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Application Note Electron Channeling Contrast Imaging Performed by ZEISS GeminiSEM 500

Electron Channeling Contrast Imaging Performed by ZEISS ... · ZEISS Microscopy, Germany Date: March 2017 Electron channeling contrast imaging (ECCI) is a technique for quantitative

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Page 1: Electron Channeling Contrast Imaging Performed by ZEISS ... · ZEISS Microscopy, Germany Date: March 2017 Electron channeling contrast imaging (ECCI) is a technique for quantitative

Application Note

Electron Channeling Contrast Imaging Performed by ZEISS GeminiSEM 500

Page 2: Electron Channeling Contrast Imaging Performed by ZEISS ... · ZEISS Microscopy, Germany Date: March 2017 Electron channeling contrast imaging (ECCI) is a technique for quantitative

Application Note

2

Electron Channeling Contrast Imaging Performed by ZEISS GeminiSEM 500

Author: Luyang Han ZEISS Microscopy, Germany

Date: March 2017

Electron channeling contrast imaging (ECCI) is a technique for quantitative characterization of deformation

structures in scanning electron microscopy (SEM). Relative orientation of crystalline lattice and incident

electron beam influence back scattered electrons (BSE). ECCI makes use of this. ECCI in SEM is especially useful

for imaging crystallographic defects such as dislocations, stacking faults and twin boundaries and thus starts

to have an impact on materials science.

Introduction

The BSE yield of crystalline samples depends on the relative

orientation of the electron beam to the crystalline lattice [1].

In particular when the incident electron beam fulfils the

Bragg condition with respect to the lattice, the backscat-

tered electron yield will have an abrupt change (Fig. 1a).

This variation of signal can be used to qualitatively distin-

guish materials with different crystalline orientations.

A particularly interesting feature of channeling contrast is

that the BSE yield has a very large change around the Bragg

condition. Even small changes in crystallographic direction

can be detected when the electron beam and the sample are

aligned to fulfil the Bragg condition. The distorted lattice

around the defects in crystalline materials can thus be

imaged. An example for a dislocation is shown where an

extra half-plane of atoms is introduced (Fig. 1b). This extra atomic plan causes local distortion of the crystal-

line lattice, which can be detected due to the large variation

of BSE yield around the Bragg condition.

Electron channeling contrast imaging

of crystalline defects

In order to effectively image defects in material using ECCI,

it is important to adjust the orientation of the sample such

that the Bragg condition is fulfilled for the incident electron

beam. This condition can be achieved when imaging a single

crystalline sample where the orientation of the sample can

be readily determined.

Epitaxial GaN thin film is imaged using ECCI. The GaN thin

film is grown by molecular chemical vapor deposition

Figure 1: Mechanism of channeling contrast imaging. (a) back scattered electron yield with respect to crystallographic orientation. (b) situation of channeling contrast due to a dislocation.

Page 3: Electron Channeling Contrast Imaging Performed by ZEISS ... · ZEISS Microscopy, Germany Date: March 2017 Electron channeling contrast imaging (ECCI) is a technique for quantitative

Application Note

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(MOCVD) along the [0001] direction of single crystalline

sapphire substrate. Because of the lattice mismatch between

sapphire and GaN, various kinds of dislocations are pro-

duced [2]. When scanning across the sample in low magnifi-

cation, the incident angle of the electron beam with respect

to crystalline direction changes continuously. The obtained

signal variation is called electron channeling pattern (ECP)

(Fig. 2a). The lines across the ECP indicate where the Bragg

condition is fulfilled. By tilting and rotating the sample,

the center of the ECP is brought to coincide with the line

patterns.Two different Bragg conditions are selected by

tilting the sample to 4.5° and 7.1(Fig. 2b-c).

The point-like features in the image indicate the presence

of dislocations where the lattice distortion around the dis-

location is manifested as a dipole shape contrast variation

around the dislocation points [3] (Fig. 3).

Figure 2: Principle of electron channeling pattern (ECP) obtained by scanning across a large area on a single crystalline sample (a) and ECP obtained on epitaxial GaN thin film with 4.5° tilt (b) and 7.1° tilt (c). The red circles indicate the center of the image.

Figure 3: Channeling contrast imaging of dislocations on epitaxial GaN thin film. The sample is imaged at 30 kV electron beam energy and tilted by 4.5° (a) and 7.1° (b).

Page 4: Electron Channeling Contrast Imaging Performed by ZEISS ... · ZEISS Microscopy, Germany Date: March 2017 Electron channeling contrast imaging (ECCI) is a technique for quantitative

Application Note

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In polycrystalline material, the grain size is usually at the

micrometer range and is too small to be obtained by ECP.

However, due to its random crystalline orientation, some

grains will always match a certain diffraction condition.

This can be observed as particularly bright or dark grains

in the BSE image. An example is demonstrated on a highly

deformed stainless steel sample. Multiple grains of several

micrometers in size, as well as a strong contrast variation

within each grain can be observed.

The deformation results in strong crystalline orientation

changes within the grains (Fig. 4a). Higher magnifications

reveal the dislocation networks formed by the deformation

(Fig. 4b) as well as by individual dislocation points and lines

(Fig. 4c-d).

Optimizing channeling contrast imaging condition

The amount of channeling contrast is influenced by the

properties of the incident electron beam and the detector.

An increase of primary electron energy decreases the chan-

neling contrast and simultaneously increases the penetration

depth of the electron [1]. This avoids multiple scattering from

surface layers and facilitates the obtaining of channeling

contrast. Thus, there is an optimum electron energy, which

depends on the material and its thickness. Under normal

SEM working conditions, higher electron beam energy

usually leads to better channeling contrast. The effect of

increase in electron beam energy on channeling contrast is

demonstrated on a gold thin film on carbon (Fig. 5). At 5 kV

and at 10 kV beam energy most of the contrast is due to

surface topography. The strongest channeling contrast is

observed at 30 kV.

Figure 4: Channeling contrast imaging of dislocation network in highly deformed stainless steel. The sample is imaged at 30 kV electron beam energy. (a) Strong crystalline orientation changes within the grains. (b) Dislocation networks formed by the deformation. (c-d) High magnicifation of dislocation lines.

Page 5: Electron Channeling Contrast Imaging Performed by ZEISS ... · ZEISS Microscopy, Germany Date: March 2017 Electron channeling contrast imaging (ECCI) is a technique for quantitative

Application Note

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Figure 5: Influence of electron beam energy to the channeling contrast. The gold islands on carbon substrate are imaged at 5 kV (a), 10 kV (b), 20 kV (c) and 30 kV (d) beam energy.

The channeling contrast will also increase with decreasing

take-off angle. This effect is demonstrated by changing the

working distance of the sample (Fig. 6).

Page 6: Electron Channeling Contrast Imaging Performed by ZEISS ... · ZEISS Microscopy, Germany Date: March 2017 Electron channeling contrast imaging (ECCI) is a technique for quantitative

Application Note

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References:

[1] L. Reimer, Scanning Electron Microscopy, 2nd. Edition (Springer) (1985) p.359

[2] Fong Kwong Yam et al, Optoelectronics - Materials and Techniques ed. P. Predeep (InTech) (2011) p. 99.

[3] G. Naresh-Kumar et al, Physical Review Letters, 108 (2012), p.135503.

Smaller working distance places the sample closer to the

annular BSE detector under the pole piece, leading to a

smaller take off angle. The image taken at the smallest

working distance used here shows the strongest channeling

contrast. However, BSE with low take-off angle also enhances

the topographic contrast, which can be seen as a strong

signal variation around the edges of the gold islands.

A sample suitable for channeling contrast imaging needs

to be flat and ideally have a polished surface to reduce

topographic contrast.

Figure 6: Influence of BSE angle to the channeling contrast. The gold islands on carbon substrate is imaged at 30 kV beam energy. The working distances vary from 4 mm to 13 mm: 4 mm, image with the strongest channeling contrast (a), 7 mm (b), 10 mm (c), 13 mm (d).

Summary

• Strongest channeling contrast is observed when orien-

tation of the incident electron and the crystalline lattice

fulfil the Bragg condition.

• Lattice defects such as dislocations can be observed by

channeling contrast.

• Higher electron beam energy and lower working distance

are suitable for getting good results in channeling

contrast.

• Ideally the sample should have a polished surface.

Page 7: Electron Channeling Contrast Imaging Performed by ZEISS ... · ZEISS Microscopy, Germany Date: March 2017 Electron channeling contrast imaging (ECCI) is a technique for quantitative

Carl Zeiss Microscopy GmbH 07745 Jena, Germany [email protected] www.zeiss.com/microscopy

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