Argon ion beam scanning electron microscope double-beam system and in-situ sample analysis method

Abstract

The invention provides an argon ion beam scanning electron microscope double-beam system and an in-situ sample analysis method, an electron optical lens barrel of the system generates a high-energy electron beam for scanning the surface of a sample for imaging; the ion optical lens cone generates a high-energy argon ion beam for sample surface polishing; the sample chamber is used for accommodating samples and providing a vacuum environment; the sample table is used for accurately controlling the position and angle of a sample; and the detector is used for collecting signals generated by interaction of the electron beam and the sample for imaging analysis. According to the invention, a sample transfer step is eliminated, so that the sample preparation and analysis efficiency is greatly improved; a millimeter-scale large-size sample can be treated, and a sample with a flat and smooth surface can be obtained; sample polishing and imaging are carried out in the same vacuum environment, so that sample pollution is reduced to the greatest extent, and the accuracy of an analysis result is improved; by combining argon ion beam polishing and scanning electron microscope imaging technologies, efficient, high-precision and in-situ analysis of the sample is realized, so that more comprehensive and more accurate microstructure information is obtained.

Description

Technical Field

[0001] The invention relates to the technical field of scanning electron microscopes, and in particular to an argon ion beam scanning electron microscope double-beam system and an in-situ sample analysis method. Background Art

[0002] Scanning electron microscope (SEM) is a key analytical tool in many fields such as materials science and life science. However, the growing scientific research needs have put forward higher requirements on sample analysis efficiency. The existing technology uses argon ion beam polishing equipment to polish the sample surface, obtain high-quality sample surface, and then manually transfer it to SEM for imaging analysis. This process has significant shortcomings:

[0003] Low efficiency: The sample needs to be manually transferred between the ion beam polishing equipment and the SEM, which is inefficient and increases the probability of error due to manual operation. In addition, the lack of in-situ observation capability makes it impossible to determine whether the polishing has reached the desired position, resulting in repeated transfer operations, further reducing efficiency. For complex samples (such as biological tissues), it is difficult to re-position the target area for continuous observation after transfer.

[0004] Contamination risk: The manual transfer process increases the risk of sample contamination, affecting the accuracy of subsequent SEM imaging and analysis results.

[0005] Although the focused ion beam scanning electron microscope (FIB-SEM) dual beam system can realize in-situ processing and observation of samples, its focused ion beam spot size is small, the processing area is limited, and the high energy ion beam easily causes damage to the sample surface. In contrast, the argon ion beam has the ability to polish a large area with a millimeter-level beam spot, and the low energy ion beam can effectively reduce sample damage.

[0006] However, the current integration of argon ion beam polishing systems with SEM is not high, which limits its efficiency and application range. Summary of the invention

[0007] In order to achieve the above-mentioned purpose and other advantages of the present invention, the first purpose of the present invention is to provide an argon ion beam scanning electron microscope dual beam system, including an electron optical column, an ion optical column, a sample chamber, a sample stage, and a detector; wherein,

[0008] The electron optical lens tube generates a high-energy electron beam for scanning the sample surface for imaging;

[0009] The ion optical column generates a high-energy argon ion beam for polishing / milling the sample surface;

[0010] The sample chamber is used to contain samples and provide a vacuum environment;

[0011] The sample stage is used to accurately control the position and angle of the sample;

[0012] The detector is used to collect signals generated by the interaction between the electron beam and the sample for imaging analysis.

[0013] Furthermore, the ion optical lens barrel comprises an ion source and a unidirectional focusing module, wherein the ion source is used to generate an ion beam, and the unidirectional focusing module is used to unidirectionally focus a circular ion beam spot into a linear ion beam spot.

[0014] Furthermore, the one-way focusing module includes an Einzel focusing lens and an electrostatic quadrupole focusing lens, and the Einzel focusing lens is placed between the ion source and the electrostatic quadrupole focusing lens.

[0015] Furthermore, the ion optical lens barrel further comprises an angle adjustment element, and the ion optical lens barrel is mounted on the angle adjustment element, so that the incident angle of the ion beam is adjustable.

[0016] Furthermore, the angle adjustment element is an adjustable flange.

[0017] Furthermore, the ion optical lens barrel also includes a magnetic shielding sleeve, and the magnetic shielding sleeve is sleeved outside the ion optical lens barrel.

[0018] Furthermore, the detector includes a backscattered electron detector and a side secondary electron detector, and the backscattered electron detector and the side secondary electron detector are used to collect secondary electron signals and backscattered electron signals generated by the electron optical lens barrel.

[0019] Furthermore, the sample stage includes, from top to bottom, a sample nail stage, a nail stage fixing seat, a base, a piezoelectric rotation stage, a piezoelectric displacement stage, and an adapter plate. The sample nail stage is fixed to the base through the nail stage fixing seat, the base is installed on the piezoelectric rotation stage, the piezoelectric rotation stage is installed on the piezoelectric displacement stage, the piezoelectric displacement stage is fixed to the adapter plate, the sample nail stage is used to place samples, the piezoelectric displacement stage is used to achieve nanometer-level precision control in the Z direction, and the piezoelectric rotation stage can be adjusted to rotate continuously during ion beam polishing.

[0020] Furthermore, it also includes a precision layer cutting mechanism, which is used to achieve precise sample layer cutting and cooperate with ion beam polishing to obtain a high-quality sample surface.

[0021] Furthermore, the precision layer cutting mechanism includes a baffle and a baffle bracket, the baffle is provided with a groove for accommodating the sample, and the baffle is fixed to the adapter plate through the baffle bracket.

[0022] Furthermore, it also includes a sputtering contaminant capturing device, which is used to capture contaminants generated by ion beam sputtering to reduce sample contamination.

[0023] Furthermore, the sputtering contaminant capturing device includes a sputtering contaminant collector and an objective lens protection baffle. The sputtering contaminant collector and the objective lens protection baffle are both mobile devices. The sputtering contaminant collector is used to guide and collect the sputtering contaminants, and the objective lens protection baffle is used to intercept the sputtering contaminants that may fall onto the objective lens.

[0024] A second object of the present invention is to provide an in-situ sample analysis method for an argon ion beam scanning electron microscope dual-beam system, which is applied to the above-mentioned argon ion beam scanning electron microscope dual-beam system, and the method comprises the following steps:

[0025] Ion beam polishing step: the sample stage moves to the polishing position, the ion optical lens barrel is started to generate an argon ion beam, the argon ion beam is incident on the sample surface at an adjustable angle, and the sample stage moves to remove the curtain effect and increase the polishing area;

[0026] Electron beam imaging step: the ion optical lens tube is closed, the sample stage is moved to the imaging position, the electron optical lens tube emits an electron beam to scan the sample surface, and the generated electron signal is collected by the detector to form a sample image.

[0027] Furthermore, the ion beam polishing step further comprises:

[0028] Before the ion optical column starts to generate the argon ion beam, the sputtered contaminant capture device extends into the sample chamber, and then collects the sputtered contaminants in real time after the argon ion beam bombards the sample surface;

[0029] The electron beam imaging step further comprises:

[0030] After the ion optical column is closed, the sputtered contamination capture device is withdrawn.

[0031] Furthermore, the method further comprises the steps of:

[0032] Adjust the ion beam energy, ion beam current, incident angle, sample stage motion parameters, and polishing time according to the sample material and the required polishing effect;

[0033] And, as needed, repeat the ion beam polishing step and the electron beam imaging step until a satisfactory result is obtained.

[0034] Compared with the prior art, the present invention has the following beneficial effects:

[0035] The invention provides an argon ion beam scanning electron microscope dual-beam system and an in-situ sample analysis method, which can realize large-area sample processing, high-precision in-situ polishing, and high-resolution imaging analysis, eliminate the sample transfer step, simplify the operation process, and greatly improve the efficiency of sample preparation and analysis; sample polishing and imaging are performed under the same vacuum environment, which minimizes sample contamination and improves the accuracy of analysis results; large-size samples of the millimeter level can be obtained, and a flat and smooth sample surface can be obtained; by combining argon ion beam polishing and scanning electron microscope technology, in-situ three-dimensional imaging of the sample can be achieved, and more comprehensive and accurate microstructure information can be obtained; a pollutant capture device is designed to minimize the contamination of the sample and the components in the sample chamber, and ensure the stable operation of the system.

[0036] The above description is only an overview of the technical solution of the present invention. In order to more clearly understand the technical means of the present invention and implement it according to the contents of the specification, the following is a detailed description of the preferred embodiments of the present invention in conjunction with the accompanying drawings. The specific implementation of the present invention is given in detail by the following embodiments and their accompanying drawings. BRIEF DESCRIPTION OF THE DRAWINGS

[0037] The drawings described herein are used to provide a further understanding of the present invention and constitute a part of this application. The exemplary embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an improper limitation of the present invention. In the drawings:

[0038] Figure 1 Schematic diagram of the dual beam system of an argon ion beam scanning electron microscope;

[0039] Figure 2 Schematic diagram of ion beam polishing;

[0040] Figure 3 Schematic diagram of electron beam imaging;

[0041] Figure 4 Schematic diagram of the precision layer cutting mechanism and sample stage;

[0042] Figure 5 It is a schematic diagram of the assembly of the ion optical tube, angle adjustment element and magnetic shielding sleeve;

[0043] Figure 6 It is a schematic diagram of the exploded view of the ion optical tube, angle adjustment element and magnetic shielding sleeve;

[0044] Figure 7 This is a schematic diagram of the ion optical column;

[0045] Figure 8 A flow chart of an in-situ sample analysis method for an argon ion beam scanning electron microscope dual beam system;

[0046] Fig. 9This is a comparison of the ternary lithium battery electrode sample before and after ion beam polishing;

[0047] Fig.10 This is a comparison chart of molybdenum alloy samples after mechanical grinding and ion beam polishing.

[0048] In the figure: 1. electron optical lens barrel; 2. objective lens protection baffle; 3. sample chamber; 4. ion optical lens barrel; 41. ion source; 42. Einzel focusing lens; 43. electrostatic quadrupole focusing lens; 44. angle adjustment element; 45. magnetic shielding sleeve; 5. backscattered electron detector; 6. lateral secondary electron detector; 7. sample stage; 71. sample nail stage; 72. nail stage fixing seat; 73. base; 74. piezoelectric rotation stage; 75. piezoelectric displacement stage; 76. adapter plate; 8. sputtering contaminant collector; 9. sample; 10. baffle; 11. baffle bracket. DETAILED DESCRIPTION

[0049] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0050] In the drawings, the shapes and dimensions may be exaggerated for clarity, and the same reference numerals will be used throughout to designate the same or like components.

[0051] In the following description, words such as center, thickness, height, length, front, back, rear, left, right, top, bottom, upper, lower, etc. are defined relative to the structure shown in the drawings. In particular, "height" is equivalent to the dimension from top to bottom, "width" is equivalent to the dimension from left to right, and "depth" is equivalent to the dimension from front to back. They are relative concepts and may change accordingly according to their different positions and different usage states. Therefore, these or other directions should not be interpreted as restrictive terms.

[0052] Terms related to attachment, coupling, and the like (eg, "connected" and "attached") refer to either a fixed or attached relationship between structures, either directly or indirectly, and either movable or rigid attachments or relationships, unless expressly stated otherwise, of the structures to one another through intermediate structures.

[0053] Example 1

[0054] An argon ion beam scanning electron microscope dual beam system, such as Figure 1-Figure 3As shown, it includes an electron optical lens tube 1, an ion optical lens tube 4, a sample chamber 3, a sample stage 7, and a detector; wherein,

[0055] The electron optical lens tube generates a high-energy electron beam for scanning the surface of the sample 9 for imaging;

[0056] The ion optical column generates a high-energy argon ion beam for polishing / milling the sample surface;

[0057] The sample chamber is used to contain samples and provide a vacuum environment;

[0058] The sample stage is used to accurately control the position and angle of the sample; the sample stage can perform continuous rotation, linear reciprocating, swinging and other movements to remove the "curtain effect", increase the polishing area, and ensure polishing uniformity.

[0059] The detector is used to collect signals generated by the interaction between the electron beam and the sample, such as secondary electron and backscattered electron signals, for imaging analysis.

[0060] In some embodiments, Figure 5-Figure 7 As shown, the ion optical lens barrel 4 includes an ion source 41 and a unidirectional focusing module. The ion source is used to generate an ion beam, and the unidirectional focusing module is used to unidirectionally focus a circular ion beam spot into a linear ion beam spot, thereby improving polishing efficiency and reducing sputtering pollution.

[0061] like Figure 7 As shown, the one-way focusing module includes an Einzel focusing lens 42 and an electrostatic quadrupole focusing lens 43, and the Einzel focusing lens is placed between the ion source and the electrostatic quadrupole focusing lens.

[0062] like Figure 5-Figure 6 As shown, the ion optical column further comprises an angle adjustment element 44, on which the ion optical column is mounted, so that the incident angle of the ion beam is adjustable. Preferably, the angle adjustment element is an adjustable flange.

[0063] like Figure 5-Figure 6 As shown, the ion optical lens barrel further includes a magnetic shielding sleeve 45, which is sleeved outside the ion optical lens barrel.

[0064] This embodiment is equipped with a variety of detectors to obtain sample morphology and composition information. Specifically, the detectors include a backscattered electron detector 5 and a lateral secondary electron detector 6, which are used to collect secondary electron signals and backscattered electron signals generated by the electron optical lens barrel.

[0065] In some embodiments, Figure 4As shown, the sample stage 7 includes, from top to bottom, a sample nail stage 71, a nail stage fixing seat 72, a base 73, a piezoelectric rotating stage 74, a piezoelectric displacement stage 75, and an adapter plate 76. The sample nail stage is fixed to the base through the nail stage fixing seat, the base is mounted on the piezoelectric rotating stage, the piezoelectric rotating stage is mounted on the piezoelectric displacement stage, the piezoelectric displacement stage is fixed to the adapter plate, the sample nail stage is used to place samples, the piezoelectric displacement stage is used to achieve nanometer-level precision control in the Z direction, and the piezoelectric rotating stage can be adjusted to rotate continuously during ion beam polishing.

[0066] In some embodiments, a precision layer cutting mechanism is also included, and the precision layer cutting mechanism is used to achieve precise sample layer cutting and cooperate with ion beam polishing to obtain a high-quality sample surface.

[0067] like Figure 4 As shown, the precision layer cutting mechanism includes a baffle 10 and a baffle bracket 11. The baffle is provided with a groove for accommodating a sample, and the baffle is fixed to the adapter plate through the baffle bracket.

[0068] In actual use, the baffle 10 is fixed, the Z-direction piezoelectric displacement stage 75 can achieve nanometer-level precision control, and the piezoelectric rotation stage 74 can be adjusted to rotate continuously during polishing to avoid the curtain effect.

[0069] In some embodiments, a sputtering contaminant capture device is also included, and the sputtering contaminant capture device is used to capture contaminants generated by ion beam sputtering to reduce sample contamination.

[0070] like Figure 1-Figure 3 As shown, the sputtering contaminant capturing device includes a sputtering contaminant collector 8 and an objective lens protection baffle 2. The sputtering contaminant collector and the objective lens protection baffle are both mobile devices. The sputtering contaminant collector is used to guide and collect the sputtering contaminants, and the objective lens protection baffle is used to intercept the sputtering contaminants that may fall onto the objective lens.

[0071] Specifically, the sputtering contaminant collector 8 extends above the sample during ion beam polishing, completely covers the ion beam and the sample, and guides the sputtering contaminants to the multi-layer collection area, preventing the sputtering contaminants from diffusing to other areas of the sample chamber, thereby effectively reducing sample contamination; when the electron beam scans and images, the sputtering contaminant collector 8 retreats to the inner wall of the sample chamber to avoid blocking the imaging light path.

[0072] Optionally, the sputtering contaminant collector 8 includes an outer capture cover and an inner collector, wherein the outer capture cover is used to limit the diffusion of the sputtering contaminants, and the inner collector is used to collect the sputtering contaminants.

[0073] Specifically, during ion beam polishing, the objective lens protection baffle 2 moves to the bottom of the objective lens to intercept sputtered contaminants that may fall onto the objective lens; during electron beam scanning imaging, the objective lens protection baffle 2 retreats to the inner wall of the sample chamber to avoid blocking the imaging light path.

[0074] During actual use, during ion beam polishing: the sputtered contaminant capture device extends above the sample, and the ion optical barrel emits the ion beam, wherein the ion optical barrel is installed on an adjustable flange, and the ion beam incident angle is adjustable; the ion gun has a unidirectional focusing module, which can focus the unidirectional line into a linear ion beam spot, thereby improving the polishing efficiency and reducing sputtering contamination; the sample stage can perform continuous rotation, linear reciprocating, swinging and other motion modes to remove the curtain effect and increase the polishing area; the ion beam bombards the sample surface, and the sputtered contaminants are captured and collected by the mobile debris capture device.

[0075] During electron beam imaging: the ion gun is turned off, the sputtered contaminant capture device is withdrawn, the electron beam scans the sample surface, and the generated secondary electron signals and backscattered electron signals are collected by the detectors respectively to form an image.

[0076] The workflow of the above-mentioned argon ion beam scanning electron microscope dual beam system is as follows:

[0077] 1. Sample loading: Load the sample onto the sample stage.

[0078] 2. Vacuum extraction: Pump the sample chamber to a high vacuum state.

[0079] 3. Ion beam polishing: Start the ion gun, and the argon ion beam is incident on the sample surface at an adjustable angle. The sample stage can perform continuous rotation, linear reciprocating or swinging motion, and the sputtered pollutants are collected in real time by a mobile capture device.

[0080] 4. Polishing parameter adjustment: According to the sample material and the required polishing effect, adjust the ion beam energy, ion beam current, incident angle, sample stage motion parameters, and polishing time.

[0081] 5. Electron beam imaging: turn off the ion gun, the mobile capture device exits the sample chamber, the electron beam scans the sample surface, and the detector collects the signal to form a sample image.

[0082] 6. Image analysis: Analyze the obtained images to obtain information such as sample morphology and composition.

[0083] 7. Repeat steps 3-6: Repeat the ion beam polishing step and electron beam imaging step as needed until a satisfactory result is obtained.

[0084] The working principle of the above-mentioned argon ion beam scanning electron microscope dual beam system is:

[0085] Ion beam polishing: Figure 2As shown, the sample stage 7 moves to the designated polishing position, the sputtered contaminant capture device (objective lens protection baffle 2 and sputtered contaminant collector 8) extends above the sample, the ion optical lens barrel 4 starts to generate an ion beam, and the sample stage 7 can perform continuous rotation, linear reciprocating, swinging and other motion modes to remove the curtain effect and increase the polishing area; the ion beam bombards the sample surface, and the sputtered contaminants are captured and collected by the mobile sputtered contaminant collector 8.

[0086] Electron beam imaging: Figure 3 As shown, the ion optical lens tube 4 is closed, the sputtering contaminant capture device (objective lens protection baffle 2 and sputtering contaminant collector 8) is withdrawn, the sample stage 7 is moved to the specified imaging position, and the electron optical lens tube 1 emits an electron beam to scan the sample surface. The generated secondary electron signal and backscattered electron signal are collected by the backscattered electron detector 5 and the side secondary electron detector 6 respectively, thereby forming an image.

[0087] The ternary lithium battery electrode samples were polished by argon ion beam scanning electron microscope before and after cross-section polishing. Fig. 9 As shown in (a) and (b), before polishing, the electrode surface is rough, the particle boundaries are blurred, and it is difficult to observe a clear internal structure; after ion beam polishing, the sample surface is flat and smooth, and the particle boundaries are clearly visible, allowing particle size distribution analysis, morphology observation, and particle packing density evaluation.

[0088] The results of mechanical polishing and argon ion beam scanning electron microscope plane polishing of the metal molybdenum sample are as follows: Fig.10 As shown in (a) and (b), after mechanical grinding and polishing, there are many tiny scratches on the surface of the sample; after ion beam polishing, the mechanical damage layer is eliminated, showing a clear grain structure.

[0089] This embodiment provides an integrated argon ion beam scanning electron microscope dual-beam system to achieve sample ion beam in-situ polishing and electron beam online imaging, and efficiently integrate sample preparation and characterization to improve analysis efficiency, reduce operation difficulty, and reduce contamination risks, thereby obtaining high-quality analysis results.

[0090] Example 2

[0091] An in-situ sample analysis method for an argon ion beam scanning electron microscope dual beam system is applied to the above-mentioned argon ion beam scanning electron microscope dual beam system. For a detailed description of the system, reference can be made to the corresponding description in the above-mentioned system embodiment, which will not be repeated here. Figure 8 As shown, the method comprises the following steps:

[0092] S100, ion beam polishing step: the sample stage moves to the polishing position, the ion optical lens barrel is started to generate an argon ion beam, the argon ion beam is incident on the sample surface at an adjustable angle, and the sample stage performs continuous rotation, linear reciprocating, swinging and other movements to remove the curtain effect and increase the polishing area;

[0093] S200, electron beam imaging step: the ion optical lens tube is closed, the sample stage is moved to the imaging position, the electron optical lens tube emits an electron beam to scan the sample surface, and the generated electron signal is collected by the detector. For example, the generated secondary electron signal and backscattered electron signal are collected by the backscattered electron detector and the side secondary electron detector, respectively, to form a sample image.

[0094] In order to capture contaminants generated by ion beam sputtering and reduce sample contamination, in some embodiments, the ion beam polishing step further includes:

[0095] Before the ion optical column starts to generate an argon ion beam, a sputtered contaminant capture device extends into the sample chamber, and then collects the sputtered contaminants in real time after the argon ion beam bombards the sample surface;

[0096] Specifically, the sputtered contaminant collector extends above the sample during ion beam polishing, completely covers the ion beam and the sample, and guides the sputtered contaminants to the multi-layer collection area, preventing the sputtered contaminants from spreading to other areas of the sample chamber, effectively reducing sample contamination;

[0097] During ion beam polishing, the objective lens protection baffle moves under the objective lens to intercept sputtered contaminants that may fall onto the objective lens.

[0098] The electron beam imaging step further comprises:

[0099] After the ion optical column is closed, the sputtered contamination capture device is withdrawn.

[0100] Specifically, when the electron beam is scanning and imaging, the sputtered contaminant collector is retracted to the inner wall of the sample chamber to avoid blocking the imaging light path.

[0101] When the electron beam is scanning and imaging, the objective lens protection baffle is retracted to the inner wall of the sample chamber to avoid blocking the imaging light path.

[0102] Combining the above ion beam polishing step and electron beam imaging step, the workflow of the above argon ion beam scanning electron microscope dual beam system is as follows:

[0103] 1. Sample loading: Load the sample onto the sample stage.

[0104] 2. Vacuum extraction: Pump the sample chamber to a high vacuum state.

[0105] 3. Ion beam polishing: Start the ion gun, and the argon ion beam is incident on the sample surface at an adjustable angle. The sample stage can perform continuous rotation, linear reciprocating or swinging motion, and the sputtered contaminants are collected in real time by the sputtered contaminant collector.

[0106] 4. Polishing parameter adjustment: According to the sample material and the required polishing effect, adjust the ion beam energy, ion beam current, incident angle, sample stage motion parameters, and polishing time.

[0107] 5. Electron beam imaging: turn off the ion gun, the sputtered contaminant collector exits the sample chamber, the electron beam scans the sample surface, and the detector collects the signal to form a sample image.

[0108] 6. Image analysis: Analyze the obtained images to obtain information such as sample morphology and composition.

[0109] 7. Repeat steps 3-6: Repeat the ion beam polishing step and electron beam imaging step as needed until a satisfactory result is obtained.

[0110] This embodiment provides an in-situ sample analysis method of an argon ion beam scanning electron microscope dual beam system, which has the following advantages:

[0111] Improved efficiency: Eliminating sample transfer steps greatly improves the efficiency of sample preparation and analysis.

[0112] Simplified operation: The automated control system simplifies the operation process, reduces the difficulty of operation, and reduces human errors.

[0113] Reduced contamination risk: Performing sample polishing and imaging in the same vacuum environment minimizes sample contamination and improves the accuracy of analytical results.

[0114] Achieve in-situ three-dimensional imaging: By combining argon ion beam polishing and scanning electron microscopy technology, in-situ three-dimensional imaging of samples can be achieved to obtain more comprehensive and accurate microstructural information.

[0115] The number of devices and processing scales described here are used to simplify the description of the present invention. Applications, modifications and variations of the present invention will be obvious to those skilled in the art.

[0116] Although the embodiments of the present invention have been disclosed as above, they are not limited to the applications listed in the specification and implementation modes. They can be fully applied to various fields suitable for the present invention. For those familiar with the art, additional modifications can be easily implemented. Therefore, without departing from the general concept defined by the claims and the scope of equivalents, the present invention is not limited to the specific details and the illustrations shown and described herein.

[0117] It should also be noted that the terms "include", "comprises" or any other variations thereof are intended to cover non-exclusive inclusion, so that a process, method, commodity or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, commodity or device. In the absence of more restrictions, the elements defined by the sentence "comprises a ..." do not exclude the existence of other identical elements in the process, method, commodity or device including the elements.

[0118] The specification may be described in the general context of computer-executable instructions executed by a computer, such as program units. Generally, program units include routines, programs, objects, components, data structures, etc. that perform specific tasks or implement specific abstract data types. The specification may also be practiced in distributed computing environments where tasks are performed by remote processing devices connected via a communications network. In a distributed computing environment, program units may be located in local and remote computer storage media, including storage devices.

[0119] Each embodiment in this specification is described in a progressive manner, and the same or similar parts between the embodiments can be referred to each other, and each embodiment focuses on the differences from other embodiments. In particular, for the system embodiment, since it is basically similar to the method embodiment, the description is relatively simple, and the relevant parts can be referred to the partial description of the method embodiment.

[0120] The above description is only an embodiment of this specification and is not intended to limit one or more embodiments of this specification. For those skilled in the art, one or more embodiments of this specification may have various changes and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of one or more embodiments of this specification shall be included in the scope of the claims of one or more embodiments of this specification.

Claims

1. An argon ion beam scanning electron microscope dual beam system, characterized in that: It includes an electron optical lens tube, an ion optical lens tube, a sample chamber, a sample stage, and a detector; wherein, The electron optical lens tube generates a high-energy electron beam for scanning the sample surface for imaging; The ion optical column generates a high-energy argon ion beam for polishing / milling the sample surface; The sample chamber is used to contain samples and provide a vacuum environment; The sample stage is used to accurately control the position and angle of the sample; The detector is used to collect signals generated by the interaction between the electron beam and the sample for imaging analysis.

2. An argon ion beam scanning electron microscope dual beam system as claimed in claim 1, characterized in that: The ion optical lens barrel comprises an ion source and a unidirectional focusing module. The ion source is used to generate an ion beam, and the unidirectional focusing module is used to unidirectionally focus a circular ion beam spot into a linear ion beam spot.

3. An argon ion beam scanning electron microscope dual beam system as claimed in claim 2, characterized in that: The one-way focusing module comprises an Einzel focusing lens and an electrostatic quadrupole focusing lens, and the Einzel focusing lens is placed between the ion source and the electrostatic quadrupole focusing lens.

4. The argon ion beam scanning electron microscope dual beam system according to claim 1, characterized in that: The ion optical column further comprises an angle adjustment element, and the ion optical column is mounted on the angle adjustment element so that the incident angle of the ion beam is adjustable.

5. An argon ion beam scanning electron microscope dual beam system as claimed in claim 4, characterized in that: The angle adjustment element is an adjustable flange.

6. The argon ion beam scanning electron microscope dual beam system according to claim 1, characterized in that: The ion optical lens barrel further comprises a magnetic shielding sleeve, and the magnetic shielding sleeve is sleeved outside the ion optical lens barrel.

7. The argon ion beam scanning electron microscope dual beam system according to claim 2, characterized in that: The detector comprises a backscattered electron detector and a lateral secondary electron detector, and the backscattered electron detector and the lateral secondary electron detector are used to collect secondary electron signals and backscattered electron signals generated by the electron optical lens barrel.

8. The argon ion beam scanning electron microscope dual beam system according to claim 1, characterized in that: The sample stage includes, from top to bottom, a sample nail stage, a nail stage fixing seat, a base, a piezoelectric rotating stage, a piezoelectric displacement stage, and an adapter plate. The sample nail stage is fixed to the base through the nail stage fixing seat, the base is installed on the piezoelectric rotating stage, the piezoelectric rotating stage is installed on the piezoelectric displacement stage, the piezoelectric displacement stage is fixed to the adapter plate, the sample nail stage is used to place samples, the piezoelectric displacement stage is used to achieve nanometer-level precision control in the Z direction, and the piezoelectric rotating stage can be adjusted to rotate continuously during ion beam polishing.

9. An argon ion beam scanning electron microscope dual beam system as claimed in claim 8, characterized in that: It also includes a precision layer cutting mechanism, which is used to achieve precise sample layer cutting and cooperate with ion beam polishing to obtain a high-quality sample surface.

10. An argon ion beam scanning electron microscope dual beam system as claimed in claim 9, characterized in that: The precision layer cutting mechanism comprises a baffle and a baffle support. The baffle is provided with a groove for accommodating a sample, and the baffle is fixed to the adapter plate through the baffle support.

11. The argon ion beam scanning electron microscope dual beam system according to claim 1, characterized in that: It also includes a sputtering contaminant capturing device, which is used to capture contaminants generated by ion beam sputtering to reduce sample contamination.

12. An argon ion beam scanning electron microscope dual beam system as claimed in claim 11, characterized in that: The sputtering contaminant capturing device includes a sputtering contaminant collector and an objective lens protection baffle. The sputtering contaminant collector and the objective lens protection baffle are both mobile devices. The sputtering contaminant collector is used to guide and collect the sputtering contaminants, and the objective lens protection baffle is used to intercept the sputtering contaminants that may fall onto the objective lens.

13. An in-situ sample analysis method for an argon ion beam scanning electron microscope dual beam system, characterized in that: Applied to an argon ion beam scanning electron microscope dual beam system as claimed in any one of claims 1 to 12, the method comprises the following steps: Ion beam polishing step: the sample stage moves to the polishing position, the ion optical lens barrel is started to generate an argon ion beam, the argon ion beam is incident on the sample surface at an adjustable angle, and the sample stage moves to remove the curtain effect and increase the polishing area; Electron beam imaging step: the ion optical lens tube is closed, the sample stage is moved to the imaging position, the electron optical lens tube emits an electron beam to scan the sample surface, and the generated electron signal is collected by the detector to form a sample image.

14. The in-situ sample analysis method of an argon ion beam scanning electron microscope dual beam system according to claim 13, characterized in that: The ion beam polishing step further comprises: Before the ion optical column starts to generate an argon ion beam, a sputtered contaminant capture device extends into the sample chamber, and then collects the sputtered contaminants in real time after the argon ion beam bombards the sample surface; The electron beam imaging step further comprises: After the ion optical column is closed, the sputtered contamination capture device is withdrawn.

15. The in-situ sample analysis method of an argon ion beam scanning electron microscope dual beam system according to claim 13, characterized in that: Also includes the steps: Adjust the ion beam energy, ion beam current, incident angle, sample stage motion parameters, and polishing time according to the sample material and the required polishing effect; And, as needed, repeat the ion beam polishing step and the electron beam imaging step until a satisfactory result is obtained.

Images