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Procedia Manufacturing 30 (2019) 173–179
Procedia Manufacturing 00 (2017) 000–000
14th Global Congress on Manufacturing and Management (GCMM-2018)
www.elsevier.com/locate/procedia

Crystallite
14th Globalsize determination
Congress of and
on Manufacturing thermally deposited
Management Gold
(GCMM-2018)
Nanoparticles
Crystallite size determination of thermally deposited Gold
ab, ac 2017, MESIC 2017, 28-30 June
Olasupo Daniel
Manufacturing OgundareSociety
Engineering , OjoInternational
Jeremiah Akinribide
Nanoparticles Conference *, Adelana Rasak Adetunjib,
2017, Vigo
Mosobalaje Oyebanji (Pontevedra),
Adeoye b
, PeterSpain
Apata Olubambic
Olasupo Daniel Ogundareab, , Ojo Jeremiah Akinribideac *, Adelana Rasak Adetunjib,
CostingResearch
models for
Sciencecapacity optimization inUniversity,
Industry 4.0:
and Developent Department, Engineering Materialsb Development Institute,611,Ondo road Akure,
Trade-off
Nigeria
a
c
Mosobalaje
Materialb
and Oyebanji Adeoye
Engineering Department, , Peter
Obafemi Apata
Awolowo Olubambi
Ile-Ife, Nigeria.
c
Centre for Nanoengineering and Tribocorossion, University of Johannesburg, Johannesburg 2028, South Africa
a
between used capacity and operational efficiency
Research andDepartment
b
DevelopentofDepartment,
metallurgy, Engineering
University ofMaterials Development
Johannesburg, Institute,611,Ondo
Johannesburg, 2028, Southroad Akure, Nigeria
Africa
Material Science and Engineering Department, Obafemi Awolowo University, Ile-Ife, Nigeria.
c
Centre for Nanoengineering and Tribocorossion, University of Johannesburg, Johannesburg 2028, South Africa
A. Santana , P. Afonso , A. Zanin , R. Wernke
a University of Johannesburg,
Department of metallurgy, a,* b
Johannesburg, 2028, SouthbAfrica
Abstract a
University of Minho, 4800-058 Guimarães, Portugal
b
Unochapecó, 89809-000 Chapecó, SC, Brazil
This paper has x-rayed an approach to investigate the crystallite size of thermally deposited gold nanoparticles on a glass
Abstract
substrate. The mined and beneficiated gold sample was deposited on glass slide in Nano-38 thermal depositor after the substrate
has been technically prepared. The crystallite size and profile fitting of the nanoparticles were determined by X-ray
This paper has x-rayed an approach to investigate the crystallite size of thermally deposited gold nanoparticles on a glass
Diffractometer (XRD). The result showed that the average crystallite size of Au nanoparticles thermally deposited on glass slide
substrate. The mined and beneficiated gold sample was deposited on glass slide in Nano-38 thermal depositor after the substrate
Abstract
was 14.4 ± 6.7 nm with lattice constants: a, b, c; 4.0789, 4.0789, and 4.0789 (Å) respectively. The TEM images have confirmed
has been technically prepared. The crystallite size and profile fitting of the nanoparticles were determined by X-ray
that high quality spherical Au NPs that were between 18 nm – 24 nm were successfully synthesized. The XRD has shown that the
Diffractometer
Under (XRD).of The"Industry
result showed that the averageprocesses
crystallite size
willofNarrow
Aupushed
nanoparticles
bethermally deposited on glass slide
materialthe concept
of the gold nanoparticles is4.0",
gold production
and crystalline in structure. be size to increasingly
distribution and smallinterconnected,
monosize gold
was 14.4 ± 6.7 nm with
information alattice constants:
basisa,and,
b, c; necessarily,
4.0789, 4.0789, and more
4.0789 (Å) respectively. The TEMcapacity
images have confirmed
nanoparticles based on may
produced real timeadvantages
proffer much
for self-assembled monolayerefficient.
formationInand
this context,
enhanced surface area.optimization
that high quality spherical Au NPs that were between 18 nm – 24 nm were successfully synthesized. The XRD has shown that the
goes beyond the traditional aim of capacity maximization, contributing also for organization’s profitability and value.
material of the gold nanoparticles is gold and crystalline in structure. Narrow size distribution and small monosize gold
Indeed, leanproduced
nanoparticles management and advantages
may proffer continuousforimprovement approachesformation
self-assembled monolayer suggestandcapacity
enhancedoptimization
surface area. instead of
maximization. The study of capacity optimization and costing models is an important research topic that deserves
contributions from both the practical and theoretical perspectives. This paper presents and discusses a mathematical
©
© 2018
2019forThe Authors. Published
Thecapacity
Authors. Published byby Elsevier
Elsevier Ltd.
Ltd.
model
This is an open accessmanagement
article under based
the CC on differentlicense
BY-NC-ND costing models (ABC and TDABC). A generic) model has been
(https://creativecommons.org/licenses/by-nc-nd/4.0/
This is an open access article under the CC BY-NC-ND license (https://creativecommons.org/licenses/by-nc-nd/4.0/)
developed
Selection and
and it was used
peer-review to
underanalyze idle capacity and to design strategies towards the maximization of organization’s
Selection
© 2018 The andAuthors.
peer-review underbyresponsibility
Published responsibility of the scientific committee of the 14th Global Congress on Manufacturing
Elsevier Ltd. of the scientific committee of the 14th Global Congress on Manufacturing and
and
value. The
Management
Management trade-off capacity
(GCMM-2018).
(GCMM-2018). maximization vs operational efficiency is highlighted and it is shown that capacity
This is an open access article under the CC BY-NC-ND license (https://creativecommons.org/licenses/by-nc-nd/4.0/)
optimization
Selection and might hide operational
peer-review inefficiency.
under responsibility of the scientific committee of the 14th Global Congress on Manufacturing and
Keywords:
© 2017 Thecrystallite
Authors. size, thermal deposition,
Published by Elseviergold nanoparticles, XRD
B.V.
Management (GCMM-2018).
Peer-review under responsibility of the scientific committee of the Manufacturing Engineering Society International Conference
2017.
Keywords: crystallite size, thermal deposition, gold nanoparticles, XRD

Keywords: Cost Models; ABC; TDABC; Capacity Management; Idle Capacity; Operational Efficiency

* Corresponding author. Cell.: +27 73 5042962

E-mail address: akinribideojo@yahoo.com
1. Introduction
* Corresponding author. Cell.: +27 73 5042962
2351-9789 © 2018 The Authors. Published by Elsevier Ltd.
E-mail address: akinribideojo@yahoo.com
ThisThe
is ancost
openof idle
access capacity
article underisthe
a fundamental
CC BY-NC-NDinformation for companies and their management of extreme importance
license (https://creativecommons.org/licenses/by-nc-nd/4.0/)
in modern
Selection andproduction systems.
peer-review under In general,
responsibility of theitscientific
is defined as unused
committee of thecapacity orCongress
14th Global production potential and
on Manufacturing andcan be measured
Management
2351-9789 © 2018 The Authors. Published by Elsevier Ltd.
in several
(GCMM-2018). ways: tons of production, available hours of manufacturing, etc. The management
This is an open access article under the CC BY-NC-ND license (https://creativecommons.org/licenses/by-nc-nd/4.0/)
of the idle capacity
* Paulo Afonso. Tel.: +351 253 510 761; fax: +351 253 604 741
Selection and peer-review under responsibility of the scientific committee of the 14th Global Congress on Manufacturing and Management
E-mail address: psafonso@dps.uminho.pt
(GCMM-2018).

2351-9789
2351-9789©©2017
2019The
TheAuthors.
Authors. Published by Elsevier
Published B.V. Ltd.
by Elsevier
Peer-review underaccess
This is an open responsibility
article of the scientific
under committee oflicense
the CC BY-NC-ND the Manufacturing Engineering Society International Conference 2017.
(https://creativecommons.org/licenses/by-nc-nd/4.0/)
Selection and peer-review under responsibility of the scientific committee of the 14th Global Congress on Manufacturing and Management
(GCMM-2018).
10.1016/j.promfg.2019.02.025
174 Olasupo Daniel Ogundare et al. / Procedia Manufacturing 30 (2019) 173–179
Ogundare, et al. / Procedia Manufacturing 00 (2018) 000–000 2

1.0 Introduction

In the current decade, much attention has been given to the synthesis of metal nanoparticles. This demanding
interest has motivated by unique properties displayed by nanoparticles in catalysis, medicine, optics and materials
science [1-3]. Alloying metal nanoparticles have portrayed promising attempt to enhance the antibacterial and
optical performance in the field of nanotechnology [4-8]. This could be a channel to produce multi-functionalized
nanoparticles [9]. Pure silver and gold nanoparticles as well as AgAu nanoalloys in the size of 4 nm have been
successfully analyzed using pulsed laser ablation [10].

In the past few years, functionalizing nanoparticles has been a major area of research that have been generating
ripples due to its interdisciplinary nature and diverse functionalities [11– 17]. Au NPs loaded carbon nanotubes have
been recently prepared by mixed acids treatment process with a view to determining its electrocatalytic properties
[18]. Also, the nanoparticles of Au (Au NPs) bearing starch polymer have been prepared and characterized. The
catalytic property of starch-borne Au NPs alloyed with phenylboronic acid in water as well as other several
parameters has been studied [19].

The aim of this work was to deepen our understanding of the crystal size in thermally deposited gold nanoparticles
with a view to ascertaining its response to optical properties. Here, we have reported the average crystallite size and
lattice constant of Au nanoparticles thermally deposited on glass slide.

2.0 Experimental section

2.1 Material and preparation process

The gold sample used in this work was mined, beneficiated and processed from Itagunmodi deposit following
standard procedure as outlined [20]. Pure Au solid target, washed with ethanol and de-ionized water, was immersed
in 5 ml de-ionized water filled in quartz cuvette in order to remove any impurity. Glass substrate with the dimension
25mm x 12mm2 was used for the experiment. Vacuum evaporation was performed at room deposition temperature,
total pressure of about 2x10-5 Pa, molybdenum container with source current more than 5Amp. The gold deposition
was accomplished at room temperature using the gold target. The thickness of the deposited Au was determined
from profilometer to be 5nm. The procedure was repeated thrice in order to minimize error, which could occur from
using a single sample.

The substrate was approximately 25mm x 12mm wide glass slide piece with a shiny deposition of Au nanoparticles
on one side. The sample was mounted to an aluminium stub with double sided tape and the stub was mounted on an
x-y-z goniometer stage.

Plate 1 has shown low magnification image from the gold nanoparticles deposited on glass slide with the analysis
area located at the intersection of the crosshairs on the image. Data was acquired on a Bruker GADDS
microdiffractometer equipped with a Copper x-ray tube, incident-beam monochromator, 500micron pinhole
collimator, laser alignment system and 2D detector. Unlike traditional point detectors, the 2D detector accepts
diffraction from crystallites oriented in a wide variety of tilt angles with respect to the incident x-ray beam. This
resulted in reasonable diffraction intensity even though the spot size analyzed was very small. To ensure that the
sample height was correct, the GADDS employed a laser and camera system oriented so that the sample was in the
correct position when the laser beam was in the center of the camera system.

Plate 2 has shown the image from the alignment camera for the sample. On the photo, the laser spot located at the
crosshairs was observable but weak due to the reflective nature of the sample.
 Olasupo Daniel Ogundare et al. / Procedia Manufacturing 30 (2019) 173–179 175
Ogundare, et al. / Procedia Manufacturing 00 (2018) 000–000 3

X100 X1000

Figure 1: Low magnification photo of Figure 2: High magnification alignment

Au nanoparticles thermally deposited on glass slide image of Au nanoparticles thermally deposited on glass slide

3.0 Results and Discussion

Figure 3: SEM images of the morphologies of the gold ore (a) (x100), c (x1000) and the extracted gold grains (b) (x100), (d) (x1000) [20]

The SEM image (Figs. 3a and c) has illustrated that the surface structure of the particles of Au ore from Itagunmodi
deposit are in trihedron shapes. The SEM (in Figs. 3b and d) image has confirmed that the morphology of the
particles of Au mined was in tetrahedron and hexahedron shapes.

The TEM images obtained from the Au NPs synthesis were shown in Fig. 4. The TEM images has elucidated that
the gold colloids were in monodispersional state, this may not be unconnected to the negatively charged layer of
citrate ions which repel from each other. This monodispersity could be attributed to the probe preparation and
generation of color signal in chromatographic strip assay. Moreover, the TEM images have stipulated that most of
the Au nanospheres were round or spherical in shape. The size range of the NPs could be noted to be between 21-29
nm. The average size of Au NPs has been evaluated by measuring the diameter of three particles on TEM images.
The average diameter of colloidal gold was in the range of 24.2 nm with few particles of higher size distribution.
Also, it could be noticed that the Au NPs are the dark spherical shaped dots with smooth surface morphology.
176 Olasupo Daniel Ogundare et al. / Procedia Manufacturing 30 (2019) 173–179
Ogundare, et al. / Procedia Manufacturing 00 (2018) 000–000 4

Figure 4: TEM image of synthesized Au NPs

Figure 1 has shown the XRD scan data from the sample along with the selected background and the reference
markers from the International Centre Diffraction Data / Inorganic Crystal Structure Database (ICDD/ICSD) for Au.
The irregular background was due to amorphous scattering from the underlying glass slide. The positions of the
reference markers have been indicated where in 2Θ an expected diffraction peak would occur and the height of the
markers was related to the expected height of an experimental peak if the sample were fine grained and randomly
oriented. 2Θ represented the Bragg’s angle between the incident and reflection x-ray beams. In XRD, you have
crystallites in all orientations. Only those crystallites whose Bragg planes are at angle of Θ with respect to the
incident angle will diffract at an angle of 2Θ with respect to the incident beam. Note that the Au (111) peak is much
more intense than the other Au peaks which is reflected in profile fit results for Au nanoparticles, Thermal deposited
in Fig 6 . This indicates that there is some moderate texture (i.e. preferred orientation) of the Au on the glass slide.

The broadening of an observed diffraction peak can be characterized in a simplistic way by its FWHM (Full Width
at Half Maximum) value at a particular 2 angle as 38o, 43o, 65o, 78o and 82o respectively. Because the apparent
FWHM of a peak is a mathematical combination (convolution) of the specimen broadening FW(S) and the
instrumental broadening FW (I), instrumental broadening is subtracted from that of the observed diffraction peak. If
the crystallites (crystalline domains) in the specimen are free of lattice strain, their average size can be estimated
from the specimen broadening FW(S) of any single peak in the observed pattern according to the Scherrer formula:

Crystallite Size = K * λ / (FW(S) * Cos ()),[1]

where  is the peak position and K is the dimensionless shape factor of the average crystallite, λ is the x-ray
wavelength, FW(S) is the line broadening at half the maximum intensity (FWHM),  is the Bragg angle.

Profile fitting is required to determine the peak positions and widths used for calculating the average crystallite size.
Figure 2 shows the profile fitting results for the Au nanoparticles thermally deposited on glass. The fitting details
are shown in the table below the profile fit figure. The XS column shows the crystallite size in Angstroms for each
peak based on the Scherer equation. The average crystallite size is shown in Table 1 for the Au peaks in the sample.
Also shown in Table 1 is the Au structure (FCC) and lattice constants from the ICDD/ICSD data file. The
ICDD/ICSD reference and peak data are shown in the Table 2.
 Olasupo Daniel Ogundare et al. / Procedia Manufacturing 30 (2019) 173–179 177
Ogundare, et al. / Procedia Manufacturing 00 (2018) 000–000 5

Table1. The average crystallite size

Average Crystallite size
Sample ID Phase
(nm)

Gold Au
Cubic, S.G: Fm-3m (225)
Au nanoparticles
Lattice Constants:
thermally
a, b, c; 4.0789, 4.0789, 4.0789 (Å) 14.4 ± 6.7 nm
deposited on glass
α, β, γ ;<90.00°, 90.00°, 90.00°>
slide
Phase Info [01-075-6560]

Table 2: ICDD/ICSD reference and peak data

Crystallite
2Θ Angle d(Å) I%(f) ( h k l) θ(°) 1/(2d) 2π/d
size #

1 38.185 2.3550 100.0 ( 1 1 1) 19.092 0.2123 2.6680

2 44.382 2.0395 47.1 ( 2 0 0) 22.191 0.2452 3.0808
3 64.571 1.4421 25.0 ( 2 2 0) 32.286 0.3467 4.3569
4 77.560 1.2299 25.4 ( 3 1 1) 38.780 0.4066 5.1089
5 81.716 1.1775 7.0 ( 2 2 2) 40.858 0.4246 5.3361
6 98.119 1.0197 3.0 ( 4 0 0) 49.060 0.4903 6.1616
7 110.806 0.9358 9.2 ( 3 3 1) 55.403 0.5343 6.7144
8 115.247 0.9121 8.7 ( 4 2 0) 57.624 0.5482 6.8889
9 135.384 0.8326 7.4 ( 4 2 2) 67.692 0.6005 7.5464

Figure 5: Phase identification and (hkl)’s of Au nanoparticles thermally deposited on glass slide.
178 Olasupo Daniel Ogundare et al. / Procedia Manufacturing 30 (2019) 173–179
Ogundare, et al. / Procedia Manufacturing 00 (2018) 000–000 6

Figure 6: Profile fit results for Au nanoparticles, Thermal deposited

Angle(°) d(Å) Height Area(α1) Area(α1)% FWHM(°) XS(Å) ( h k l)

1 38.265 2.3502 1974.8 1421.6 100.0 0.487 253 ( 1 1 1)
2 44.371 2.0400 218.7 375.9 26.4 1.114 84 ( 2 0 0)
3 64.688 1.4398 106.7 133.4 9.4 0.864 120 ( 2 2 0)
4 77.624 1.2290 95.3 134.5 9.5 1.035 106 ( 3 1 1)
5 81.799 1.1765 80.7 82.6 5.8 0.755 157 ( 2 2 2)

R=3.78% (related to goodness of fit; lower R implies better fit)

Conclusions
The TEM images have confirmed that high quality spherical Au NPs that were between 18 nm – 24 nm were
successfully synthesized. The XRD has shown that the material of the gold nanoparticles is gold and crystalline in
structure. Narrow size distribution and small monosize thermally deposited gold nanoparticles produced may proffer
advantages for self-assembled monolayer formation and enhanced surface area. These findings imply that the atomic
scale interface structure plays an important role when continuous ultra- thin films are being considered.

Competing interests

All authors have pronounced that no contending intrigues exist.

Acknowledgements

The authors are appreciative to Engineering Materials Development Institute (EMDI) Akure Nigeria for the bench
Work, National Agency for Science and Engineering Infrastructure (NASENI) Abuja Nigeria and International
Foundation for Science (IFS) Stockholm, Sweden (No F/5085-1) for the financing.
 Olasupo Daniel Ogundare et al. / Procedia Manufacturing 30 (2019) 173–179 179
Ogundare, et al. / Procedia Manufacturing 00 (2018) 000–000 7

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