Device and method for collaborative analysis of microstructure and chemical structure

Abstract

The invention discloses a device and a method for collaborative analysis of a microstructure and a chemical structure. The device comprises an AFM system, a hollow motion extension mechanism, an XY plane double-axis electric displacement table and an inverted fluorescence Raman microscope, the hollowed-out movement extending mechanism is provided with a hollowed-out part used for containing a sample, and the hollowed-out movement extending mechanism is connected with the table top of the XY plane double-axis electric displacement table; the AFM system is arranged above the hollowed-out movement extension mechanism and is used for measuring the surface topography structure information and the friction performance of the target sample; and the inverted fluorescent Raman microscope is arranged below the hollow movement extension mechanism and is used for representing the chemical components of the regional sample. According to the integrated AFM and inverted fluorescent Raman microscope provided by the invention, local information of chemical components, forms, phases and molecular vibration of the material can be in one-to-one correspondence with the microscopic physical structure and size distribution of the material, and information unification of the microscopic physical structure morphology and the internal chemical component structure of the same area of the tested material is realized.

Description

Technical Field

[0001] The present invention relates to a material analysis device and method, and in particular to a device and method for collaboratively analyzing microscopic morphology and chemical structure. Background Art

[0002] When studying the functional properties of various materials, clarifying their microscopic physical structure morphology and internal chemical composition structure is of great guiding significance for clarifying specific scientific principles. In order to obtain multi-dimensional characterization information of the research material, traditional characterization technology usually adopts "multi-equipment multi-project" testing of the same material. Although the single test has extremely high precision resolution (nanometer level), the regional deviation of the research object between the two tests brings certain technical errors to the collaborative analysis of the characterization information.

[0003] Patent CN201780084916.1 discloses a method and apparatus for enhanced photothermal imaging and spectroscopy, using a multifunctional platform combining analysis and imaging techniques including dual-beam photothermal spectroscopy with confocal microscopy, Raman spectroscopy, fluorescence detection, various vacuum analysis techniques, and / or mass spectrometry to perform chemical spectroscopy analysis on samples from nanometers to millimeters and above. Patent CN201780084288.7 discloses a method and apparatus for chemical imaging atomic force microscopy infrared spectroscopy, using infrared light to illuminate the sample and read out the resulting sample deformation with a focused UV / visible beam and / or AFM tip. The combination of the two technologies provides fast and large-area measurement scans using UV / visible light and high-resolution measurements using an AFM tip.

[0004] Although the above patents demonstrate the technical capability of a single device to collect multi-faceted characterization information of samples, it is actually impossible to achieve true in-situ collaborative analysis and testing. Summary of the invention

[0005] Purpose of the invention: The purpose of the present invention is to provide a device for collaborative analysis of microscopic morphology and chemical structure, which can achieve the information unification of the microscopic physical structure morphology and the internal chemical component structure of the same area of ​​the test material;

[0006] The second object of the present invention is to provide a method for collaboratively analyzing microscopic morphology and chemical structure using the above-mentioned device.

[0007] Technical solution: The device for collaborative analysis of microscopic morphology and chemical structure described in the present invention comprises an AFM system, a hollow motion extension mechanism, an XY plane biaxial electric translation stage and an inverted fluorescence Raman microscope; the hollow motion extension mechanism is provided with a hollow portion for holding samples, and the hollow motion extension mechanism is connected to the table top of the XY plane biaxial electric translation stage to enable the sample to perform nanometer resolution scanning movement in the XY plane; the AFM system is arranged above the hollow motion extension mechanism, and the AFM system utilizes the scanning movement of the AFM needle tip to achieve regional sample characterization with nanometer resolution, thereby achieving measurement of the surface morphology structure information and friction performance of the target sample; the inverted fluorescence Raman microscope is arranged below the hollow motion extension mechanism, and the inverted fluorescence Raman microscope faces the bottom surface of the sample, and is used to complete the emission of excitation light and the collection of fluorescence or Raman signals, and cooperate with the scanning movement of the XY plane biaxial electric translation stage to achieve chemical component characterization of the regional sample.

[0008] Wherein, the needle tip of the AFM system is arranged above the hollow part of the hollow motion extension mechanism, and the inverted fluorescence Raman microscope is arranged below the hollow part of the hollow motion extension mechanism.

[0009] Wherein, the deflection angle range of the XY plane dual-axis electric translation stage is between -120 and 120 μrad.

[0010] Wherein, the pitch angle range of the XY plane dual-axis electric translation stage is between -80 and 80 μrad.

[0011] A method for collaboratively analyzing microscopic morphology and chemical structure using the above-mentioned device is used. The above-mentioned device is used to perform both surface morphology testing and fluorescence Raman testing on the same area of ​​the sample with nanometer resolution, and the test results of the above two areas are matched one by one according to the spatial distribution, so as to collaboratively analyze the physical structure information and chemical composition information of the sample.

[0012] Specifically, the following steps are included:

[0013] (1) Surface morphology test: Use the contact and tapping modes of AFM to test the surface morphology and friction performance of the sample;

[0014] (2) Fluorescence Raman test: adjusting the focal length of the objective lens of the inverted fluorescence Raman microscope so that the excitation light spot is focused on the lower surface of the sample to collect signals, controlling the XY plane biaxial electric translation stage to perform scanning motion, and recording the regional Raman spectrum of the sample;

[0015] (3) The test results of the above two regions are matched one by one according to the spatial distribution, and the physical structure information and chemical composition information of the samples are analyzed collaboratively.

[0016] Wherein, in step (1), the friction performance includes lateral friction, stick-slip friction and micro-area friction difference.

[0017] Among them, in step (2), the motion range and step length parameters of the XY plane biaxial electric translation stage for scanning motion are consistent with the AFM test parameters. The test parameters are: laser power of 0.5 to 30 mW, scanning range of 0 to 10000 μm 2 The single-point integration time is 0.05 to 30 s, and the unidirectional step size in the plane is 0.01 to 2 μm.

[0018] Wherein, in step (3), the collaborative analysis method is: to maintain the consistency of the spatial distribution of the sample area between the AFM test and the fluorescence Raman test, specifically including the test area, the scanning range and the unidirectional step length.

[0019] Beneficial effects: Compared with the prior art, the present invention achieves the following significant effects:

[0020] (1) The integrated AFM and inverted fluorescence Raman microscope provided by the present invention can correspond the local information of the chemical composition, morphology, phase and molecular vibration of the material to the microscopic physical structure and size distribution of the material, so as to unify the information of the microscopic physical structure morphology and the internal chemical component structure of the same area of ​​the test material; (2) The regional scanning Raman characterization of the present invention uses a high-precision piezoelectric displacement stage to drive the sample, which has a more accurate resolution than scanning the sample by moving the focused spot with a galvanometer. (3) Through the scanning movement of the atomic force microscope (AFM) needle tip, the device can obtain physical information such as the surface morphology and roughness of the sample in the area. (4) With the help of the scanning movement capability of the electric displacement stage and the optical analysis function of the fluorescence Raman microscope, the present invention can obtain the Raman spectrum of the sample in the area and analyze its molecular structure and chemical composition. By combining the AFM test with the Raman characterization results, the device can achieve a close correspondence between the physical structure morphology and chemical composition content of the sample within the range at the nanoscale. The synergistic analysis results are of great positive significance for studying the mechanism of action of composite thin film materials in electrochemistry, micro-nano friction and photoelectrocatalysis. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 It is a schematic diagram of the structure of the device of the present invention. DETAILED DESCRIPTION

[0022] The present invention is described in further detail below.

[0023] Example 1

[0024] like Figure 1As shown, the present invention provides a device for collaboratively analyzing microscopic morphology and chemical structure, including an AFM system 1, a hollow motion extension mechanism 4, an XY plane biaxial electric translation stage 5 and an inverted fluorescence Raman microscope 3; the hollow motion extension mechanism 4 is provided with a hollow portion 4-1 for holding a sample 2, and the hollow motion extension mechanism 4 is connected to the table of the XY plane biaxial electric translation stage 5 to enable the sample 2 to perform nanometer resolution scanning movement in the XY plane; the AFM system 1 is arranged above the hollow motion extension mechanism 4, and the AFM system 1 uses the scanning movement of the AFM needle tip to achieve regional sample characterization with nanometer resolution, thereby achieving measurement of the surface morphology structure information and friction performance of the target sample; the inverted fluorescence Raman microscope 3 is arranged below the hollow motion extension mechanism 4, and the inverted fluorescence Raman microscope 3 faces the bottom surface of the sample 2, and is used to complete the emission of excitation light and the collection of fluorescence or Raman signals, and cooperate with the scanning movement of the XY plane biaxial electric translation stage 5 to achieve chemical component characterization of the regional sample 2.

[0025] The needle tip of the AFM system 1 is disposed above the hollow portion 4 - 1 of the hollow motion extension mechanism 4 , and the inverted fluorescence Raman microscope 3 is disposed below the hollow portion 4 - 1 of the hollow motion extension mechanism 4 .

[0026] The yaw angle range of the XY plane biaxial electric translation stage 5 is between -120 and 120 μrad; the pitch angle range of the XY plane biaxial electric translation stage 5 is between -80 and 80 μrad.

[0027] The friction characteristics and component distribution of the thin film material are uniformly characterized. The sample material composition is a mixture of MXene and MoS2. The method of using the above-mentioned device to collaboratively analyze the surface morphology structure and internal components of the material is as follows:

[0028] 1. AFM tests the adhesion and surface morphology of samples. The specific steps are as follows:

[0029] (1) Fixing the sample on the hollow motion extension mechanism 4, and adjusting the longitudinal height of the AFM system 1 so that the probe tip is roughly close to the sample surface;

[0030] (2) Setting feedback, using the AFM motor to approach the sample and lower the needle, setting the contact mode;

[0031] (3) Select a scanning range and perform AFM imaging in a range of 80 × 80 μm with a unidirectional step size of 50 nm to test the surface adhesion of the sample.

[0032] 2. Inverted Raman fluorescence chemical analysis, the specific steps are:

[0033] (1) Adjust the longitudinal position between the inverted lens and the sample so that the laser spot is focused on the upper surface of the glass, i.e., the lower surface of the sample, through the supporting glass;

[0034] (2) Set the sample scanning area in the XY plane dual-axis electric translation stage 5 software, and the range size and step length are consistent with the AFM scanning process;

[0035] (3) Perform Raman test spectrum imaging on the above-mentioned set area with a power of 5 mW and an integration time of 3 s.

[0036] 3. Coordinated microscopic physical morphology and chemical component analysis. The specific steps are as follows:

[0037] (1) Based on the Raman scattering peaks of different molecular structures, the content distribution, molecular vibration and structural phase of MXene and MoS2 in the scanning area are analyzed;

[0038] (2) The chemical information is matched one by one with the surface morphology measured by AFM according to the step area, realizing in-situ collaborative physical and chemical two-dimensional characterization.

[0039] Example 2

[0040] The device structure is the same as that of Example 1. The surface morphology and chemical structure of the composite functional material are uniformly characterized, and the sample material composition is porous MoS2 and ReS2. The method of using the device to collaboratively analyze the surface morphology and chemical structure of the composite functional material is as follows:

[0041] 1. AFM tests the surface morphology of samples. The specific steps are:

[0042] (1) Fixing the sample on the hollow motion extension mechanism 4, and adjusting the longitudinal height of the AFM system 1 so that the probe tip is roughly close to the sample surface;

[0043] (2) Setting feedback, using the AFM motor to approach the sample and lower the needle, setting the contact mode;

[0044] (3) Select a scanning range and perform AFM imaging in a 50 × 50 μm range with a unidirectional step size of 10 nm to test the surface morphology of the sample, including the pore size and corresponding distribution.

[0045] 2. Inverted Raman fluorescence chemical analysis, the specific steps are:

[0046] (1) Adjust the longitudinal position between the inverted lens and the sample so that the laser spot is focused on the upper surface of the glass, i.e., the lower surface of the sample, through the supporting glass;

[0047] (2) Set the sample scanning area in the XY plane dual-axis electric translation stage 5 software, and the range size and step length are consistent with the AFM scanning process;

[0048] (3) Perform Raman test spectrum imaging on the above-mentioned set area with a power of 10 mW and an integration time of 5 s.

[0049] 3. Coordinated microscopic physical morphology and chemical component analysis. The specific steps are as follows:

[0050] (1) Based on the Raman scattering peaks of different molecular structures, the content distribution, molecular vibration and structural phase of MoS2 and ReS2 in the scanning area are analyzed;

[0051] (2) The chemical information is matched one by one with the surface morphology measured by AFM according to the step area, realizing in-situ collaborative physical and chemical two-dimensional characterization.

Claims

1. A device for collaborative analysis of microscopic morphology and chemical structure, characterized in that: The invention comprises an AFM system (1), a hollow motion extension mechanism (4), an XY plane biaxial electric translation stage (5), and an inverted fluorescence Raman microscope (3); the hollow motion extension mechanism (4) is provided with a hollow portion (4-1) for holding a sample (2); the hollow motion extension mechanism (4) is connected to the table top of the XY plane biaxial electric translation stage (5) to enable the sample (2) to perform nanometer resolution scanning movement in the XY plane; the AFM system (1) is arranged above the hollow motion extension mechanism (4); the AFM The system (1) uses the scanning motion of the AFM needle tip to achieve regional sample characterization with nanometer-level resolution, thereby achieving measurement of surface morphology structure information and friction performance of the target sample; the inverted fluorescence Raman microscope (3) is arranged below the hollow motion extension mechanism (4), and the inverted fluorescence Raman microscope (3) faces the bottom surface of the sample (2) and is used to complete the emission of excitation light and the collection of fluorescence or Raman signals, and cooperates with the scanning motion of the XY plane biaxial electric translation stage (5) to achieve chemical component characterization of the regional sample.

2. The device for collaborative analysis of microscopic morphology and chemical structure according to claim 1, characterized in that: The needle tip of the AFM system (1) is arranged above the hollow portion (4-1) of the hollow motion extension mechanism (4), and the inverted fluorescence Raman microscope (3) is arranged below the hollow portion (4-1) of the hollow motion extension mechanism (4).

3. The device for collaborative analysis of microscopic morphology and chemical structure according to claim 1, characterized in that: The deflection angle range of the XY plane dual-axis electric translation stage (5) is between -120 and 120 μrad.

4. The device for collaborative analysis of microscopic morphology and chemical structure according to claim 1, characterized in that: The pitch angle range of the XY plane dual-axis electric translation stage (5) is between -80 and 80 μrad.

5. A method for collaboratively analyzing microscopic morphology and chemical structure using the device of claim 1, characterized in that: The device described in claim 1 is used to perform nanometer-level resolution surface morphology testing and fluorescence Raman testing on the same area of ​​the sample, and the test results of the two areas are matched one by one according to spatial distribution, so as to collaboratively analyze the physical structure information and chemical composition information of the sample.

6. The method for collaborative analysis of micromorphology and chemical structure according to claim 5, characterized in that: The specific steps include: (A) Surface morphology test: The surface morphology and friction performance of the sample (2) were tested using the contact and tapping modes of AFM. (B) Fluorescence Raman test: adjusting the focal length of the objective lens of the inverted fluorescence Raman microscope (3) so that the excitation light spot is focused on the lower surface of the sample (2) to collect signals, controlling the XY plane biaxial electric translation stage (5) to perform scanning motion, and recording the regional Raman spectrum of the sample (2); (C) The above two regional test results are matched one by one according to the spatial distribution, and the physical structure information and chemical composition information of the sample (2) are analyzed in a coordinated manner.

7. The method for collaborative analysis of micromorphology and chemical structure according to claim 5, characterized in that: In step (B), the motion range and step length parameters of the XY plane biaxial electric translation stage (5) for scanning motion are controlled to be consistent with the AFM test parameters.

8. The method for collaborative analysis of micromorphology and chemical structure according to claim 7, characterized in that: Test parameters: laser power 0.5 ~ 30mW, scanning range 0 ~ 10000μm 2 The single-point integration time is 0.05 to 30 s, and the unidirectional step size in the plane is 0.01 to 2 μm.

9. The method for collaborative analysis of microscopic morphology and chemical structure according to claim 7, characterized in that: In step (C), the collaborative analysis method is to keep the spatial distribution of the AFM test and the fluorescence Raman test consistent in the sample area, specifically including the test area, scanning range and unidirectional step length.

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