 1022 to the half mirror 1023, and then incident to the sample surface for illuminating and observing the view field, and the images of the sample and the probe are reflected by the half mirror 1023 to the CCD detector 101 for imaging.
The invention discloses a multifunctional coupling detection device for scanning probe microscopic measurement and elliptical polarized light measurement for in-situ detection, which has the working principle that:
an external light source 109 in a coaxial illumination observation mechanism arranged right above a probe of the scanning probe micro-measurement mechanism emits a beam of white light, the white light is collimated by a light collimating mirror 1021, reflected by a reflecting mirror 1022 to a semi-reflecting mirror 1023 and then enters a sample surface illumination observation field, images of a sample and the probe are reflected to a CCD detector 101 through the semi-reflecting mirror 1023 to be imaged, the distance between the probe and the sample surface of the scanning probe micro-measurement mechanism 1 is respectively adjusted in an electric and manual mode through a Z-axis piezoelectric coarse motion scanning mechanism of an XYZ coarse motion scanner 205 and a spiral micrometer 108 according to the formed images, the probe is arranged at the center position of a laser incidence light spot of a sample stage of an elliptical polarization light measurement mechanism 2, and the spot is recorded as a measurement origin;
by taking a measurement origin as a reference and controlling the XY coarse-fine motion scanning platform to move a certain relative XY coordinate, namely a scanning area, in a horizontal plane, the scanning probe driving controller 106 and the preamplifier 107 respectively provide detection and pre-amplification of an excitation signal of the probe and an excitation signal modulated by the surface topography of the sample, so that the scanning probe micro-measurement mechanism of the micro-topography of the sample to be measured measures and records a scanning track;
moving a probe of the scanning probe micro-measuring mechanism 1 out of the range of an incident light spot of the elliptical polarized light measuring mechanism 2 through a coarse movement scanner and a micro movement scanner of a Z axis along the Z axis direction, and restoring the XY micro movement scanner 4 to a measuring original point position according to a scanning track;
according to the scanning area and the scanning track, the elliptical polarized light measuring mechanism 2 changes non-polarized light emitted by the laser source 201 into linearly polarized light after passing through the polarizer 202, adjusts the polarizer 202 to change the polarization direction of the light beam, changes the linearly polarized light into elliptically polarized light after passing through a lambda/4 wave plate, changes the polarization state of the elliptically polarized light after irradiating on the film sample, and measures the polarization state (amplitude and phase) of the reflected light of the elliptically polarized light by using the analyzer 203 to obtain the point-by-point optical and material characteristics of the sample acquired by the scanning area;
thus, each scanning point actually contains (Ψ, Δ, X, Y, Z) ij, i being a scanning point number, which includes both optical information (Ψ, Δ) ij and surface topography information (X, Y, Z) ij.
The coordinate and the track of a scanning point of the scanning probe microscopic measurement and the elliptical polarized light measurement are the same, and in-situ measurement is formed; the scanning probe micro-measuring mechanism 1 is used for measuring the center of an incident light spot by a probe in elliptical polarized light and contacting or not contacting a measured surface. When the distance between the scanning probe and the measured surface of the sample is less than 20nm during non-contact measurement, although elliptical polarized light cannot be measured simultaneously, the measurement time is short (second order) by adopting spectral elliptical polarized light and the microscopic measurement time (grading) by adopting the scanning probe, and the simultaneous measurement can be approximately considered.
According to the embodiment, the innovative design of the system can be used for testing the macroscopic optical characteristic parameters, the thickness information and the microscopic geometric quantity information of the thin film material in situ, synchronously and in real time, more accurately analyzing the corresponding relation and the modulation effect of the microstructure on the optical information and directly explaining the change of the thin film optical characteristic caused by the change of the microstructure of the thin film material.
The invention provides a scanning probe-elliptical polarization multifunctional coupling in-situ measurement method. As shown in fig. 4, the specific implementation steps are as follows:
a coaxial illumination observation mechanism 102 and an imaging CCD detector 101 which are arranged right above a probe of the scanning probe micro-measurement mechanism 1 are utilized to enable the probe of the scanning probe micro-measurement mechanism 1 to be close to the surface of a sample through Z-axis out-of-plane coarse scanning of an XYZ coarse movement scanner 205 and a Z-axis piezoelectric micro-movement scanner 103, the probe is arranged at the center position of a laser spot on an incident sample of the elliptical polarized light measurement mechanism 2, and the point is recorded as a measurement origin; taking a measurement origin as a reference, carrying out scanning probe microscopic measurement on the microscopic appearance of the sample to be measured by controlling an XY micro-scanner to move a certain relative XY coordinate, namely a scanning area, in a horizontal plane, and recording a scanning track; returning the XY micro-scanner to the position of the measurement origin according to the scanning track, and then moving the scanning probe micro-measurement mechanism out of the range of the incident light spot of the elliptical polarized light measurement mechanism along the Z-axis direction; and (3) performing elliptical polarized light measurement to obtain point-by-point optical and material characteristics of the sample obtained by the scanning area according to the scanning area and the scanning track. Thus, each scanning point actually contains (Ψ, Δ, X, Y, Z) ij, i being a scanning point number, which includes both optical information (Ψ, Δ) ij and surface topography information (X, Y, Z) ij.
In the above embodiment, the Z-axis off-plane coarse movement of the scanning probe micro-measuring mechanism 1 is provided by the XYZ coarse movement scanner 205 of the ellipsometric measuring mechanism 2, and the Z-axis fine movement scanning tracking is provided by the Z-axis piezoelectric fine movement scanner 103 fixed on the micrometer screw 108; XY jogging scanning is provided by XY jogging scanner 4 which is also used as a sample stage, the sample is fixed on a sample stage bracket 3 by utilizing air negative pressure or magnetism, and the sample stage bracket is connected with the XY jogging scanner; the XY micro-motion scanner 4 is fixedly connected with an XYZ coarse motion scanner 205 of the elliptical polarized light measuring mechanism 2, and the XYZ coarse motion scanner 205 provides coarse motion scanning of the scanning probe micro-measuring mechanism 1; the scanning probe micro-measuring mechanism 1 and the coaxial illumination observation mechanism 102 therein are fixedly connected with the elliptical polarized light measuring mechanism 2 through a base 5. Under the condition of certain temperature and pressure intensity, the sample is measured by the scanning probe micro-measurement-elliptical polarized light measurement multifunctional coupling detection method based on in-situ detection, and the macro optical property and thickness information and microstructure information of in-situ, synchronous and real-time sample devices can be obtained under the same measurement condition.
And (3) comparative analysis: the microstructure and the macroscopic optical performance of the sample are respectively tested by using a scanning probe microscope and an elliptical polarized light measuring instrument, so that the obtained independent microstructure, optical performance parameters and thickness under the same measurement condition, in the same measurement area and in the same measurement area are obtained, and the test result cannot explain the correspondence or modulation relationship between the microstructure and the macroscopic optical parameters of the sample.
According to the embodiment and the comparative example, the innovative design of the system can be used for testing the macroscopic optical characteristic parameters, the thickness information and the microstructure information of the thin film material in situ, synchronously and in real time, more accurately analyzing the corresponding relation and the modulation effect of the microstructure on the optical information and directly explaining the change of the optical characteristic of the thin film caused by the change of the microstructure of the thin film material.
It should be noted that although the above description and examples describe the present invention in more detail, these descriptions are only provided for the simplicity of description of the design idea of the present invention, and are not meant to limit the concept idea of the present invention. Any combination, addition or modification not exceeding the design idea of the present invention falls within the scope of the present invention.
Claims (5)
1. A scanning probe-elliptical polarization multifunctional coupling in-situ measurement method comprises the following steps:
the method comprises the following steps: a coaxial illumination observation mechanism (102) and an imaging CCD detector (101) of a scanning probe micro-measurement mechanism (1) are used for enabling a probe of the scanning probe micro-measurement mechanism (1) to be close to the surface of a sample and be arranged at the center of a laser spot on an incident sample of an elliptical polarized light measurement mechanism (2) through Z-axis off-plane coarse motion scanning of an XYZ coarse motion scanner (205) and micro-motion feeding of a Z-axis piezoelectric micro-motion scanner (103);
step two: controlling an XY micro-motion scanner (4) to move a certain relative XY coordinate, namely a scanning area, in a horizontal plane by taking the central position of a light spot as a measurement origin, carrying out scanning probe micro-measurement on the micro-topography of a sample to be measured, and recording a scanning track to obtain (X, Y, Z) ij, wherein i and j are scanning point serial numbers in an XY plane;
step three: roughly adjusting the probe of the scanning probe micro-measuring mechanism (1) along the Z axis by a micrometer screw (108) of the coaxial illumination observation mechanism (102) along the Z axis to move out of the range of an incident light spot of the elliptical polarized light measuring mechanism (2), and simultaneously restoring the XY micro-motion scanner to the position of a measurement origin according to a scanning track;
step four: performing elliptical polarized light measurement according to the scanning track to obtain point-by-point optical and material characteristics (psi, delta) ij of the sample;
step five: data coupling processing: each scan point in the scan region contains (Ψ, Δ, X, Y, Z) ij, wherein: (Ψ, Δ) ij is the optical information, (X, Y, Z) ij is the surface topography information, and the scanning process ends.
2. The scanning probe-ellipsometric multifunctional coupling in-situ measurement method as claimed in claim 1, wherein: the scanning point coordinates and the scanning track of the scanning probe micro-measuring mechanism (1) and the scanning point coordinates and the scanning track of the elliptical polarized light measuring mechanism (2) in the first step are the same, and in-situ measurement is formed.
3. The scanning probe-ellipsometric multifunctional coupling in-situ measurement method as claimed in claim 1, wherein: the scanning probe micro-measuring mechanism (1) is used for measuring the center of an incident light spot of the elliptical polarized light measuring mechanism (2) and contacting or not contacting the measured surface.
4. The scanning probe-ellipsometric multifunctional coupling in-situ measurement method as claimed in claim 3, wherein: and the distance between the scanning probe and the measured surface of the sample in the non-contact measurement is less than 20 nm.
5. The scanning probe-ellipsometric multifunctional coupling in-situ measurement method as claimed in claim 1, wherein: the probe was moved away from the spot area of the spectroscopic ellipsometer along the Z-axis, and then the ellipsometer was measured.
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| CN107144529A (en) * | 2017-06-06 | 2017-09-08 | 大连理工大学 | A kind of device and method that measurement is accurately positioned for ellipsometer |
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| US9395173B2 (en) * | 2014-10-22 | 2016-07-19 | National Applied Research Laboratories | Multi-functioned optical measurement device and method for optically measuring a plurality of parameters |
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| CN1255625A (en) * | 1998-12-02 | 2000-06-07 | 西门子公司 | Device and method for measuring critical measurement by ellipsometry |
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| CN202329574U (en) * | 2011-11-15 | 2012-07-11 | 武汉理工大学 | Elliptical polarization three-dimensional scanning device |
| CN106595521A (en) * | 2016-12-12 | 2017-04-26 | 武汉颐光科技有限公司 | Vertical objective lens type Muller matrix imaging ellipsometer based on liquid crystal phase modulation |
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