CN110954568B - Electron microscope observation sample and preparation method thereof - Google Patents
Electron microscope observation sample and preparation method thereof Download PDFInfo
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- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
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- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
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- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
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- G01N23/2202—Preparing specimens therefor
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- G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
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- 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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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Abstract
The embodiment of the application discloses an electron microscope observation sample and a preparation method thereof, wherein the method comprises the following steps: providing a test specimen comprising a target sample layer; dividing a sample preparation area on the sample, and exposing the side wall of a target sample layer in the sample preparation area; forming a support frame, wherein the support frame at least covers the side wall of the target sample layer; thinning the test sample in the sample preparation area after the support frame is formed to obtain a target sample with preset thickness in the target sample layer; wherein the material hardness of the support frame is greater than the material hardness of the target sample layer.
Description
Technical Field
The application relates to the field of semiconductor manufacturing, in particular to an electron microscope observation sample and a preparation method thereof.
Background
The Electron Back Scattering Diffraction (EBSD) technique is to add a set of EBSD collection hardware and analysis system in a Scanning Electron Microscope (SEM), so as to analyze the micro-domain crystal structure and orientation information of a sample in the SEM, and to correspond the micro-domain crystal structure and orientation information to the microstructure morphology. The EBSD technology has a large analysis area and a large number of obtained grains, becomes an effective analysis means for fast, high-efficiency and quantitative statistical research on microstructure and texture of materials, and is widely applied to the fields of materials, geology, microelectronics and the like. The extremely high resolution and the extremely high analytical capability of EBSD requires the electron beam to penetrate the sample, thus requiring the sample to be thinned to a certain thickness when preparing the sample.
Currently, a Transmission Electron Microscope (TEM) sample preparation method is generally used to prepare an EBSD sample, i.e., a thicker sample containing a target sample layer is adhered to a carbon film copper mesh (Grid), and then both sides of the sample are thinned by using a Focused Ion Beam (FIB) process. However, when the EBSD sample of soft material (e.g., cu, al, etc.) is prepared by this method, if the sample is thinned to 200nm or less, the sample is very easily deformed, thereby affecting the subsequent thinning process, and even causing sample preparation failure.
Disclosure of Invention
The embodiment of the application provides an electron microscope observation sample and a preparation method thereof for solving at least one problem in the prior art.
In order to achieve the above purpose, the technical solution of the embodiment of the present application is implemented as follows:
in a first aspect, an embodiment of the present application provides a method for preparing an electron microscope observation sample, where the method includes:
providing a test specimen comprising a target sample layer;
dividing a sample preparation area on the sample, and exposing the side wall of a target sample layer in the sample preparation area;
forming a support frame, wherein the support frame at least covers the side wall of the target sample layer;
thinning the test sample in the sample preparation area after the supporting frame is formed to obtain a target sample with a preset thickness in the target sample layer;
wherein the material hardness of the support frame is greater than the material hardness of the target sample layer.
In an alternative embodiment, the thinning of the sample is performed using a focused ion beam FIB process; wherein the FIB is projected to the support frame and the target sample layer in a direction perpendicular to the thickness direction of the specimen to cut off a portion of the specimen other than the target sample of the preset thickness.
In an alternative embodiment, the sample preparation area satisfies a predetermined pattern condition, such that the exposed sidewall of the target sample layer satisfies the following condition:
when the sample is thinned by adopting an FIB process, any surface on the side wall is not parallel to the projection direction of the FIB.
In an alternative embodiment, the preset graphics conditions include:
the sample preparation area is a polygon, the polygon at least comprises one side, and included angles between the side and other sides of the polygon are not right angles.
In an alternative embodiment, the dividing a sample preparation area on the test sample, and exposing a sidewall of a target sample layer in the sample preparation area, includes: etching a groove surrounding the sample preparation area on the sample, wherein the depth of the groove is more than or equal to the thickness from the surface of the sample to the bottom surface of the target sample layer, so that the side wall of the target sample layer is exposed;
said forming a support frame comprising: depositing a frame material in the groove, wherein the deposition thickness of the frame material is greater than or equal to the thickness of the target sample layer, so that the support frame is formed to cover at least the side wall of the target sample layer;
the method further comprises the following steps: and cutting along the outer edge of the supporting frame to separate the test sample in the sample preparation area with the supporting frame.
In an alternative embodiment, at least one of the steps of etching a trench around the sample preparation area, depositing frame material in the trench, and cutting along the outer edge of the support frame is performed using a FIB process.
In a second aspect, embodiments of the present application provide an electron microscope observation sample, including:
a target sample;
a support frame that encases the sidewalls of the target sample;
wherein the support frame has a material hardness greater than a material hardness of the target sample.
In an alternative embodiment, the sidewall of the target sample is a polygon, the polygon includes at least one side, and the side and the other sides of the polygon form an included angle different from a right angle.
In an alternative embodiment, the target sample is obtained by thinning by using a FIB process; and the surface of the side wall of the target sample, on which the side is located, is used as a cutting surface when the FIB process is thinned, and the FIB is projected along the direction vertical to the cutting surface.
The embodiment of the application provides an electron microscope observation sample and a preparation method thereof, wherein the method comprises the following steps: providing a test specimen comprising a target sample layer; dividing a sample preparation area on the sample, and exposing the side wall of a target sample layer in the sample preparation area; forming a support frame, wherein the support frame at least covers the side wall of the target sample layer; thinning the test sample in the sample preparation area after the support frame is formed to obtain a target sample with preset thickness in the target sample layer; wherein the material hardness of the support frame is greater than the material hardness of the target sample layer. In the embodiment of the application, a material with hardness greater than that of the target sample layer is used as a frame material to provide support for the target sample, so that the deformation of the target sample in the thinning process is reduced.
Drawings
Fig. 1 is a first schematic flow chart of an implementation of a method for preparing an electron microscope observation sample according to an embodiment of the present disclosure;
fig. 2 is a schematic flow chart of an implementation of a method for preparing an electron microscope observation sample according to an embodiment of the present application;
FIG. 3 is a schematic diagram of an electron microscope observation sample during preparation according to an embodiment of the present application;
fig. 4 is an electron microscope observation sample provided in the embodiment of the present application.
Detailed Description
Exemplary embodiments disclosed in the present application will be described in more detail below with reference to the accompanying drawings. While exemplary embodiments of the present application are shown in the drawings, it should be understood that the present application may be embodied in various forms and should not be limited to the specific embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art.
In the following description, numerous specific details are set forth in order to provide a more thorough understanding of the present application. It will be apparent, however, to one skilled in the art, that the present application may be practiced without one or more of these specific details. In other instances, well-known features have not been described in order to avoid obscuring the present application; that is, not all features of an actual embodiment are described herein, and well-known functions and structures are not described in detail.
In the drawings, the size of layers, regions, elements, and relative sizes may be exaggerated for clarity. Like reference numerals refer to like elements throughout.
It will be understood that when an element or layer is referred to as being "on," "8230;" \8230 "", "adjacent to," "connected to," or "coupled to" other elements or layers, it can be directly on, adjacent to, connected to, or coupled to the other elements or layers, or intervening elements or layers may be present. In contrast, when an element is referred to as being "directly on," "8230," "over," "with," "8230," "directly adjacent," "directly connected to," or "directly coupled to" other elements or layers, there are no intervening elements or layers present. It will be understood that, although the terms first, second, third, etc. may be used to describe various elements, components, regions, layers and/or sections, these elements, components, regions, layers and/or sections should not be limited by these terms. These terms are only used to distinguish one element, component, region, layer or section from another element, component, region, layer or section. Thus, a first element, component, region, layer or section discussed below could be termed a second element, component, region, layer or section without departing from the teachings of the present application. And the discussion of a second element, component, region, layer or section does not imply that a first element, component, region, layer or section is necessarily present in the application.
Spatial relational terms such as "in 8230," "below," "in 8230," "below," "8230," "above," "above," and the like may be used herein for convenience of description to describe the relationship of one element or feature to another element or feature illustrated in the figures. It will be understood that the spatially relative terms are intended to encompass different orientations of the device in use or operation in addition to the orientation depicted in the figures. For example, if the device in the figures is turned over, then elements or features described as "below" or "beneath" other elements or features would then be oriented "above" the other elements or features. Thus, the exemplary terms "at 8230; \8230; below" and "at 8230; \8230; below" may include both upper and lower orientations. The device may be otherwise oriented (rotated 90 degrees or at other orientations) and the spatial descriptors used herein interpreted accordingly.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It will be further understood that the terms "comprises" and/or "comprising," when used in this specification, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof. As used herein, the term "and/or" includes any and all combinations of the associated listed items.
So that the manner in which the features and elements of the present embodiments can be understood in detail, a more particular description of the embodiments, briefly summarized above, may be had by reference to embodiments, some of which are illustrated in the appended drawings.
The embodiment of the present application provides a method for preparing an electron microscope observation sample, and fig. 1 is a schematic implementation flow diagram of the method for preparing an electron microscope observation sample provided in the embodiment of the present application, where the method mainly includes the following steps:
In the embodiment of the present application, a test sample including a target sample layer is provided, and it should be noted that the test sample may be a chip manufactured by an integrated circuit manufacturing process, and the test sample may include a dielectric layer, a semiconductor layer, a metal layer, and the like. The target sample layer can be made of a material which is low in hardness and easy to deform in the thinning process, such as aluminum or copper.
In this embodiment, a sample preparation region is firstly divided from the sample, and specifically, a trench surrounding the sample preparation region is etched on the sample by an etching process, so as to expose a sidewall of a target sample layer in the sample preparation region. The specific process of etching the groove comprises the following steps: and etching a groove surrounding the sample preparation area on the sample by using an FIB (focused ion beam) process, wherein the depth of the groove is more than or equal to the thickness from the surface of the sample to the bottom surface of the target sample layer, so that the side wall of the target sample layer is exposed.
In the embodiment of the present application, the sample preparation area needs to satisfy a predetermined pattern condition, so that the exposed sidewall of the target sample layer satisfies the following condition: when the FIB process is adopted to thin the sample, any surface on the side wall is not parallel to the projection direction of the FIB. It can be understood that, the sample preparation area is a preset pattern, and the top view of the sidewall of the target sample layer is also a preset pattern, that is, the shape surrounded by the sidewall of the target sample layer is the same as the shape of the sample preparation area, so that when the FIB process is used to thin the sample, any surface of the sidewall of the target sample layer is not parallel to the projection direction of the FIB, thereby greatly avoiding the curtain effect caused by the hardness difference between the support frame and the target sample layer during the thinning process. In some embodiments, an included angle between any one of the side walls of the target sample layer and the projection direction of the FIB is preferably greater than or equal to 5 degrees, so that a curtain effect in a thinning process can be better avoided, and the success rate of sample preparation is improved. .
Wherein the preset graphics conditions include: the sample preparation area is a polygon, and the polygon may be a quadrilateral, but in this embodiment, the polygon includes at least one side, and an included angle between the side and another side on the polygon is not a right angle, for example: 85 degrees or less or 95 degrees or more.
For example, the polygon may be a parallelogram, and then two included angles are formed between at least one side of the parallelogram and the other sides of the parallelogram, one included angle is smaller than or equal to 85 degrees, and the other included angle is greater than or equal to 95 degrees;
for another example, the polygon may be a trapezoid, and then two included angles are formed between at least one side (upper bottom) of the trapezoid and the other sides of the trapezoid, where both the two included angles are greater than or equal to 95 degrees; two included angles are formed between at least one edge (lower bottom) of the trapezoid and other edges of the trapezoid, and the two included angles are both smaller than or equal to 85 degrees; two included angles are formed between at least one edge (inclined edge) of the trapezoid and other edges of the trapezoid, wherein one included angle is smaller than or equal to 85 degrees, and the other included angle is larger than or equal to 95 degrees; for another example, the polygon may be non-quadrilateral, such as a pentagon, a hexagon, or other polygons, and an included angle formed between at least one side of the polygon and the other side of the polygon is equal to or less than 85 degrees or equal to or greater than 95 degrees. Therefore, when the FIB process is adopted to thin the sample of the preset graph, the FIB is projected along the direction perpendicular to the cutting edge based on the edge of the sample preparation area of the preset graph as the cutting edge, and other edges of the sample preparation area of the preset graph except the cutting edge are not parallel to the projection direction of the FI B, namely any one surface on the side wall of the target sample layer is not parallel to the projection direction of the FIB. Thereby being capable of avoiding the curtain effect generated by the hardness difference between the supporting frame and the target sample layer in the thinning process to the great extent. In some embodiments, an included angle between any surface of the sidewall of the target sample layer and the projection direction of the FIB is preferably greater than or equal to 5 degrees, so that a curtain effect during thinning can be better avoided.
103, forming a supporting frame, wherein the supporting frame at least covers the side wall of the target sample layer; wherein the material hardness of the support frame is greater than the material hardness of the target sample layer.
In the embodiment of the application, a frame material is deposited in the groove surrounding the sample preparation area through a FIB process to form a support frame, and the deposition thickness of the frame material is greater than or equal to the thickness of the target sample layer, so that the support frame is formed to cover at least the side wall of the target sample layer. And cutting along the outer edge of the supporting frame by using an FIB (focused ion beam) process to separate the sample in the sample preparation area with the supporting frame. Wherein the material hardness of the support frame is greater than the material hardness of the target sample layer. In practical applications, the material of the supporting frame may be tungsten or platinum, etc. with relatively high hardness. In the embodiment of the application, a frame material with higher hardness is used as a supporting frame to support a target sample layer, so that the deformation condition caused by the fact that the material of the target sample is softer in the thinning process is reduced.
And 104, thinning the test sample in the sample preparation area after the support frame is formed, and obtaining a target sample with preset thickness in the target sample layer.
In this application embodiment, form behind the braced frame, adopt FIB technology will have braced frame sample in the system appearance region separates to separating to have braced frame sample in the system appearance region thins, and the FIB is along the perpendicular to throw in the thickness direction of sample to braced frame and target sample layer to cut off on the sample except the part of the target sample of predetermineeing thickness, thereby obtain to be located the target sample of predetermineeing thickness in the target sample layer. In practical application, the preset thickness is less than or equal to 100nm.
It should be noted that, when the FIB process is used to thin the sample in the sample preparation region with the support frame, any interface between the support frame and the target sample layer is not parallel to the projection direction of the FIB, and an included angle between any surface on the side wall of the target sample layer and the projection direction of the FIB is preferably greater than or equal to 5 degrees. Therefore, the curtain effect caused by the hardness difference between the supporting frame and the target sample layer in the thinning process can be avoided to the greatest extent, and the success rate of sample preparation is improved.
In embodiments of the present application, the target sample may be used for EBSD detection. The electron microscope may be specifically a SEM; it should be noted that the electron microscope observation sample and the preparation method thereof provided in the embodiments of the present application can also be applied to other electron microscopes with similar sample requirements, including but not limited to TEM.
The electron microscope observation sample and the preparation method thereof provided by the embodiment of the application comprise the following steps: providing a test specimen comprising a target sample layer; dividing a sample preparation area on the sample, and exposing the side wall of a target sample layer in the sample preparation area; forming a support frame, wherein the support frame at least covers the side wall of the target sample layer; thinning the test sample in the sample preparation area after the support frame is formed to obtain a target sample with preset thickness in the target sample layer; wherein the material hardness of the support frame is greater than the material hardness of the target sample layer. In the embodiment of the application, a material with hardness greater than that of the target sample layer is used as a frame material to provide support for the target sample, so that the deformation of the target sample in the thinning process is reduced.
The following describes the preparation method of the electron microscope observation sample provided in the embodiment of the present application in detail with reference to fig. 2. Fig. 2 is a schematic view of a second implementation flow chart of a method for preparing an electron microscope observation sample, provided in an embodiment of the present application, where the method mainly includes the following steps:
In the embodiment of the present application, a test sample including a target sample layer is provided, and it should be noted that the test sample may be a chip manufactured by an integrated circuit manufacturing process, and the test sample may include a dielectric layer, a semiconductor layer, a metal layer, and the like. The target sample layer may be made of a material with a relatively low hardness, such as aluminum or copper. When a certain area (target sample layer) in the test sample needs to be tested, a sample preparation area needs to be selected on the test sample. In the embodiment of the application, the sample preparation area is firstly divided to expose the side wall of the target sample layer; specifically, a groove surrounding the sample preparation region may be etched on the sample by an etching process to divide the sample preparation region. The specific process of etching the groove is as follows: and etching a groove surrounding the sample preparation area on the sample by using an FIB (focused ion beam) process, wherein the depth of the groove is more than or equal to the thickness from the surface of the sample to the bottom surface of the target sample layer, so that the side wall of the target sample layer is exposed.
In this application embodiment, the system appearance region needs to satisfy a predetermined pattern condition to make the lateral wall of the target sample layer that exposes adopt FIB technology to when the sample carries out the attenuate, arbitrary one on the lateral wall with FIB's projection direction is not parallel. It can be understood that, the sample preparation area is a preset pattern, and the top view of the sidewall of the target sample layer is also a preset pattern, that is, the shape surrounded by the sidewall of the target sample layer is the same as the shape of the sample preparation area, so that when the FIB process is used to thin the sample, any surface of the sidewall of the target sample layer is not parallel to the projection direction of the FIB, thereby greatly avoiding the curtain effect caused by the hardness difference between the support frame and the target sample layer during the thinning process. In some embodiments, an included angle between any one of the side walls of the target sample layer and the projection direction of the FIB is preferably greater than or equal to 5 degrees, so that a curtain effect in a thinning process can be better avoided, and the success rate of sample preparation is improved.
Wherein the preset graphics conditions include: the sample preparation area is a polygon, which may be a quadrangle, but in this embodiment, the polygon includes at least one side, and an included angle between the side and another side of the polygon is not a right angle, for example: 85 degrees or less or 95 degrees or more. For example, the polygon may be a parallelogram, and two included angles are formed between at least one side of the parallelogram and the other sides of the parallelogram, one included angle is less than or equal to 85 degrees, and the other included angle is greater than or equal to 95 degrees; for another example, the polygon may be a trapezoid, and then two included angles are formed between at least one side (upper bottom) of the trapezoid and the other sides of the trapezoid, where both the two included angles are greater than or equal to 95 degrees; two included angles are formed between at least one edge (lower bottom) of the trapezoid and other edges of the trapezoid, and the two included angles are both smaller than or equal to 85 degrees; two included angles are formed between at least one edge (inclined edge) of the trapezoid and other edges of the trapezoid, wherein one included angle is smaller than or equal to 85 degrees, and the other included angle is larger than or equal to 95 degrees; for example, the polygon may be non-quadrilateral, such as a pentagon, a hexagon, and other polygons, and an included angle formed between at least one side of the polygon and the other side of the polygon is 85 degrees or less or 95 degrees or more. Therefore, when the sample of the preset graph is thinned by adopting an FIB process, the FIB is projected along the direction perpendicular to the cutting edge based on the edge of the sample preparation area of the preset graph, and other edges of the sample preparation area of the preset graph except the cutting edge are not parallel to the projection direction of the FIB, namely any one surface on the side wall of the target sample layer is not parallel to the projection direction of the FIB. Thereby avoiding the curtain effect caused by the hardness difference between the support frame and the target sample layer in the thinning process to the utmost extent. In some embodiments, an included angle between any surface of the sidewall of the target sample layer and the projection direction of the FIB is preferably greater than or equal to 5 degrees, so that a curtain effect during thinning can be better avoided.
In the embodiment of the application, a frame material is deposited in the groove surrounding the sample preparation area through a FIB (focused ion beam) process to form a support frame, and the deposition thickness of the frame material is greater than or equal to the thickness of the target sample layer, so that the support frame is formed to at least cover the side wall of the target sample layer. Wherein the material hardness of the support frame is greater than the material hardness of the target sample layer. In practical applications, the material of the support frame may be tungsten or platinum, which has a relatively high hardness. In the embodiment of the application, a frame material with higher hardness is used as a supporting frame to support a target sample layer, so that the deformation condition caused by the fact that the material of the target sample is softer in the thinning process is reduced.
And step 203, cutting along the outer edge of the supporting frame to separate the sample in the sample preparation area with the supporting frame.
In the embodiment of the application, FIB process is used to cut along the outer edge of the support frame to separate the sample in the sample preparation area with the support frame.
And 204, thinning the test sample in the sample preparation area with the supporting frame to obtain a target sample with preset thickness in the target sample layer.
In the embodiment of the application, the FIB process is adopted to thin the sample separated from the sample preparation area with the supporting frame; wherein the FIB is projected to the support frame and the target sample layer along a direction perpendicular to the thickness direction of the test sample to cut off the test sample except the target sample with the preset thickness, so as to obtain the target sample with the preset thickness in the target sample layer. In practical application, the preset thickness is less than or equal to 100nm.
It should be noted that, when the FIB process is used to thin the sample in the sample preparation region with the support frame, any interface between the support frame and the target sample layer is not parallel to the projection direction of the FIB, and an included angle between any surface on the sidewall of the target sample layer and the projection direction of the FIB is preferably greater than or equal to 5 degrees. Therefore, the curtain effect caused by the hardness difference between the supporting frame and the target sample layer in the thinning process can be avoided to the great extent, and the success rate of sample preparation is greatly improved.
In embodiments of the present application, the target sample may be used for EBSD detection. The electron microscope may specifically be a SEM; it should be noted that the electron microscope observation sample and the preparation method thereof provided in the embodiments of the present application may also be applied to other electron microscopes with similar sample requirements, including but not limited to TEM.
The technical solution provided by the present embodiment is described in more detail below with reference to specific application scenarios.
Fig. 3 is a schematic structural diagram of an electron microscope observation sample provided in a specific example of the present application during a preparation process. In an embodiment of the present application, as shown in fig. 3, a test specimen is provided that includes a target sample layer that is located in an intermediate layer of the test specimen, the test specimen including three layers of material. When preparing an electron microscope observation sample, etching a groove surrounding the sample preparation area on the sample by using an FIB (focused ion beam) process to expose the side wall of a target sample layer in the sample preparation area, wherein the depth of the groove is required to be greater than or equal to the thickness from the surface of the sample to the bottom surface of the target sample layer in order to expose the side wall of the target sample layer in the sample preparation area. The groove surrounding the sample preparation area is a parallelogram, the groove divides the sample into two sub-areas, one sub-area is an area outside the groove, the other sub-area is an area inside the groove, and the shape of the sub-area (sample preparation area) inside the groove is also a parallelogram. Depositing a frame material in the groove surrounding the sample preparation area through an FIB process to form a parallelogram-shaped support frame, wherein the deposition thickness of the frame material is greater than or equal to the thickness of the target sample layer, so that the formed parallelogram-shaped support frame at least covers the side wall of the target sample layer. And cutting along the outer edge of the supporting frame by using an FIB (focused ion beam) process to separate the sample in the sample preparation area with the supporting frame. And finally, thinning the sample separated out from the sample preparation area with the supporting frame by adopting an FIB (focused ion beam) process, and projecting FIB (focused ion beam) to the supporting frame and the target sample layer along the direction perpendicular to the thickness direction of the sample so as to cut off the part of the sample except the target sample with the preset thickness, thereby obtaining the target sample with the supporting frame and positioned at the preset thickness in the target sample layer. The obtained target sample with the support frame can be used as an SEM (EBS D) detection sample or a TEM detection sample. Wherein the material hardness of the support frame is greater than the material hardness of the target sample layer. The embodiment of the application uses the higher frame material of hardness to provide the support as braced frame for the target sample layer to reduce the condition that target sample warp among the attenuate process, and optimize braced frame's shape into parallelogram in the embodiment of the application, thereby it is right to have braced frame when sample in the system appearance region carries out the attenuate, arbitrary interface between braced frame and the target sample layer with contained angle more than or equal to 5 degrees between the projection direction of FIB have avoided the curtain effect among the attenuate process from this, have greatly improved the success rate of sample preparation.
The embodiment of the application also provides an electron microscope observation sample prepared by adopting the method in any one of the embodiments. The following description will be given taking the support frame as a parallelogram as an example, and fig. 4 shows the prepared electron microscope observation sample; as shown, the electron microscopy observation of the sample includes: target sample 401, support frame 402; wherein the material hardness of the support frame 402 is greater than the material hardness of the target sample 401.
The embodiment of the present application further provides an electron microscope observation sample, including: a target sample; a support frame that encases the sidewalls of the target sample; wherein the material hardness of the support frame is greater than the material hardness of the target sample. The shape enclosed by the side walls of the target sample is a polygon, the polygon at least comprises one side, and the included angle between the side and the other sides of the polygon is not a right angle. The target sample is obtained by thinning by using an FIB (focused ion beam) process; wherein the target sample is obtained by thinning by using an FIB process; and the surface of the side wall of the target sample, on which the side is located, is used as a cutting surface when the FIB process is thinned, and the FIB is projected along the direction vertical to the cutting surface.
The above description is only for the specific embodiments of the present application, but the scope of the present application is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present application, and shall be covered by the scope of the present application. Therefore, the protection scope of the present application shall be subject to the protection scope of the claims.
It should be appreciated that reference throughout this specification to "one embodiment" or "an embodiment" means that a particular feature, structure or characteristic described in connection with the embodiment is included in at least one embodiment of the present application. Thus, the appearances of the phrases "in one embodiment" or "in an embodiment" in various places throughout this specification are not necessarily all referring to the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments. It should be understood that, in the various embodiments of the present application, the sequence numbers of the above-mentioned processes do not imply any order of execution, and the order of execution of the processes should be determined by their functions and inherent logic, and should not constitute any limitation to the implementation process of the embodiments of the present application. The above-mentioned serial numbers of the embodiments of the present application are merely for description and do not represent the merits of the embodiments.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrases "comprising a component of' 8230; \8230;" does not exclude the presence of another like element in a process, method, article, or apparatus that comprises the element.
In the several embodiments provided in the present application, it should be understood that the disclosed method and apparatus may be implemented in other manners. The above-described terminal embodiments are merely illustrative, for example, the division of the unit is only one logical function division, and there may be other division ways in actual implementation, such as: multiple units or components may be combined, or may be integrated into another system, or some features may be omitted, or not implemented. In addition, the coupling, direct coupling or communication connection between the components shown or discussed may be through some interfaces, and the indirect coupling or communication connection between the devices or units may be electrical, mechanical or in other forms.
The units described as separate parts may or may not be physically separate, and parts displayed as units may or may not be physical units, that is, may be located in one place, or may be distributed on a plurality of network units; some or all of the units can be selected according to actual needs to achieve the purpose of the solution of the embodiment.
In addition, all functional units in the embodiments of the present application may be integrated into one processing module, or each unit may be separately used as one unit, or two or more units may be integrated into one unit; the integrated unit may be implemented in the form of hardware, or in the form of hardware plus a software functional unit. Those of ordinary skill in the art will understand that: all or part of the steps for implementing the method embodiments may be implemented by hardware related to program instructions, and the program may be stored in a computer readable storage medium, and when executed, the program performs the steps including the method embodiments; and the aforementioned storage medium includes: a mobile storage device, a Read-Only Memory (ROM), a Random Access Memory (RAM), a magnetic disk or an optical disk, and various media capable of storing program codes.
The methods disclosed in the several method embodiments provided in the present application may be combined arbitrarily without conflict to obtain new method embodiments.
The features disclosed in the several product embodiments presented in this application can be combined arbitrarily, without conflict, to arrive at new product embodiments.
The features disclosed in the several method or apparatus embodiments provided herein may be combined in any combination to arrive at a new method or apparatus embodiment without conflict.
The above description is only for the specific embodiments of the present application, but the scope of the present application is not limited thereto, and any person skilled in the art can easily think of the changes or substitutions within the technical scope of the present application, and shall be covered by the scope of the present application. Therefore, the protection scope of the present application shall be subject to the protection scope of the claims.
Claims (4)
1. A method for preparing an electron microscope observation sample, the method comprising:
providing a test specimen comprising a target sample layer;
dividing a sample preparation area on the sample, and exposing the side wall of a target sample layer in the sample preparation area;
forming a support frame, wherein the support frame at least covers the side wall of the target sample layer;
thinning the test sample in the sample preparation area after the supporting frame is formed to obtain a target sample with a preset thickness in the target sample layer; thinning the sample and executing by using a focused ion beam FIB (focused ion beam) process;
the sample preparation area meets a preset pattern condition, so that the exposed side wall of the target sample layer meets the following conditions: when the sample is thinned by adopting an FIB process, the FIB is projected to the supporting frame and the target sample layer along a direction vertical to the thickness direction of the sample so as to cut off the part of the sample except the target sample with the preset thickness; an included angle between any surface of the side wall of the target sample layer and the projection direction of the FIB is more than or equal to 5 degrees; the sample preparation area is a polygon, the polygon at least comprises one side, and an included angle between the side and the other sides of the polygon is less than or equal to 85 degrees or greater than or equal to 95 degrees;
wherein the material hardness of the support frame is greater than the material hardness of the target sample layer.
2. The method of claim 1, wherein said segmenting a sample area on said test specimen, exposing sidewalls of a target sample layer within said sample area, comprises: etching a groove surrounding the sample preparation area on the sample, wherein the depth of the groove is more than or equal to the thickness from the surface of the sample to the bottom surface of the target sample layer, so that the side wall of the target sample layer is exposed;
said forming a support frame comprising: depositing a frame material in the groove, wherein the deposition thickness of the frame material is greater than or equal to the thickness of the target sample layer, so that the support frame is formed to at least cover the side wall of the target sample layer;
the method further comprises the following steps: and cutting along the outer edge of the supporting frame to separate the test sample in the sample preparation area with the supporting frame.
3. The method of claim 2,
at least one of the steps of etching a trench around the sample preparation area, depositing frame material in the trench, and cutting along the outer edge of the support frame is performed using a FIB process.
4. An electron microscopy specimen comprising:
a target sample; the target sample is obtained by thinning through an FIB (focused ion beam) process; the shape defined by the side walls of the target sample is a polygon, the polygon at least comprises one side, and the included angle between the side and the other sides of the polygon is less than or equal to 85 degrees or greater than or equal to 95 degrees; the surface of the side wall of the target sample, on which the edge is located, is used as a cutting surface when the FIB process is thinned, and the FIB is projected along a direction vertical to the cutting surface; an included angle between any one surface of the side wall of the target sample and the projection direction of the FIB is more than or equal to 5 degrees;
a support frame that encases the sidewalls of the target sample;
wherein the material hardness of the support frame is greater than the material hardness of the target sample.
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