CN111537533B - Preparation method of spherical aberration correction TEM sample of spinel micron particles - Google Patents
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Abstract
The invention discloses a preparation method of a spherical aberration correction TEM sample of spinel microparticles, which belongs to the technical field of material processing and is characterized by comprising the following steps: s1, preparing samples and screening particles, wherein the sample preparation process comprises the following steps: firstly, preparing a silicon wafer with the length of 1cm multiplied by 1cm, dipping a proper amount of powder sample by using a toothpick or a cotton swab, and rubbing the powder sample on the silicon wafer; then intermittently blowing 5-10 times by using a high-pressure nitrogen gun; finally, fixing the silicon wafer on a sample stage by using a double-sided carbon tape; the particle screening process comprises the following steps: firstly, after sample injection, a sample stage is moved, and individual particles which are free of abrasion and have cross sections to be observed perpendicular to the surface of a silicon wafer are searched under SEM; then, by rotating the sample stage, the cross-sectional direction of the particles to be extracted is flattened; s2, depositing a pt protective layer; s3, digging a large groove; s4, U-shaped cutting, S5, extracting slices; s6, lofting; s7, thinning and low-voltage cleaning.
Description
Technical Field
The invention belongs to the technical field of material processing, and particularly relates to a preparation method of a spherical aberration correction TEM sample of spinel microparticles.
Background
Transmission Electron Microscopy (TEM) is one of the very important characterization means in the scientific research fields of materials, physics, chemistry, biology, etc., which can characterize the microstructure of materials. With the development of transmission electron microscopy technology, an spherical aberration correcting transmission electron microscope (spherical aberration TEM) equipped with an spherical aberration corrector can observe the atomic structure of the material. The preparation quality of the TEM sample plays a key role on the TEM characterization result. The focused ion beam scanning electron microscope (FIB-SEM) is a dual-beam system with a focusing ion beam lens barrel added on the basis of the SEM, is provided with accessories such as a nanometer manipulator, a gas injection system and the like, has high-precision processing capability and high-resolution imaging capability, and can be used for rapidly preparing TEM samples. Compared with an ion thinning method, an electrolytic double-spraying method and an ultrathin section method, the FIB-SEM has unique advantages in preparing a TEM sample, and can be used for preparing a TEM sample with a specific position and a specific orientation; the damage to the original sample is small; the sample preparation time is short; in situ heating, powering up, stretching a TEM sample may be prepared.
The traditional method of preparing high resolution TEM samples based on FIB is the U-cut method. As shown in fig. 1, the steps are mainly divided into six steps: a. depositing a pt protective layer, namely ion beam assisted deposition of a pt protective layer of 10 μm×2 μm×1 μm in a target area; b. digging large grooves, namely digging large grooves on two sides of a target area to obtain a thin sheet with the thickness of about 1 micrometer; c.U, i.e. U-shaped cutting the sheet, completely cutting the bottom and one end of the sheet while leaving a portion of the other end; d. the extraction is that the nano manipulator is slowly lowered to lightly contact one end of the slice in the air, then the deposition pt firmly welds the slice and the nano manipulator, then the other end of the slice is cut off, and then the nano manipulator is slowly lifted to lift the slice; e. setting out, namely moving a sample table to enable a copper net to move to the center of a visual field, lowering the nano manipulator welded with the sheet sample again to be in contact with the side face of a column on the copper net, depositing pt to firmly weld the sheet and the column on the copper net, cutting off one end of the sheet connected with the nano manipulator, and removing the nano manipulator to finish the transfer of the sheet; f. thinning and low-voltage cleaning, namely firstly thinning the sheet to about 150nm by using an ion beam with 30kv accelerating voltage, and then cleaning and thinning the sheet to about 50nm by using 5kv accelerating voltage.
Spinel particles are polyhedral particles, the length of diagonal vertexes is between 500nm and 2um, and a cross-section spherical aberration TEM sample penetrating through a vertex angle platform needs to be manufactured to observe the atomic structure of the sample. The preparation difficulty of the sample mainly comprises the following points: the particle size is small, and the manipulator cannot extract one particle alone; the particle apex angle plateau size is small (100 nm-200 nm), and the thinning process needs to be precisely controlled, so that the final thin region remains in the plateau range.
Disclosure of Invention
The invention provides a preparation method of a spherical aberration correction TEM sample of spinel micron particles, which is technically improved on the basis of a traditional U-cut method, wherein particles are prepared on a silicon substrate slice, electron beam assisted deposition Pt is adopted before ion beam assisted deposition Pt, the total thickness of the deposited Pt is thicker, and the method comprises the steps of accurate thinning, step-by-step cleaning and the like, so that a high-quality spinel spherical aberration TEM sample is successfully prepared.
The invention aims to provide a preparation method of a spherical aberration correction TEM sample of spinel microparticles, wherein the length range between diagonal vertexes of the particles is 500 nm-2 um; the method comprises the following steps:
s1, preparing samples and screening particles, wherein the preparation method comprises the following steps:
sample preparation: firstly, preparing a silicon wafer with the length of 1cm multiplied by 1cm, dipping a proper amount of powder sample by using a toothpick or a cotton swab, and rubbing the powder sample on the silicon wafer; then intermittently blowing 5-10 times by using a high-pressure nitrogen gun; finally, fixing the silicon wafer on a sample stage by using a double-sided carbon tape;
the particle screening process comprises the following steps: firstly, after sample injection, a sample stage is moved, and individual particles which are in a regular octahedron shape, have no abrasion and have a section to be observed vertical to the surface of a silicon wafer are searched under an SEM; then, by rotating the sample stage, the cross-sectional direction of the particles to be extracted is flattened;
s2, depositing a pt protective layer; the method comprises the following steps:
firstly, carrying out electron beam assisted Pt deposition in a target area, and then carrying out ion beam assisted Pt deposition to fill gaps between particles and a substrate; the total thickness of the electron beam and ion beam assisted deposition Pt is 1-2 microns.
S3, digging large grooves, namely digging the large grooves on two sides of the target area to obtain a thin sheet with the thickness ranging from 1um to 1.5 um;
s4, U-shaped cutting, namely, U-shaped cutting is carried out on the thin sheet, the bottom and one end of the thin sheet are completely cut off, and a part of the other end is left;
s5, extracting, namely lowering the nano manipulator to enable the nano manipulator to contact one end of the thin sheet in the air, depositing pt to weld the thin sheet and the nano manipulator, cutting off the other end of the thin sheet, raising the nano manipulator, and lifting the thin sheet;
s6, lofting, namely moving a sample table to enable the copper net to move to the center of a visual field, lowering the nano manipulator welded with the sheet sample again to be in contact with the side face of the column on the copper net, depositing pt to firmly weld the sheet and the column on the copper net, cutting off one end of the sheet connected with the nano manipulator, and removing the nano manipulator to finish the transfer of the sheet;
s7, thinning and low-voltage cleaning, namely firstly thinning a sheet to 140-160 nm by using an ion beam with 30kv accelerating voltage, then cleaning and thinning the sheet to 40-60 nm by using 5kv accelerating voltage, and finally cleaning and thinning the sheet to 20-40 nm by using 2kv accelerating voltage, wherein the steps are as follows:
and (3) thinning: firstly, thinning one observable side of an SEM, firstly, thinning the observable side by using conditions of 30kv and 700pA, when the section of particles can be seen, continuously thinning by changing the beam current of 30kv and 50pA, observing and measuring the top edge length of a front cutting surface in real time, stopping immediately when the length W=w1, wherein W1 is the top edge length of the front cutting surface when the middle position of a thin area with the thickness of 150nm remained after sample thinning is consistent with the middle position of a top angle platform (target area); then thinning the other side until the sample thin area is transparent under the SEM acceleration voltage of 5kv and the secondary electron probe in the sample chamber, wherein the thickness of the sample thin area is 140-160 nm, and the middle position of the thin area in the thickness direction is basically consistent with the middle position of the vertex angle platform (target area);
the low-voltage cleaning process comprises the following steps: firstly, under the conditions that the acceleration voltage and beam current of an ion beam are 5kv and 10pA, alternately and symmetrically processing samples on the front side and the rear side, and gradually reducing the cleaning time of each side until a thin area of the sample is transparent under the SEM acceleration voltage of 3kv and a secondary electron probe in the sample chamber, wherein the thickness of the thin area is 40-60 nm; then the ion beam voltage and beam current are switched to 2kv and 10pA, the sample is continuously and symmetrically processed in an alternating mode, and the cleaning time of each side is reduced step by step until the thin area of the sample is transparent under the SEM acceleration voltage of 2kv and the secondary electron probe, and the thickness of the thin area is 20-40 nm.
Further, s2 is a pt protective layer of 10 μm×2 μm×x μm, which is in the range of 1 to 2, which is electron beam and ion beam assisted deposition in the target region.
Further, the final thin region of the sheet has a thickness of 20 to 40nm. .
The invention has the advantages and positive effects that:
the invention is technically improved on the basis of the traditional U-cut method, mainly comprises the steps of preparing particles on a silicon substrate slice, adopting electron beam assisted deposition Pt before ion beam assisted deposition Pt, and adopting measures such as thicker total thickness of the deposited Pt, accurate thinning, step-by-step cleaning and the like to successfully prepare a high-quality spinel spherical aberration TEM sample; the spherical TEM samples prepared were very thin and had few damaged layers.
Drawings
FIG. 1 is a schematic flow chart of a TEM sample prepared by a conventional U-cut method;
FIG. 2 is a schematic representation of the correspondence of the front cutting surface of the present invention in plan and cross-sectional views;
fig. 3 is an SEM image of spinel particles of the present invention at sample stage tilt angles t=0° (a) and 54 ° (b);
FIG. 4 is an SEM image of the present invention after cutting has stopped at a front section (a) and a rear section (b);
FIG. 5 is an SEM image after low voltage cleaning of the present invention;
fig. 6 is an image of HAADF at atomic resolution of a cross-section of an experimental spinel particle after application of the teachings of the present invention.
Detailed Description
For a further understanding of the invention, its features and advantages, reference is now made to the following examples, which are illustrated in the accompanying drawings in which:
referring to fig. 2 to 6, a method for preparing a spherical aberration correcting TEM sample of spinel microparticles, comprises:
s1, preparing samples and screening particles;
the traditional U-cut sample preparation method can be used for preparing a block body, a film sample or a large-size powder sample (the single particle is larger than 10 mu m), no special treatment is needed in the sample preparation process, and the sample is directly fixed on a sample table by using a double-sided carbon tape. However, for this spinel powder sample, the length between the diagonal vertices of the particles is between 500nm and 2um, the size is too small and the nanomachining arm cannot extract one particle alone, the improvement here is to disperse the particles onto the substrate sheet and extract the particles together with a portion of the substrate sheet at the time of extraction. First, a clean silicon wafer of 1 cm. Times.1 cm was prepared. A proper amount of powder sample is dipped by a toothpick or a cotton swab and is rubbed on the silicon wafer, and then the silicon wafer is intermittently blown for 5 to 10 times by a high-pressure nitrogen gun, so that the residual particles can be firmly and electrostatically adsorbed on the surface of the silicon wafer. And finally, fixing the silicon wafer on a sample stage by using a double-sided carbon tape.
Compared with the traditional U-cut sample preparation method, the preparation of the spinel TEM sample has strict requirements and special treatment on the selection of target areas (particles). First, after sample introduction, the sample stage was moved and individual, abrasion-free particles were found under SEM with the cross section to be observed perpendicular to the wafer surface. Then, by rotating the sample stage, the cross-sectional direction of the particles to be extracted is flattened. Fig. 2 is a schematic diagram of the correspondence between the front side cutting surface (front cutting surface) in the particle thinning process in a plan view and a cross-sectional view, W is the top edge length of the front cutting surface, and W1 is the top edge length of the front cutting surface when the middle position of the remaining 150nm thick thin area in the thickness direction after sample thinning is consistent with the middle position of the particle vertex angle platform. In order to facilitate the judgment of the thinning position in the later thinning process, it is necessary to photograph the particles at the sample stage inclination angles t=0° and 54 ° (as shown in fig. 3), respectively, and measure the w1 length;
s2, depositing a pt protective layer;
the purpose of depositing the Pt protective layer is to protect the sample from damage by the ion beam during the final thinning. There are mainly two improvements in this step. First, since the subsequent TEM experiments require characterization of atomic structures in a region a few nanometers deep from the particle surface, and ion beam assisted deposition of Pt damages a region about 30nm deep from the sample surface, electron beam assisted deposition of Pt is performed before ion beam assisted deposition of Pt, which damages less than 5nm to the sample surface. Secondly, because there is a large gap between the particles and the substrate, which becomes larger and larger with the subsequent thinning process, resulting in the risk of cracking and flaking of the final TEM sample, it is desirable to deposit Pt thicker than in the conventional U-cut sample preparation method to fill the gap as much as possible. The total thickness of the electron beam and ion beam assisted deposition Pt is 1-2 microns.
S3, digging large grooves, namely digging the large grooves on two sides of the target area to obtain a thin sheet with the thickness ranging from 1um to 1.5 um;
s4, U-shaped cutting, namely, U-shaped cutting is carried out on the thin sheet, the bottom and one end of the thin sheet are completely cut off, and a part of the other end is left;
s5, extracting, namely lowering the nano manipulator to enable the nano manipulator to contact one end of the thin sheet in the air, depositing pt to weld the thin sheet and the nano manipulator, cutting off the other end of the thin sheet, raising the nano manipulator, and lifting the thin sheet;
s6, lofting, namely moving a sample table to enable the copper net to move to the center of a visual field, lowering the nano manipulator welded with the sheet sample again to be in contact with the side face of the column on the copper net, depositing pt to firmly weld the sheet and the column on the copper net, cutting off one end of the sheet connected with the nano manipulator, and removing the nano manipulator to finish the transfer of the sheet;
s7, thinning and low-voltage cleaning; firstly, thinning a sheet to 140-160 nm by using an ion beam with 30kv accelerating voltage, then cleaning and thinning the sheet to 40-60 nm by using 5kv accelerating voltage, and finally cleaning and thinning the sheet to 20-40 nm by using 2kv accelerating voltage;
the traditional U-cut sample preparation method only needs to thin at two sides alternately in the thinning stage, the thickness of the final thin area is controlled, and whether the position to be observed is in the range of the final thin area or not does not need to be concerned, because the whole area covered by Pt is a target area for the samples. Whereas for the spinel particle TEM sample preparation herein, the final thin zone needs to be controlled within the range of the particle apex angle plateau, i.e. the target area is the apex angle plateau of the particle. In this stage, a precise thinning method is proposed. The SEM can be thinned first on the side (pre-cut surface) observed, thinned with 30kv 700pa, and when the cross section of the particle can be seen, the thinning is continued with a beam change of 30kv 50pa, and the top edge length of the pre-cut surface is observed and measured in real time, stopping immediately when its length w=w1, as shown in fig. 4 a. And then the other side (rear cutting surface) is thinned until the thin sample area is transparent under the SEM acceleration voltage of 5kv and the secondary electron probe in the sample chamber (as shown in figure 4 b), wherein the thickness of the thin sample area is about 140-160 nm, and the middle position of the thin sample area in the thickness direction is basically consistent with the middle position of the platform.
The low voltage cleaning stage plays a very critical role for the quality of the TEM sample. The spherical TEM sample is required to be thinner and have fewer damaged layers than the HRTEM sample, and the amount of the damaged layers is influenced by the accelerating voltage, so that the thinner the sample is, the less resistant to ion beam bombardment, and a step-by-step cleaning method is required. Firstly, under the condition that the acceleration voltage and beam current of the ion beam are 5kv10pA, the sample is alternately and symmetrically processed on the front side and the rear side, and the cleaning time of each side is gradually reduced until a thin area of the sample is transparent under the SEM acceleration voltage of 3kv and a secondary electron probe in the sample chamber, and the thickness of the thin area is 40-60 nm. Then the ion beam voltage and beam current are switched to 2kv10pA, the sample is continuously processed in an alternating and symmetrical mode, and the cleaning time of each side is reduced step by step until the thin area of the sample is transparent under the SEM acceleration voltage of 2kv and the secondary electron probe, and the thickness of the thin area is 20-40 nm at the moment, as shown in figure 5.
Fig. 6 is a HAADF image of a prepared sample using STEM mode photography of a spherical TEM, model JEOL JEM-ARM300F, in which a clear atomic image is seen and the scale is uniform. This indicates that the prepared spherical aberration TEM samples were very thin and had few damaged layers.
The above-described embodiments are only for illustrating the technical spirit and features of the present invention, and it is intended to enable those skilled in the art to understand the content of the present invention and to implement it accordingly, and the scope of the present invention is not limited to the embodiments, i.e. equivalent changes or modifications to the spirit of the present invention are still within the scope of the present invention.
Claims (3)
1. A preparation method of a spherical aberration correction TEM sample of spinel micron particles, wherein the length range between diagonal peaks of the particles is 500 nm-2 um; the method is characterized by comprising at least the following steps:
s1, preparing samples and screening particles, wherein the method comprises the following steps:
sample preparation: firstly, preparing a silicon wafer with the length of 1cm multiplied by 1cm, dipping a proper amount of powder sample by using a toothpick or a cotton swab, and rubbing the powder sample on the silicon wafer; then intermittently blowing 5-10 times by using a high-pressure nitrogen gun; finally, fixing the silicon wafer on a sample stage by using a double-sided carbon tape;
the particle screening process comprises the following steps: firstly, after sample injection, a sample stage is moved, and individual particles which are free of abrasion and have cross sections to be observed perpendicular to the surface of a silicon wafer are searched under SEM; then, by rotating the sample stage, the cross-sectional direction of the particles to be extracted is flattened;
s2, depositing a pt protective layer; the method comprises the following steps:
firstly, carrying out electron beam assisted Pt deposition in a target area, and then carrying out ion beam assisted Pt deposition to fill gaps between particles and a substrate; the total thickness of the electron beam and ion beam assisted deposition Pt is 1-2 microns;
s3, digging large grooves, namely digging the large grooves on two sides of the target area to obtain a thin sheet with the thickness ranging from 1um to 1.5 um;
s4, U-shaped cutting, namely, U-shaped cutting is carried out on the thin sheet, the bottom and one end of the thin sheet are completely cut off, and a part of the other end is left;
s5, extracting, namely lowering the nano manipulator to enable the nano manipulator to contact one end of the thin sheet in the air, depositing pt to weld the thin sheet and the nano manipulator, cutting off the other end of the thin sheet, raising the nano manipulator, and lifting the thin sheet;
s6, lofting, namely moving a sample table to enable the copper net to move to the center of a visual field, lowering the nano manipulator welded with the sheet sample again to be in contact with the side face of the column on the copper net, depositing pt to firmly weld the sheet and the column on the copper net, cutting off one end of the sheet connected with the nano manipulator, and removing the nano manipulator to finish the transfer of the sheet;
s7, thinning and low-voltage cleaning, namely firstly thinning the sheet to 140-160 nm by using an ion beam with 30kv accelerating voltage, then cleaning and thinning the sheet to 40-60 nm by using 5kv accelerating voltage, and finally cleaning and thinning the sheet to 20-40 nm by using 2kv accelerating voltage, wherein the method specifically comprises the following steps:
and (3) thinning: firstly, thinning one observable side of an SEM, firstly, thinning the observable side by using conditions of 30kv and 700pA, when the section of the particle can be seen, continuously thinning by changing the beam current of 30kv and 50pA, observing and measuring the top edge length of a front cutting surface in real time, stopping immediately when the length W=w1, wherein W1 is the top edge length of the front cutting surface when the middle position of a thin area with the thickness of 150nm remained after sample thinning is consistent with the middle position of a target area in the thickness direction; then thinning the other side until the sample thin area is transparent under the SEM acceleration voltage of 5kv and the secondary electron probe in the sample chamber, wherein the thickness of the sample thin area is 140-160 nm, and the middle position of the thin area in the thickness direction is basically consistent with the middle position of the target area;
the low-voltage cleaning process comprises the following steps: firstly, under the conditions that the acceleration voltage and beam current of an ion beam are 5kv and 10pA, alternately and symmetrically processing samples on the front side and the rear side, and gradually reducing the cleaning time of each side until a thin area of the sample is transparent under the SEM acceleration voltage of 3kv and a secondary electron probe in the sample chamber, wherein the thickness of the thin area is 40-60 nm; then the ion beam voltage and beam current are switched to 2kv and 10pA, the sample is continuously and symmetrically processed in an alternating mode, and the cleaning time of each side is reduced step by step until the thin area of the sample is transparent under the SEM acceleration voltage of 2kv and the secondary electron probe, and the thickness of the thin area is 20-40 nm.
2. The method for preparing a spherical aberration correcting TEM sample of spinel microparticles according to claim 1 wherein s2 is a pt protective layer deposited at 10 μm X2 μm X μm with the assistance of electron and ion beams in the target zone; the above range of X is 1 to 2.
3. The method for preparing a spherical aberration correcting TEM sample of spinel microparticles according to claim 2 wherein the final thin zone thickness of the flakes is 20-40 nm.
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