SlideShare a Scribd company logo
1 of 24
Download to read offline
1
MEMORANDUM
Date: 5 May 2017
To: Dr. Charles E. Lyman, Supervisor
From: Tech Tanasarnsopaporn
Subject: Investigation of Material Composition in Mysterious Historical Subject: Metal Fence
Executive Summary
The objective of this investigation is to identify the metallographic composition of the
sample and to determine the possible manufacturing process of the fence. The material is
composed of approximately 81.12% α-Fe and cementite pearlitic matrix, 17.2% graphite,
10.21% Fe3P, 1.52% TiC, 0.51% TiN, 2.85% MnS, and 1.6% pores by volume fraction. It is
concluded that the metal fence is a pearlitic gray cast iron ASTM A48 casted in a sand mold for
a low-volume production. The presence of alloying elements resulted in phases including iron
phosphide (Fe3P) which increases flowability and allows more complex designs to be made,
titanium carbide (TiC) which increases strength, titanium nitride (TiN) which increases wear
resistance, manganese sulfide (MnS) which removes sulfur contaminants to increase strength and
flowability, and silicon-iron matrix which increases the corrosion resistance.
Background
An unknown specimen under investigation is a section of a metal fence procured from a
household region of Bethlehem, Pennsylvania and was made in the mid-to-late 18th
century
(Appendix 3, figure 1). The sample was a small section with rough surface covered with thick
layer of red-colored rust. The objective of this investigation is to identify the composition of the
sample and to conclude the possible manufacturing process of the fence.
Method
The preliminary examination includes an unaided color observation of rust (oxide layer)
2
and metallic piece it enveloped, the density of the metallic piece using Archimedes’ method
(ASTM B962-15), and the magnetic property using a magnet test (Appendix 1, section 1). The
sample was then metallographically prepared (ASTM E3-11) and observed under Light Optical
Microscope (LOM) (ASTM E562) (Appendix 1, section 2), Scanning Electron Microscope and
Energy-Dispersive Spectrometry (SEM/EDS) (ASTM E1508), Powder X-ray Diffraction (XRD)
(ASTM D3906), and Transmission Electron Microscope (TEM) with Selected Area Diffraction
(SAD). The collected data was finally analyzed and compared with the information from various
accepted literatures listed in the reference section.
Result
The investigation shows that the material is comprises of pearlite (α-Fe and cementite),
graphite, iron phosphide (Fe3P), titanium carbide (TiC), titanium nitride (TiN), and manganese
sulfide (MnS) with porous regions scattered throughout the sample. The evidence for each phase
is described under the subheadings below. All procedures and methods of calculation are
included in Appendix 1; tables are in Appendix 2; and. figures are in Appendix 3. The detailed
results are summarized in table 1.
Ferrite
The material has silvery-gray color with dark red oxide layer and exhibits
ferromagnetism, all of which suggests a high composition of iron (Fe) in the sample. This result
is reaffirmed with the strong characteristic x-ray peaks in XRD (Table 5) and the EDS result of
89.90 ± 0.50% α-Fe volume fraction (Table 4). LOM and SEM also show pearlitic
microstructures with volume fraction of the matrix phase of 70.4 ± 3.0% which confirm the
presence of ferrite (α-Fe) (Table 3).
Cementite
The strong characteristic x-ray peaks in XRD of Fe3C are the evidence of cementite
3
(Table 5). The pearlitic microstructures found in LOM and SEM also confirm the presence of
cementite (Fe3C) within the matrix phase (Table 3). Cementite within each pearlite colony has a
characteristic of a lamella with 0.3 ± 0.05 µm wide on average, aligned in the same direction,
suggesting that the colonies are fine pearlite (Table 1) [1]. Moreover, the density of the sample
was found to be 6.6 ± 0.5 g/mL, closely resembles that of cast iron with density of 6.8-7.8 g/mL
(Figure 1) [1]. The density lower than that of pure iron can be explained by corrosion which was
seen as rust and the presence of 1.6 ± 1.0% porosity by volume fraction as analyzed from optical
micrographs (Table 1). The size of the pores was also found to be 4 ± 0.5 µm in diameter on
average (Table 1).
Graphite Flakes
A significant amount of black carbon flakes was also seen in LOM and SEM. In various
areas on the sample, EDS x-ray mapping also shows pure carbon composition (Figure 5-6); thus,
these regions must contain some stable allotropes of carbon. The XRD result further confirms
that the carbon phase present is in graphite form (Table 5). In the optical micrograph and SEM,
the graphite phases were seen to be in the form of rosette flake graphite with 80 µm diameter and
2 ± 0.5 µm x 30 ± 0.5 µm per flake (ASTM Type B) (Table 1) [3]. These flakes have the
characteristics of rosette grouping in random orientations pointing out radially from the center of
the group. Some nodular graphite with 7 µm diameter (ISO Form VI) was also observed (Table
1, Figure 2-3) [3]. Under LOM, the volume fractions of flake graphite and nodular graphite are
found to be 15.6 ± 2.5 % and 1.6 ± 1.0 %, respectively (Table 1).
Iron Phosphide
In addition to α-Fe and Fe3C, the Fe-P phase was observed in EDS, XRD, and TEM. The
X-ray pattern in TEM-SAD identified a 10 ± 0.5µm x 10 ± 0.5µm region with non-homogeneous
characteristics and well-distributed white dots to be a phase containing phosphorus and iron
4
peaks. With EDS x-ray mapping, the volume fraction of this Fe-P phase was estimated to be
10.21 ± 0.30% (Table 4). The more accurate analysis with XRD was then able to reveal the
tertiary ferritic phase to be iron phosphide or Fe3P (Table 5). TEM-SAD was then used to
determine the dhkl of this region, which corresponds to the accepted values of Fe3P in The
International Centre for Diffraction Data (ICDD)’s Powder Diffraction File (PDF) database [2].
Titanium Carbide
While the LOM shows the carbon phases to have the total of 17.2 ± 3.5% (Table 3), the
EDS result shows the volume fraction of carbon-containing regions to be 22.92 ± 3.44% (Table
4). This discrepancy can be explained with the discovery of Ti-C phase in EDS x-ray mapping,
which shows the overlaps of titanium and carbon regions. The volume fraction of Ti-C region is
approximately 1.52 ± 0.04% with the cubic crystal shape and 2 ± 0.5 µm x 5 ± 0.5 µm in size
(Table 1). While small percent volume fraction is present, the XRD detected faint signal of TiC
phase in the sample (Table 5). The TEM-SAD further reaffirms that the unique faceted region
containing Ti-C has the Fm3m space group crystal, and the dhkl matching that of Titanium
Carbide or TiC (Table 6) [4].
Titanium Nitride
While the XRD cannot be used to accurately detect phases with percent volume fraction
less than 1% [5], the small cubic crystalline precipitates (2 µm x 2 µm) found in LOM were
investigated under EDS and TEM (Table 1). The EDS x-ray mapping shows regions containing
both titanium and nitrogen with the volume fraction of approximately 0.51 ± 0.06% (Table 4).
TEM-SAD suggests that the unique region containing Ti-N has the Fm3m space group crystal
and the dhkl matching that of Titanium Nitride or TiN [6] (Table 6).
Manganese Sulfide
The EDS x-ray mapping shows another region with manganese and sulfur with 2.85 ±
5
1.79% volume fraction (Table 4). TEM-SAD suggests that the small (2µm x 2µm) cubic crystals
containing Mn-S has the Fm3m space group crystal and the dhkl matching that of manganese
sulfide or MnS (Table 6) [7]. As MnS crystal has a light pink color, this agrees with the pink
color of the cubic crystal found in various sites throughout the LOM micrograph (Figure 3) [8].
Silicon
Silicon was observed throughout the sample when using EDS x-ray mapping with the
volume fraction of 59.20 ± 3.72% (Table 5). By looking closely at the x-ray mapping, it appears
that silicon is scattered almost uniformly over the region containing iron. This can be explained
as the matrix of iron and silicon, which is commonly seen in a high silicon cast iron [18].
Discussion
The result of the investigation shows that The material is composed of approximately
81.12% α-Fe and cementite pearlitic matrix, 17.2% graphite, 10.21% Fe3P, 1.52% TiC, 0.51%
TiN, 2.85% MnS, and 1.6% pores by volume fraction. The calculated weight fraction shows
carbon with over 2.14 wt%, which suggests that the specimen is a type of cast iron (Table 7) [9,
10]. By considering the Fe-C phase diagram at 3.23 wt%C (Figure 22-23), the Fe-C system
should form graphite precipitates and a large amount of pearlite which is confirmed by the result
shown in Table 1 [11]. By comparing the weight percent composition and other experimental
results with ASTM alloy designation of cast irons [9, 11], this unknown specimen was found to
be Gray Cast Iron ASTM A48 (Table 7), an easily machined and ductile alloy [11].
Another important clue to find out the original manufacturing process is its rosette
graphite flakes that can only be found in gray cast iron [11]. Since manufacturing pearlitic gray
cast iron involves fast cooling during tempering process to form pearlite colonies, the evidence
from LOM and SEM showing the large volume fraction of fine pearlite suggests that this cast
iron is indeed a pearlitic gray cast iron (Table 3) [9].
6
Furthermore, the presence of Fe3P, TiC, TiN, MnS, and Si displays some interesting
alloying technologies that might have been used during the production of this fence. Since the
quality of casting depends on the fluidity of molten iron, phosphorus is sometimes added to form
a network of low-melting-point phosphorous eutectic phase (Fe3P) to increase flowability and
widen processing window [12]. During 19th
century, titanium was traditionally considered a
contaminant from the iron ore extraction process, and it was not widely used an alloy element
However, titanium can combine with carbon to form hard TiC precipitates which increase
strength [13]. When molten titanium combines with nitrogen in the hot air and forms TiN
precipitate, the wear resistance will also be improved [14]. Moreover, as sulfur is another major
contaminant from iron ore processing which causes the molten iron to be viscous, manganese is
added to form MnS which neutralizes the effect [15]. Furthermore, the high level of silicon
means that excess silicon might be intentionally used in alloying. As shown in high silicon cast
iron (HSCI), silicon is an inexpensive alloying element to improve the corrosion resistance [15].
Other observations include the low dimensional details such as the high curvature around
the corner of the specimen which indicates that the mold material has low resolution (Figure 1).
Thus, it is likely that this metal fence is casted in a sand mold – a fast and inexpensive metal
manufacturing process typically used during that period [16]. The small porous voids also
suggest that the fence was casted by a small volume at a time i.e. few kilograms [17]. Moreover,
the ASTM type B rosette-shaped graphite flakes are a characteristic of a thin-walled casting (i.e.
die casting), which is suitable for a small- to medium-sized casting [18].
To conclude, the metal fence under investigation is a pearlitic gray cast iron (ASTM
A48) casted in sand mold for a low-volume production while various alloying elements
including Fe3P, TiC, TiN, MnS, and Si were included to improve wear resistance and strength of
the fence and to allow the more complex designs to be made.
7
Appendix 1: Procedure and methods of calculation
Section 1. Preliminary Examination: ASTM B962-15 [19]
With a simple magnet test, the metal was discovered to be magnetic. Then, density
measurements were made before and after the oxide layer of the metal was scraped off. These
measurements were 5.7 g/mL and 6.6 g/mL, respectively.
Section 2. Light Optical Microscopy: ASTM E3-11, ASTM E562 [20,21]
A sample of the metal was mounted in Bakelite and metallographically prepared. Using
Pax-It and the Olympus TH3 light microscope, images of the unetched sample were captured.
The sample was then etched in 4% Picral for 1 second, followed by 1 second in 2% Nital. Images
of the etched sample were captured. Then, to measure volume fractions of these phases, the
ASTM E562 point count method was performed with a reticle on the ocular of a microscope [1].
Only the flake graphite, nodular graphite, and matrix, believed to be both ferrite and pearlite,
were visible under the light microscope without the contrast manipulation feature of Pax-it. After
etching, however, the other five phases, including pores, became much more visible. The results
of all ten point counts are seen below in Appendix 2, Table 3.
Section 3: Comments on uncertainty of the experiment:
It is important to note that the experimental results may contain some margin of error in
the data for the small, non-ferrous phases from LOM and SEM observations. This is because
while the point counting method has the limitation of 0.5%, these phases may be present at less
than 1% [11]. Moreover, as outlined in Section 5, the volume fraction of elements observed in
EDS x-ray mapping is subjected to the error in threshold values for each phase.
Section 4: Precision Calculation: ASTM D4460-97 [22]
Precision of experimental data can be calculated as the average deviation of the dataset:
𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝐷𝑒𝑣𝑖𝑎𝑡𝑖𝑜𝑛 =
∑|𝑥−𝜇|
𝑛
, where 𝑥 is the data points, 𝜇 is the mean value of dataset, and 𝑛
8
is the number of data points. For example, in LOM point counting,
𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝐷𝑒𝑣𝑖𝑎𝑡𝑖𝑜𝑛 =
(13−15.6)+(19−15.6)+(15−15.6)+(13−15.6)+(18−15.6)
5
% = 2.5%
Section 5: Image-J Processing [23]
In using the EDS x-ray mapping data, there exist the background noise that can let the
experimenter to misinterpret the actual volume percent of each element. This is because of the
resolution of the SEM/EDS. In order to reduce the noise, the automated software can be used.
Image-J, for example, can readjust the color threshold of the photo such that only when the
contrast threshold exceed certain value will the pixel will be counted.
First, open the photo in Image-J and go to Process>Binary>Options. Check the "Black
Background" box. This is so that pixels with value 0 are shown as black, and those with 255 as
white, after the thresholding operation. Open the Threshold tool: Image>Adjust>Threshold.
Check the "Dark Background" box. The brighter pixels will be highlighted in red. These red
pixels will be mapped to white and the rest to black. Keep the higher threshold (bottom slider) at
255. Click “Auto-Adjust” to let Image-J analyze the background noise and eliminate. Click on
the "Apply" button to get a binary image. An effective way to do calculate volume ratio is to
look at the histogram by pressing Crtl+H. Then, click “copy” to copy the values and paste into an
Excel spreadsheet. The ratio of phases or elements can be found by dividing the number of pixel
with threshold at 255 and the total number of pixels of the image. The results are shown in
Appendix 3, figure 7.
9
Appendix 2: Tables
Table 1. The detailed summary of results from LOM, SEM, EDS, XRD, and TEM/SAD. D-
values and space groups were obtained by comparing raw data to ICDD database.
Table 2. TEM SAD: Calibration data using diffraction ring pattern of Pure Aluminum observed
in TEM. The interplanar spacing is calculated using the ICDD database [3].
Ring diameter=2R (mm) hkl dhkl (Å) 2Rd=2λL λL (mm Å)
23.0 111 2.3380 53.774 26.8
26.5 200 2.0248 53.657 26.8
37.5 220 1.4317 53.689 26.8
Table 3. LOM: Shown in the table below are the results of the point counts of all 10 of the
Phase
Volume
%
Size Shape Elements
Largest
measured
d-value
PDF
value
PDF card #
Space
group
Pearlite 81.2
Span across
sample
Colonies Fe, C N/A N/A N/A N/A
- Ferrite N/A
Span across
colonies
N/A Fe 2.04 2.026 00-006-0696 Im3m
- Cementite N/A
Varied length,
0.3 µm wide
Long, thin
strands
Fe, C 2.541 2.541 00-035-0772 Pnma
Rosette
Graphite
15.6
80 µm diameter,
2µm x 30µm per
flake
Rosette, long
flakes
C 3.357 3.355 00-056-0159
P63/mmc
Nodular
Graphite
1.6 7 µm diameter Circular C 3.357 3.355 00-056-0159 P63/mmc
Iron
Phosphide
10.21
10 µm x
10 µm
Non-
homogeneous,
long dots
Fe, P 6.469 6.43962 00-051-0943 Fm3m
Titanium
Carbide
1.52
2 µm x
5 µm
Cubic shape Ti, C 2.14 2.1637 00-032-1383 Fm3m
Titanium
Nitride
0.51
2 µm x
2 µm
Cubic shape Ti, N 2.43 2.44917 00-038-1420 Fm3m
Manganese
Sulfide
2.85
2 µm x
2 µm
Cubic shape Mn, S 3.063 3.015 00-006-0518 Fm3m
Pores 1.6
4 µm x
4 µm
Irregular,
round edges
N/A N/A N/A N/A N/A
10
phases observed under the Olympus TH3 light microscope with the assistance of a Pax-it
camera. For each phase, five fields of view were chosen at random for the point counting.
Microconstituent I II III IV V Volume% Precision (±)
Flake Graphite 13 19 15 13 18 15.60 2.5
Nodular Graphite 3 2 2 1 0 1.60 1.0
Pearlite (Gray
matrix phase)
83 78 82 83 82 81.20 1.4
Manganese Sulfide
(Pink Cube)
1 0 0 1 0 0.40 0.5
Titanium Carbide
(Blue Cube)
1 0 0 1 0 0.40 0.5
Iron Phosphide
(Orange Phase)
0 0 0 0 1 0.20 0.4
Pores 1 2 2 3 0 1.60 1.0
Table 4. EDS: Volume fractions calculated from element x-ray mapping images taken by FEI Scios
FIB. The data was then auto correct to reduce background noise using Image-J (Appendix 1, section
5). The average values were calculated and used in analysis.
Element
Vol%
(FEI – raw data)
Vol%
(Auto-Correct)
Average Vol% Precision (±)
C K 26.35 19.48% 22.92 3.44
Fe K 90.40 89.40% 89.90 0.50
Mn K 4.63 1.06% 2.85 1.79
Si K 55.48 62.92% 59.20 3.72
S K 1.99 2.12% 2.06 0.07
Ti K 1.99 2.06% 2.03 0.04
N K 0.57 0.44% 0.51 0.06
P K 10.51 9.91% 10.21 0.30
11
Table 5. XRD: Diffraction pattern for various phases observed in XRD as shown in Appendix 3,
figure 2-6. The peaks were compared with the standard index diffraction pattern [2].
Phase
Measured
2ϴ
Measured
dhkl (Å)
dhkl from
PDF card
(Å)
Difference
in d-value
(Å)
% Deviation hkl PDF card #
Fe 44.36 2.040 2.046800 0.00680 0.33% 110
00-006-069665.14 1.431 1.433200 0.00220 0.15% 200
82.46 1.16 1.170200 0.01020 0.87% 220
Fe3C 35.29 2.541 2.545160 0.00416 0.16% 220
00-035-077239.83 2.217 2.218570 0.00157 0.07% 201
49 1.858 1.853400 0.00460 0.25% 221
TiC 35.42 2.532 2.500000 0.03200 1.28% 111
00-03201383
41.5 2.174 2.166000 0.00800 0.37% 200
60.85 1.521 1.531000 0.01000 0.65% 220
75.57 1.258 1.305000 0.04700 3.60% 311
C 35.42 3.293 3.355300 0.06230 1.86% 002
00-056-015942.36 2.132 2.131900 0.00010 0.00% 100
54.66 1.679 1.677700 0.00130 0.08% 004
Fe3P 35.46 2.510 2.529000 0.01900 0.75% 120
00-051-094342.80 2.07 1.990000 0.08000 4.02% 201
45.82 19.940 19.33000 0.61000 3.16% 220
12
Table 6. SAD: Diffraction pattern for various phases observed in TEM/SAD. The interplanar
spacing is calculated using camera constant found in Table 2. The ratios of the principal spot
spacing were calculated and compared with the standard index diffraction pattern [2].
Phase
Measured
distance from
diffraction
pattern (mm)
λL
(mm Å)
Measured
dhkl (Å)
dhkl from
PDF card
(Å)
hkl
Difference in
d-value (Å)
% Accuracy
PDF
card #
MnS (35÷4)= 8.750 26.8 3.06 3.015 111 0.048 1.59
00-006-
0518
(43÷3)=14.333 26.8 1.87 1.847 220 0.023 1.25
(50÷3)=16.667 26.8 1.61 1.575 311 0.033 2.1
Fe3P (29÷7)= 4.143 26.8 6.47 6.43962 110 0.029 0.45
00-051-
0943(26.5÷3)=12.167 26.8 2.20 2.19874 321 0.004 0.18
TiN 11 26.8 2.43 2.44917 111 –0.019 0.78
00-038-
142012.5 26.8 2.14 2.12071 200 0.019 0.9
TiC 12.5 26.8 2.14 2.1637 200 -0.0237 1.1
00-032-
1383
17.5 26.8 1.53 1.5302 220 -0.0002 0.01
20.5 26.8 1.30 1.3047 311 -0.0047 0.36
Table 7. Weight percent calculation for each element. Atomic weight information is cited from
an accepted literature [10]. Weight fraction was then calculated from the values of volume
fraction by EDS mapping and the atomic weight of each element.
Element Volume %
Atomic
Weight
(g/mol) [12]
Molecular
Weight
Contribution
(g/mol)
Weight %
Wt% of Gray
cast iron,
Class ASTM
A48 [11]
Fe 89.40% 55.8470 49.93 68.97 N/A
C 19.48% 12.0110 2.34 3.23 3.10-3.40
Mn 1.06% 54.9380 0.58 0.81 0.70-1.00
Si 62.92% 28.0855 17.67 24.41 2.10-1.08
S 2.12% 32.0600 0.68 0.94 0.15
P 10.21% 30.9738 3.16 4.19 0.08
Ti 2.06% 47.9000 0.99 1.36 N/A
N 0.44% 14.0067 0.06 0.08 N/A
13
Appendix 3: Figures
Figure 1. An unknown object is a portion of a fence produced in the mid-to-late 1800s
Figure 2. An image of the unetched mystery metal under a light microscope. The matrix is made
up of pearlite and a ferrite. The circles enclose the rosette, which is made up mainly of graphite
flakes. The image was taken in Pax-it at 230X magnification.
14
Figures 3. A picture taken of the unetched microstructure. The image was taken at 800X
magnification. The high magnification levels help distinguish the differences between the
multiple small phases in the mystery material. Phases noted: Blue cube, flake graphite, hexagon,
pink cube, triangular structure, and nodular graphite.
Figure 4. Site 1 of material at 1000x magnification. The dark phase is flake graphite, and the
pearlite stands out strongly as a lamella pattern.
Manganese Sulfide
(Pink Cube)
Titanium Carbide
(Blue Cube)
Graphite
15
Figure 5. X-ray mapping of unetched sample from FEI Scios FIB EDS at 800x magnification.
Figure 6. X-ray mapping of unetched sample from FEI Scios FIB EDS corrected for background
detection using Image-J software Auto-Adjust Threshold as described in Appendix 1, section 5.
16
Figure 7. XRD Pattern of the iron peaks in unknown material. The corresponding hkl values are
shown in Table 5. PDF card # 00-006-0696
Figure 8. XRD Pattern of Cementite peaks in material. The corresponding hkl values are shown
in Table 5. PDF card # 00-035-0772
2.217
17
Figure 9. XRD Pattern of Titanium Carbide in metal. The corresponding hkl values are shown in
Table 5. PDF card # 00-03201383
Figure 10. XRD Pattern of Graphite. The corresponding hkl values are shown in Table 5. PDF
card # 00-056-0159
18
Figure 11. XRD Pattern of Iron Phosphide in the unknown. The corresponding hkl values are
shown in Table 5. PDF card # 00-051-0943
Figure 12. Adapted from the TEM/SAD diffraction pattern of MnS with camera length of 0.6 m,
a high voltage of 120kV. The labels show the corresponding zone axis of electron diffraction
patterns, and measured d-values are noted. PDF# 00-006-0518
Fe3P
2θ = 35.46º
d = 2.510
2θ = 45.82º
d = 1.940
2θ = 42.80º
d = 2.070
[220] 1.87Å
[311] 1.61Å
[111]
3.06Å
19
Figure 13. Adapted from the TEM/SAD diffraction pattern of Fe3P with camera length of 0.6 m,
a high voltage of 120kV. The labels show the corresponding zone axis of electron diffraction
patterns, and measured d-values are noted. PDF# 00-051-0943
Figure 14. Adapted from the TEM/SAD diffraction pattern of TiN with camera length of 0.6 m,
a high voltage of 120kV. The labels show the corresponding zone axis of electron diffraction
patterns, and measured d-values are noted. PDF# 00-038-1420
[200] 2.14Å
[111]
2.43Å
[110] 6.47Å
[321] 2.20Å
20
Figure 15. Adapted from the TEM/SAD diffraction pattern of TiC (facetted particle) with
camera length of 0.6 m, a high voltage of 120kV. The labels show the corresponding zone axis of
electron diffraction patterns, and measured d-values are noted. PDF# 00-032-1383
Figure 16. Excerpt of ICDD Ferrite XRD Pattern PDF Card # 00-006-0696
Figure 17. Excerpt of ICDD Cementite XRD Pattern PDF Card # 00-035-0772
[200] 2.14Å
[220] 1.53Å
21
Figure 18. Excerpt of ICDD Graphite XRD Pattern PDF Card # 00-056-0159
Figure 19. Excerpt of ICDD Iron Phosphide XRD Pattern PDF Card # 00-051-0943
Figure 20. Excerpt of ICDD Titanium Carbide XRD Pattern PDF Card # 00-03201383
Figure 21. Excerpt of ICDD Titanium Nitride XRD Pattern PDF Card # 00-038-1420
Figure 22. Excerpt of ICDD Manganese Sulfide XRD Pattern PDF Card # 00-006-0518
22
Figure 23. The iron-carbon phase diagram with graphite instead of cementite as stable phase,
explaining the formation of graphite flakes in cast iron. [9]
Figure 24. The iron-carbon phase diagram with cementite as stable phase, explaining the
formation of pearlite in cast iron. [9]
23
References
[1] ASM Engineered Materials Reference Book, Second Edition, Michael Bauccio, Ed. ASM
International, Materials Park, OH, 1994.
[2] ICDD. PDF# 00-051-0943. Mayo, W., H&M Analytical Services, Inc., Allentown, NJ,
USA. ICDD Grant-in-Aid (1999).
[3] Casting design and performance. Materials Park, OH: ASM International, 2009. Print.
[4] ICDD. PDF# 00-03201383. Natl. Bur. Stand. (U. S.) Monogr. 25 18, 73 (1981).
[5] Charles Lyman. “Lecture: Scanning Electron Microscopy (SEM) and X-ray
Microanalysis.” Bethlehem, PA, Lehigh University, 2017
[6] ICDD. PDF# 00-038-1420. Wong-Ng, W., McMurdie, H., Paretzkin, B., Hubbard, C.,
Dragoo, A., NBS, Gaithersburg, MD, USA. ICDD Grant-in-Aid (1987).
[7] ICDD. PDF# 00-006-0518. Wong-Ng, W., McMurdie, H., Paretzkin, B., Hubbard, C.,
Dragoo, A., NBS, Gaithersburg, MD, USA. ICDD Grant-in-Aid (1987).
[8] Silas H Douglas. Guide to a systematic course of qualitative chemical analysis, prepared
for the chemical laboratory at the University of Michigan. Ann Arbor, MI: Dr. Chase's
steam printing House, 1868. Print.
[9] William D. Callister and David G. Rethwisch., Fundamentals of materials science and
engineering: an integrated approach. Hoboken (N.J.): Wiley, 2016. Print.
[10] Sargent-Welch Scientific, “Periodic Table of the Elements”, Skokie, Illinois, N.D.
[11] ASM Metals Reference Book, Third edition, Michael Bauccio, Ed. ASM International,
Materials Park, OH, 1993.
[12] Dawson and Hollinger, “The Effect of Metallurgical Variables on the Machinability of
Compacted Graphite Iron”, SinterCast Technologies AB, Sweden, 2001
[13] "Giesserei Lexikon." Foundry - Lexicon. N.p., n.d. Web. 20 Apr. 2017.
24
[14] Morrogh, “The Status of the Metallurgy of Cast Irons,” Journal of the Iron and Steel
Institute, Jan. 1968, pp. 1-10.
[15] John Campbell. Complete casting handbook: metal casting processes, metallurgy,
techniques and design. Amsterdam: Elsevier/Butterworth-Heinemann, 2015. P.277.
[16] History of Metal Casting, “History of Metal Casting: Brief History”
[17] LaRoux K. Gillespie. Troubleshooting manufacturing processes: adapted from the Tool
and manufacturing engineers handbook: a reference book for manufacturing engineers,
managers, and technicians. Dearborn, MI: Society of Manufacturing Engineers, 1988.
[18] Veselinka Đorđević, Corrosion Resistant High Silicon Cast Iron, BMC, Ohrid, R.
Macedonia, 2003
[19] ASTM B962, Standard Test Methods for Density Using Archimedes’ Principle, ASTM
International, West Conshohocken, PA, 2015.
[20] ASTM E3-11, Standard Guide for Preparation of Metallographic Specimens, ASTM
International, West Conshohocken, PA, 2011.
[21] ASTM E562-11, Standard Test Method for Determining Volume Fraction by Systematic
Manual Point Count, ASTM International, West Conshohocken, PA, 2011.
[22] ASTM D4460-97(2015) Standard Practice for Calculating Precision Limits Where Values
are Calculated from Other Test Methods, ASTM International, West Conshohocken, PA,
2015.
[23] "Image Intensity Processing." ImageJ. N.p., n.d. Web. 05 May 2017.

More Related Content

What's hot

1st research article
1st research article1st research article
1st research articleSravani Pappu
 
Mechanochemical reduction of MoO3 powder by silicone to synthesize nanocrysta...
Mechanochemical reduction of MoO3 powder by silicone to synthesize nanocrysta...Mechanochemical reduction of MoO3 powder by silicone to synthesize nanocrysta...
Mechanochemical reduction of MoO3 powder by silicone to synthesize nanocrysta...Hossein Ramezanalizadeh
 
Synthesis, characterization and DC Conductivity Studies of NaCF3SO3 -PEO Dope...
Synthesis, characterization and DC Conductivity Studies of NaCF3SO3 -PEO Dope...Synthesis, characterization and DC Conductivity Studies of NaCF3SO3 -PEO Dope...
Synthesis, characterization and DC Conductivity Studies of NaCF3SO3 -PEO Dope...IJERA Editor
 
Influence of Y2O3 on the structure of Y2O3-doped BaTiO3 powder and ceramics
Influence of Y2O3 on the structure of Y2O3-doped BaTiO3 powder and ceramicsInfluence of Y2O3 on the structure of Y2O3-doped BaTiO3 powder and ceramics
Influence of Y2O3 on the structure of Y2O3-doped BaTiO3 powder and ceramicsIJOEAR Agriculture Research Journal
 
On the role of mechanical milling on structural and morphological features of...
On the role of mechanical milling on structural and morphological features of...On the role of mechanical milling on structural and morphological features of...
On the role of mechanical milling on structural and morphological features of...Hossein Ramezanalizadeh
 
Preparation of mo si2–al2o3 nano composite via mashs route
Preparation of mo si2–al2o3 nano composite via mashs routePreparation of mo si2–al2o3 nano composite via mashs route
Preparation of mo si2–al2o3 nano composite via mashs routeHossein Ramezanalizadeh
 
1 s2.0-s092583881402461 x-main
1 s2.0-s092583881402461 x-main1 s2.0-s092583881402461 x-main
1 s2.0-s092583881402461 x-mainXiomara Lopez
 
The microstructural revolution of al 10%al3 mg2 nanocomposite during mechanic...
The microstructural revolution of al 10%al3 mg2 nanocomposite during mechanic...The microstructural revolution of al 10%al3 mg2 nanocomposite during mechanic...
The microstructural revolution of al 10%al3 mg2 nanocomposite during mechanic...Hossein Ramezanalizadeh
 
Wear behavior of al cma-type al3 mg2nanocomposites fabricated by mechanical m...
Wear behavior of al cma-type al3 mg2nanocomposites fabricated by mechanical m...Wear behavior of al cma-type al3 mg2nanocomposites fabricated by mechanical m...
Wear behavior of al cma-type al3 mg2nanocomposites fabricated by mechanical m...Hossein Ramezanalizadeh
 
Influence of Ruthenium doping on Structural and Morphological Properties of M...
Influence of Ruthenium doping on Structural and Morphological Properties of M...Influence of Ruthenium doping on Structural and Morphological Properties of M...
Influence of Ruthenium doping on Structural and Morphological Properties of M...IJERA Editor
 

What's hot (18)

Crystal growth and Design
Crystal growth and DesignCrystal growth and Design
Crystal growth and Design
 
1st research article
1st research article1st research article
1st research article
 
duplex artigo
duplex artigoduplex artigo
duplex artigo
 
F0363341
F0363341F0363341
F0363341
 
Effects of addition of BaTiO3 Nano particles on the conductivity of PVdF/PMMA...
Effects of addition of BaTiO3 Nano particles on the conductivity of PVdF/PMMA...Effects of addition of BaTiO3 Nano particles on the conductivity of PVdF/PMMA...
Effects of addition of BaTiO3 Nano particles on the conductivity of PVdF/PMMA...
 
20120140504007 2
20120140504007 220120140504007 2
20120140504007 2
 
Mechanochemical reduction of MoO3 powder by silicone to synthesize nanocrysta...
Mechanochemical reduction of MoO3 powder by silicone to synthesize nanocrysta...Mechanochemical reduction of MoO3 powder by silicone to synthesize nanocrysta...
Mechanochemical reduction of MoO3 powder by silicone to synthesize nanocrysta...
 
Synthesis, characterization and DC Conductivity Studies of NaCF3SO3 -PEO Dope...
Synthesis, characterization and DC Conductivity Studies of NaCF3SO3 -PEO Dope...Synthesis, characterization and DC Conductivity Studies of NaCF3SO3 -PEO Dope...
Synthesis, characterization and DC Conductivity Studies of NaCF3SO3 -PEO Dope...
 
Cx34600604
Cx34600604Cx34600604
Cx34600604
 
Influence of Y2O3 on the structure of Y2O3-doped BaTiO3 powder and ceramics
Influence of Y2O3 on the structure of Y2O3-doped BaTiO3 powder and ceramicsInfluence of Y2O3 on the structure of Y2O3-doped BaTiO3 powder and ceramics
Influence of Y2O3 on the structure of Y2O3-doped BaTiO3 powder and ceramics
 
On the role of mechanical milling on structural and morphological features of...
On the role of mechanical milling on structural and morphological features of...On the role of mechanical milling on structural and morphological features of...
On the role of mechanical milling on structural and morphological features of...
 
Preparation of mo si2–al2o3 nano composite via mashs route
Preparation of mo si2–al2o3 nano composite via mashs routePreparation of mo si2–al2o3 nano composite via mashs route
Preparation of mo si2–al2o3 nano composite via mashs route
 
1 s2.0-s092583881402461 x-main
1 s2.0-s092583881402461 x-main1 s2.0-s092583881402461 x-main
1 s2.0-s092583881402461 x-main
 
The microstructural revolution of al 10%al3 mg2 nanocomposite during mechanic...
The microstructural revolution of al 10%al3 mg2 nanocomposite during mechanic...The microstructural revolution of al 10%al3 mg2 nanocomposite during mechanic...
The microstructural revolution of al 10%al3 mg2 nanocomposite during mechanic...
 
Wear behavior of al cma-type al3 mg2nanocomposites fabricated by mechanical m...
Wear behavior of al cma-type al3 mg2nanocomposites fabricated by mechanical m...Wear behavior of al cma-type al3 mg2nanocomposites fabricated by mechanical m...
Wear behavior of al cma-type al3 mg2nanocomposites fabricated by mechanical m...
 
Structure revision of asperjinone using computer assisted structure elucidati...
Structure revision of asperjinone using computer assisted structure elucidati...Structure revision of asperjinone using computer assisted structure elucidati...
Structure revision of asperjinone using computer assisted structure elucidati...
 
Influence of Ruthenium doping on Structural and Morphological Properties of M...
Influence of Ruthenium doping on Structural and Morphological Properties of M...Influence of Ruthenium doping on Structural and Morphological Properties of M...
Influence of Ruthenium doping on Structural and Morphological Properties of M...
 
Ijmet 10 01_079
Ijmet 10 01_079Ijmet 10 01_079
Ijmet 10 01_079
 

Similar to Mat 203 - memo to supervisor

Selective Oxidation of Cyclohexene, Toluene and Ethyl Benzene Catalyzed by Bi...
Selective Oxidation of Cyclohexene, Toluene and Ethyl Benzene Catalyzed by Bi...Selective Oxidation of Cyclohexene, Toluene and Ethyl Benzene Catalyzed by Bi...
Selective Oxidation of Cyclohexene, Toluene and Ethyl Benzene Catalyzed by Bi...Iranian Chemical Society
 
Thickness Dependent Structure and Magnetic Properties in Fe/Ti/Co Multilayers
Thickness Dependent Structure and Magnetic Properties in Fe/Ti/Co MultilayersThickness Dependent Structure and Magnetic Properties in Fe/Ti/Co Multilayers
Thickness Dependent Structure and Magnetic Properties in Fe/Ti/Co MultilayersDr. Vishal Jain
 
2000 guerman-pyrochemistry technetium
2000 guerman-pyrochemistry technetium2000 guerman-pyrochemistry technetium
2000 guerman-pyrochemistry technetiumKonstantin German
 
Scholar Day Presentation Poster
Scholar Day Presentation PosterScholar Day Presentation Poster
Scholar Day Presentation PosterBrandon Alexander
 
Synthesis & Bio-Evaluation of 4-Amino-5-Benzyl-2, 4-Dihydro-3H-1, 2, 4-Triazo...
Synthesis & Bio-Evaluation of 4-Amino-5-Benzyl-2, 4-Dihydro-3H-1, 2, 4-Triazo...Synthesis & Bio-Evaluation of 4-Amino-5-Benzyl-2, 4-Dihydro-3H-1, 2, 4-Triazo...
Synthesis & Bio-Evaluation of 4-Amino-5-Benzyl-2, 4-Dihydro-3H-1, 2, 4-Triazo...IJERA Editor
 
Hydrothermal alteration zones
Hydrothermal alteration zonesHydrothermal alteration zones
Hydrothermal alteration zonesOmer M. Ahmed
 
Annual Report 2022-23_TEM Facility Activities (2022-2023).pdf
Annual Report 2022-23_TEM Facility Activities (2022-2023).pdfAnnual Report 2022-23_TEM Facility Activities (2022-2023).pdf
Annual Report 2022-23_TEM Facility Activities (2022-2023).pdfAmbujMishra77
 
Minerals 08-00601 (1)- carmeltazite - new mineral
Minerals 08-00601 (1)- carmeltazite - new mineralMinerals 08-00601 (1)- carmeltazite - new mineral
Minerals 08-00601 (1)- carmeltazite - new mineralJames AH Campbell
 
Minerals 08-00601 Carmeltazite- new mineral
Minerals 08-00601 Carmeltazite- new mineralMinerals 08-00601 Carmeltazite- new mineral
Minerals 08-00601 Carmeltazite- new mineralJames AH Campbell
 
surface characteristics and electrochemical impedance investigation of spark-...
surface characteristics and electrochemical impedance investigation of spark-...surface characteristics and electrochemical impedance investigation of spark-...
surface characteristics and electrochemical impedance investigation of spark-...mohammad fazel
 
Investigation of the distribution of lead in three different combinations of ...
Investigation of the distribution of lead in three different combinations of ...Investigation of the distribution of lead in three different combinations of ...
Investigation of the distribution of lead in three different combinations of ...Rautomead Limited
 
1 s2.0-s0167577 x10009705-main
1 s2.0-s0167577 x10009705-main1 s2.0-s0167577 x10009705-main
1 s2.0-s0167577 x10009705-mainRiyan Angela
 
Performance Analysis of Low Loss Gas Filled Hollow Core Photonic Crystal Fibe...
Performance Analysis of Low Loss Gas Filled Hollow Core Photonic Crystal Fibe...Performance Analysis of Low Loss Gas Filled Hollow Core Photonic Crystal Fibe...
Performance Analysis of Low Loss Gas Filled Hollow Core Photonic Crystal Fibe...IOSRJECE
 
AusteniticAndFerriticStainlessSteelsInHighTemperatureCokingAtmosphere
AusteniticAndFerriticStainlessSteelsInHighTemperatureCokingAtmosphereAusteniticAndFerriticStainlessSteelsInHighTemperatureCokingAtmosphere
AusteniticAndFerriticStainlessSteelsInHighTemperatureCokingAtmosphereSteven Acker
 
2011 Acta Materialia A P T Steel Fe Mn
2011  Acta  Materialia  A P T  Steel  Fe  Mn2011  Acta  Materialia  A P T  Steel  Fe  Mn
2011 Acta Materialia A P T Steel Fe MnDierk Raabe
 
Structure and band gap energies of nano titanium dioxide doped with the fifth...
Structure and band gap energies of nano titanium dioxide doped with the fifth...Structure and band gap energies of nano titanium dioxide doped with the fifth...
Structure and band gap energies of nano titanium dioxide doped with the fifth...Alexander Decker
 
10.1016@j.jorganchem.2014.11.025
10.1016@j.jorganchem.2014.11.02510.1016@j.jorganchem.2014.11.025
10.1016@j.jorganchem.2014.11.025Gleb Denisov
 
Improve1_MyFinalPresentation
Improve1_MyFinalPresentationImprove1_MyFinalPresentation
Improve1_MyFinalPresentationJojo Pak
 

Similar to Mat 203 - memo to supervisor (20)

Selective Oxidation of Cyclohexene, Toluene and Ethyl Benzene Catalyzed by Bi...
Selective Oxidation of Cyclohexene, Toluene and Ethyl Benzene Catalyzed by Bi...Selective Oxidation of Cyclohexene, Toluene and Ethyl Benzene Catalyzed by Bi...
Selective Oxidation of Cyclohexene, Toluene and Ethyl Benzene Catalyzed by Bi...
 
Thickness Dependent Structure and Magnetic Properties in Fe/Ti/Co Multilayers
Thickness Dependent Structure and Magnetic Properties in Fe/Ti/Co MultilayersThickness Dependent Structure and Magnetic Properties in Fe/Ti/Co Multilayers
Thickness Dependent Structure and Magnetic Properties in Fe/Ti/Co Multilayers
 
2000 guerman-pyrochemistry technetium
2000 guerman-pyrochemistry technetium2000 guerman-pyrochemistry technetium
2000 guerman-pyrochemistry technetium
 
Scholar Day Presentation Poster
Scholar Day Presentation PosterScholar Day Presentation Poster
Scholar Day Presentation Poster
 
Synthesis & Bio-Evaluation of 4-Amino-5-Benzyl-2, 4-Dihydro-3H-1, 2, 4-Triazo...
Synthesis & Bio-Evaluation of 4-Amino-5-Benzyl-2, 4-Dihydro-3H-1, 2, 4-Triazo...Synthesis & Bio-Evaluation of 4-Amino-5-Benzyl-2, 4-Dihydro-3H-1, 2, 4-Triazo...
Synthesis & Bio-Evaluation of 4-Amino-5-Benzyl-2, 4-Dihydro-3H-1, 2, 4-Triazo...
 
Hydrothermal alteration zones
Hydrothermal alteration zonesHydrothermal alteration zones
Hydrothermal alteration zones
 
Annual Report 2022-23_TEM Facility Activities (2022-2023).pdf
Annual Report 2022-23_TEM Facility Activities (2022-2023).pdfAnnual Report 2022-23_TEM Facility Activities (2022-2023).pdf
Annual Report 2022-23_TEM Facility Activities (2022-2023).pdf
 
Minerals 08-00601 (1)- carmeltazite - new mineral
Minerals 08-00601 (1)- carmeltazite - new mineralMinerals 08-00601 (1)- carmeltazite - new mineral
Minerals 08-00601 (1)- carmeltazite - new mineral
 
Minerals 08-00601 Carmeltazite- new mineral
Minerals 08-00601 Carmeltazite- new mineralMinerals 08-00601 Carmeltazite- new mineral
Minerals 08-00601 Carmeltazite- new mineral
 
2005 tc c-tc-met-jn6316
2005 tc c-tc-met-jn63162005 tc c-tc-met-jn6316
2005 tc c-tc-met-jn6316
 
surface characteristics and electrochemical impedance investigation of spark-...
surface characteristics and electrochemical impedance investigation of spark-...surface characteristics and electrochemical impedance investigation of spark-...
surface characteristics and electrochemical impedance investigation of spark-...
 
Investigation of the distribution of lead in three different combinations of ...
Investigation of the distribution of lead in three different combinations of ...Investigation of the distribution of lead in three different combinations of ...
Investigation of the distribution of lead in three different combinations of ...
 
Masters Poster Final Draft
Masters Poster Final DraftMasters Poster Final Draft
Masters Poster Final Draft
 
1 s2.0-s0167577 x10009705-main
1 s2.0-s0167577 x10009705-main1 s2.0-s0167577 x10009705-main
1 s2.0-s0167577 x10009705-main
 
Performance Analysis of Low Loss Gas Filled Hollow Core Photonic Crystal Fibe...
Performance Analysis of Low Loss Gas Filled Hollow Core Photonic Crystal Fibe...Performance Analysis of Low Loss Gas Filled Hollow Core Photonic Crystal Fibe...
Performance Analysis of Low Loss Gas Filled Hollow Core Photonic Crystal Fibe...
 
AusteniticAndFerriticStainlessSteelsInHighTemperatureCokingAtmosphere
AusteniticAndFerriticStainlessSteelsInHighTemperatureCokingAtmosphereAusteniticAndFerriticStainlessSteelsInHighTemperatureCokingAtmosphere
AusteniticAndFerriticStainlessSteelsInHighTemperatureCokingAtmosphere
 
2011 Acta Materialia A P T Steel Fe Mn
2011  Acta  Materialia  A P T  Steel  Fe  Mn2011  Acta  Materialia  A P T  Steel  Fe  Mn
2011 Acta Materialia A P T Steel Fe Mn
 
Structure and band gap energies of nano titanium dioxide doped with the fifth...
Structure and band gap energies of nano titanium dioxide doped with the fifth...Structure and band gap energies of nano titanium dioxide doped with the fifth...
Structure and band gap energies of nano titanium dioxide doped with the fifth...
 
10.1016@j.jorganchem.2014.11.025
10.1016@j.jorganchem.2014.11.02510.1016@j.jorganchem.2014.11.025
10.1016@j.jorganchem.2014.11.025
 
Improve1_MyFinalPresentation
Improve1_MyFinalPresentationImprove1_MyFinalPresentation
Improve1_MyFinalPresentation
 

More from Tech Tanasarnsopaporn

Interview of Arnett Edwards about LPC, and teachers & students from Coral Mon...
Interview of Arnett Edwards about LPC, and teachers & students from Coral Mon...Interview of Arnett Edwards about LPC, and teachers & students from Coral Mon...
Interview of Arnett Edwards about LPC, and teachers & students from Coral Mon...Tech Tanasarnsopaporn
 
60e2fab4-8222-41a9-a256-cab9c59949f2-170109183050
60e2fab4-8222-41a9-a256-cab9c59949f2-17010918305060e2fab4-8222-41a9-a256-cab9c59949f2-170109183050
60e2fab4-8222-41a9-a256-cab9c59949f2-170109183050Tech Tanasarnsopaporn
 
Lehigh Hyperloop Preliminary Design Briefing 2017 (2)
Lehigh Hyperloop Preliminary Design Briefing 2017 (2)Lehigh Hyperloop Preliminary Design Briefing 2017 (2)
Lehigh Hyperloop Preliminary Design Briefing 2017 (2)Tech Tanasarnsopaporn
 

More from Tech Tanasarnsopaporn (6)

Interview of Arnett Edwards about LPC, and teachers & students from Coral Mon...
Interview of Arnett Edwards about LPC, and teachers & students from Coral Mon...Interview of Arnett Edwards about LPC, and teachers & students from Coral Mon...
Interview of Arnett Edwards about LPC, and teachers & students from Coral Mon...
 
Inverts presentation -2
Inverts presentation -2Inverts presentation -2
Inverts presentation -2
 
Coral Monitoring QC Service Fair_v2
Coral Monitoring QC Service Fair_v2Coral Monitoring QC Service Fair_v2
Coral Monitoring QC Service Fair_v2
 
coral eco 2013-14 interim report r1
coral eco 2013-14 interim report r1coral eco 2013-14 interim report r1
coral eco 2013-14 interim report r1
 
60e2fab4-8222-41a9-a256-cab9c59949f2-170109183050
60e2fab4-8222-41a9-a256-cab9c59949f2-17010918305060e2fab4-8222-41a9-a256-cab9c59949f2-170109183050
60e2fab4-8222-41a9-a256-cab9c59949f2-170109183050
 
Lehigh Hyperloop Preliminary Design Briefing 2017 (2)
Lehigh Hyperloop Preliminary Design Briefing 2017 (2)Lehigh Hyperloop Preliminary Design Briefing 2017 (2)
Lehigh Hyperloop Preliminary Design Briefing 2017 (2)
 

Recently uploaded

Introduction to Artificial Intelligence and History of AI
Introduction to Artificial Intelligence and History of AIIntroduction to Artificial Intelligence and History of AI
Introduction to Artificial Intelligence and History of AISheetal Jain
 
Research Methodolgy & Intellectual Property Rights Series 1
Research Methodolgy & Intellectual Property Rights Series 1Research Methodolgy & Intellectual Property Rights Series 1
Research Methodolgy & Intellectual Property Rights Series 1T.D. Shashikala
 
ALCOHOL PRODUCTION- Beer Brewing Process.pdf
ALCOHOL PRODUCTION- Beer Brewing Process.pdfALCOHOL PRODUCTION- Beer Brewing Process.pdf
ALCOHOL PRODUCTION- Beer Brewing Process.pdfMadan Karki
 
Dynamo Scripts for Task IDs and Space Naming.pptx
Dynamo Scripts for Task IDs and Space Naming.pptxDynamo Scripts for Task IDs and Space Naming.pptx
Dynamo Scripts for Task IDs and Space Naming.pptxMustafa Ahmed
 
Linux Systems Programming: Semaphores, Shared Memory, and Message Queues
Linux Systems Programming: Semaphores, Shared Memory, and Message QueuesLinux Systems Programming: Semaphores, Shared Memory, and Message Queues
Linux Systems Programming: Semaphores, Shared Memory, and Message QueuesRashidFaridChishti
 
What is Coordinate Measuring Machine? CMM Types, Features, Functions
What is Coordinate Measuring Machine? CMM Types, Features, FunctionsWhat is Coordinate Measuring Machine? CMM Types, Features, Functions
What is Coordinate Measuring Machine? CMM Types, Features, FunctionsVIEW
 
Module-III Varried Flow.pptx GVF Definition, Water Surface Profile Dynamic Eq...
Module-III Varried Flow.pptx GVF Definition, Water Surface Profile Dynamic Eq...Module-III Varried Flow.pptx GVF Definition, Water Surface Profile Dynamic Eq...
Module-III Varried Flow.pptx GVF Definition, Water Surface Profile Dynamic Eq...Nitin Sonavane
 
Artificial Intelligence in due diligence
Artificial Intelligence in due diligenceArtificial Intelligence in due diligence
Artificial Intelligence in due diligencemahaffeycheryld
 
The Entity-Relationship Model(ER Diagram).pptx
The Entity-Relationship Model(ER Diagram).pptxThe Entity-Relationship Model(ER Diagram).pptx
The Entity-Relationship Model(ER Diagram).pptxMANASINANDKISHORDEOR
 
Augmented Reality (AR) with Augin Software.pptx
Augmented Reality (AR) with Augin Software.pptxAugmented Reality (AR) with Augin Software.pptx
Augmented Reality (AR) with Augin Software.pptxMustafa Ahmed
 
Autodesk Construction Cloud (Autodesk Build).pptx
Autodesk Construction Cloud (Autodesk Build).pptxAutodesk Construction Cloud (Autodesk Build).pptx
Autodesk Construction Cloud (Autodesk Build).pptxMustafa Ahmed
 
5G and 6G refer to generations of mobile network technology, each representin...
5G and 6G refer to generations of mobile network technology, each representin...5G and 6G refer to generations of mobile network technology, each representin...
5G and 6G refer to generations of mobile network technology, each representin...archanaece3
 
Maher Othman Interior Design Portfolio..
Maher Othman Interior Design Portfolio..Maher Othman Interior Design Portfolio..
Maher Othman Interior Design Portfolio..MaherOthman7
 
Tembisa Central Terminating Pills +27838792658 PHOMOLONG Top Abortion Pills F...
Tembisa Central Terminating Pills +27838792658 PHOMOLONG Top Abortion Pills F...Tembisa Central Terminating Pills +27838792658 PHOMOLONG Top Abortion Pills F...
Tembisa Central Terminating Pills +27838792658 PHOMOLONG Top Abortion Pills F...drjose256
 
8th International Conference on Soft Computing, Mathematics and Control (SMC ...
8th International Conference on Soft Computing, Mathematics and Control (SMC ...8th International Conference on Soft Computing, Mathematics and Control (SMC ...
8th International Conference on Soft Computing, Mathematics and Control (SMC ...josephjonse
 
Involute of a circle,Square, pentagon,HexagonInvolute_Engineering Drawing.pdf
Involute of a circle,Square, pentagon,HexagonInvolute_Engineering Drawing.pdfInvolute of a circle,Square, pentagon,HexagonInvolute_Engineering Drawing.pdf
Involute of a circle,Square, pentagon,HexagonInvolute_Engineering Drawing.pdfJNTUA
 
Passive Air Cooling System and Solar Water Heater.ppt
Passive Air Cooling System and Solar Water Heater.pptPassive Air Cooling System and Solar Water Heater.ppt
Passive Air Cooling System and Solar Water Heater.pptamrabdallah9
 
Geometric constructions Engineering Drawing.pdf
Geometric constructions Engineering Drawing.pdfGeometric constructions Engineering Drawing.pdf
Geometric constructions Engineering Drawing.pdfJNTUA
 
Lab Manual Arduino UNO Microcontrollar.docx
Lab Manual Arduino UNO Microcontrollar.docxLab Manual Arduino UNO Microcontrollar.docx
Lab Manual Arduino UNO Microcontrollar.docxRashidFaridChishti
 
21scheme vtu syllabus of visveraya technological university
21scheme vtu syllabus of visveraya technological university21scheme vtu syllabus of visveraya technological university
21scheme vtu syllabus of visveraya technological universityMohd Saifudeen
 

Recently uploaded (20)

Introduction to Artificial Intelligence and History of AI
Introduction to Artificial Intelligence and History of AIIntroduction to Artificial Intelligence and History of AI
Introduction to Artificial Intelligence and History of AI
 
Research Methodolgy & Intellectual Property Rights Series 1
Research Methodolgy & Intellectual Property Rights Series 1Research Methodolgy & Intellectual Property Rights Series 1
Research Methodolgy & Intellectual Property Rights Series 1
 
ALCOHOL PRODUCTION- Beer Brewing Process.pdf
ALCOHOL PRODUCTION- Beer Brewing Process.pdfALCOHOL PRODUCTION- Beer Brewing Process.pdf
ALCOHOL PRODUCTION- Beer Brewing Process.pdf
 
Dynamo Scripts for Task IDs and Space Naming.pptx
Dynamo Scripts for Task IDs and Space Naming.pptxDynamo Scripts for Task IDs and Space Naming.pptx
Dynamo Scripts for Task IDs and Space Naming.pptx
 
Linux Systems Programming: Semaphores, Shared Memory, and Message Queues
Linux Systems Programming: Semaphores, Shared Memory, and Message QueuesLinux Systems Programming: Semaphores, Shared Memory, and Message Queues
Linux Systems Programming: Semaphores, Shared Memory, and Message Queues
 
What is Coordinate Measuring Machine? CMM Types, Features, Functions
What is Coordinate Measuring Machine? CMM Types, Features, FunctionsWhat is Coordinate Measuring Machine? CMM Types, Features, Functions
What is Coordinate Measuring Machine? CMM Types, Features, Functions
 
Module-III Varried Flow.pptx GVF Definition, Water Surface Profile Dynamic Eq...
Module-III Varried Flow.pptx GVF Definition, Water Surface Profile Dynamic Eq...Module-III Varried Flow.pptx GVF Definition, Water Surface Profile Dynamic Eq...
Module-III Varried Flow.pptx GVF Definition, Water Surface Profile Dynamic Eq...
 
Artificial Intelligence in due diligence
Artificial Intelligence in due diligenceArtificial Intelligence in due diligence
Artificial Intelligence in due diligence
 
The Entity-Relationship Model(ER Diagram).pptx
The Entity-Relationship Model(ER Diagram).pptxThe Entity-Relationship Model(ER Diagram).pptx
The Entity-Relationship Model(ER Diagram).pptx
 
Augmented Reality (AR) with Augin Software.pptx
Augmented Reality (AR) with Augin Software.pptxAugmented Reality (AR) with Augin Software.pptx
Augmented Reality (AR) with Augin Software.pptx
 
Autodesk Construction Cloud (Autodesk Build).pptx
Autodesk Construction Cloud (Autodesk Build).pptxAutodesk Construction Cloud (Autodesk Build).pptx
Autodesk Construction Cloud (Autodesk Build).pptx
 
5G and 6G refer to generations of mobile network technology, each representin...
5G and 6G refer to generations of mobile network technology, each representin...5G and 6G refer to generations of mobile network technology, each representin...
5G and 6G refer to generations of mobile network technology, each representin...
 
Maher Othman Interior Design Portfolio..
Maher Othman Interior Design Portfolio..Maher Othman Interior Design Portfolio..
Maher Othman Interior Design Portfolio..
 
Tembisa Central Terminating Pills +27838792658 PHOMOLONG Top Abortion Pills F...
Tembisa Central Terminating Pills +27838792658 PHOMOLONG Top Abortion Pills F...Tembisa Central Terminating Pills +27838792658 PHOMOLONG Top Abortion Pills F...
Tembisa Central Terminating Pills +27838792658 PHOMOLONG Top Abortion Pills F...
 
8th International Conference on Soft Computing, Mathematics and Control (SMC ...
8th International Conference on Soft Computing, Mathematics and Control (SMC ...8th International Conference on Soft Computing, Mathematics and Control (SMC ...
8th International Conference on Soft Computing, Mathematics and Control (SMC ...
 
Involute of a circle,Square, pentagon,HexagonInvolute_Engineering Drawing.pdf
Involute of a circle,Square, pentagon,HexagonInvolute_Engineering Drawing.pdfInvolute of a circle,Square, pentagon,HexagonInvolute_Engineering Drawing.pdf
Involute of a circle,Square, pentagon,HexagonInvolute_Engineering Drawing.pdf
 
Passive Air Cooling System and Solar Water Heater.ppt
Passive Air Cooling System and Solar Water Heater.pptPassive Air Cooling System and Solar Water Heater.ppt
Passive Air Cooling System and Solar Water Heater.ppt
 
Geometric constructions Engineering Drawing.pdf
Geometric constructions Engineering Drawing.pdfGeometric constructions Engineering Drawing.pdf
Geometric constructions Engineering Drawing.pdf
 
Lab Manual Arduino UNO Microcontrollar.docx
Lab Manual Arduino UNO Microcontrollar.docxLab Manual Arduino UNO Microcontrollar.docx
Lab Manual Arduino UNO Microcontrollar.docx
 
21scheme vtu syllabus of visveraya technological university
21scheme vtu syllabus of visveraya technological university21scheme vtu syllabus of visveraya technological university
21scheme vtu syllabus of visveraya technological university
 

Mat 203 - memo to supervisor

  • 1. 1 MEMORANDUM Date: 5 May 2017 To: Dr. Charles E. Lyman, Supervisor From: Tech Tanasarnsopaporn Subject: Investigation of Material Composition in Mysterious Historical Subject: Metal Fence Executive Summary The objective of this investigation is to identify the metallographic composition of the sample and to determine the possible manufacturing process of the fence. The material is composed of approximately 81.12% α-Fe and cementite pearlitic matrix, 17.2% graphite, 10.21% Fe3P, 1.52% TiC, 0.51% TiN, 2.85% MnS, and 1.6% pores by volume fraction. It is concluded that the metal fence is a pearlitic gray cast iron ASTM A48 casted in a sand mold for a low-volume production. The presence of alloying elements resulted in phases including iron phosphide (Fe3P) which increases flowability and allows more complex designs to be made, titanium carbide (TiC) which increases strength, titanium nitride (TiN) which increases wear resistance, manganese sulfide (MnS) which removes sulfur contaminants to increase strength and flowability, and silicon-iron matrix which increases the corrosion resistance. Background An unknown specimen under investigation is a section of a metal fence procured from a household region of Bethlehem, Pennsylvania and was made in the mid-to-late 18th century (Appendix 3, figure 1). The sample was a small section with rough surface covered with thick layer of red-colored rust. The objective of this investigation is to identify the composition of the sample and to conclude the possible manufacturing process of the fence. Method The preliminary examination includes an unaided color observation of rust (oxide layer)
  • 2. 2 and metallic piece it enveloped, the density of the metallic piece using Archimedes’ method (ASTM B962-15), and the magnetic property using a magnet test (Appendix 1, section 1). The sample was then metallographically prepared (ASTM E3-11) and observed under Light Optical Microscope (LOM) (ASTM E562) (Appendix 1, section 2), Scanning Electron Microscope and Energy-Dispersive Spectrometry (SEM/EDS) (ASTM E1508), Powder X-ray Diffraction (XRD) (ASTM D3906), and Transmission Electron Microscope (TEM) with Selected Area Diffraction (SAD). The collected data was finally analyzed and compared with the information from various accepted literatures listed in the reference section. Result The investigation shows that the material is comprises of pearlite (α-Fe and cementite), graphite, iron phosphide (Fe3P), titanium carbide (TiC), titanium nitride (TiN), and manganese sulfide (MnS) with porous regions scattered throughout the sample. The evidence for each phase is described under the subheadings below. All procedures and methods of calculation are included in Appendix 1; tables are in Appendix 2; and. figures are in Appendix 3. The detailed results are summarized in table 1. Ferrite The material has silvery-gray color with dark red oxide layer and exhibits ferromagnetism, all of which suggests a high composition of iron (Fe) in the sample. This result is reaffirmed with the strong characteristic x-ray peaks in XRD (Table 5) and the EDS result of 89.90 ± 0.50% α-Fe volume fraction (Table 4). LOM and SEM also show pearlitic microstructures with volume fraction of the matrix phase of 70.4 ± 3.0% which confirm the presence of ferrite (α-Fe) (Table 3). Cementite The strong characteristic x-ray peaks in XRD of Fe3C are the evidence of cementite
  • 3. 3 (Table 5). The pearlitic microstructures found in LOM and SEM also confirm the presence of cementite (Fe3C) within the matrix phase (Table 3). Cementite within each pearlite colony has a characteristic of a lamella with 0.3 ± 0.05 µm wide on average, aligned in the same direction, suggesting that the colonies are fine pearlite (Table 1) [1]. Moreover, the density of the sample was found to be 6.6 ± 0.5 g/mL, closely resembles that of cast iron with density of 6.8-7.8 g/mL (Figure 1) [1]. The density lower than that of pure iron can be explained by corrosion which was seen as rust and the presence of 1.6 ± 1.0% porosity by volume fraction as analyzed from optical micrographs (Table 1). The size of the pores was also found to be 4 ± 0.5 µm in diameter on average (Table 1). Graphite Flakes A significant amount of black carbon flakes was also seen in LOM and SEM. In various areas on the sample, EDS x-ray mapping also shows pure carbon composition (Figure 5-6); thus, these regions must contain some stable allotropes of carbon. The XRD result further confirms that the carbon phase present is in graphite form (Table 5). In the optical micrograph and SEM, the graphite phases were seen to be in the form of rosette flake graphite with 80 µm diameter and 2 ± 0.5 µm x 30 ± 0.5 µm per flake (ASTM Type B) (Table 1) [3]. These flakes have the characteristics of rosette grouping in random orientations pointing out radially from the center of the group. Some nodular graphite with 7 µm diameter (ISO Form VI) was also observed (Table 1, Figure 2-3) [3]. Under LOM, the volume fractions of flake graphite and nodular graphite are found to be 15.6 ± 2.5 % and 1.6 ± 1.0 %, respectively (Table 1). Iron Phosphide In addition to α-Fe and Fe3C, the Fe-P phase was observed in EDS, XRD, and TEM. The X-ray pattern in TEM-SAD identified a 10 ± 0.5µm x 10 ± 0.5µm region with non-homogeneous characteristics and well-distributed white dots to be a phase containing phosphorus and iron
  • 4. 4 peaks. With EDS x-ray mapping, the volume fraction of this Fe-P phase was estimated to be 10.21 ± 0.30% (Table 4). The more accurate analysis with XRD was then able to reveal the tertiary ferritic phase to be iron phosphide or Fe3P (Table 5). TEM-SAD was then used to determine the dhkl of this region, which corresponds to the accepted values of Fe3P in The International Centre for Diffraction Data (ICDD)’s Powder Diffraction File (PDF) database [2]. Titanium Carbide While the LOM shows the carbon phases to have the total of 17.2 ± 3.5% (Table 3), the EDS result shows the volume fraction of carbon-containing regions to be 22.92 ± 3.44% (Table 4). This discrepancy can be explained with the discovery of Ti-C phase in EDS x-ray mapping, which shows the overlaps of titanium and carbon regions. The volume fraction of Ti-C region is approximately 1.52 ± 0.04% with the cubic crystal shape and 2 ± 0.5 µm x 5 ± 0.5 µm in size (Table 1). While small percent volume fraction is present, the XRD detected faint signal of TiC phase in the sample (Table 5). The TEM-SAD further reaffirms that the unique faceted region containing Ti-C has the Fm3m space group crystal, and the dhkl matching that of Titanium Carbide or TiC (Table 6) [4]. Titanium Nitride While the XRD cannot be used to accurately detect phases with percent volume fraction less than 1% [5], the small cubic crystalline precipitates (2 µm x 2 µm) found in LOM were investigated under EDS and TEM (Table 1). The EDS x-ray mapping shows regions containing both titanium and nitrogen with the volume fraction of approximately 0.51 ± 0.06% (Table 4). TEM-SAD suggests that the unique region containing Ti-N has the Fm3m space group crystal and the dhkl matching that of Titanium Nitride or TiN [6] (Table 6). Manganese Sulfide The EDS x-ray mapping shows another region with manganese and sulfur with 2.85 ±
  • 5. 5 1.79% volume fraction (Table 4). TEM-SAD suggests that the small (2µm x 2µm) cubic crystals containing Mn-S has the Fm3m space group crystal and the dhkl matching that of manganese sulfide or MnS (Table 6) [7]. As MnS crystal has a light pink color, this agrees with the pink color of the cubic crystal found in various sites throughout the LOM micrograph (Figure 3) [8]. Silicon Silicon was observed throughout the sample when using EDS x-ray mapping with the volume fraction of 59.20 ± 3.72% (Table 5). By looking closely at the x-ray mapping, it appears that silicon is scattered almost uniformly over the region containing iron. This can be explained as the matrix of iron and silicon, which is commonly seen in a high silicon cast iron [18]. Discussion The result of the investigation shows that The material is composed of approximately 81.12% α-Fe and cementite pearlitic matrix, 17.2% graphite, 10.21% Fe3P, 1.52% TiC, 0.51% TiN, 2.85% MnS, and 1.6% pores by volume fraction. The calculated weight fraction shows carbon with over 2.14 wt%, which suggests that the specimen is a type of cast iron (Table 7) [9, 10]. By considering the Fe-C phase diagram at 3.23 wt%C (Figure 22-23), the Fe-C system should form graphite precipitates and a large amount of pearlite which is confirmed by the result shown in Table 1 [11]. By comparing the weight percent composition and other experimental results with ASTM alloy designation of cast irons [9, 11], this unknown specimen was found to be Gray Cast Iron ASTM A48 (Table 7), an easily machined and ductile alloy [11]. Another important clue to find out the original manufacturing process is its rosette graphite flakes that can only be found in gray cast iron [11]. Since manufacturing pearlitic gray cast iron involves fast cooling during tempering process to form pearlite colonies, the evidence from LOM and SEM showing the large volume fraction of fine pearlite suggests that this cast iron is indeed a pearlitic gray cast iron (Table 3) [9].
  • 6. 6 Furthermore, the presence of Fe3P, TiC, TiN, MnS, and Si displays some interesting alloying technologies that might have been used during the production of this fence. Since the quality of casting depends on the fluidity of molten iron, phosphorus is sometimes added to form a network of low-melting-point phosphorous eutectic phase (Fe3P) to increase flowability and widen processing window [12]. During 19th century, titanium was traditionally considered a contaminant from the iron ore extraction process, and it was not widely used an alloy element However, titanium can combine with carbon to form hard TiC precipitates which increase strength [13]. When molten titanium combines with nitrogen in the hot air and forms TiN precipitate, the wear resistance will also be improved [14]. Moreover, as sulfur is another major contaminant from iron ore processing which causes the molten iron to be viscous, manganese is added to form MnS which neutralizes the effect [15]. Furthermore, the high level of silicon means that excess silicon might be intentionally used in alloying. As shown in high silicon cast iron (HSCI), silicon is an inexpensive alloying element to improve the corrosion resistance [15]. Other observations include the low dimensional details such as the high curvature around the corner of the specimen which indicates that the mold material has low resolution (Figure 1). Thus, it is likely that this metal fence is casted in a sand mold – a fast and inexpensive metal manufacturing process typically used during that period [16]. The small porous voids also suggest that the fence was casted by a small volume at a time i.e. few kilograms [17]. Moreover, the ASTM type B rosette-shaped graphite flakes are a characteristic of a thin-walled casting (i.e. die casting), which is suitable for a small- to medium-sized casting [18]. To conclude, the metal fence under investigation is a pearlitic gray cast iron (ASTM A48) casted in sand mold for a low-volume production while various alloying elements including Fe3P, TiC, TiN, MnS, and Si were included to improve wear resistance and strength of the fence and to allow the more complex designs to be made.
  • 7. 7 Appendix 1: Procedure and methods of calculation Section 1. Preliminary Examination: ASTM B962-15 [19] With a simple magnet test, the metal was discovered to be magnetic. Then, density measurements were made before and after the oxide layer of the metal was scraped off. These measurements were 5.7 g/mL and 6.6 g/mL, respectively. Section 2. Light Optical Microscopy: ASTM E3-11, ASTM E562 [20,21] A sample of the metal was mounted in Bakelite and metallographically prepared. Using Pax-It and the Olympus TH3 light microscope, images of the unetched sample were captured. The sample was then etched in 4% Picral for 1 second, followed by 1 second in 2% Nital. Images of the etched sample were captured. Then, to measure volume fractions of these phases, the ASTM E562 point count method was performed with a reticle on the ocular of a microscope [1]. Only the flake graphite, nodular graphite, and matrix, believed to be both ferrite and pearlite, were visible under the light microscope without the contrast manipulation feature of Pax-it. After etching, however, the other five phases, including pores, became much more visible. The results of all ten point counts are seen below in Appendix 2, Table 3. Section 3: Comments on uncertainty of the experiment: It is important to note that the experimental results may contain some margin of error in the data for the small, non-ferrous phases from LOM and SEM observations. This is because while the point counting method has the limitation of 0.5%, these phases may be present at less than 1% [11]. Moreover, as outlined in Section 5, the volume fraction of elements observed in EDS x-ray mapping is subjected to the error in threshold values for each phase. Section 4: Precision Calculation: ASTM D4460-97 [22] Precision of experimental data can be calculated as the average deviation of the dataset: 𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝐷𝑒𝑣𝑖𝑎𝑡𝑖𝑜𝑛 = ∑|𝑥−𝜇| 𝑛 , where 𝑥 is the data points, 𝜇 is the mean value of dataset, and 𝑛
  • 8. 8 is the number of data points. For example, in LOM point counting, 𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝐷𝑒𝑣𝑖𝑎𝑡𝑖𝑜𝑛 = (13−15.6)+(19−15.6)+(15−15.6)+(13−15.6)+(18−15.6) 5 % = 2.5% Section 5: Image-J Processing [23] In using the EDS x-ray mapping data, there exist the background noise that can let the experimenter to misinterpret the actual volume percent of each element. This is because of the resolution of the SEM/EDS. In order to reduce the noise, the automated software can be used. Image-J, for example, can readjust the color threshold of the photo such that only when the contrast threshold exceed certain value will the pixel will be counted. First, open the photo in Image-J and go to Process>Binary>Options. Check the "Black Background" box. This is so that pixels with value 0 are shown as black, and those with 255 as white, after the thresholding operation. Open the Threshold tool: Image>Adjust>Threshold. Check the "Dark Background" box. The brighter pixels will be highlighted in red. These red pixels will be mapped to white and the rest to black. Keep the higher threshold (bottom slider) at 255. Click “Auto-Adjust” to let Image-J analyze the background noise and eliminate. Click on the "Apply" button to get a binary image. An effective way to do calculate volume ratio is to look at the histogram by pressing Crtl+H. Then, click “copy” to copy the values and paste into an Excel spreadsheet. The ratio of phases or elements can be found by dividing the number of pixel with threshold at 255 and the total number of pixels of the image. The results are shown in Appendix 3, figure 7.
  • 9. 9 Appendix 2: Tables Table 1. The detailed summary of results from LOM, SEM, EDS, XRD, and TEM/SAD. D- values and space groups were obtained by comparing raw data to ICDD database. Table 2. TEM SAD: Calibration data using diffraction ring pattern of Pure Aluminum observed in TEM. The interplanar spacing is calculated using the ICDD database [3]. Ring diameter=2R (mm) hkl dhkl (Å) 2Rd=2λL λL (mm Å) 23.0 111 2.3380 53.774 26.8 26.5 200 2.0248 53.657 26.8 37.5 220 1.4317 53.689 26.8 Table 3. LOM: Shown in the table below are the results of the point counts of all 10 of the Phase Volume % Size Shape Elements Largest measured d-value PDF value PDF card # Space group Pearlite 81.2 Span across sample Colonies Fe, C N/A N/A N/A N/A - Ferrite N/A Span across colonies N/A Fe 2.04 2.026 00-006-0696 Im3m - Cementite N/A Varied length, 0.3 µm wide Long, thin strands Fe, C 2.541 2.541 00-035-0772 Pnma Rosette Graphite 15.6 80 µm diameter, 2µm x 30µm per flake Rosette, long flakes C 3.357 3.355 00-056-0159 P63/mmc Nodular Graphite 1.6 7 µm diameter Circular C 3.357 3.355 00-056-0159 P63/mmc Iron Phosphide 10.21 10 µm x 10 µm Non- homogeneous, long dots Fe, P 6.469 6.43962 00-051-0943 Fm3m Titanium Carbide 1.52 2 µm x 5 µm Cubic shape Ti, C 2.14 2.1637 00-032-1383 Fm3m Titanium Nitride 0.51 2 µm x 2 µm Cubic shape Ti, N 2.43 2.44917 00-038-1420 Fm3m Manganese Sulfide 2.85 2 µm x 2 µm Cubic shape Mn, S 3.063 3.015 00-006-0518 Fm3m Pores 1.6 4 µm x 4 µm Irregular, round edges N/A N/A N/A N/A N/A
  • 10. 10 phases observed under the Olympus TH3 light microscope with the assistance of a Pax-it camera. For each phase, five fields of view were chosen at random for the point counting. Microconstituent I II III IV V Volume% Precision (±) Flake Graphite 13 19 15 13 18 15.60 2.5 Nodular Graphite 3 2 2 1 0 1.60 1.0 Pearlite (Gray matrix phase) 83 78 82 83 82 81.20 1.4 Manganese Sulfide (Pink Cube) 1 0 0 1 0 0.40 0.5 Titanium Carbide (Blue Cube) 1 0 0 1 0 0.40 0.5 Iron Phosphide (Orange Phase) 0 0 0 0 1 0.20 0.4 Pores 1 2 2 3 0 1.60 1.0 Table 4. EDS: Volume fractions calculated from element x-ray mapping images taken by FEI Scios FIB. The data was then auto correct to reduce background noise using Image-J (Appendix 1, section 5). The average values were calculated and used in analysis. Element Vol% (FEI – raw data) Vol% (Auto-Correct) Average Vol% Precision (±) C K 26.35 19.48% 22.92 3.44 Fe K 90.40 89.40% 89.90 0.50 Mn K 4.63 1.06% 2.85 1.79 Si K 55.48 62.92% 59.20 3.72 S K 1.99 2.12% 2.06 0.07 Ti K 1.99 2.06% 2.03 0.04 N K 0.57 0.44% 0.51 0.06 P K 10.51 9.91% 10.21 0.30
  • 11. 11 Table 5. XRD: Diffraction pattern for various phases observed in XRD as shown in Appendix 3, figure 2-6. The peaks were compared with the standard index diffraction pattern [2]. Phase Measured 2ϴ Measured dhkl (Å) dhkl from PDF card (Å) Difference in d-value (Å) % Deviation hkl PDF card # Fe 44.36 2.040 2.046800 0.00680 0.33% 110 00-006-069665.14 1.431 1.433200 0.00220 0.15% 200 82.46 1.16 1.170200 0.01020 0.87% 220 Fe3C 35.29 2.541 2.545160 0.00416 0.16% 220 00-035-077239.83 2.217 2.218570 0.00157 0.07% 201 49 1.858 1.853400 0.00460 0.25% 221 TiC 35.42 2.532 2.500000 0.03200 1.28% 111 00-03201383 41.5 2.174 2.166000 0.00800 0.37% 200 60.85 1.521 1.531000 0.01000 0.65% 220 75.57 1.258 1.305000 0.04700 3.60% 311 C 35.42 3.293 3.355300 0.06230 1.86% 002 00-056-015942.36 2.132 2.131900 0.00010 0.00% 100 54.66 1.679 1.677700 0.00130 0.08% 004 Fe3P 35.46 2.510 2.529000 0.01900 0.75% 120 00-051-094342.80 2.07 1.990000 0.08000 4.02% 201 45.82 19.940 19.33000 0.61000 3.16% 220
  • 12. 12 Table 6. SAD: Diffraction pattern for various phases observed in TEM/SAD. The interplanar spacing is calculated using camera constant found in Table 2. The ratios of the principal spot spacing were calculated and compared with the standard index diffraction pattern [2]. Phase Measured distance from diffraction pattern (mm) λL (mm Å) Measured dhkl (Å) dhkl from PDF card (Å) hkl Difference in d-value (Å) % Accuracy PDF card # MnS (35÷4)= 8.750 26.8 3.06 3.015 111 0.048 1.59 00-006- 0518 (43÷3)=14.333 26.8 1.87 1.847 220 0.023 1.25 (50÷3)=16.667 26.8 1.61 1.575 311 0.033 2.1 Fe3P (29÷7)= 4.143 26.8 6.47 6.43962 110 0.029 0.45 00-051- 0943(26.5÷3)=12.167 26.8 2.20 2.19874 321 0.004 0.18 TiN 11 26.8 2.43 2.44917 111 –0.019 0.78 00-038- 142012.5 26.8 2.14 2.12071 200 0.019 0.9 TiC 12.5 26.8 2.14 2.1637 200 -0.0237 1.1 00-032- 1383 17.5 26.8 1.53 1.5302 220 -0.0002 0.01 20.5 26.8 1.30 1.3047 311 -0.0047 0.36 Table 7. Weight percent calculation for each element. Atomic weight information is cited from an accepted literature [10]. Weight fraction was then calculated from the values of volume fraction by EDS mapping and the atomic weight of each element. Element Volume % Atomic Weight (g/mol) [12] Molecular Weight Contribution (g/mol) Weight % Wt% of Gray cast iron, Class ASTM A48 [11] Fe 89.40% 55.8470 49.93 68.97 N/A C 19.48% 12.0110 2.34 3.23 3.10-3.40 Mn 1.06% 54.9380 0.58 0.81 0.70-1.00 Si 62.92% 28.0855 17.67 24.41 2.10-1.08 S 2.12% 32.0600 0.68 0.94 0.15 P 10.21% 30.9738 3.16 4.19 0.08 Ti 2.06% 47.9000 0.99 1.36 N/A N 0.44% 14.0067 0.06 0.08 N/A
  • 13. 13 Appendix 3: Figures Figure 1. An unknown object is a portion of a fence produced in the mid-to-late 1800s Figure 2. An image of the unetched mystery metal under a light microscope. The matrix is made up of pearlite and a ferrite. The circles enclose the rosette, which is made up mainly of graphite flakes. The image was taken in Pax-it at 230X magnification.
  • 14. 14 Figures 3. A picture taken of the unetched microstructure. The image was taken at 800X magnification. The high magnification levels help distinguish the differences between the multiple small phases in the mystery material. Phases noted: Blue cube, flake graphite, hexagon, pink cube, triangular structure, and nodular graphite. Figure 4. Site 1 of material at 1000x magnification. The dark phase is flake graphite, and the pearlite stands out strongly as a lamella pattern. Manganese Sulfide (Pink Cube) Titanium Carbide (Blue Cube) Graphite
  • 15. 15 Figure 5. X-ray mapping of unetched sample from FEI Scios FIB EDS at 800x magnification. Figure 6. X-ray mapping of unetched sample from FEI Scios FIB EDS corrected for background detection using Image-J software Auto-Adjust Threshold as described in Appendix 1, section 5.
  • 16. 16 Figure 7. XRD Pattern of the iron peaks in unknown material. The corresponding hkl values are shown in Table 5. PDF card # 00-006-0696 Figure 8. XRD Pattern of Cementite peaks in material. The corresponding hkl values are shown in Table 5. PDF card # 00-035-0772 2.217
  • 17. 17 Figure 9. XRD Pattern of Titanium Carbide in metal. The corresponding hkl values are shown in Table 5. PDF card # 00-03201383 Figure 10. XRD Pattern of Graphite. The corresponding hkl values are shown in Table 5. PDF card # 00-056-0159
  • 18. 18 Figure 11. XRD Pattern of Iron Phosphide in the unknown. The corresponding hkl values are shown in Table 5. PDF card # 00-051-0943 Figure 12. Adapted from the TEM/SAD diffraction pattern of MnS with camera length of 0.6 m, a high voltage of 120kV. The labels show the corresponding zone axis of electron diffraction patterns, and measured d-values are noted. PDF# 00-006-0518 Fe3P 2θ = 35.46º d = 2.510 2θ = 45.82º d = 1.940 2θ = 42.80º d = 2.070 [220] 1.87Å [311] 1.61Å [111] 3.06Å
  • 19. 19 Figure 13. Adapted from the TEM/SAD diffraction pattern of Fe3P with camera length of 0.6 m, a high voltage of 120kV. The labels show the corresponding zone axis of electron diffraction patterns, and measured d-values are noted. PDF# 00-051-0943 Figure 14. Adapted from the TEM/SAD diffraction pattern of TiN with camera length of 0.6 m, a high voltage of 120kV. The labels show the corresponding zone axis of electron diffraction patterns, and measured d-values are noted. PDF# 00-038-1420 [200] 2.14Å [111] 2.43Å [110] 6.47Å [321] 2.20Å
  • 20. 20 Figure 15. Adapted from the TEM/SAD diffraction pattern of TiC (facetted particle) with camera length of 0.6 m, a high voltage of 120kV. The labels show the corresponding zone axis of electron diffraction patterns, and measured d-values are noted. PDF# 00-032-1383 Figure 16. Excerpt of ICDD Ferrite XRD Pattern PDF Card # 00-006-0696 Figure 17. Excerpt of ICDD Cementite XRD Pattern PDF Card # 00-035-0772 [200] 2.14Å [220] 1.53Å
  • 21. 21 Figure 18. Excerpt of ICDD Graphite XRD Pattern PDF Card # 00-056-0159 Figure 19. Excerpt of ICDD Iron Phosphide XRD Pattern PDF Card # 00-051-0943 Figure 20. Excerpt of ICDD Titanium Carbide XRD Pattern PDF Card # 00-03201383 Figure 21. Excerpt of ICDD Titanium Nitride XRD Pattern PDF Card # 00-038-1420 Figure 22. Excerpt of ICDD Manganese Sulfide XRD Pattern PDF Card # 00-006-0518
  • 22. 22 Figure 23. The iron-carbon phase diagram with graphite instead of cementite as stable phase, explaining the formation of graphite flakes in cast iron. [9] Figure 24. The iron-carbon phase diagram with cementite as stable phase, explaining the formation of pearlite in cast iron. [9]
  • 23. 23 References [1] ASM Engineered Materials Reference Book, Second Edition, Michael Bauccio, Ed. ASM International, Materials Park, OH, 1994. [2] ICDD. PDF# 00-051-0943. Mayo, W., H&M Analytical Services, Inc., Allentown, NJ, USA. ICDD Grant-in-Aid (1999). [3] Casting design and performance. Materials Park, OH: ASM International, 2009. Print. [4] ICDD. PDF# 00-03201383. Natl. Bur. Stand. (U. S.) Monogr. 25 18, 73 (1981). [5] Charles Lyman. “Lecture: Scanning Electron Microscopy (SEM) and X-ray Microanalysis.” Bethlehem, PA, Lehigh University, 2017 [6] ICDD. PDF# 00-038-1420. Wong-Ng, W., McMurdie, H., Paretzkin, B., Hubbard, C., Dragoo, A., NBS, Gaithersburg, MD, USA. ICDD Grant-in-Aid (1987). [7] ICDD. PDF# 00-006-0518. Wong-Ng, W., McMurdie, H., Paretzkin, B., Hubbard, C., Dragoo, A., NBS, Gaithersburg, MD, USA. ICDD Grant-in-Aid (1987). [8] Silas H Douglas. Guide to a systematic course of qualitative chemical analysis, prepared for the chemical laboratory at the University of Michigan. Ann Arbor, MI: Dr. Chase's steam printing House, 1868. Print. [9] William D. Callister and David G. Rethwisch., Fundamentals of materials science and engineering: an integrated approach. Hoboken (N.J.): Wiley, 2016. Print. [10] Sargent-Welch Scientific, “Periodic Table of the Elements”, Skokie, Illinois, N.D. [11] ASM Metals Reference Book, Third edition, Michael Bauccio, Ed. ASM International, Materials Park, OH, 1993. [12] Dawson and Hollinger, “The Effect of Metallurgical Variables on the Machinability of Compacted Graphite Iron”, SinterCast Technologies AB, Sweden, 2001 [13] "Giesserei Lexikon." Foundry - Lexicon. N.p., n.d. Web. 20 Apr. 2017.
  • 24. 24 [14] Morrogh, “The Status of the Metallurgy of Cast Irons,” Journal of the Iron and Steel Institute, Jan. 1968, pp. 1-10. [15] John Campbell. Complete casting handbook: metal casting processes, metallurgy, techniques and design. Amsterdam: Elsevier/Butterworth-Heinemann, 2015. P.277. [16] History of Metal Casting, “History of Metal Casting: Brief History” [17] LaRoux K. Gillespie. Troubleshooting manufacturing processes: adapted from the Tool and manufacturing engineers handbook: a reference book for manufacturing engineers, managers, and technicians. Dearborn, MI: Society of Manufacturing Engineers, 1988. [18] Veselinka Đorđević, Corrosion Resistant High Silicon Cast Iron, BMC, Ohrid, R. Macedonia, 2003 [19] ASTM B962, Standard Test Methods for Density Using Archimedes’ Principle, ASTM International, West Conshohocken, PA, 2015. [20] ASTM E3-11, Standard Guide for Preparation of Metallographic Specimens, ASTM International, West Conshohocken, PA, 2011. [21] ASTM E562-11, Standard Test Method for Determining Volume Fraction by Systematic Manual Point Count, ASTM International, West Conshohocken, PA, 2011. [22] ASTM D4460-97(2015) Standard Practice for Calculating Precision Limits Where Values are Calculated from Other Test Methods, ASTM International, West Conshohocken, PA, 2015. [23] "Image Intensity Processing." ImageJ. N.p., n.d. Web. 05 May 2017.