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Sample transfer method of chip type in-situ transmission electron microscope

A technology for sample transfer and transmission electron microscopy, which is used in material analysis, measurement devices, instruments, etc. using wave/particle radiation, which can solve the limitations of chip-type in-situ transmission electron microscopy. question

Active Publication Date: 2021-09-03
INST OF PHYSICS - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since the transfer of micron-scale samples is a key technical difficulty and bottleneck, this limits the wide application of chip-based in situ TEM research.
That is to say, traditional sample transfer methods cannot transfer micron-scale large particle materials according to specific crystallographic directions, so a new sample transfer method needs to be invented for on-chip in situ TEM research

Method used

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  • Sample transfer method of chip type in-situ transmission electron microscope
  • Sample transfer method of chip type in-situ transmission electron microscope
  • Sample transfer method of chip type in-situ transmission electron microscope

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] This example is used to illustrate the method for micron-sized particles with thinner sample edges in the examples of the present application.

[0064] First, lithium cobalt oxide LiCoO with thinner edges was 2 The (LCO) particle sample was dispersed into a suspension, and a dropper was used to drop 2 drops of the suspension on the electron microscope microgrid with coordinates. After drying in an oven or naturally drying, the microgrid sample was put into the TEM. Randomly select one of the particle samples, and observe the thinner part of the sample edge, and use the diffraction technique to measure the α and β deflection angles of the crystal zone axis of the sample relative to the actual observation direction. Select the particle samples several times until a particle sample is found, and the deviation angle of the crystal zone axis to be observed relative to the actual observation direction is within the allowable range (α image 3 As shown in (a), record the coordi...

Embodiment 2

[0066] This example is used to illustrate the method for micron-sized particles with thicker sample edges in the examples of the present application.

[0067] First, use ethanol solvent to disperse the LCO particle sample with thicker edges into a suspension, use a dropper to drop 2 drops of the suspension on the microgrid of an ordinary electron microscope, dry it in an oven or dry it naturally, then put the microgrid sample into a focused ion beam instrument (FIB). like Figure 4 As shown in (a,b), the sample is selected according to the shape characteristics, the sample is transferred to the FIB special carrier net by the micro-nano processing manipulator, and a small part of the sample is thinned by the ion beam. Put the grid sample into a transmission electron microscope (TEM), observe the thinned part of the sample, and use the diffraction technique to measure the deflection angle of the sample crystal band axis relative to the actual observation direction as α=12.4° an...

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Abstract

The invention discloses a sample transfer method of a chip type in-situ transmission electron microscope. The sample transfer comprises the following steps of: dispersing a particle sample into suspension liquid by utilizing a solvent, dripping a plurality of drops of suspension liquid on a micro-grid of the electron microscope, and drying to obtain a micro-grid sample; putting the micro-grid sample into a focused ion beam (FIB) instrument, selecting the sample and transferring the sample to a special grid of the FIB instrument , and thinning a part of the sample by using an ion beam to obtain a grid sample; putting the grid sample into the transmission electron microscope (TEM), observing the thinned part in the grid sample, and measuring deflection angles alpha and beta of a crystal belt axis of the grid sample relative to an actual observation direction; taking out the grid sample from the TEM, and adjusting the in-plane rotation angle of the grid relative to the sample rod of the transmission electron microscope so as to make the crystal belt axis of the grid sample rotates along with the grid sample until only the deflection angle alpha is left relative to the optical axis of the TEM; and transferring the grid sample into the FIB instrument, and transferring the grid sample to a specified position of an in-situ chip by utilizing the tilting compensation deflection angle alpha of the sample table.

Description

technical field [0001] The present application generally relates to the field of transmission electron microscopy under the field of condensed matter physics and materials, and specifically relates to a sample transfer method for a chip-type in-situ transmission electron microscope. Background technique [0002] In-situ transmission electron microscopy (in-situ TEM analysis) can observe the structural evolution process of the sample in situ and in real time at the atomic scale, and has been obtained in the fields of condensed matter physics, inorganic materials science, catalysis, and electrochemistry. a wide range of applications. Micro-electromechanical systems (MEMS)-based in-situ TEM research has the advantages of high mechanical stability, high measurement accuracy, and versatility, and is one of the main research methods in the field of in-situ TEM research. [0003] The principle of chip-type in-situ TEM research is to use a special in-situ chip (in-situ chip) to loa...

Claims

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Application Information

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IPC IPC(8): G01N23/20025G01N23/20008
CPCG01N23/20025G01N23/20008
Inventor 刘效治张庆华时金安谷林
Owner INST OF PHYSICS - CHINESE ACAD OF SCI