Analyzing the features of fractured samples by scanning electron

microscopy (SEM)

Muayad Alhilal

UNC Charlotte, Department of Mechanical Engineering, ME3152; Mechanics and

Materials Laboratory

Preformed on: March 22, 2018

Reported on: March 27, 2018
Table of Contents
Table of Contents ................................................................................................................. 2
Abstract................................................................................................................................ 3
Equipment and Procedure ................................................................................................... 3
References ............................................................................................................................ 5
Appendices ........................................................................................................................... 6

2
Abstract

The purpose of the experiment was to analyze the microstructure of fractured samples and correlate
the features of the surface to identify the failure mode by scanning electron microscopy (SEM). In
addition, one goal was to practice and get familiar with the principles of an SEM. A total of eight
samples were analyzed from previous experiments which were 360 brass and A20 cast iron from
tensile test, 1018 steel (fractured at 77K,373K and 473K) and 7075 aluminum (fractured at 77k
and 473K) from impact test, and A36 steel fractured at 384 cycles at 4500 lb. from fatigue test.
JEOL 6480 SEM was used to observe the fracture surfaces. All samples were loaded into a
specimen holder and was placed into the specimen stage. A PC was used to control the parameters
of the SEM machine and to observe the features of the surfaces. Finally, the microstructures of the
surfaces were recorded and saved. Furthermore, the final results indicated a higher number of
vacancy defects on the brass while none on the cast iron in tensile test. In addition, it was observed
that there were no vacancy defects on the steel at 77K while there were some defects at 373K and
474K. The aluminum had some defects at 77K while it did not have defects at 474K. Moreover, a
line of the crack in the fatigue zone on the steel was observed while it was observed that there were
some defects in the rupture zone. In summary, the features of the fractured surfaces could correlate
to the fracture mode. The presence of the vacancy defects indicates a ductile fracture while no
vacancy defects indicates a brittle fracture. Furthermore, the number of defects increases at high
temperatures on the steel while no change of the defects with respect to temperature on aluminum.

Equipment and Procedure

Eight samples from previous experiments were collected to be analyzed. Table 1 shows the
samples that were used in this experiment.

Table 1 samples of Fractography Experiment

# Material Test Details
1 360 Brass N/A
Tensile Test
2 A20 Cast Iron N/A
3 at 77K
4 1018 Steel at 373K
5 Impact Test at 474K
6 at 77K
7075 Aluminum
7 at 474K
8 A36 Steel Fatigue Test 384 cycles at 4500 lb.

The procedure started with starting up the JEOL 6480 SEM machine by the teaching assistant. The
JEOL program was started by clicking on its icon on the PC desktop. A pre-check of the SEM
system status was carried out by checking the [EVAC] button to be green, the HT button to be [HT
OFF], and the default position of the stage to be x = 0, y = 0, R = 0, T = 0, and z = 20 mm. The
IR camera from the PC desktop was opened to monitor the distance between the stage and the
detectors.

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 Figure 1 Location of Samples on the Specimen Holder

Figure 1 shows how the samples were loaded into the specimen holder. The specimen chamber
was vented by pressing [VENT] button on the column control panel. Then, the specimen holder
was placed on the specimen stage in the STM machine using the Specimen Exchange Tool. Next,
the chamber was closed and evacuated by pressing [EVAC] button. After the HT button changed
to [HT OFF], the system was ready for observation. Table 2 shows the parameters that were used
for each sample in order to obtain the features of the surface. (Refer to Table1 for sample #/
Material)

Table 2 Summary of Parameters Used in the Experiment

Acceleration Working
Sample # Operation Mode
Voltage (kV) Distance (mm)
1 15
2 17
3 24
4 23
BSE 20
5 22
6 22
7 17
8 15

Furthermore, the stage was moved from a sample to another one by adjusting the stage position
from the Stage Control window. Also, the [Z] position was adjusted to focus and to obtain clear
observations. Then, the [HT] icon was clicked so that it changes to [HT ON] before a SEM image
appears. The magnification and focus were adjusted as needed to observe the features of the
surface. After obtaining clear STM features, SEM images were saved on a file.

To turn off the SEM machine, the [HT] button was clicked so it changes to [HT OFF]. The stage
position was returned to the start position (i.e. x = 0, y = 0, R = 0, T = 0, and z = 20 mm). The
specimen chamber was vented and the specimen holder was unloaded. Then, the door was closed
tightly before the specimen chamber was evacuated by pressing [EVAC] button. Lastly, the
programs were closed before logging off from the PC.1

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References
1. Xu, Terry, Hodgins, Garry, and Chen, Xiaoxue. 2018. “Lab 7: Fractography of Metals”
MEGR 3152 Mechanics and Materials Lab: Lab Instruction for Students.

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Appendices