Lodz University of Technology
Faculty of Chemistry
INSTRUCTION
SEM-EDS LABORATORY
Investigation of Chemical Composition and
Surface Structure
by Scanning Electron Microscopy with X-ray
Microanalysis Attachment
1. OBJECTIVE OF THE EXERCISE
The goal of the exercise "Investigation of the chemical composition and surface
structure of hair, cosmetics, and other samples using scanning electron microscopy with
X-ray microanalysis (SEM-EDS)" is to examine the morphology and elemental
composition of the surface layers of selected samples. This exercise aims to familiarize
students with the research capabilities and applications of the SEM-EDS method for
analyzing solid surface materials.
2. INTRODUCTION
Modern scientific research equipment enables progress in many areas of science and
technology. In recent years, the study of the surfaces of biological, medical, electronic,
polymeric materials, as well as catalysts and adsorbents, has gained significant
importance due to the availability of methods for analyzing the elemental composition
of surfaces and their distribution on selected microareas, as well as identifying chemical
forms on the surface. Among these methods, scanning electron microscopy (SEM) is a
valuable research tool for examining the surfaces of various solids in many scientific
fields due to its high resolution and large depth of field. These features allow direct
observation of surfaces at magnifications ranging from 20 to 500,000, or even up to
1,000,000 times. This enables the detailed study of the smallest organisms (bacteria and
viruses), the examination of crystal structures and their defects, and the investigation of
various materials and their properties. This technique has also found broad application
in forensics, dentistry, and industry, including product quality control.
3. EXERCISE PROCEDURE
3.1. Measuring Equipment
The scanning electron microscope with field emission, Hitachi S-4700, with X-ray
microanalysis attachment ThermoScientific (USA). The SEM is equipped with:
• two independent SE (Secondary Electrons Detector) detectors,
• YAG BSE (Backscattered Electrons Detector),
• Energy Dispersive Spectrometer (EDS).
The microscope resolution at a working distance of 12 mm and at 15 kV is 1.5 nm with the
SE detector and 3 nm with the BSE detector. The magnification range of the apparatus:
High-mag mode: 50–500,000 times
Low-mag mode: 20–10,000 times
3.2. Execution of the Exercise
1. Presentation of the SEM-EDS method – structure, basic applications in surface
analysis of solids.
2. Discussion of the samples intended for SEM-EDS analysis.
3. Preparation of samples for analysis.
4. Selection of operating parameters for the microscope and the spectrometer for micro-
X-ray analysis.
5. Registration of microscopic images of the sample surfaces at various magnifications
(SEM).
6. Registration of X-ray spectra for selected microareas (EDS).
7. Mapping the distribution of selected elements on the surface of the sample.
8. Discussion and analysis of the obtained results.
9. REPORT PREPARATION
4.1. Objective of the Exercise
The objective of the exercise is to investigate the morphology of surface layers of samples and
determine their elemental composition and surface distribution of elements depending on the
method, stage, and conditions of their preparation using scanning electron microscopy with X-
ray microanalysis attachment.
4.2. Measurement Methodology
In the electron microscope, the image of the object is created by scanning a high-energy electron
beam (1–30 keV) over the surface of the sample. The interaction between the electrons and the
atoms of the sample causes physicochemical phenomena, such as the generation of low-energy
secondary electrons (SE), high-energy backscattered electrons (BSE), and X-ray radiation. The
signals from SE, BSE, and EDS detectors are analyzed. The SE and BSE signals are used to
create images of the sample morphology, while the EDS attachment analyzes the elemental
composition of the surface (X-ray spectra) and the distribution of these elements on the sample
surface (EDS maps).
4.3. Measurement Results
The report should include the following results:
• Microscopic images obtained with the SE and/or BSE detectors at various magnifications,
describing the observed surface structure and crystal sizes.
• X-ray spectra of the tested samples – point spectra and spectra collected from selected
microareas.
• Maps of the distribution of elements on the surface of the studied microareas, with a
description of the observed surface morphology, areas with uniform or elevated
concentrations of elements.
4.4. Results Analysis
Based on the obtained results, students will determine the morphology and elemental
composition of the surface of the tested catalyst samples. The analysis should include:
• Description of the surface morphology,
• Estimation of the size of objects visible in microscopic images,
• Evaluation of the elemental composition of the surface,
• Description of element distribution maps in selected microareas,
• Analysis of the impact of the methods and conditions of sample preparation on the state of
the surface, assessment of morphological changes.
4.5. Conclusions
Based on the results obtained, students should evaluate the impact of sample preparation
processes on the morphology and elemental composition of the surface layers. They will
perform qualitative and semi-quantitative analysis of the content and distribution of individual
elements in selected microareas. They will familiarize themselves with the research capabilities
of the microscope using various types of detectors (SE, EDS), assess the advantages and
limitations of using SEM-EDS for surface analysis, and draw conclusions regarding the study
of the morphology of other solid samples. They will also evaluate the impact of microscope and
EDS spectrometer parameters on the quality of images and results.
7. LITERATURE
[1] SEM-EDS Laboratory Instruction: “Investigation of the chemical composition and surface
structure of catalysts using scanning electron microscopy with X-ray microanalysis,”
developed by Prof. Dr. Hab. M. I. Szynkowska-Jóźwik.
[2] Szynkowska, Małgorzata Iwona, Scanning Electron Microscopy, in Encyclopedia of
Analytical Science, Second Edition (Paul J. Worsfold, Alan Townshend, and Colin F. Poole,
eds.) Elsevier, Oxford, 2005, Vol.4, pp.134-142.
[3] Najbar, Mieczysława (ed.), Fizykochemiczne metody badań katalizatorów kontaktowych,
Wyd. Uniwersytetu Jagiellońskiego, Kraków, 2000, 48-56.
[4] X-ray elements – Bing images.
