CN112067405B - Preparation method of plane TEM sample and plane TEM sample - Google Patents
Preparation method of plane TEM sample and plane TEM sample Download PDFInfo
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- CN112067405B CN112067405B CN202011075854.8A CN202011075854A CN112067405B CN 112067405 B CN112067405 B CN 112067405B CN 202011075854 A CN202011075854 A CN 202011075854A CN 112067405 B CN112067405 B CN 112067405B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01Q—SCANNING-PROBE TECHNIQUES OR APPARATUS; APPLICATIONS OF SCANNING-PROBE TECHNIQUES, e.g. SCANNING PROBE MICROSCOPY [SPM]
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Abstract
The application discloses a preparation method of a plane TEM sample and the plane TEM sample, wherein the preparation method comprises the steps of placing a sample to be detected on a sample table; controlling the sample table to incline to 52 degrees; constructing a target sample preparation area on the surface of a sample to be detected; etching by using an ion beam to obtain a target rectangular sample; controlling the sample table to incline to-10 degrees; etching by using an ion beam to obtain a target wedge-shaped body, wherein the intersection of the first wedge-shaped surface and the second wedge-shaped surface of the target wedge-shaped body can be used for cutting the bottom of the target wedge-shaped body from a sample to be detected; inclining the sample table to zero degree; and controlling the nano manipulator to extract the target wedge, rotating by 90 degrees, welding the target wedge to a standard copper net, and thinning to a target thickness to obtain a planar TEM sample. According to the preparation method, the inclination angle of the sample platform is controlled, so that the target wedge-shaped body is divided from the sample to be detected in the process of meeting two wedge-shaped surfaces in the target wedge-shaped body.
Description
Technical Field
The application relates to the technical field of semiconductor manufacturing, in particular to a preparation method of a planar TEM sample and the planar TEM sample.
Background
A Transmission Electron Microscope (TEM) is the most widely used type of TEM, and its working principle is as follows: the electron beam penetrates through a TEM sample, and then is imaged on a fluorescent screen after being amplified by multi-stage electrons, so that an image of the TEM sample is formed, and then the image of the TEM sample is measured and analyzed.
Because the substance has a strong ability to scatter the electron beam, the TEM sample must be made very thin to allow the electron beam to pass through. At present, a Focused Ion Beam (FIB) instrument is often used to prepare a TEM sample, that is, a FIB is used to directly cut a film for TEM research from a sample to be tested in a nanometer or micrometer scale. The preparation process roughly comprises the following steps: firstly, a sample to be detected is placed on a sample table, a metal protective layer is plated on an interested area of the sample to be detected for protection, then a thicker small piece is cut out from the sample to be detected by directly using FIB, the small piece is transferred to a specially-made standard copper net in an FIB sample cavity by using a nano manipulator, and finally the small piece is thinned to the final thickness by using FIB, so that the preparation of a TEM sample is realized.
At present, in order to cut out a small piece parallel to the surface of a sample to be measured to obtain a planar TEM sample, a sample table is usually kept horizontal, and materials below a sample preparation position need to be completely removed to completely cut out the small piece from the sample to be measured.
Disclosure of Invention
In order to solve the technical problem that the sample is difficult to be completely cut in the existing preparation process of the plane TEM sample, the application discloses a preparation method of the plane TEM sample and the plane TEM sample.
The application discloses in a first aspect a method for preparing a planar TEM sample, comprising:
placing a sample to be detected on a sample table;
controlling the sample table to incline to 52 degrees;
depositing a metal protective layer on the surface of the sample to be detected to construct a target sample preparation area;
etching a channel with a fixed shape around the target sample preparation area by using an ion beam to obtain a target rectangular sample, wherein a connecting bridge exists between the target rectangular sample and the rest part of the sample to be detected;
controlling the sample table to incline to-10 degrees;
etching two long sides of the target rectangular sample by using an ion beam to obtain a target wedge, wherein the target wedge comprises a first wedge surface and a second wedge surface, and the intersection of the first wedge surface and the second wedge surface is used for cutting the bottom of the target wedge from the sample to be detected;
controlling the sample stage to incline to zero degree;
controlling the nano mechanical arm to extract the target wedge-shaped body;
controlling the nanometer mechanical arm to rotate by 90 degrees, so that the target wedge body rotates by 90 degrees;
welding the rotated target wedge to a standard copper mesh;
and thinning the target wedge welded on the standard copper mesh to a target thickness to obtain a plane TEM sample.
Optionally, the etching, by using an ion beam, two long sides of the target rectangular sample to obtain a target wedge includes:
etching one long side of the target rectangular sample by using an ion beam to form a first wedge-shaped surface on the target rectangular sample;
controlling the sample table to rotate 180 degrees;
and etching the other long side of the target rectangular sample by using the ion beam to form a second wedge-shaped surface on the target rectangular sample, wherein in the process of forming the second wedge-shaped surface, the second wedge-shaped surface and the first wedge-shaped surface are intersected so that the bottom of the finally obtained target wedge-shaped body is cut off.
Optionally, depositing a metal protection layer on the surface of the sample to be tested to construct a target sample preparation area, including:
selecting an interested area on the sample to be tested;
and depositing four metal protective layers around the region of interest by using an ion beam to construct the target sampling region.
Optionally, the channel with the fixed shape is a C-shaped channel, and the opening of the C-shaped channel is the position of the connecting bridge.
Optionally, the controlling the nano manipulator to extract the target wedge includes:
controlling the nanometer mechanical arm to be close to the target end surface of the target wedge body, wherein the target end surface is positioned at the other end of the end surface where the connecting bridge is positioned;
welding the target wedge to the nanomachinery manipulator by depositing a metal layer;
severing the connecting bridge using an ion beam;
and controlling the nano manipulator to extract the target wedge body according to the original position.
Optionally, before the controlling the sample stage to tilt to zero, the method for preparing a planar TEM sample further includes:
and observing by using a scanning electron microscope, judging whether the bottom of the target wedge-shaped body is cut off, and if so, controlling the sample stage to incline to zero.
In a second aspect, a planar TEM sample is disclosed, which is prepared by the method of preparing a planar TEM sample according to the first aspect of the present invention.
The application discloses a preparation method of a plane TEM sample and the plane TEM sample, wherein in the preparation method, the sample to be detected is placed on a sample stage; controlling the sample table to incline to 52 degrees; constructing a target sample preparation area on the surface of a sample to be detected; etching a channel with a fixed shape around a target sample preparation area by using an ion beam to obtain a target rectangular sample; controlling the sample table to incline to-10 degrees; etching two long sides of a target rectangular sample by using an ion beam to obtain a target wedge-shaped body, wherein the intersection of the first wedge-shaped surface and the second wedge-shaped surface of the target wedge-shaped body can divide the bottom of the target wedge-shaped body from the sample to be detected; controlling the sample table to incline to zero degree; and controlling the nano manipulator to extract the target wedge body, rotating the target wedge body by 90 degrees, welding the target wedge body to a standard copper net, and thinning the target wedge body to a target thickness to obtain a planar TEM sample. In the preparation method, the target wedge-shaped body is etched in the sample to be detected by controlling the inclination angle of the sample platform, and the target wedge-shaped body is separated from the sample to be detected in the process of meeting two wedge-shaped surfaces in the target wedge-shaped body.
Drawings
In order to more clearly explain the technical solution of the present application, the drawings needed to be used in the embodiments are briefly described below, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a schematic workflow diagram of a method for preparing a planar TEM sample disclosed in an embodiment of the present application;
FIG. 2 is a schematic diagram of a target sample preparation region constructed in a method for preparing a planar TEM sample according to an embodiment of the present disclosure;
FIG. 3 is a schematic diagram of a rectangular target sample obtained in a method for preparing a planar TEM sample disclosed in an embodiment of the present application;
FIG. 4 is a schematic diagram of a target wedge structure obtained in a method for preparing a planar TEM sample according to an embodiment of the present disclosure;
FIG. 5 is a schematic diagram of a target wedge being extracted during a method of preparing a planar TEM sample according to an embodiment of the present disclosure;
FIG. 6 is a schematic illustration of a rotated target wedge welded to a standard copper mesh in a method of making a planar TEM sample as disclosed in an example of the present application.
Detailed Description
In order to solve the technical problem that the sample is difficult to be cut completely in the existing preparation process of the plane TEM sample, the application discloses a preparation method of the plane TEM sample and the plane TEM sample through the following implementation.
The first embodiment of the present application discloses a method for preparing a planar TEM sample, which is shown in fig. 1 as a schematic workflow diagram, and includes:
step S101, placing the sample 10 to be measured on a sample table.
And step S102, controlling the sample table to incline to 52 degrees.
Step S103, depositing a metal protection layer on the surface of the sample 10 to be tested, and constructing a target sample preparation area 20.
Specifically, a metal protection layer is deposited on the surface of the sample 10 to be tested, and a target sample preparation area 20 is constructed by the following steps:
a region of interest is selected on the sample 10 to be tested.
The target patterning area 20 is constructed by depositing four protective layers of metal around the region of interest using ion beams.
Referring to fig. 2, the four metal protective layers are a first metal protective layer 201, a second metal protective layer 202, a third metal protective layer 203, and a fourth metal protective layer 204, respectively, which form marks having rectangular shapes, build the target patterning region 20, and also protect from redeposition of a large amount of material during a sputtering process.
Step S104, etching a channel with a fixed shape around the target sample preparation area 20 by using an ion beam to obtain a target rectangular sample 30, wherein a connecting bridge 50 exists between the target rectangular sample 30 and the rest part of the sample 10 to be detected.
In some embodiments, the fixed-shape channel is a C-shaped channel 40, and the opening of the C-shaped channel 40 is the location of the connecting bridge 50. Referring to fig. 3, the target rectangular sample 30 is isolated from the rest of the sample 10 to be tested by a C-shaped channel 40, the only connecting channel being where the bridge 50 is located. In the etching process, large beam current regular cross section etching is firstly used, and then smaller beam current cleaning cross section etching is gradually carried out.
And step S105, controlling the sample stage to incline to-10 degrees.
Step S106, etching two long sides of the target rectangular sample 30 by using an ion beam to obtain a target wedge 60, where the target wedge 60 includes a first wedge surface 601 and a second wedge surface 602, and a junction of the first wedge surface 601 and the second wedge surface 602 can separate the bottom of the target wedge 60 from the sample 10 to be measured.
Specifically, the etching of two long sides of the target rectangular sample 30 by using the ion beam to obtain the target wedge 60 includes:
a first wedge surface 601 is formed on the target rectangular sample 30 by etching with an ion beam for one of the long sides of the target rectangular sample 30.
And controlling the sample table to rotate by 180 degrees.
And etching the other long side of the target rectangular sample 30 by using the ion beam to form a second wedge surface 602 on the target rectangular sample 30, wherein in the process of forming the second wedge surface 602, the second wedge surface 602 meets the first wedge surface 601 so that the bottom of the finally obtained target wedge 60 is cut off, and the structure of the target wedge 60 is shown in fig. 4.
It should be noted that, in the process of controlling the inclination angle of the sample stage, the sample stage is controlled to rotate according to the target central axis to change the inclination angle of the sample stage, and the target central axis is parallel to the long side of the target rectangular sample 30. Before etching, the sample stage is controlled to be inclined to-10 degrees (belonging to the maximum negative angle of an FIB instrument), an ion beam has an incident angle, surfaces obtained by etching two long sides form a wedge, the wedge surface processed by the second long side meets the wedge surface generated by the first long side after the wedge surface processed by the second long side succeeds, and then the bottom of the target wedge 60 is cut off, at the moment, whether the bottom is cut off can be observed through an SEM (scanning electron microscope), and when the bottom is observed on the short side of a sample, the method is more obvious.
And S107, controlling the sample stage to incline to zero degree.
The upper surfaces of the target wedge 60 (the surfaces other than the first and second wedge surfaces 601, 602) are in a horizontal plane when the sample stage is horizontal.
Step S108, the nano-manipulator 70 is controlled to extract the target wedge 60.
Specifically, the nano-manipulator 70 is controlled to approach the target end surface of the target wedge 60, where the target end surface is located at the other end of the end surface where the connecting bridge 50 is located.
The target wedge 60 is welded to the nanomachinery robot 70 by depositing a metal layer. Because of the wedge geometry, the flat sample is much larger than the cross-sectional sample, and therefore, a thicker metal layer is required to more securely weld to the nanotechnology tool 70.
The connecting bridges 50 are cut using a rectangular pattern of ion beams. Whether the target wedge 60 is separated from the substrate is monitored by Scanning Electron Microscope (SEM) imaging. After the separation is confirmed, the nano-manipulator 70 is controlled to extract the target wedge 60 in situ, and the upper surface of the target wedge 60 is always kept parallel to the horizontal plane during the extraction process.
Step S109, the nano manipulator 70 is controlled to rotate 90 degrees, so that the target wedge 60 rotates 90 degrees.
After the target wedge 60 is lifted to a certain height, the rotation of 90 degrees is performed by using the nano manipulator 70 with the rotation function together with the target wedge 60. The result of the rotation is shown in figure 5, where the upper surface of the target wedge 60 is in a vertical orientation.
In step S110, the rotated target wedge 60 is welded to the standard copper mesh 80.
And step S111, thinning the target wedge-shaped body 60 welded on the standard copper mesh 80 to a target thickness to obtain a plane TEM sample.
Referring to FIG. 6, the target wedge 60 is transferred to a standard copper mesh 80 for welding, and then the target wedge 60 is thinned using a standard cross-section sample thinning method to complete the sample preparation and obtain a planar TEM sample.
The embodiment discloses a preparation method of a planar TEM sample, wherein in the preparation method, a sample 10 to be detected is placed on a sample table; controlling the sample table to incline to 52 degrees; constructing a target sample preparation area 20 on the surface of a sample 10 to be detected; etching a channel with a fixed shape around the target sample preparation area 20 by using an ion beam to obtain a target rectangular sample 30; controlling the sample platform to incline to-10 degrees; etching two long sides of the target rectangular sample 30 by using an ion beam to obtain a target wedge 60, wherein the intersection of the first wedge surface 601 and the second wedge surface 602 of the target wedge 60 can divide the bottom of the target wedge 60 from the sample 10 to be measured; controlling the sample table to incline to zero degree; and controlling the nanometer manipulator 70 to extract the target wedge 60, rotating the target wedge 60 by 90 degrees, welding the target wedge 60 to a standard copper mesh 80, and thinning the target wedge to a target thickness to obtain a planar TEM sample. In the preparation method, the target wedge 60 is etched in the sample 10 to be detected by controlling the inclination angle of the sample stage, and the target wedge 60 is separated from the sample 10 to be detected by the intersection of the two wedge surfaces in the target wedge 60.
Further, before the controlling the sample stage to tilt to zero, the method for preparing a planar TEM sample further comprises:
observing by using a Scanning Electron Microscope (SEM), judging whether the bottom of the target wedge 60 is cut off, and if so, controlling the sample stage to incline to zero degree.
A second embodiment of the present application discloses a planar TEM sample prepared by the method of preparing a planar TEM sample as described in the first embodiment of the present application.
The preparation method of the plane TEM sample disclosed by the embodiment of the application can realize plane TEM sample preparation in the designated area and improve the sample preparation diversity. Compared with the prior FIB cutting method, the new cutting geometry reduces the etching area, provides a larger visual angle to judge the separation condition of the sample and the substrate more intuitively and conveniently, and greatly improves the success rate of extracting the sample. Therefore, the new preparation method improves the success rate and efficiency of the FIB-enhanced planar TEM sample preparation technology. The target rectangular sample is prepared by the geometrical shape of the isolated cuboid, so that the wedging process in the subsequent steps is efficient, a clear visual angle is provided for the milling process between the monitoring steps, the damage to surrounding materials is avoided to the maximum extent, and the problem of judging whether the sample is completely separated from bulk materials is solved.
The present application has been described in detail with reference to specific embodiments and illustrative examples, but the description is not intended to limit the application. Those skilled in the art will appreciate that various equivalent substitutions, modifications or improvements may be made to the embodiments and implementations thereof without departing from the spirit and scope of the present application, and are within the scope of the present application. The protection scope of this application is subject to the appended claims.
Claims (6)
1. A method for preparing a planar TEM sample, which is characterized by comprising:
placing a sample to be detected on a sample table;
controlling the sample table to incline to 52 degrees;
depositing a metal protective layer on the surface of the sample to be detected to construct a target sample preparation area;
etching a channel with a fixed shape around the target sample preparation area by using an ion beam to obtain a target rectangular sample, wherein a connecting bridge exists between the target rectangular sample and the rest part of the sample to be detected;
controlling the sample table to incline to-10 degrees;
etching two long sides of the target rectangular sample by using ion beams to obtain a target wedge, comprising:
etching one long side of the target rectangular sample by using an ion beam to form a first wedge-shaped surface on the target rectangular sample;
controlling the sample table to rotate 180 degrees;
etching the other long side of the target rectangular sample by using the ion beam to form a second wedge-shaped surface on the target rectangular sample, wherein in the process of forming the second wedge-shaped surface, the second wedge-shaped surface and the first wedge-shaped surface are intersected to cut off the bottom of the finally obtained target wedge-shaped body;
controlling the sample stage to incline to zero degree;
controlling the nano mechanical arm to extract the target wedge-shaped body;
controlling the nanometer mechanical arm to rotate by 90 degrees, so that the target wedge body rotates by 90 degrees;
welding the rotated target wedge to a standard copper mesh;
and thinning the target wedge welded on the standard copper mesh to a target thickness to obtain a plane TEM sample.
2. The method of preparing a planar TEM sample according to claim 1, wherein depositing a metal protective layer on the surface of the sample to be tested to create a target sample preparation area comprises:
selecting an interested area on the sample to be tested;
and depositing four metal protective layers around the region of interest by using an ion beam to construct the target sampling region.
3. A method of preparing a planar TEM sample according to claim 1, wherein the fixed-shape channel is a C-shaped channel, and the opening of the C-shaped channel is the location of the bridge.
4. The method of claim 1, wherein said controlling the nanomachinery manipulator to extract the target wedge comprises:
controlling the nanometer mechanical arm to be close to the target end face of the target wedge body, wherein the target end face is positioned at the other end of the end face where the connecting bridge is positioned;
welding the target wedge to the nanomachinery manipulator by depositing a metal layer;
severing the connecting bridge using an ion beam;
and controlling the nanometer mechanical arm to extract the target wedge body according to the original position.
5. The method of preparing a planar TEM sample according to claim 1, wherein prior to said controlling the tilt of the sample stage to zero degrees, the method further comprises:
and observing by using a scanning electron microscope, judging whether the bottom of the target wedge-shaped body is cut off, and if so, controlling the sample stage to incline to zero.
6. A planar TEM sample prepared by the method of preparing a planar TEM sample according to any one of claims 1 to 5.
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| CN112881439A (en) * | 2021-03-09 | 2021-06-01 | 洪启集成电路(珠海)有限公司 | OLED TEM sample preparation method and OLED TEM sample |
| CN113466268B (en) * | 2021-06-30 | 2022-06-07 | 长江存储科技有限责任公司 | Combined sample and preparation method thereof |
| CN113588372B (en) * | 2021-08-13 | 2022-09-02 | 胜科纳米(苏州)股份有限公司 | Sample preparation method and detection method for measuring element diffusion of VCSEL device multilayer film |
| CN114235478A (en) * | 2021-12-17 | 2022-03-25 | 桂林理工大学 | In-situ micro-area sampling method for underground sample |
| CN114486324A (en) * | 2022-01-30 | 2022-05-13 | 上海季丰电子股份有限公司 | Preparation method of transmission electron microscope sample |
| CN115096639B (en) * | 2022-05-27 | 2023-03-28 | 中国科学院地质与地球物理研究所 | Micro-area sampling and micro-analysis method for rock |
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