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A kind of preparation method of transmission electron microscope sample

A technology for transmission electron microscope samples and samples, which is applied in the preparation of test samples and other directions, can solve the problems of increasing sample preparation cost and time-consuming, and achieves the effects of high cost, long time-consuming and reducing preparation cost.

Active Publication Date: 2019-09-20
SHANGHAI DOESUN ENERGY TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the film layer is very thick, in order to cut off the bottom (depth direction), the width of the two side incisions at the sampling place is much larger, and the depth is also deeper than the film thickness, so it takes a long time, which significantly increases the sample preparation. cost

Method used

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  • A kind of preparation method of transmission electron microscope sample
  • A kind of preparation method of transmission electron microscope sample
  • A kind of preparation method of transmission electron microscope sample

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Sample: 4 micron GaN film epitaxially grown on the c-axis of sapphire, observe the cross section of the sample.

[0031] Sample preparation steps for TEM section:

[0032] In the preparatory work, the sample is divided into two similar 1x3mm rectangles by wire cutting, and the 3mm side is 11-20 direction. Two rectangular film surfaces were bonded together with M-bond 610 epoxy resin and cured at high temperature.

[0033] Step 1, the cured sample 1 is mechanically ground and polished to reduce the thickness of the section to less than 50 microns.

[0034] Step 2, bond the mechanically thinned sample 1 to the copper ring 2 with an outer diameter of 3 mm and an inner diameter of 2 mm for a transmission electron microscope, and use an ion thinner to perform double-sided polishing. The polished sample 1 and copper ring 2 are schematically shown as figure 1 As shown, a wedge-shaped region with a thickness less than 20 nm was obtained at the edge of sample 1. Using a trans...

Embodiment 2

[0040] Sample: ceramic sample.

[0041] TEM sample preparation steps:

[0042] Step 1: Cut sample 1 into a 1x3mm rectangle with a wire. The cut sample was mechanically ground and polished to reduce the thickness of sample 1 to less than 50 microns.

[0043] Step 2: Bond the mechanically thinned sample 1 to a copper ring 2 with an outer diameter of 3 mm and an inner diameter of 2 mm for a transmission electron microscope, and perform double-sided polishing with an ion thinner to obtain a wedge-shaped area with a thickness of less than 20 nanometers at the edge of the sample. Using a transmission electron microscope to observe the wedge-shaped edge of the sample, a clear high-resolution lattice structure image can be obtained; but if the observation is reduced at this time, it is difficult to obtain a full picture of a sufficient number of crystal grains.

[0044] Step 3: Use laser cutting to cut the sample after high-resolution image observation into two parts. The cutting li...

Embodiment 3

[0047] Sample: martensitic bearing steel sample.

[0048] TEM planar sample preparation steps:

[0049] Step 1: Cut sample 1 into a 1x3mm rectangle with a wire. The cut sample was mechanically ground and polished to reduce the thickness of sample 1 to less than 50 microns.

[0050] Step 2: Cut the mechanically thinned sample 1 into a disc with a diameter of 3 mm, and perform double-sided polishing with an electrochemical double-jet device, and obtain a wedge-shaped area with a thickness of less than 20 nanometers in the edge of the sample . Using a transmission electron microscope to observe the wedge-shaped edge of the sample, a clear high-resolution lattice structure image can be obtained; but if the observation is reduced at this time, it is difficult to obtain a full picture of a sufficient number of crystal grains.

[0051] Step 3: Cut the sample after the high-resolution image observation into two parts by laser cutting, and the cutting line passes through the perfora...

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Abstract

The invention provides a transmission electron microscope sample preparation method. The method comprises the steps of at first conducting mechanical grinding and polishing to a sample, then using a ion thinning apparatus or directly using a electrochemical twin-jet polisher to conduct double side polishing of the mechanically ground and polished sample, cutting the sample loading ring or directly cutting the sample, finally using a focused ion beam to thin the thickness of a target area all to less than 200nm. The method can acquire high quality, high resolution and low magnification images in a same sample, and can considerably reduce the sample preparation cost.

Description

technical field [0001] The invention relates to the technical field of semiconductor device analysis, in particular to a method for preparing a transmission electron microscope sample. Background technique [0002] The TEM cross-section is made by the classic method of mechanical and ion thinning, because the thinned sample is often larger than several hundred microns including the substrate, thus forming a wedge-shaped thin region. Assuming that the wedge angle is 2 degrees and the radian value is about 0.03, it can be known from the geometric ratio that for a coating or coating of 5 microns, there will be a region with a thickness greater than 200 nm in the cross section of the entire film. The absorption and scattering of the electron beam by the sample larger than 200nm will cause obvious mass-thickness contrast, especially in the contrast with a thickness smaller than 20nm, we will find that it is difficult to obtain a complete and clear low-magnification image of the w...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/28
Inventor 孙明达
Owner SHANGHAI DOESUN ENERGY TECH