Scanning electron microscope imaging and spectrum in-situ detection combined system and detection method

Abstract

The invention discloses a scanning electron microscope imaging and spectrum in-situ detection combined system and a detection method, the scanning electron microscope imaging and spectrum in-situ detection combined system comprises a scanning electron microscope and an optical fiber coupling optical path module, the scanning electron microscope comprises a scanning electron microscope chamber, and an excitation source and a secondary electron detector arranged in the scanning electron microscope chamber; during detection, a sample is arranged in a scanning electron microscope chamber, and the excitation source is arranged right above the sample to be detected and can emit an electron beam to vertically irradiate a position A of the sample to generate a secondary electronic signal; and the secondary electron detector is positioned on the inclined side above the sample and is used for receiving a secondary electron signal. Laser emitted by the laser excitation source is focused by the optical fiber coupling light path module to irradiate the position A of a sample and stimulate to generate a to-be-measured light signal, the optical fiber coupling light path module is connected with the spectrograph, and the to-be-measured light signal is transmitted to the spectrograph for detection, so that high-precision in-situ, real-time and co-site observation and analysis of the sample are realized; and the morphology, composition and chemical state information of the sample can be synchronously obtained.

Description

Technical Field

[0001] This invention relates to the field of sample detection technology, and more specifically, to a system and method for combining scanning electron microscopy imaging with in-situ spectral detection. Background Technology

[0002] Scanning electron microscopy (SEM), a core material characterization technique, acquires high-resolution nanoscale images of a material's microstructure, composition, and structure by focusing an electron beam to scan the sample surface and collecting the generated signals (such as secondary electrons and backscattered electrons). It is widely used in materials science, nanotechnology, and life sciences. Spectroscopic techniques can detect and analyze internal information of samples. For example, Raman spectroscopy provides rich chemical and structural information, such as molecular vibrations, crystal structure, chemical bonds, and stress states, by analyzing the inelastic scattering spectrum of a sample to monochromatic laser light. It is a powerful tool for identifying material composition and studying surface reaction dynamics. Fluorescence spectroscopy detects the photoluminescence signal (fluorescence emission spectrum) generated after a sample is excited, analyzing its wavelength distribution and intensity characteristics to obtain information such as the material's electronic energy level structure, defect state distribution, carrier dynamics, molecular configuration, and environmental interactions. However, a single detection method cannot comprehensively analyze the multi-dimensional information of complex material systems in dynamic processes, such as the real-time correlation between morphological evolution and chemical state changes, and the interaction between local stress distribution and microstructure.

[0003] Existing SEM and spectral detection combined solutions mostly adopt a split design, requiring frequent sample transfer between different instruments, making it difficult to achieve truly high-precision in-situ, real-time, and co-localized observation and analysis. Summary of the Invention

[0004] This invention provides a system and method for combining scanning electron microscopy imaging with Raman in-situ detection, enabling the combined use of scanning electron microscopy imaging and spectral detection to achieve in-situ, real-time, and co-located observation and analysis of samples.

[0005] To achieve the above objectives, the technical solution provided by the present invention is as follows:

[0006] A scanning electron microscope imaging and in-situ spectral detection combined system is used for sample detection.

[0007] It includes a scanning electron microscope, a fiber-coupled optical path module, and a laser excitation source. The scanning electron microscope includes a scanning electron microscope chamber and an excitation source and a secondary electron detector disposed within the scanning electron microscope chamber.

[0008] During detection, the sample is placed inside the scanning electron microscope chamber, the excitation source is positioned directly above the sample to be detected and is capable of emitting an electron beam that vertically irradiates point A on the sample to generate a secondary electron signal; the secondary electron detector is located at an angle above the sample and is used to receive the secondary electron signal.

[0009] The laser excitation source is connected to the fiber-coupled optical path module; the laser emitted by the laser excitation source is focused by the fiber-coupled optical path module onto the sample A and simultaneously generates a light signal to be measured, which is emitted in different directions closer to the sample; the fiber-coupled optical path module is also connected to a spectrometer and collects the light signal to be measured and transmits it to the spectrometer for detection.

[0010] As a further improvement, when the fiber-coupled optical path module is located directly above the sample A to collect the optical signal to be measured, a through hole is opened on the fiber-coupled optical path module to allow the electron beam to pass through.

[0011] As a further improvement, the fiber-coupled optical path module is an off-axis parabolic mirror probe, which includes an off-axis parabolic mirror disposed at one end of the off-axis parabolic mirror probe and an achromatic lens located inside the off-axis parabolic mirror probe; the off-axis parabolic mirror is located directly below the excitation source, and the through hole is formed on the off-axis parabolic mirror; the off-axis parabolic mirror faces the sample on one side, and an opening is formed on the off-axis parabolic mirror probe.

[0012] As a further improvement, the fiber-coupled optical path module is a planar mirror probe, which includes a planar mirror disposed at one end of the planar mirror probe and a rear achromatic lens and a front achromatic lens located inside the planar mirror probe. The front achromatic lens is disposed at the end close to the planar mirror. The planar mirror is located directly below the excitation source, and the through hole is formed on the planar mirror. The side of the planar mirror facing the sample has an opening.

[0013] As a further improvement, the optical signal to be measured includes a Raman optical signal or a fluorescence signal.

[0014] As a further improvement, the fiber-coupled optical path module is located in the scanning electron microscope chamber and placed on an adjustment frame, which is also connected to the focusing assembly, which is used to adjust the position of the fiber-coupled optical path module.

[0015] As a further improvement, the focusing component includes,

[0016] X-axis direction adjustment component, used to move the fiber optic coupled optical path module along the X-axis direction;

[0017] The Y-axis adjustment component is connected to the X-axis adjustment component and is used to move the fiber optic coupled optical path module along the Y-axis direction.

[0018] The Z-axis adjustment component is connected to the Y-axis adjustment component and is used to move the fiber optic coupled optical path module along the Z-axis direction.

[0019] As a further improvement, the X-axis direction adjustment component includes a lead screw and a first slider connected to the lead screw;

[0020] The Y-axis direction adjustment component includes a third slider located on the first slider and a third lead screw connected to the third slider;

[0021] The Z-axis direction adjustment component includes a second slider connected to the third slider and a second lead screw connected to the second slider.

[0022] As a further improvement, the diameter of the through hole is 1-10 mm.

[0023] This invention also provides a detection method using a combined scanning electron microscopy imaging and in-situ spectral detection system.

[0024] For testing samples, it includes a scanning electron microscope, a fiber-coupled optical path module, and a laser excitation source. The scanning electron microscope includes a scanning electron microscope chamber and an excitation source and a secondary electron detector disposed within the scanning electron microscope chamber.

[0025] During the detection, the sample is placed inside the scanning electron microscope chamber, and the excitation source is placed directly above the sample to be detected and emits an electron beam that vertically irradiates point A of the sample to generate secondary electrons.

[0026] The secondary electron detector is positioned at an angle above the sample to receive the secondary electrons;

[0027] The laser excitation source is connected to the fiber-coupled optical path module; the laser emitted by the laser excitation source is focused by the fiber-coupled optical path module onto the sample A, thereby generating a light signal to be measured, which is emitted in different directions closer to the sample; the fiber-coupled optical path module is also connected to a spectrometer and collects the light signal to be measured, which is then transmitted to the spectrometer for detection.

[0028] Compared with existing technologies, the technical solution provided by this invention has the following advantages: The sample is placed inside the scanning electron microscope (SEM) chamber. The excitation source in the SEM emits an electron beam that irradiates point A of the sample, generating a secondary electron signal. The secondary electron detector receives the secondary electron signal, thereby obtaining the sample surface morphology information. Simultaneously, point A of the sample can be excited by other optical signals to generate a test optical signal. This test optical signal is collected by the fiber-coupled optical path module and transmitted to a spectrometer for detection. The spectrometer simultaneously analyzes the internal information of the sample, achieving high-precision in-situ, real-time, and co-situ observation and analysis of the sample, thus enabling the simultaneous and accurate acquisition of sample morphology, composition, and chemical state information. Attached Figure Description

[0029] Figure 1 This is a schematic diagram of a sample being irradiated by an excitation source.

[0030] Figure 2 A schematic diagram of an off-axis parabolic mirror probe structure;

[0031] Figure 3 This is a schematic diagram of the plane mirror probe structure;

[0032] Figure 4 Schematic diagram of the optical signal acquisition principle of the fiber-coupled optical path module using an off-axis parabolic mirror probe;

[0033] Figure 5 Schematic diagram of optical signal acquisition by a plane mirror probe in an optical fiber coupled optical path module;

[0034] Figure 6 When the fiber-coupled optical path module is an off-axis parabolic mirror probe, it is used in Raman or fluorescence measurement.

[0035] Figure 7 When the fiber-coupled optical path module is a planar mirror probe, it is used in Raman or fluorescence measurement.

[0036] Figure 8 This is a schematic diagram of a scanning electron microscope (SEM) image.

[0037] Figure 9 This is a top view of the focusing component structure;

[0038] Figure 10 This is the main view of the focusing component structure;

[0039] Figure 11 A schematic diagram showing the off-axis parabolic mirror probe located inside the scanning electron microscope chamber and connected to the focusing assembly when the fiber-coupled optical path module is an off-axis parabolic mirror probe.

[0040] Figure 12 This diagram illustrates the situation where the optical fiber coupled optical path module is a planar reflector probe, located within the scanning electron microscope chamber and connected to the focusing assembly.

[0041] Label Explanation:

[0042] 1. Excitation source; 2. Sample; 3. Electron beam; 4. Scanning electron microscope chamber; 6. Optical fiber; 7. Off-axis parabolic mirror; 14. Through-hole;

[0043] 101. Optical signal under test; 102. Laser; 202. Rotary motor;

[0044] 28. Achromatic lens; 29. ​​Off-axis parabolic mirror fiber optic adapter;

[0045] 32. Laser excitation source; 33. First converging lens; 34. Dichroic mirror; 35. Long-pass filter; 36. Second converging lens; 37. Spectrometer; 38. Bandpass filter;

[0046] 38. Plane mirror; 39. Plane mirror holder;

[0047] 40. Plane mirror fiber optic adapter; 41. Plane mirror rear achromatic lens; 42. Plane mirror front achromatic lens; 43. Plane mirror lens sleeve;

[0048] 401. Secondary electronic detector; 402. Secondary electronic signal;

[0049] 70. First motor; 71. Lead screw; 72. Third slider; 73. Second motor; 74. First slider; 75. Third motor; 76. Second slider; 77. First slide rail. Detailed Implementation

[0050] To further understand the content of this invention, a detailed description of the invention will be provided in conjunction with the accompanying drawings and embodiments.

[0051] The structures, proportions, sizes, etc., shown in the accompanying drawings of this specification are only for the purpose of assisting those skilled in the art in understanding and reading the content disclosed in the specification, and are not intended to limit the conditions under which the present invention can be implemented. Therefore, they have no substantial technical significance. Any modifications to the structure, changes in the proportions, or adjustments to the size, without affecting the effects and objectives that the present invention can produce, should still fall within the scope of the technical content disclosed in the present invention.

[0052] It should be noted that the terms "first," "second," etc., in the specification, claims, and accompanying drawings of this application are used to distinguish similar objects and are not necessarily used to describe a specific order or sequence. It should be understood that such use of data can be interchanged where appropriate for the embodiments of this application described herein.

[0053] In this application, the terms "upper," "lower," "left," "right," "front," "rear," "top," "bottom," "inner," "outer," "middle," "vertical," "horizontal," "lateral," and "longitudinal" indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. These terms are primarily for the purpose of better describing this application and its embodiments, and are not intended to limit the indicated devices, elements, or components to having a specific orientation, or to be constructed and operated in a specific orientation. Furthermore, some of the above terms may be used to indicate other meanings besides orientation or positional relationship; for example, the term "upper" may also be used in some cases to indicate a certain dependency or connection relationship. Those skilled in the art can understand the specific meaning of these terms in this application according to the specific circumstances.

[0054] This embodiment provides a scanning electron microscope imaging and in-situ spectral detection combined system for detecting sample 2.

[0055] Combination Figure 1-8 As shown, the detection system includes a scanning electron microscope, a fiber optic coupled optical path module, and a laser excitation source 32. The scanning electron microscope includes a scanning electron microscope chamber 4 and an excitation source 1 and a secondary electron detector 401 disposed in the scanning electron microscope chamber 4.

[0056] During the detection, sample 2 is placed inside the scanning electron microscope chamber 4, and excitation source 1 is placed directly above sample 2 and can emit electron beam 3 to vertically irradiate point A of sample 2 to generate secondary electron signal 402; secondary electron detector 401 is located on the oblique side above sample 2 and is used to receive secondary electron signal 402.

[0057] The laser excitation source 32 is connected to the fiber optic coupled optical path module; the laser emitted by the laser excitation source 32 is focused by the fiber optic coupled optical path module and irradiates point A of the sample 2, thereby generating the light signal to be measured 101. The light signal to be measured 101 is emitted in different directions closer to the sample 2; the fiber optic coupled optical path module is also connected to the spectrometer and collects the light signal to be measured and transmits it to the spectrometer for detection.

[0058] like Figure 1 As shown, sample 2 is placed inside the scanning electron microscope chamber 4. Excitation source 1 emits an electron beam 3 to irradiate point A of sample 2, generating a secondary electron signal 402. The secondary electron detector 401 receives the secondary electron signal 402, thereby obtaining the surface morphology information of the sample. Simultaneously, point A of sample 2 can be excited by other optical signals to generate a test optical signal 101. The test optical signal 101 is collected by the fiber-coupled optical path module and transmitted to the spectrometer for detection. At the same time, the internal information of the sample is analyzed, realizing high-precision in-situ, real-time, and co-situ observation and analysis of the sample, so as to achieve synchronous and accurate acquisition of sample morphology, composition, and chemical state information.

[0059] In a preferred embodiment, when the fiber-coupled optical path module is located directly above point A of sample 2 to collect the optical signal 101 to be measured, a through hole 14 is opened on the fiber-coupled optical path module for the electron beam 3 to pass through.

[0060] Combination Figure 2 and Figure 4 As shown, in one case, the fiber-coupled optical path module used is an off-axis parabolic mirror probe. The off-axis parabolic mirror probe includes an off-axis parabolic mirror 7 disposed at one end of the off-axis parabolic mirror probe and an achromatic lens 28 located inside the off-axis parabolic mirror probe. The off-axis parabolic mirror 7 is located directly below the excitation source 1, and a through hole 14 is formed on the off-axis parabolic mirror 7. The off-axis parabolic mirror 7 faces the sample 2 on one side, and an opening is formed on the off-axis parabolic mirror probe.

[0061] Specifically, the off-axis parabolic mirror probe also includes an off-axis parabolic mirror lens sleeve, an achromatic lens 28 is disposed in the off-axis parabolic mirror lens sleeve, an off-axis parabolic mirror 7 is installed at one end of the off-axis parabolic mirror lens sleeve, and an off-axis parabolic mirror fiber optic adapter 29 is installed at the other end of the off-axis parabolic mirror lens sleeve. An opening is provided on the off-axis parabolic mirror lens sleeve, which is located on the side of the off-axis parabolic mirror 7 facing the sample 2.

[0062] When using the off-axis parabolic mirror probe, the electron beam 3 passes through the through-hole 14 and strikes point A on the surface of sample 2. This point is the focal point of the off-axis parabolic mirror 7. Simultaneously, the laser 102, focused by the off-axis parabolic mirror 7, illuminates point A on sample 2, generating the light signal 101 to be measured. The off-axis parabolic mirror 7 collects the light signal 101, reflects it as parallel light, focuses it through the achromatic lens 28, and then enters the off-axis parabolic mirror fiber optic adapter 29, which transmits it via fiber optic cable to the spectrometer 32. The focal point of the achromatic lens 28 is the center of the fiber optic adapter. Since the wavelengths of the light signals to be measured vary depending on the sample, the achromatic lens ensures that the focal point of different wavelengths of light converges to a single point, thus maintaining a relatively constant distance between the achromatic lens and the fiber optic adapter.

[0063] Combination Figure 3 and Figure 5 As shown, in another case, the fiber-coupled optical path module is a planar mirror probe. The planar mirror probe includes a planar mirror 38 disposed at one end of the planar mirror probe, and a rear achromatic lens 41 and a front achromatic lens 42 of the planar mirror located inside the planar mirror probe. The front achromatic lens 42 of the planar mirror is disposed at the end close to the planar mirror 38. The planar mirror 38 is located directly below the excitation source 1, and a through hole 14 is opened on the planar mirror 38. The planar mirror 38 faces the sample 2, and an opening is opened on the planar mirror probe.

[0064] Specifically, the planar mirror probe also includes a planar mirror lens sleeve 43. A planar mirror holder 39 is mounted at one end of the lens sleeve 43, and a planar mirror 38 is mounted on the holder 39. A planar mirror fiber optic adapter 40 is mounted at the other end of the lens sleeve 43, and an achromatic lens 41 is positioned near the end of the adapter 40. It should be noted that the through-hole 14 needs to pass through both the planar mirror 38 and the holder 39, and the opening on the planar mirror probe is located on the lens sleeve 43.

[0065] Setting up a rear achromatic lens 41 and a front achromatic lens 42 for the plane mirror enables 4f imaging, allowing the formed image to be accurately focused at the center of the fiber optic adapter.

[0066] When the plane mirror probe is in use, the electron beam 3 passes through the through hole 14 and strikes the surface of the sample 2. In addition, the laser 102 is focused by the plane mirror 38 of the plane mirror probe and irradiates point A of the sample 2 to generate the light signal to be measured 101. The plane mirror probe then collects the light signal to be measured. The light signal to be measured is reflected by the plane mirror 38 to the front achromatic lens 42 of the plane mirror. The front achromatic lens 42 of the plane mirror converts the reflected light into parallel light. The rear achromatic lens 41 of the plane mirror focuses the light into the plane mirror fiber optic adapter 40, and then inputs it into the spectrometer 32 through the optical fiber.

[0067] It should be noted that the laser 102 emitted by the laser excitation source 32 and focused onto point A of the sample 2 through the fiber optic coupling optical path module generates a Raman light signal or a fluorescence signal.

[0068] As a further improvement, the aperture of the through hole 14 is in the millimeter range, specifically 1-10 mm, to avoid blocking the irradiation of the electron beam 3.

[0069] Combination Figure 9 and Figure 10 As shown, the fiber-coupled optical path module is located in the scanning electron microscope chamber 4 and placed on an adjustment frame. The adjustment frame is also connected to the focusing assembly, which is used to adjust the position of the fiber-coupled optical path module. During detection, sample 2 needs to be placed at the focal point where the fiber-coupled optical path module converges. Since the fiber-coupled optical path module is located inside the scanning electron microscope chamber 4, a focusing assembly is provided to facilitate adjustment.

[0070] Furthermore, the focusing assembly includes an X-axis adjustment component, a Y-axis adjustment component, and a Z-axis adjustment component. The X-axis adjustment component is used to move the fiber-coupled optical path module along the X-axis direction; the Y-axis adjustment component is connected to the X-axis adjustment component and is used to move the fiber-coupled optical path module along the Y-axis direction; the Z-axis adjustment component is connected to the Y-axis adjustment component and is used to move the fiber-coupled optical path module along the Z-axis direction.

[0071] Specifically, the X-axis adjustment component includes a lead screw 71 and a first slider 74 connected to the lead screw 71. One end of the lead screw 71 is connected to a first motor 70. The first slider 74 is mounted on a first slide rail 77. The first motor 70 drives the lead screw 71 to rotate, causing the first slider 74 to move along the first slide rail 77, thereby moving the fiber optic coupled optical path module along the X-axis. The Y-axis adjustment component includes a third slider 72 located on the first slider 74 and a third lead screw connected to the third slider 72. The first slider 74 also serves as the slide rail for the third slider 72. One end of the third lead screw is connected to a third motor 75. The third motor 75 drives the third lead screw to rotate, causing the third slider 72 to move, thereby moving the fiber optic coupled optical path module along the Y-axis. The Z-axis adjustment component includes a second slider 76 connected to the third slider 72 and a second lead screw connected to the second slider 76. One end of the second lead screw is connected to a second motor 73. The second motor 73 drives the second lead screw to rotate, causing the second slider 76 to move, thereby moving the fiber optic coupled optical path module along the Z-axis.

[0072] The second slider 76 is connected to one end of the adjustment frame via a rotary motor 202. The fiber optic coupling optical path module is located on the adjustment frame, allowing the focusing assembly to adjust it in the X, Y, and Z directions. Furthermore, the rotary motor 202 adds a degree of freedom for adjustment, facilitating the adjustment of the position of the fiber optic coupling optical path module.

[0073] When adjusting the focus of the fiber-coupled optical path module, the position of the fiber-coupled optical path module can be manually adjusted through the focus assembly, and the focus position can be determined by combining the light intensity display on the spectrometer 37, so that point A of sample 2 is located at the desired focus.

[0074] This application also provides a detection method for a scanning electron microscope imaging and in-situ spectral detection system for detecting sample 2. The system includes a scanning electron microscope and an optical fiber coupled optical path module. The scanning electron microscope includes a scanning electron microscope chamber 4 and an excitation source 1 and a secondary electron detector 401 disposed in the scanning electron microscope chamber 4.

[0075] During the test, sample 2 is placed inside the scanning electron microscope chamber 4, and excitation source 1 is placed directly above sample 2 and emits electron beam 3 vertically to point A of sample 2 to generate secondary electrons.

[0076] The secondary electron detector 401 is positioned at an angle above the sample 2 to receive the secondary electrons.

[0077] At the same time, the light signal to be measured 101 can be excited at point A of sample 2, and the light signal to be measured 101 is emitted in different directions toward the side closer to sample 2.

[0078] The fiber-coupled optical path module is connected to the spectrometer and positioned directly above point A of sample 2 to collect the light signal 101 to be measured, and the light signal to be measured is transmitted to the spectrometer for detection; and a through hole 14 is opened on the fiber-coupled optical path module for the electron beam 3 to pass through.

[0079] A detection method for a combined scanning electron microscopy imaging and in-situ spectral detection system can simultaneously and accurately acquire information on the morphology, composition, and chemical state of a sample through in-situ, real-time, and co-situ observation and analysis.

[0080] To better understand the content of this application, the following will provide a more detailed explanation of this application using different embodiments.

[0081] Example 1

[0082] In this embodiment, a scanning electron microscope imaging and in-situ spectral detection combined system is used to detect Raman light signals and simultaneously analyze the secondary electron signals of sample 2, thereby enabling simultaneous detection and analysis of the morphology, composition and chemical state information of sample 2.

[0083] Specific detection methods, such as Figure 6 and Figure 11 The diagram illustrates a specific example of using an off-axis parabolic mirror probe to detect Raman signals. The off-axis parabolic mirror probe is positioned above sample 2, with the lens sleeve of the off-axis parabolic mirror parallel to the surface of sample 2, and the off-axis parabolic mirror 7 located directly above sample 2. An electron beam 3 passes through the through-hole 14, through the off-axis parabolic mirror 7, and enters sample 2 to excite a secondary electron signal 402.

[0084] In this embodiment, a laser excitation source 32 is used to excite the Raman light signal. A conversion component is also included in this embodiment. The conversion component includes a first converging lens 33, a dichroic mirror 34, a long-pass filter 35, a second converging lens 36, and a bandpass filter 388.

[0085] Specifically, see Figure 6 and Figure 11An electron beam enters through the through-hole 14 on the off-axis parabolic mirror 7 and illuminates point A of the sample 2. Simultaneously, the laser excitation source 32 emits a laser beam, which is filtered out by the bandpass filter 388 to remove stray light other than the excitation light. At this point, it can be considered as parallel light. After passing through the dichroic mirror 34, the short-wavelength light is reflected, and the long-wavelength light is transmitted. The laser beam is reflected by the dichroic mirror 34 to the first converging lens 33, which focuses the laser beam onto an optical fiber. The laser beam then enters the off-axis parabolic mirror fiber optic adapter 29 and is guided into the probe. Here, the laser beam passes through the achromatic lens 28 to become parallel light, and then passes through the off-axis parabolic mirror 7 to converge at its focal point. Point A of the sample 2 to be tested should be placed at this focal point to generate a Raman light signal. Raman light is generated by elastic and inelastic scattering of light when it shines on the sample 2. The scattered light from elastic scattering has the same wavelength as the excitation light, while the scattered light from inelastic scattering has components with wavelengths longer and shorter than the excitation light, which constitute the Raman light signal. The excited Raman light signal is collected by the off-axis parabolic mirror 7 and converted into parallel light. It is then focused into an optical fiber by the achromatic lens 28. The light collected by the optical fiber passes through the first converging lens 33 and the dichroic mirror 34, and after passing through the long-pass filter 35, it passes through the second converging lens 36 and is then connected to the spectrometer 37 for measurement. At the same time, the electron beam irradiates point A of the sample 2 to generate a secondary electron signal. The secondary electron detector 401 receives the secondary electron signal to obtain the surface morphology information of the sample.

[0086] The off-axis parabolic mirror probe is located inside the scanning electron microscope chamber 4 and mounted on the adjustment frame. The focusing assembly is used to position point A of sample 2 at the focal point of the off-axis parabolic mirror 7.

[0087] A hole is opened on one side of the scanning electron microscope chamber 4 for the adjustment frame to pass through. A corrugated tube is connected around the hole, and the other end of the corrugated tube is connected to the focusing assembly to maintain the airtightness of the electron microscope chamber. The optical fiber 6 passes through the corrugated tube, with one end connected to the off-axis parabolic mirror fiber optic adapter 29 and the other end connected to the first converging lens 33.

[0088] Example 2

[0089] This embodiment describes a system combining scanning electron microscopy imaging and in-situ spectral detection for detecting Raman light signals, such as... Figure 7 and Figure 12 The diagram illustrates a specific example of using a plane mirror probe to detect Raman signals. In this embodiment, the off-axis parabolic mirror probe is replaced with a plane mirror probe; the rest of the structure remains the same as in Example 1.

[0090] In this embodiment, the electron beam enters through the through-hole 14 on the off-axis parabolic mirror 7 and irradiates point A of the sample 2. Simultaneously, the laser excitation source 32 emits a laser conversion component with a first converging lens 33 that enters the plane mirror probe. The laser then passes through a rear achromatic lens 41 of the plane mirror to convert the excitation light into parallel light. After passing through a front achromatic lens 42 and the plane mirror 38, the light is focused onto its focal point. Point A of the sample 2 to be tested should also be placed at this focal point. The Raman light generated after excitation is again converted into parallel light by the front achromatic lens 42 and the plane mirror 38, and then focused by a rear achromatic lens 41 of the plane mirror onto the optical fiber. The light collected by the optical fiber passes through the first converging lens 33 and the dichroic mirror 34, and after passing through the long-pass filter 35 and the second converging lens 36, it is connected to the spectrometer 37 for measurement. At the same time, the electron beam irradiates point A of the sample 2, generating a secondary electron signal. The secondary electron detector 401 receives the secondary electron signal to obtain the surface morphology information of the sample.

[0091] It should be noted that when detecting other samples 2 in Examples 1 and 2, if the light signal to be measured excited by the laser on sample 2 is a fluorescence signal, the detection system structure and detection method are the same as in Examples 1 and 2, only the monitored samples are different.

[0092] The terms “installation,” “setup,” “equipped with,” and “connection” used herein should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral structure; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium, or an internal connection between two devices, components, or parts. Those skilled in the art can understand the specific meaning of these terms in this application based on the specific circumstances.

[0093] The present invention and its embodiments have been described above illustratively. This description is not restrictive, and the figures shown are only one embodiment of the present invention; the actual structure is not limited thereto. Therefore, if those skilled in the art are inspired by this description and design similar structures and embodiments without departing from the spirit of the present invention, such designs should fall within the protection scope of the present invention.

Claims

1. A scanning electron microscope imaging and in-situ spectral detection combined system for detecting sample (2), characterized in that: It includes a scanning electron microscope, a fiber-coupled optical path module and a laser excitation source (32). The scanning electron microscope includes a scanning electron microscope chamber (4) and an excitation source (1) and a secondary electron detector (401) disposed in the scanning electron microscope chamber (4). During the detection, the sample (2) is placed inside the scanning electron microscope chamber (4), the excitation source (1) is placed directly above the sample (2) to be detected and is able to emit an electron beam (3) to vertically irradiate point A of the sample (2) to generate a secondary electron signal; the secondary electron detector (401) is located on the oblique side above the sample (2) and is used to receive the secondary electron signal. The laser excitation source (32) is connected to the fiber-coupled optical path module; the laser emitted by the laser excitation source (32) is focused by the fiber-coupled optical path module and irradiates point A of the sample (2) to generate a test light signal (101), which is emitted in different directions closer to the sample (2); the fiber-coupled optical path module is also connected to a spectrometer and collects the test light signal and transmits it to the spectrometer for detection.

2. The scanning electron microscope imaging and in-situ spectral detection combined system according to claim 1, characterized in that: When the fiber-coupled optical path module is located directly above the sample (2)A to collect the optical signal to be tested (101), a through hole (14) is opened on the fiber-coupled optical path module for the electron beam (3) to pass through.

3. The scanning electron microscope imaging and in-situ spectral detection combined system according to claim 2, characterized in that: The fiber-coupled optical path module is an off-axis parabolic mirror probe. The off-axis parabolic mirror probe includes an off-axis parabolic mirror (7) disposed at one end of the off-axis parabolic mirror probe and an achromatic lens (28) located inside the off-axis parabolic mirror probe. The off-axis parabolic mirror (7) is located directly below the excitation source (1), and the through hole (14) is opened on the off-axis parabolic mirror (7). The off-axis parabolic mirror (7) faces the sample (2) on one side, and an opening is opened on the off-axis parabolic mirror probe.

4. The scanning electron microscope imaging and in-situ spectral detection combined system according to claim 2, characterized in that: The fiber-coupled optical path module is a planar mirror probe. The planar mirror probe includes a planar mirror (38) disposed at one end of the planar mirror probe and a rear achromatic lens (41) and a front achromatic lens (42) of the planar mirror located inside the planar mirror probe. The front achromatic lens (42) of the planar mirror is disposed at one end close to the planar mirror (38). The planar mirror (38) is located directly below the excitation source (1). The through hole (14) is opened on the planar mirror (38). The planar mirror (38) faces the sample (2) and an opening is opened on the planar mirror probe.

5. The scanning electron microscope imaging and in-situ spectral detection combined system according to claim 3 or 4, characterized in that: The optical signal to be tested (101) includes Raman optical signal or fluorescence signal.

6. The scanning electron microscope imaging and in-situ spectral detection combined system according to claim 3 or 4, characterized in that: The fiber-coupled optical path module is located in the scanning electron microscope chamber (4) and placed on the adjustment frame. The adjustment frame is also connected to the focusing assembly, which is used to adjust the position of the fiber-coupled optical path module.

7. The scanning electron microscope imaging and in-situ spectral detection combined system according to claim 6, characterized in that: The focusing component includes, X-axis direction adjustment component, used to move the fiber optic coupled optical path module along the X-axis direction; The Y-axis adjustment component is connected to the X-axis adjustment component and is used to move the fiber optic coupled optical path module along the Y-axis direction. The Z-axis adjustment component is connected to the Y-axis adjustment component and is used to move the fiber optic coupled optical path module along the Z-axis direction.

8. The scanning electron microscope imaging and in-situ spectral detection combined system according to claim 7, characterized in that: The X-axis direction adjustment component includes a lead screw (71) and a first slider (74) connected to the lead screw (71); The Y-axis direction adjustment component includes a third slider (72) located on the first slider (74) and a third lead screw connected to the third slider (72); The Z-axis direction adjustment component includes a second slider (76) connected to the third slider (72) and a second lead screw connected to the second slider (76).

9. The scanning electron microscope imaging and in-situ spectral detection combined system according to claim 1, characterized in that: The diameter of the through hole (14) is 1-10 mm.

10. A detection method using a combined scanning electron microscopy imaging and in-situ spectral detection system, characterized in that: The device is used to detect the sample (2), including a scanning electron microscope, a fiber optic coupled optical path module and a laser excitation source (32). The scanning electron microscope includes a scanning electron microscope chamber (4) and an excitation source (1) and a secondary electron detector (401) disposed in the scanning electron microscope chamber (4). During the detection, the sample (2) is placed in the scanning electron microscope chamber (4), and the excitation source (1) is placed directly above the sample (2) to be detected and emits an electron beam (3) to vertically irradiate point A of the sample (2) to generate secondary electrons; The secondary electron detector (401) is positioned at an oblique angle above the sample (2) to receive the secondary electrons; The laser excitation source (32) is connected to the fiber-coupled optical path module; the laser emitted by the laser excitation source (32) is focused by the fiber-coupled optical path module and irradiates point A of the sample (2) to generate a test light signal (101), which is emitted in different directions closer to the sample (2); the fiber-coupled optical path module is also connected to a spectrometer and the test light signal is collected and transmitted to the spectrometer for detection.

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