CN210400620U - Angle-resolved micro-Raman spectrum detection device - Google Patents
Angle-resolved micro-Raman spectrum detection device Download PDFInfo
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- CN210400620U CN210400620U CN201921106024.XU CN201921106024U CN210400620U CN 210400620 U CN210400620 U CN 210400620U CN 201921106024 U CN201921106024 U CN 201921106024U CN 210400620 U CN210400620 U CN 210400620U
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Abstract
The utility model provides a micro-raman spectrum detection device of angle resolution relates to optical measurement equipment technical field, and the micro-raman spectrum detection device of angle resolution includes: a Raman detection mechanism and an inclination angle control mechanism; the Raman detection mechanism is provided with a signal inlet and a signal outlet, the signal inlet and the signal outlet correspond to the sample, and the Raman detection mechanism can emit laser signals to the surface of the sample, collect scattering signals excited on the surface of the sample and carry out Raman spectrum analysis; the Raman detection mechanism is connected with the inclination angle control mechanism, and the inclination angle control mechanism is used for adjusting the connection angle of the Raman detection mechanism and the inclination angle control mechanism so as to adjust the angle of the detection inclination angle of the angle resolution micro-Raman spectrum detection device. The scattering signals of the same measuring point on the surface of the sample at different detection inclination angles are collected to obtain spectral data of the same measuring point at different detection inclination angles, so that the sample can be finely measured.
Description
Technical Field
The invention relates to the technical field of optical measurement equipment, in particular to an angle-resolved micro-Raman spectrum detection device.
Background
The micro-Raman spectrum technology is a micro-scale nondestructive detection technology commonly used in the fields of materials, biology, archaeology, chemistry, mechanics and the like, can acquire information such as chemical components, crystal orientation, stress or strain of materials by collecting Raman scattering signals and analyzing the spectrum of the Raman scattering signals, and is widely applied to experimental analysis in various fields. Existing devices, whether commercial or institutional, already exist in many types of micro-raman spectroscopy devices.
The requirements of micro-nano science and technology on accurate, in-situ and online measurement research of complex materials and structures are increasing day by day, for example, the research requirements of crystal orientation identification, Raman tensor coefficient calibration, complex stress state decoupling analysis of complex crystal structures, multi-angle all-dimensional measurement of special-shaped samples and the like are required.
However, the geometry of the existing micro-raman spectroscopy detection devices is usually fixed, and most of them is that the incident excitation light coincides with the normal direction of the surface of the sample to be detected. Because the existing instruments and devices cannot perform Raman excitation and detection at any geometric angle and polarization configuration, many fine and complex spectral analyses are difficult to perform, and further the research requirements of micro-nano science and technology on fine detection of complex materials and structures cannot be met.
Disclosure of Invention
The invention aims to provide an angle-resolved micro-Raman spectrum detection device, and aims to solve the problem that in the prior art, the micro-Raman spectrum detection device cannot realize refined measurement on a sample due to the fact that the geometric configuration of the detection on the sample is fixed.
The invention provides an angle-resolved microscopic Raman spectrum detection device, which comprises: a Raman detection mechanism and an inclination angle control mechanism;
the Raman detection mechanism is provided with a signal inlet and a signal outlet, the signal inlet and the signal outlet correspond to the sample, and the Raman detection mechanism is used for emitting laser signals to the surface of the sample, collecting scattering signals excited on the surface of the sample and carrying out Raman spectrum analysis;
the Raman detection mechanism is connected with the inclination angle control mechanism, the inclination angle control mechanism is used for adjusting the connection angle of the Raman detection mechanism and the inclination angle control mechanism so as to adjust the angle of the detection inclination angle of the angle resolution micro-Raman spectrum detection device, and the detection inclination angle is the included angle between the optical axis of the incident exciting light and the normal direction of the sample.
Further, the tilt angle control mechanism is configured to make the detected tilt angle an adjustable angle of 0 degree or more and 90 degrees or less.
Furthermore, the angle-resolved micro-Raman spectrum detection device also comprises a sample stage and an in-situ rotating mechanism;
the sample table is used for placing a sample;
the in-situ rotating mechanism is arranged below the sample stage and connected with the in-situ rotating mechanism, and the in-situ rotating mechanism is used for driving the sample stage to rotate in situ so as to adjust the angle of a detection corner of the angle resolution micro-Raman spectrum detection device, wherein the detection corner is a corner generated along the normal direction of the sample by the optical axis of incident exciting light and the plane where the normal direction of the sample is located.
Further, the home position rotation mechanism is configured to make the detection rotation angle be an adjustable angle greater than or equal to 0 degree and less than or equal to 360 degrees.
Further, the Raman detection mechanism comprises a Raman detection module, a laser, a spectrograph and a microscope lens;
the signal inlet and outlet is arranged on the microscope head;
an incident light path and a scattering light path are arranged in the Raman detection module, the laser is arranged at one end of the incident light path of the Raman detection module and is connected with the Raman detection module, the spectrograph is arranged at one end of the scattering light path of the Raman detection module and is connected with the Raman detection module;
the microscope lens is arranged at the other end of the incident light path and the other end of the reflection light path on the Raman detection module, and one end of the microscope lens, which is far away from the signal inlet and the signal outlet, is connected with the Raman detection module.
Further, the Raman detection mechanism also comprises a polarization control module;
the polarization control module is arranged in the Raman detection module and used for adjusting the polarization angle of the incident exciting light and the collected scattered light, the polarization angle of the incident exciting light is the angle of the azimuth angle of the polarization direction of the incident exciting light on the optical axis wave front plane, and the polarization angle of the collected scattered light is the angle of the azimuth angle of the polarization direction of the collected scattered light on the optical axis wave front plane.
Further, the inclination angle control mechanism comprises a base, a support rod and a connecting piece;
the base is connected with one end of the supporting rod, and the other end of the supporting rod is connected with the Raman detection module through the connecting piece.
Further, the raman detection mechanism further includes an introduction part and a discharge part;
the laser is connected with the Raman detection module through the leading-in part, and the spectrograph is connected with the Raman detection module through the leading-out part;
the leading-in part comprises a leading-in optical fiber and a leading-in optical fiber coupler, one end of the leading-in optical fiber is connected with the laser, the other end of the leading-in optical fiber is connected with the leading-in optical fiber coupler, and the leading-in optical fiber coupler is connected with the Raman detection module;
the leading-out part comprises a leading-out optical fiber and a leading-out optical fiber coupler, one end of the leading-out optical fiber is connected with the spectrograph, the other end of the leading-out optical fiber is connected with the leading-out optical fiber coupler, and the leading-out optical fiber coupler is connected with the Raman detection module.
Furthermore, a first three-dimensional shifter is arranged between the base and the supporting rod, one end of the first three-dimensional shifter is connected with the supporting rod, and the other end of the first three-dimensional shifter is connected with the base;
the in-situ rotating mechanism comprises a rotating platform and a second three-dimensional shifter, and the second three-dimensional shifter is arranged below the rotating platform; and the second three-dimensional shifter is connected with the rotating platform.
Compared with the prior art, the angle-resolved microscopic Raman spectrum detection device provided by the invention has the following advantages:
when the angle-resolved micro-Raman spectrum detection device provided by the invention is used, the signal inlet and outlet of the Raman detection mechanism correspond to the measuring point on the surface of the sample, namely the measuring point on the surface of the sample is on the extension line of the optical axis of the incident exciting light of the Raman detection mechanism.
The angle of the detection inclination angle of the angle resolution micro-Raman spectrum detection device is adjusted by adjusting the connection angle of the Raman detection mechanism and the inclination angle control mechanism, so that the angle resolution micro-Raman spectrum detection device can collect scattering signals of the same measuring point on the surface of a sample at different detection inclination angles, and perform Raman spectrum analysis on the scattering signals respectively to obtain spectrum data of the same measuring point at different detection inclination angles, and further realize the research of fine measurement such as the decoupling analysis of the complex stress state of the sample.
Drawings
In order to more clearly illustrate the detailed description of the invention or the technical solutions in the prior art, the drawings that are needed in the detailed description of the invention or the prior art will be briefly described below. It is obvious that the drawings in the following description are some embodiments of the invention, and that for a person skilled in the art, other drawings can be derived from them without inventive effort.
Fig. 1 is a schematic structural diagram of an angle-resolved micro-raman spectroscopy detection apparatus provided in an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of an angle-resolved micro-Raman spectroscopy apparatus according to another embodiment of the present invention;
FIG. 3 is a schematic structural diagram of an angle-resolved micro-Raman spectrum detection apparatus according to another embodiment of the present invention;
fig. 4 is a schematic structural diagram of a raman detection module, a polarization control module and a microscope lens in the angle-resolved micro-raman spectroscopy detection apparatus according to the embodiment of the present invention;
FIG. 5 is a schematic diagram of an angle-resolved micro-Raman spectroscopy apparatus according to an embodiment of the present invention;
FIG. 6 is a schematic structural diagram of an angle-resolved micro-Raman spectroscopy apparatus according to an embodiment of the present invention;
fig. 7 is a schematic structural diagram of an angle-resolved micro-raman spectroscopy apparatus according to another embodiment of the present invention.
Reference numerals:
a 100-angle resolution micro-Raman spectrum detection device; 11-a Raman detection module; 111-a first collimator; 112-a raman filter; 113-a first mirror; 114-a second collimator; 115-polarizer; 116-a first high pass filter; 117-a second high pass filter; 118-a half-wave plate; 119-a pluggable mirror; 1110-a second mirror; 1111-half reflecting and half transmitting mirror; 1112-a CCD camera; 12-a laser; 121-an introduction part; 13-spectrograph; 131-a lead-out section; 14-micro lens; 141-one-dimensional displacer; 15-a polarization control module; 16-a signal light path module; 17-observation light path module; 21-a base; 211-a first three-dimensional displacer; 22-a support bar; 231-a fixing plate; 232-bolt; 3-a sample stage; 31-sample; 4-an in-situ rotation mechanism; 5-a second three-dimensional shifter; 6-optical axis of incident excitation light; 7-a rotating shaft of the in-situ rotation mechanism; 8-detection optical axis.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that, as the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", "front", "rear", etc. appear, their indicated orientations or positional relationships are based on those shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" as appearing herein are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Fig. 1 is a schematic structural diagram of an angle-resolved micro-raman spectroscopy detection apparatus provided in an embodiment of the present invention; fig. 2 is a schematic structural diagram of an angle-resolved micro-raman spectroscopy apparatus according to another embodiment of the present invention.
As shown in fig. 1-2, the present embodiment provides an angle-resolved micro-raman spectroscopy apparatus 100, including: a Raman detection mechanism and an inclination angle control mechanism; the raman detection mechanism is provided with a signal inlet 142, the signal inlet 142 corresponds to the sample, and the raman detection mechanism is used for emitting laser signals to the surface of the sample 31, collecting scattering signals excited on the surface of the sample 31 and carrying out raman spectrum analysis; the raman detection mechanism is connected to the tilt angle control mechanism, the tilt angle control mechanism is configured to adjust a connection angle between the raman detection mechanism and the tilt angle control mechanism, so as to adjust an angle of a detection tilt angle of the angle-resolved micro-raman spectroscopy detection apparatus 100, the detection tilt angle is an included angle between an optical axis 6 of the incident excitation light and a normal direction of the sample 31, and in fig. 1, the detection tilt angle is represented by "Ψ".
The inclination control mechanism is configured to make the detected inclination Ψ an adjustable angle of 0 degree or more and 90 degrees or less.
The angle-resolved micro-raman spectroscopy detection device 100 further comprises a sample stage 3; the sample stage 3 is used for placing a sample.
Compared with the prior art, the angle-resolved micro-raman spectroscopy detection apparatus 100 provided by the present embodiment has the following advantages:
when the angle-resolved micro-raman spectroscopy detection apparatus 100 provided in this embodiment is used, the sample 31 is placed on the sample stage 3, so that the signal inlet/outlet 142 of the raman detection mechanism corresponds to a measurement point on the surface of the sample 31 on the sample stage 3, that is, the measurement point on the surface of the sample 31 is on an extension line of the optical axis 6 of the incident excitation light of the raman detection mechanism.
By adjusting the connection angle between the raman detection mechanism and the tilt angle control mechanism, the angle of the detection tilt angle of the angle-resolved micro-raman spectrum detection device 100 is adjusted, so that the angle-resolved micro-raman spectrum detection device 100 can collect scattering signals of the same measurement point on the surface of the sample 31 at different detection tilt angles, and perform raman spectrum analysis on the scattering signals respectively to obtain spectrum data of the same measurement point at different detection tilt angles, thereby further realizing the research of fine measurement such as complex stress state decoupling analysis on the sample 31.
Further, the raman detection mechanism includes a raman detection module 11, a laser 12, a spectrograph 13 and a microscope lens 14; the signal inlet/outlet 142 is disposed on the microscope 14; an incident light path and a scattering light path are arranged in the Raman detection module 11, the laser 12 is arranged at one end of the incident light path of the Raman detection module 11, the laser 12 is connected with the Raman detection module 11, the spectrograph 13 is arranged at one end of the scattering light path of the Raman detection module 11, and the spectrograph 13 is connected with the Raman detection module 11; the microscope 14 is disposed at the other end of the incident light path and the reflected light path on the raman detection module 11, and the end of the microscope 14 away from the signal inlet/outlet 142 is connected to the raman detection module 11.
The incident optical path module and the scattering optical path module are collectively referred to as a signal optical path module 16.
The raman detection module 11 comprises a shell, an incident light path module and a scattering light path module which are arranged in the shell, wherein the shell is provided with an incident light inlet and a scattered light outlet; a laser 12 is connected to the incident light inlet of the housing and a spectrograph 13 is connected to the scattered light outlet of the housing. The incident light path module includes a first collimator 111, a raman filter 112, and a first mirror 113; the first collimator 111, the raman filter 112 and the first reflector 113 are all arranged in the shell and are respectively connected with the shell; the scattered light path module comprises a second collimator 114, a first high-pass filter 116 and a second high-pass filter 117; the second collimator 114, the first high-pass filter 116 and the second high-pass filter 117 are all arranged in the shell and are respectively connected with the shell; the incident light path module forms a traveling path of incident light, the laser 12 emits a laser signal, and the laser signal enters the microscope 14 through the first collimator 111, the raman filter 112, the first reflector 113, and the second high-pass filter 117, and finally irradiates to a measurement point of the sample 31. At this time, the scattering signal excited on the surface of the sample 31 enters the microscope 14, and then enters the spectrograph 13 after passing through the second high-pass filter 117, the first high-pass filter 116 and the second collimator 114, so that the scattering light path module forms a traveling path of the scattering signal excited on the surface of the sample 31, and the spectrograph 13 performs raman spectrum analysis on the scattering signal excited on the surface of the sample 31 to obtain spectral data.
In the angle-resolved micro-raman spectroscopy detection apparatus 100 provided in the above embodiment, the optical axis 6 of the incident excitation light in the microlens 14 coincides with the optical axis of the collected scattered light.
In this specification, the optical axis 6 of the incident excitation light refers to the optical axis of the incident excitation light within the microlens 14.
A one-dimensional shifter 141 may be disposed between the raman detection module 11 and the microscope 14, and a displacement direction of the one-dimensional shifter 141 is along the optical axis 6 direction of the incident excitation light, so as to adjust the focus of the microscope 14.
Fig. 5 is a schematic diagram of an angle-resolved micro-raman spectroscopy detection apparatus 100 according to an embodiment of the present invention.
In fig. 5, the detection optical axis 8 refers to the optical axis 6 of the incident excitation light; x, Y, Z respectively represent three directions of three-dimensional linear displacement of the sample stage 3, the rotation axis 7 of the in-situ rotation mechanism is parallel to the Z axis, and the wave front plane of the detection optical axis 8 is in the X '-Y' plane, on which the excitation light e is incidentiAnd collecting scattered light esThe included angles α, β between the polarization direction of (A) and X' are respectively called the incident excitation light eiAnd collecting scattered light esThe polarization angle of (c).
Preferably, in order to further enable the angle-resolved micro-raman spectroscopy detection apparatus 100 to realize refined measurement on the sample 31, in the angle-resolved micro-raman spectroscopy detection apparatus 100 provided in this embodiment, as shown in fig. 1-2, the angle-resolved micro-raman spectroscopy detection apparatus 100 further includes an in-situ rotation mechanism; the in-situ rotating mechanism is arranged below the sample table 3, the sample table 3 is connected with the in-situ rotating mechanism, the in-situ rotating mechanism is used for driving the sample table 3 to rotate in situ so as to adjust the angle of a detection corner of the angle resolution micro-Raman spectrum detection device, and the detection corner is a corner generated along the normal direction of the sample 31 by the plane where the optical axis 6 of the incident exciting light and the normal direction of the sample 31 are located.
By controlling the in-situ rotating mechanism, the sample table 3 can carry the sample 31 to realize in-situ rotation, so that the angle-resolved micro-raman spectroscopy detection device 100 can measure the sample 31 at different detection angles, thereby obtaining spectral data at the same measurement point at different detection angles, and further realizing the research of fine measurement such as complex stress state decoupling analysis on the sample 31.
The detection rotation angle refers to a rotation angle of the optical axis 6 of the incident excitation light from the plane of the normal direction of the sample 31 along the normal direction of the sample 31, and is represented by "δ" in fig. 5.
The home position rotation mechanism is configured to make the detection rotation angle at an adjustable angle of 0 degree or more and 360 degrees or less. In the process of rotating the sample table 3, the sample table 3 and the sample 31 are always kept rotating in situ, namely the position of the measuring point is kept unchanged.
Further, in order to enable the angle-resolved micro-raman spectroscopy detection apparatus 100 to realize refined measurement on the sample 31, in the angle-resolved micro-raman spectroscopy detection apparatus 100 provided in this embodiment, as shown in fig. 1-2 and fig. 5, the raman detection mechanism further includes a polarization control module 15; the polarization control module 15 is disposed in the raman detection module 11, and is configured to adjust a polarization angle between the incident excitation light and the collected scattered light, where the polarization angle of the incident excitation light is an angle of an azimuth angle of a polarization direction of the incident excitation light on the optical axis wavefront plane, and the polarization angle of the collected scattered light is an angle of an azimuth angle of the polarization direction of the collected scattered light on the optical axis wavefront plane.
Incident excitation light eiAnd collecting scattered light esThe azimuth angle of the polarization direction of (1) on the optical axis wavefront plane is referred to as the polarization angle of the incident excitation light and the polarization angle of the collected scattered light, the polarization angle of the incident excitation light is represented by "α", and the polarization angle of the collected scattered light is represented by "β".
The polarization control module 15 includes a polarizer 115 and a half-wave plate 118, the polarizer 115 is disposed between the second collimator 114 and the first high-pass filter 116, and the polarizer 115 is connected to the housing; half-wave plate 118 is disposed between second high-pass filter 117 and microlens 14, and half-wave plate 118 is connected to the housing.
The laser 12 emits a laser signal, and the laser signal enters the microscope 14 through the first collimator 111, the raman filter 112, the first mirror 113, the second high-pass filter 117, and the half-wave plate 118, and finally irradiates to a measurement point of the sample 31. At this time, the scattering signal excited on the surface of the sample 31 enters the microscope 14, and then enters the spectrograph 13 after passing through the half-wave plate 118, the second high-pass filter 117, the first high-pass filter 116, the polarizer 115, and the second collimator 114, and the spectrograph 13 performs raman spectrum analysis on the scattering signal excited on the surface of the sample 31 to obtain spectral data.
By adjusting the polarizer 115 and the half-wave plate 118, the incident excitation light e can be adjustediAnd collecting scattered light esThe polarization angle of (c).
During the experiment, firstly, the imaging focus of the microscope 14 is adjusted to the measuring point position on the surface of the sample 31 by adjusting the sample stage 3; then, the angle-resolved micro-raman spectroscopy apparatus 100 performs spectroscopic analysis on the sample 31 under the combination of a plurality of detection inclination angles, detection rotation angles, and polarization angles, so as to realize fine measurement of the sample 31, such as complex stress state decoupling analysis.
Preferably, the raman detection module 11 further includes an observation light path module 17, the observation light path module 17 includes a pluggable reflector 119, a second reflector 1110, a transflective mirror 1111 and a CCD camera 1112, the pluggable reflector 119, the second reflector 1110 and the transflective mirror 1111 are all disposed in the housing and are respectively connected with the housing, the pluggable reflector 119 is disposed between the first high-pass filter and the second high-pass filter, the CCD camera 1112 is disposed outside the housing, and the CCD camera 1112 is connected with the housing.
When a user wants to observe whether the measuring point of the sample 31 is on the optical axis 6 of the incident exciting light through the raman detection module 11, the pluggable reflector 119 can be inserted between the first high-pass filter and the second high-pass filter, the user can observe through the CCD, and after the user finishes observing the sample 31, the pluggable reflector 119 is pulled out, and the angle-resolved micro-raman spectroscopy detection device 100 is continuously used for measuring the sample 31.
Further, in order to better realize the adjustment of the angle of the detection tilt angle of the angle-resolved micro-raman spectroscopy detection apparatus 100 so as to perform a refined measurement on the sample 31, in the angle-resolved micro-raman spectroscopy detection apparatus 100 provided in this embodiment, as shown in fig. 3, the tilt angle control mechanism includes a base 21, a support rod 22 and a connecting member; the base 21 is connected with one end of the support rod 22, and the other end of the support rod 22 is connected with the raman detection module 11 through a connecting piece.
The connector includes a fixing plate 231 and a bolt 232; the fixing plate 231 is connected with the raman detection module 11; first threaded holes are formed in the supporting rod 22, second threaded holes are formed in the fixing plate 231, and the bolts 232 penetrate through the first threaded holes and the second threaded holes in sequence, so that the supporting rod 22 is connected with the fixing plate 231.
Through rotating bolt 232 to adjust the angle of connection between raman detection module 11 and the bracing piece 22, and then the angle of the detection inclination of angle resolution micro-raman spectrum detection device 100, after waiting to adjust and accomplish, screw up bolt 232 and fixed plate 231, thereby obtain the spectral data when different detection inclinations, in order to realize the measurement of refining to sample 31.
Further, in order to firmly connect the laser 12 and the spectrograph 13 with the raman detection module 11 and ensure that the laser signal can better enter the raman detection module 11, and the scattering signal excited on the surface of the sample 31 can better enter the spectrograph 13, in the angle-resolved micro-raman spectroscopy detection apparatus 100 provided in this embodiment, as shown in fig. 1-2, the raman detection mechanism further includes an introducing part 121 and an deriving part 131; the laser 12 is connected to the raman detection module 11 through the introduction unit 121, and the spectrograph 13 is connected to the raman detection module 11 through the derivation unit 131.
The lead-in part 121 includes a lead-in optical fiber and a lead-in optical fiber coupler, one end of the lead-in optical fiber is connected with the laser 12, the other end of the lead-in optical fiber is connected with the lead-in optical fiber coupler, and the lead-in optical fiber coupler is connected with the raman detection module 11; the derivation unit 131 includes a derivation optical fiber and a derivation optical fiber coupler, one end of the derivation optical fiber is connected to the spectrograph 13, the other end of the derivation optical fiber is connected to the derivation optical fiber coupler, and the derivation optical fiber coupler is connected to the raman detection module 11.
The optical fiber has a good optical signal conduction function, so that the laser 12 is connected with the raman detection module 11 through the lead-in part 121, and the spectrograph 13 is connected with the raman detection module 11 through the lead-out part 131, so that the laser signal can be ensured to well enter the raman detection module 11, and the scattering signal excited on the surface of the sample 31 can well enter the spectrograph 13 for raman spectrum analysis.
Further, in order to facilitate the user to adjust the positions of the supporting rod 22 and the sample stage 3 in the three-dimensional direction, and further adjust the positions of the raman detection module 11 and the sample 31 in the three-dimensional direction, so as to facilitate the user to complete the alignment work of the incident excitation light of the raman detection mechanism and the surface measurement point of the sample 31, in the angle-resolved micro-raman spectroscopy detection apparatus 100 provided in this embodiment, as shown in fig. 2, a first three-dimensional shifter 211 is arranged between the base 21 and the supporting rod 22; one end of the first three-dimensional shifter 211 is connected with the support rod 22, and the other end is connected with the base 21; the in-situ rotating mechanism comprises a rotating platform 4 and a second three-dimensional shifter 5, and the second three-dimensional shifter 5 is arranged below the rotating platform 4; and a second three-dimensional displacer 5 is connected to the rotary table 4.
The first three-dimensional shifter 211 or/and the second three-dimensional shifter 5 is/are used for adjusting the spatial positions of the inclination angle control mechanism and the raman detection mechanism relative to the sample so as to adjust the detection optical axis of the raman detection mechanism, and the detection optical axis is aligned to the spatial position of the measuring point on the surface of the sample and is kept in place in the process of adjusting the detection inclination angle, the detection rotation angle and the polarization angle of the raman detection mechanism.
The positions of the raman detection module 11 and the sample stage 3 in the three-dimensional direction are adjusted by adjusting the first three-dimensional shifter 211 and the second three-dimensional shifter 5, so that the surface measuring point of the sample 31 is always on the optical axis 6 of the incident excitation light in the process of adjusting the detection inclination angle, the detection rotation angle and the polarization angle, and further, a user can conveniently use the angle-resolved micro-raman spectroscopy detection device 100 to perform fine measurement on the sample 31.
By controlling the in-situ rotating mechanism, the sample table 3 can carry the sample 31 to realize in-situ rotation, so that the angle-resolved micro-raman spectroscopy detection device 100 can measure the sample 31 at different detection angles, thereby obtaining spectral data at the same measurement point at different detection angles, and further realizing the research of fine measurement such as complex stress state decoupling analysis on the sample 31.
Also, the home position rotating mechanism may include a closed loop control function.
Fig. 6 is a schematic structural diagram of the angle-resolved micro-raman spectroscopy detection apparatus 100 according to the embodiment of the present invention; fig. 7 is a schematic structural diagram of an angle-resolved micro-raman spectroscopy detection apparatus 100 according to another embodiment of the present invention.
The first embodiment is as follows:
the angle-resolved micro-raman spectroscopy apparatus 100 can perform a refined measurement on the sample 31, for example, a complex stress state decoupling analysis.
Taking the measurement of the stress component of the single crystal silicon with the {100} crystal plane under the non-equal biaxial stress state as an example, the step of decoupling and measuring the stress in the single crystal silicon sample 31 surface by adopting the analysis method of realizing the bidirectional stress decoupling of the single crystal silicon with the {100} crystal plane through the Raman detection of changing the inclination angle is as follows:
first, sample 31 preparation: the {100} crystal plane single crystal silicon cut to a specific size is taken as a sample 31 to be measured, the length, width and height directions of the sample are respectively along the [100] crystal direction, [010] crystal direction and the [001] crystal direction, as shown in fig. 6-7, and the sample 31 is ground to meet the requirements of raman measurement and loading on the surface flatness of the sample 31.
Second, example calculation: taking θ as 0 ° as an example, the angle-resolved micro-raman spectroscopy detection apparatus 100 is set to a vertical backscattering geometry, as shown in fig. 6, and is vertically polarized, and the frequency shift-stress relation is obtained as follows: Δ ωobs1＝-2.298(σθ+σθ′) Then, the detection inclination angle of the angle-resolved microscopic raman spectrum detection apparatus 100 is changed to Ψ equal to 30 °, that is, an oblique backscattering configuration, as shown in fig. 7, the vertical polarization is also adopted, and the frequency shift-stress relationship after raman selection rule selection is obtained by calculation as follows: Δ ωobs2＝-2.298σθ-2.005σθ′And then two stress components sigma can be obtained by measuring frequency shift quantities under two geometric configurations and connecting vertical frequency shift-stress expressions in parallelθAnd σθ′。
If atUnder the above conditions, the sample 31 was subjected to confining pressure in the direction along the single crystal silicon [100]]The strain of the sample 31 in the confining pressure direction is zero in the crystal direction, and the two in-plane principal stress sigma can be obtained based on the generalized Hooke's lawθAnd σθ′There is a relationship between: sigmaθ′＝0.279σθThus, the frequency shift-stress relationship in the vertical backscatter geometry is simplified to: Δ ωobs1＝-2.939σθThe frequency shift-stress relation under the oblique backscattering geometric configuration is simplified as follows: Δ ωobs2＝-2.857σθ。
Step three, verifying the experiment: and verifying the calculated frequency shift-stress relation expression under two geometrical conditions in the second step, wherein the specific operation steps are as follows: 1. adjusting the angle-resolved micro-raman spectroscopy detection apparatus 100 to a vertical back-scattering geometry configuration, i.e., psi ═ 0 °, as shown in fig. 6, vertically polarizing, and then placing the monocrystalline silicon sample 31 on a loading platform; 2. the initial state of the sample 31 is stress-free, single-point measurement is carried out for 20 times, and Raman spectrum information of the sample is collected; 3. carrying out confining pressure loading on a monocrystalline silicon sample 31, wherein the loading direction is along the crystal direction of monocrystalline silicon [100], the loading step length is 150N, single-point measurement is carried out for 20 times after each loading is finished, Raman spectrum information is collected until 2300N is loaded, spectrum information under different loading states is finally obtained, and the frequency shift mean value and the standard deviation are extracted, and the corresponding data are shown in table 1; 4. unloading the sample 31, then adjusting the measurement system to the oblique backscattering geometry, i.e. Ψ ═ 30 °, and vertically polarizing, repeating the operation steps 2 and 3 to obtain the raman spectrum information under the oblique backscattering configuration, and extracting the frequency shift mean and standard deviation under different loading, where the corresponding data are shown in table 2.
The Raman frequency shift factor under the vertical back scattering geometric configuration is obtained by fitting the slope of the frequency shift-stress distribution function measured under the condition of the non-equal biaxial stress loading of the monocrystalline silicon－1PerGPa, with a theoretical result of-2.94 cm－1the/GPa is almost consistent; the raman shift factor at an oblique backscatter geometry with a probe tilt psi of 30 deg. is about-3.04 cm－1PerGPa, with a theoretical result of-2.86 cm－1The ratio of the specific surface area to the specific surface area is similar to that of the specific surface area per GPa. The above materialsThe experimental results show that the stress component can be quickly and simply decoupled by changing the inclination angle of Raman detection by using the analytical method to carry out experimental analysis on the non-equal biaxial stress state in the monocrystalline silicon surface.
Table 1: mean value and standard deviation of Raman frequency shift measured by vertical backscattering geometric configuration under different loading states
Table 2: mean and standard deviation of Raman frequency shifts measured under different loading states by oblique backscattering geometric configuration
Example two:
taking the example of "fine analysis of unidirectional residual stress of unknown crystal orientation of epitaxially grown (001) single crystal silicon thin film", the device of the present invention was used to perform a test experiment. The material to be measured is a monocrystalline silicon film which grows in an epitaxial mode, the surface of the monocrystalline silicon film is a (001) crystal face, unidirectional residual stress caused by technological factors exists in the face, and the magnitude and the direction of the stress are measured. The direction of the stress cannot be measured by the existing Raman system.
The specific steps for carrying out the residual stress analysis by adopting the method are as follows:
firstly, system construction: as shown in fig. 1 or fig. 4, the respective components are connected;
second, sample 31 installation: the sample 31 is placed on the sample stage 3 and the geometrical relationship as shown in fig. 5 is established; wherein [001] crystal direction, which is the external normal direction of the sample 31, is set as the Z direction, and [100] crystal direction and [010] crystal direction in the surface to be measured are the X direction and the Y direction, respectively;
step three, measuring point selection: the spatial position of a measuring point of the system is adjusted to the surface of the sample 31 by regulating the sample table 3, and then the measuring point is adjusted to the position to be measured on the surface of the sample 31 by utilizing the observation function of the Raman detection module 11;
fourthly, parameter setting, namely regulating and controlling technical parameters of the system according to measured requirements, wherein the detection inclination angle psi is 30 degrees, the polarization angle α is 90 degrees, and the detection inclination angle β is 0 degree;
fifthly, detecting the spectrum; respectively carrying out Raman spectrum detection when the detection inclination angle delta is 0 degrees and delta is 45 degrees to obtain Raman spectrum information; wherein 20 different spot information on the surface of the sample 31 is taken under the same system parameters.
Sixthly, analyzing data: fitting the actually measured Raman frequency shifts to obtain respective frequency shifts and average values thereof, as shown in Table 3; based on the fact that the measured data is substituted into the formula (1) of the inclined Raman detection of the monocrystalline silicon (001):
wherein, Δ ω0For detecting the amount of frequency shift, Δ ω, at a rotation angle of 0 °45Detecting the frequency shift quantity delta omega when the rotation angle is 45 degrees45Theta is the direction of the stress to be measured, sigmaθThe unidirectional stress to be measured; obtain the stress size sigma1159.93MPa, and the stress direction theta is 42.66 degrees.
Table 3: actual and average values of Raman frequency shift at 0 deg. and 45 deg. at different measuring points
| Measuring point | 1 | 2 | 3 | 4 | 5 | 6 | 7 |
| Δω0(cm-1) | -0.341 | -0.328 | -0.374 | -0.330 | -0.358 | -0.342 | -0.348 |
| Δω45(cm-1) | -0.420 | -0.534 | -0.465 | -0.487 | -0.397 | -0.448 | -0.453 |
| |
8 | 9 | 10 | 11 | 12 | 13 | 14 |
| Δω0(cm-1) | -0.354 | -0.335 | -0.319 | -0.339 | -0.351 | -0.347 | -0.363 |
| Δω45(cm-1) | -0.486 | -0.479 | -0.450 | -0.438 | -0.436 | -0.477 | -0.602 |
| |
15 | 16 | 17 | 18 | 19 | 20 | Average |
| Δω0(cm-1) | -0.320 | -0.351 | -0.357 | -0.344 | -0.348 | -0.333 | -0.344 |
| Δω45(cm-1) | -0.454 | -0.451 | -0.462 | -0.465 | -0.379 | -0.439 | -0.461 |
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (9)
1. An angle-resolved micro-raman spectroscopy apparatus, comprising: a Raman detection mechanism and an inclination angle control mechanism;
the Raman detection mechanism is provided with a signal inlet and a signal outlet, the signal inlet and the signal outlet correspond to the sample, and the Raman detection mechanism is used for emitting laser signals to the surface of the sample, collecting scattering signals excited on the surface of the sample and carrying out Raman spectrum analysis;
the Raman detection mechanism is connected with the inclination angle control mechanism, the inclination angle control mechanism is used for adjusting the connection angle of the Raman detection mechanism and the inclination angle control mechanism so as to adjust the angle of the detection inclination angle of the angle resolution micro-Raman spectrum detection device, and the detection inclination angle is the included angle between the optical axis of the incident exciting light and the normal direction of the sample.
2. The angle-resolved micro-raman spectrum detection apparatus according to claim 1, wherein the tilt control mechanism is configured to make the detection tilt an adjustable angle of 0 degree or more and 90 degrees or less.
3. The angle-resolved micro-raman spectroscopy apparatus of claim 1, further comprising a sample stage and an in-situ rotation mechanism;
the sample table is used for placing a sample;
the in-situ rotating mechanism is arranged below the sample stage and connected with the in-situ rotating mechanism, and the in-situ rotating mechanism is used for driving the sample stage to rotate in situ so as to adjust the angle of a detection corner of the angle resolution micro-Raman spectrum detection device, wherein the detection corner is a corner generated along the normal direction of the sample by the optical axis of incident exciting light and the plane where the normal direction of the sample is located.
4. The angle-resolved micro-raman spectroscopy apparatus according to claim 3, wherein the in-situ rotation mechanism is configured to make the detection rotation angle at an adjustable angle of 0 degree or more and 360 degrees or less.
5. The angle-resolved micro-raman spectroscopy apparatus of claim 3, wherein the raman detection mechanism comprises a raman detection module, a laser, a spectrograph, and a microscope lens;
the signal inlet and outlet is arranged on the microscope head;
an incident light path and a scattering light path are arranged in the Raman detection module, the laser is arranged at one end of the incident light path of the Raman detection module and is connected with the Raman detection module, the spectrograph is arranged at one end of the scattering light path of the Raman detection module and is connected with the Raman detection module;
the microscope lens is arranged at the other end of the incident light path and the other end of the reflection light path on the Raman detection module, and one end of the microscope lens, which is far away from the signal inlet and the signal outlet, is connected with the Raman detection module.
6. The angle-resolved microscopic raman spectroscopy apparatus of claim 5, wherein the raman detection mechanism further comprises a polarization control module;
the polarization control module is arranged in the Raman detection module and used for adjusting the polarization angle of the incident exciting light and the collected scattered light, the polarization angle of the incident exciting light is the angle of the azimuth angle of the polarization direction of the incident exciting light on the optical axis wave front plane, and the polarization angle of the collected scattered light is the angle of the azimuth angle of the polarization direction of the collected scattered light on the optical axis wave front plane.
7. The angle-resolved micro-raman spectroscopy apparatus of claim 5, wherein the tilt control mechanism comprises a base, a support bar, and a connector;
the base is connected with one end of the supporting rod, and the other end of the supporting rod is connected with the Raman detection module through the connecting piece.
8. The angle-resolved microscopic raman spectroscopy apparatus according to claim 5, wherein the raman detection mechanism further comprises an introduction section and a derivation section;
the laser is connected with the Raman detection module through the leading-in part, and the spectrograph is connected with the Raman detection module through the leading-out part;
the leading-in part comprises a leading-in optical fiber and a leading-in optical fiber coupler, one end of the leading-in optical fiber is connected with the laser, the other end of the leading-in optical fiber is connected with the leading-in optical fiber coupler, and the leading-in optical fiber coupler is connected with the Raman detection module;
the leading-out part comprises a leading-out optical fiber and a leading-out optical fiber coupler, one end of the leading-out optical fiber is connected with the spectrograph, the other end of the leading-out optical fiber is connected with the leading-out optical fiber coupler, and the leading-out optical fiber coupler is connected with the Raman detection module.
9. The angle-resolved micro-raman spectroscopy apparatus according to claim 7, wherein a first three-dimensional shifter is provided between the base and the support bar, one end of the first three-dimensional shifter is connected to the support bar, and the other end is connected to the base;
the in-situ rotating mechanism comprises a rotating platform and a second three-dimensional shifter, and the second three-dimensional shifter is arranged below the rotating platform; and the second three-dimensional shifter is connected with the rotating platform.
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| CN110231092A (en) * | 2019-07-15 | 2019-09-13 | 天津大学 | Angle-resolved micro Raman spectra detection device and detection method |
| CN113075195A (en) * | 2021-03-23 | 2021-07-06 | 北京大学 | Method for depth positioning of microcracks in silicon carbide based on Raman residual stress detection |
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| CN110231092A (en) * | 2019-07-15 | 2019-09-13 | 天津大学 | Angle-resolved micro Raman spectra detection device and detection method |
| CN110231092B (en) * | 2019-07-15 | 2024-04-12 | 天津大学 | Angle resolution microscopic Raman spectrum detection device and detection method |
| CN113075195A (en) * | 2021-03-23 | 2021-07-06 | 北京大学 | Method for depth positioning of microcracks in silicon carbide based on Raman residual stress detection |
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