CN113899765A - Electron microscopy three-dimensional reconstruction geological sample preparation method based on focused ion beam processing - Google Patents
Electron microscopy three-dimensional reconstruction geological sample preparation method based on focused ion beam processing Download PDFInfo
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- CN113899765A CN113899765A CN202111141302.7A CN202111141302A CN113899765A CN 113899765 A CN113899765 A CN 113899765A CN 202111141302 A CN202111141302 A CN 202111141302A CN 113899765 A CN113899765 A CN 113899765A
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N23/02—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 transmitting the radiation through the material
- G01N23/04—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 transmitting the radiation through the material and forming images of the material
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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
- 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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- 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
- G01N1/32—Polishing; Etching
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- 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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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- 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
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
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Abstract
The invention discloses an electron microscopic three-dimensional reconstruction geological sample preparation method based on focused ion beam processing, which relates to the technical field of geological industry detection, and comprises the following steps: s1, machining a geological target sample into a flat and smooth surface by adopting mechanical cutting; s2, depositing a protective layer on the region of interest, wherein the thickness of the deposited protective layer is 2-4 μm; s3, extracting a region of interest sample, and welding the extracted sample to a grid for a transmission electron microscope; and S4, processing the extracted sample into a needle shape by using a focused ion beam until the extracted sample is processed to a thickness which is penetrable by an electron beam, and then obtaining the sample which can be subjected to three-dimensional reconstruction data acquisition under a transmission electron microscope. The geological sample preparation method provided by the invention can realize 360-degree full-angle electron microscopy three-dimensional reconstruction data acquisition, and wedge-shaped data loss caused by the shape limitation of the sample can be avoided.
Description
Technical Field
The invention relates to a sample preparation method for an electron microscopic three-dimensional reconstruction geological sample, in particular to a sample preparation method for an electron microscopic three-dimensional reconstruction geological sample based on focused ion beam processing.
Background
Natural geological samples have the characteristic of complex micro-texture. Distribution characteristics of the internal microstructure of the sample in a three-dimensional space can be obtained through three-dimensional texture analysis of the geological sample, geological cause information is visually provided, and important basic data are provided for geological research.
The three-dimensional reconstruction technology can synthesize a three-dimensional image by using a series of two-dimensional images in a specific direction; the transmission electron microscope can be used for taking micrographs of samples with different tilting angles and then carrying out three-dimensional reconstruction. Because the penetration ability of electrons is weak, the sample preparation method for transmission electron microscope observation is generally performed in a manner of a sheet, and particularly, for a solid sample such as natural minerals and meteorites, a larger thin area needs to be pursued, for example, chinese patent application cn201610515722.x discloses a preparation method of a large-area thin area transmission electron microscope sample. However, the samples obtained by the conventional sheet sample preparation have certain limitation on the angle of acquisition of electron microscopic three-dimensional reconstruction data, 360-degree full-angle data cannot be obtained, wedge-shaped data loss is generated, and the reconstruction result has certain deviation from a real structure. For this reason, it is necessary to design a sample preparation method capable of realizing 360 ° full-angle electron microscopy three-dimensional reconstruction data acquisition to address this drawback.
Disclosure of Invention
The invention aims to provide a sample preparation method capable of realizing 360-degree full-angle electron microscopy three-dimensional reconstruction data acquisition, and the sample prepared by the method can realize 360-degree full-angle electron microscopy three-dimensional reconstruction data acquisition without wedge-shaped data loss caused by the shape limitation of the sample.
In order to achieve the purpose, the invention provides the following technical scheme: an electron microscopy three-dimensional reconstruction geological sample preparation method based on focused ion beam processing comprises the following steps:
s1, machining a geological target sample into a flat and smooth surface by adopting mechanical cutting;
s2, depositing a protective layer on the region of interest, wherein the thickness of the deposited protective layer is 2-4 μm, and then extracting a region of interest sample by using focused ion beam cutting and matching with a nanometer manipulator;
s3, welding the extracted region of interest sample to a grid for a transmission electron microscope;
and S4, processing the region of interest into a needle shape by using a focused ion beam until the region of interest is processed to a thickness which is penetrable by an electron beam, and then obtaining a sample which can be subjected to three-dimensional reconstruction data acquisition under a transmission electron microscope.
As a preferable technical scheme of the invention, the geological target samples are all solid geological samples which can be observed under a transmission electron microscope.
As a preferable technical scheme, the geological sample preparation method is suitable for a double-beam scanning electron microscope system with a focused ion beam and an electron beam.
As a preferred embodiment of the present invention, the region of interest processed by the focused ion beam in step S4 is needle-shaped, and specifically, the processing is performed by a ring-shaped ion beam scanning manner.
As a preferred embodiment of the present invention, the region of interest is processed into a needle shape by the focused ion beam in the step S4 until the thickness through which the electron beam can penetrate is processed, specifically, the tip of the pointer is scaled and the scale is nanometer scale, and the scale is usually 50-200 nm.
As a preferable technical scheme of the invention, the needle-tip-shaped end dimension is preferably 50-80 nm.
Compared with the prior art, the invention has the beneficial effects that:
according to the geological sample preparation method, the protective layer is deposited on the region of interest, the region of interest sample is extracted, the extracted region of interest sample is welded to the grid for the transmission electron microscope, the region of interest is processed into a needle shape by using a focused ion beam until the thickness of the region of interest is equal to the thickness of the region of interest sample which can be penetrated by an electron beam, and then the sample capable of carrying out three-dimensional reconstruction data acquisition under the transmission electron microscope is obtained, so that the geological sample preparation method capable of realizing 360-degree full-angle electron microscope three-dimensional reconstruction data acquisition is provided, and wedge-shaped data loss cannot be generated due to the shape limitation of the sample.
Drawings
FIG. 1 is a TEM image of a needle-like sample prepared by the method of the present invention;
FIG. 2 is a three-dimensional image of a needle-shaped sample reconstructed by a weighted back projection (weighted back projection) algorithm according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-2, the present invention provides a method for preparing a geological sample by electron microscopy three-dimensional reconstruction based on focused ion beam processing, which comprises the following steps:
s1, machining a geological target sample into a flat and smooth surface by adopting mechanical cutting;
s2, depositing a protective layer on the region of interest, wherein the thickness of the deposited protective layer is 2-4 mu m, and then extracting a region of interest sample by using focused ion beam cutting and matching with a nanometer manipulator;
s3, welding the extracted region of interest sample to a grid for a transmission electron microscope;
and S4, processing the region of interest into a needle shape by using a focused ion beam until the region of interest is processed to a thickness which is penetrable by an electron beam, and then obtaining a sample which can be subjected to three-dimensional reconstruction data acquisition under a transmission electron microscope.
The geological target samples are all solid geological samples which can be observed under a transmission electron microscope.
The geological sample preparation method is suitable for a double-beam scanning electron microscope system with a focused ion beam and an electron beam.
The processing of the region of interest with the focused ion beam in the step S4 is needle-shaped, specifically, the processing is performed in a manner of annular ion beam scanning.
The region of interest is machined with a focused ion beam into a needle shape as described in step S4 until the thickness is reached where the electron beam is transparent, specifically on the scale of the tip of the pointer, and on the scale of nanometers, and typically on the scale of 50-200 nm.
The tip-like end dimension is preferably 50-80 nm.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. A method for preparing a geological sample by electron microscopic three-dimensional reconstruction based on focused ion beam processing is characterized by comprising the following steps: the method comprises the following steps:
s1, machining a geological target sample into a flat and smooth surface by adopting mechanical cutting;
s2, depositing a protective layer on the region of interest, wherein the thickness of the deposited protective layer is 2-4 mu m, and then extracting a region of interest sample by using focused ion beam cutting and matching with a nanometer manipulator;
s3, welding the extracted region of interest sample to a grid for a transmission electron microscope;
and S4, processing the region of interest into a needle shape by using a focused ion beam until the region of interest is processed to a thickness which is penetrable by an electron beam, and then obtaining a sample which can be subjected to three-dimensional reconstruction data acquisition under a transmission electron microscope.
2. The electron microscopy three-dimensional reconstruction geological sample preparation method based on focused ion beam processing as claimed in claim 1, characterized in that: the geological target samples are all solid geological samples which can be observed under a transmission electron microscope.
3. The electron microscopy three-dimensional reconstruction geological sample preparation method based on focused ion beam processing as claimed in claim 1, characterized in that: the geological sample preparation method is suitable for a double-beam scanning electron microscope system with a focused ion beam and an electron beam.
4. The electron microscopy three-dimensional reconstruction geological sample preparation method based on focused ion beam processing as claimed in claim 1, characterized in that: the region of interest processed by the focused ion beam in the step S4 is needle-shaped, and is specifically processed by a ring-shaped ion beam scanning method.
5. The electron microscopy three-dimensional reconstruction geological sample preparation method based on focused ion beam processing as claimed in claim 1, characterized in that: the region of interest is machined with a focused ion beam into a needle shape as described in step S4 until the electron beam is machined to a thickness that is transparent to the electron beam, specifically on the scale of the tip of the needle, and on the scale of nanometers, and typically on the scale of 50-200 nm.
6. The electron microscopy three-dimensional reconstruction geological sample preparation method based on focused ion beam processing as claimed in claim 5, characterized in that: the tip-like end dimension is preferably 50-80 nm.
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| CN202111141302.7A CN113899765A (en) | 2021-09-27 | 2021-09-27 | Electron microscopy three-dimensional reconstruction geological sample preparation method based on focused ion beam processing |
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| CN202111141302.7A CN113899765A (en) | 2021-09-27 | 2021-09-27 | Electron microscopy three-dimensional reconstruction geological sample preparation method based on focused ion beam processing |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114518378A (en) * | 2022-01-14 | 2022-05-20 | 中国矿业大学 | Method for improving conductivity of sample in FIB-SEM three-dimensional reconstruction process |
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| JP2012002552A (en) * | 2010-06-15 | 2012-01-05 | National Institute Of Advanced Industrial & Technology | Method of manufacturing sample for electron microscope |
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| CN114518378B (en) * | 2022-01-14 | 2024-09-24 | 中国矿业大学 | Method for improving conductivity of sample in FIB-SEM three-dimensional reconstruction process |
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