Among calcium phosphates, Hydroxyapatite (HA) has become the material of choice and is commonly used in bone implantation and human teeth due to its chemical and crystal structure similar to bone apatite and excellent bioactivity. To date, HA has been successfully prepared from biogenic waste as the calcium precursor via extraction of calcium oxide from eggshells, seashells, animal bones (cow, chicken, fish) and many more via wet method. The dry method has been least preferred due to the tendency of powder contamination and non-homogeneous powder mixing during the mechanochemical activation method. However, with the proper methods, the dry method can be used in producing pure HA on a mass scale. Consequently, this work used a solid-state synthesis approach to produce HA from discarded eggshells, which provided a biogenic calcium precursor in the form of calcium carbonate. The intention was to determine how various ball milling durations affected the microstructure and phase stability of the artificially produced HA generated from eggshells. The eggshells were dried first and then subjected to calcination at 700°C for 2 hours. The eggshells, after being heated to high temperatures, were combined with dicalcium phosphate dihydrate (DCPD) by rotating at 400 rpm for 2, 4, and 6 hours. The powder combination including CaCO3 and DCPD was subjected to heat treatment at 800°C to get pure HA powder. The XRD analysis of the heat-treated powder revealed the successful production of hydroxyapatite (HA) after 2 hours of ball milling and calcination at 800°C. Extending the ball milling period to 4 hours and 6 hours would lead to intense mechanochemical activation, resulting in the powder combination transitioning into a biphasic calcium phosphate (BCP) phase including HA and β-TCP. Furthermore, the image of pure HA powder that was made after two hours of ball milling showed that the powder had a flake-like shape and was less clumped together. The BCP powder produced contained spherical particles that were agglomerated in form. The milling length of the starting materials significantly impacted the phase stability and microstructure of the synthesised calcium phosphate powder generated from eggshells.

1.
S.
Pokhrel
,
Adv. Chem. Eng. Sci.
8
,
225
240
(
2018
).
2.
R. M.
Anggraini
and
Y.
Yusuf
,
IOP Conf. Ser.: Mater. Sci. Eng.
546
,
042002
(
2019
).
3.
V. A.
Apalangya
,
V. K.
Rangari
,
B. J.
Tiimob
,
S.
Jeelani
and
T.
Samuel
,
Int. J. Biomater.
(
2019
).
4.
S.
Ramesh
,
A. N.
Natasha
,
C. Y.
Tan
,
L. T.
Bang
,
S.
Ramesh
,
C. Y.
Ching
,
H.
Chandran
,
Ceram. Int.
42
7824
7829
(
2016
).
5.
N.
Nuamsrinuan
,
W.
Kaewwiset
,
P.
Limsuwan
and
K.
Naemchanthara
,
Appl. Mech. Mater.
866
,
12
16
(
2017
).
6.
J.
Akter
,
M.
Mollah
,
S.
Ahmed
and
M.
Abu
,
Mater. Today Proc.
4
,
5497
5506
(
2017
).
7.
H.
Khandelwal
and
S.
Prakash
,
J. Miner. Mater. Charact. Eng.
4
,
119
126
. (
2016
).
8.
S. C.
Wu
,
H. C.
Hsu
,
S. K.
Hsu
,
Y. C.
Chang
and
W. F.
Ho
,
J. Asian Ceram. Soc.
4
(
1
),
85
90
(
2016
).
9.
H.
Shahid
and
S.
Kazi
,
IOP Conf. Ser. Mater. Sci. Eng.
1189
012024
(
2021
).
10.
N.
Razali
,
N.
Jumadi
,
A. Y.
Jalani
,
N. Z.
Kamarulzaman
and
K. F.
Pa’ee
,
Malays. J. Anal. Sci.
26
,
347
359
(
2022
).
11.
K. H.
Teoh
,
C.-S.
Lim
,
C.-W.
Liew
and
S.
Ramesh
and
S.
Ramesh
,
Ionics
21
,
2061
2068
(
2015
).
12.
S.
Ramesh
,
C.
Gill
and
S.
Lawson
,
J. Mater. Sci.
34
,
5457
5467
(
1999
).
13.
I.
Sopyan
,
S.
Ramesh
,
N. A.
Nawawi
,
A.
Tampieri
and
S.
Sprio
,
Ceram. Int.
37
,
3703
3715
(
2011
).
14.
I.
Sopyan
,
S.
Ramesh
and
M.
Hamdi
,
Indian J. Chem.
47A
,
1626
1631
(
2008
).
15.
L. T.
Bang
,
S.
Ramesh
,
J.
Purbolaksono
,
Y. C.
Ching
,
B. D.
Long
,
Hari
Chandran
,
S.
Ramesh
and
R.
Othman
,
Mater. Design
87
,
788
796
(
2015
).
16.
S.
Ramesh
,
A.
Yaghoubi
,
K. Y. Sara
Lee
,
K. M. Christopher
Chin
,
J.
Purbolaksono
,
M.
Hamdi
and
M. A.
Hassan
,
J. Mech. Behav. Biomed. Mater.
25
,
63
69
(
2013
).
17.
S.
Ramesh
,
C. Y.
Tan
,
R.
Tolouei
,
M.
Amiriyan
,
J.
Purbolaksono
,
I.
Sopyan
and
W. D.
Teng
,
Mater. Design
34
,
148
154
(
2012
).
18.
S.
Ramesh
,
C. Y.
Tan
,
M.
Hamdi
,
I.
Sopyan
and
W. D.
Teng
, in
Proceedings of SPIE, Vol. 6423: International Conference on Smart Materials and Nanotechnology in Engineering
, ed by
Shanyi Du
et al.
(
SPIE Digital Library
,
USA
, Nov.
2007
) Paper No. 64233A.
19.
S. T.
Auwal
,
S.
Ramesh
,
F.
Yusof
and
S. M.
Manladan
,
J. Adv. Manuf. Tech.
97
,
1071
1098
(
2018
).
20.
S.
Ramesh
,
S.
Meenaloshini
,
C. Y.
Tan
,
W. J. Kelvin
Chew
and
W. D.
Teng
,
Ceram. Int.
34
,
1603
1608
(
2008
).
21.
S. M.
Manladan
,
F.
Yusof
,
S.
Ramesh
and
M.
Fadzil
,
Int. J. Adv. Manuf. Tech.
86
,
1805
1825
(
2016
).
22.
S.
Ramesh
,
A. N.
Natasha
,
C. Y.
Tan
,
L. T.
Bang
,
A.
Niakan
,
J.
Purbolaksono
,
Hari
Chandran
,
C. Y.
Ching
,
S.
Ramesh
and
W. D.
Teng
,
Ceram. Int.
41
,
10434
10441
(
2015
).
23.
S.
Ramesh
,
C. Y.
Tan
,
C. L.
Peralta
and
W. D.
Teng
,
Sci. Tech. Adv. Mater.
8
,
257
263
(
2007
).
24.
C. Y.
Tan
,
A.
Yaghoubi
,
S.
Ramesh
,
S.
Adzila
,
J.
Purbolaksono
,
M. A.
Hassan
and
M. G.
Kutty
,
Ceram. Int.
39
,
8979
8983
(
2013
).
25.
N.
Duraisamy
,
A.
Numan
,
K.
Ramesh
,
K.-H.
Choi
,
S.
Ramesh
and
S.
Ramesh
,
Mater. Letts.
161
,
694
697
(
2015
).
26.
C.
Bowen
,
S.
Ramesh
,
C.
Gill
and
S.
Lawson
,
J. Mater. Sci.
33
,
5103
5110
(
1998
).
27.
S. M.
Manladan
,
F.
Yusof
,
S.
Ramesh
,
Y.
Zhang
,
Z.
Luo
and
Z.
Ling
,
J. Mater. Proc. Tech.
250
,
45
54
(
2017
).
28.
S.
Ramesh
,
N.
Zulkifli
,
C. Y.
Tan
,
Y. H.
Wong
,
F.
Tarlochan
,
S.
Ramesh
,
W. D.
Teng
,
I.
Sopyan
,
L. T.
Bang
and
A. A. D.
Sarhan
,
Ceram. Int.
44
,
8922
8927
(
2018
).
29.
T. M. Sampath Udeni
Gunathilake
,
Y. C.
Ching
,
C. H.
Chuah
,
H. A.
Illias
,
K. Y.
Ching
,
R.
Singh
and
L.
Nai-Shang
,
Int. J. Biological Macromolecules
,
118
,
1055
1064
(
2018
).
30.
K. A.
Francis
,
C.-W.
Liew
,
S.
Ramesh
,
K.
Ramesh
and
S.
Ramesh
,
Ionics
,
22
,
919
925
(
2016
).
31.
S.
Ramesh
,
M.
Amiriyan
,
S.
Meenaloshini
,
R.
Tolouei
,
M.
Hamdi
,
J.
Pruboloksono
and
W. D.
Teng
,
Ceram. Int.
37
,
3583
3590
(
2011
).
32.
A. Azim
Jais
,
S. A. Muhammed
Ali
,
M.
Anwar
,
M. Rao
Somalu
,
A.
Muchtar
,
W. N. R. Wan
Isahak
,
C. Y.
Tan
,
R.
Singh
and
N. P.
Brandon
,
Ceram. Int.
43
,
8119
8125
(
2017
).
33.
H.
Misran
,
R.
Singh
and
M. A.
Yarmo
,
Microporous and Mesoporous Mater.
112
,
243
253
(
2008
).
34.
M. M.
Barzani
,
A. A. D.
Sarhan
,
S.
Farahany
,
S.
Ramesh
and
I.
Maher
,
Measurement
62
,
170
178
(
2015
).
35.
W. H.
Yeo
,
A. T.
Fry
,
J.
Purbolaksono
,
S.
Ramesh
,
J. I.
Inayat-Hussain
,
H. L.
Liew
and
M.
Hamdi
,
J. Supercritical Fluids
92
,
215
222
(
2014
).
36.
Y. C.
Ching
,
T. M. S. U.
Gunathilake
,
C. H.
Chuah
,
K. Y.
Ching
,
R.
Singh
and
N.-S.
Liou
,
Cellulose
26
,
5467
5481
(
2019
).
37.
Y. Y.
Yee
,
Y. C.
Ching
,
S.
Rozali
,
N. A.
Hashim
and
S.
Ramesh
,
BioResources
11
,
2269
2286
(
2016
).
38.
S.
Ramesh
and
C.
Gill
,
Ceram. Int.
27
,
705
711
(
2001
).
39.
Y. S.
Pai
,
H. J.
Yap
and
R.
Singh
,
Proc. Inst. Mech. Eng. Part B J. Eng. Manuf.
229
,
1029
1045
(
2015
).
40.
S.
Ramesh
,
C. Y.
Tan
,
W. H.
Yeo
,
R.
Tolouei
,
M.
Amiriyan
,
I.
Sopyan
and
W. D.
Teng
,
Ceram. Int.
37
,
599
606
(
2011
).
41.
U.
Sutharsini
,
M.
Thanihaichelvan
,
C. H.
Ting
,
S.
Ramesh
,
C. Y.
Tan
,
Hari
Chandran
,
A. A. D.
Sarhan
,
S.
Ramesh
and
I.
Urriés
,
Ceram. Int.
43
,
7594
7599
(
2017
).
42.
C. Y.
Tan
,
R.
Singh
,
Y. C.
Teh
,
Y. M.
Tan
and
B. K.
Yap
,
Int. J. Appl. Ceram. Tech.
12
,
223
227
(
2015
).
43.
M.
Afshar-Mohajer
,
A.
Yaghoubi
,
S.
Ramesh
,
A. R.
Bushroa
,
K. M. C.
Chin
,
C. C.
Tin
and
W. S.
Chiu
,
Appl. Surf. Sci.
307
,
1
6
(
2014
)
44.
B.
Wen
,
N.
Musa
,
C. C.
Onn
,
S.
Ramesh
,
L.
Liang
and
W.
Wang
,
J. Cleaner Prod.
259
,
120912
(
2020
).
45.
A.
Syairah
,
M. H.
Khanmirzaei
,
N. M.
Saidi
,
N. K.
Farhana
,
S.
Ramesh
,
K.
Ramesh
and
S.
Ramesh
,
Ionics
25
,
2427
2435
(
2019
).
46.
B.
Wen
,
S. N.
Musa
,
C. C.
Onn
,
S.
Ramesh
,
L.
Liang
,
W.
Wang
and
K.
Ma
,
Building and Environment
185
,
107091
(
2020
).
47.
A. A. A.
Rahim
,
S. N.
Musa
,
S.
Ramesh
and
M. K.
Lim
,
Proc. Inst. Mech. Eng. Part L J. Mater. Design and Appl.
234
,
1032
1059
(
2020
).
48.
S. E.
Alkhatib
,
F.
Tarlochan
,
H.
Mehboob
,
R.
Singh
,
K.
Kadirgama
and
W. S. B. W.
Harun
,
Artificial Organs
43
,
E152
E164
(
2019
).
49.
M. A.
Zavareh
,
A. A. D. M.
Sarhan
,
R.
Karimzadeh
and R. S. A./
I. K.
Singh
,
Ceram. Int.
44
,
5967
5975
(
2018
).
50.
C. M.
Mardziah
,
S.
Ramesh
,
M. F. Abdul
Wahid
,
Hari
Chandran
,
A.
Sidhu
,
S.
Krishnasamy
and
J.
Purbolaksono
,
Ceram. Int.
46
,
13945
13952
(
2020
).
51.
T.
Sugumaran
,
D. S.
Silvaraj
,
N. M.
Saidi
,
N. K.
Farhana
,
S.
Ramesh
,
K.
Ramesh
and
S.
Ramesh
,
Ionics
25
,
763
771
(
2019
)
52.
H. A.
Chee
,
R. S. K.
Singh
, and
K. S.
Lee
,
Journal of Ceramic Processing Research
22
,
289
295
(
2021
).
53.
H. A.
Chee
,
R. S. K.
Singh
, and
K. S.
Lee
,
Journal of Ceramic Processing Research
21
,
495
500
(
2020
).
54.
ACH
Cheong
,
International Journal of Advanced Science and Technology
29
(
1
),
111
128
(
2020
).
55.
S.
Ramesh
,
M. M.
Khan
,
H. A.
Chee
,
Y. H.
Wong
,
P.
Ganesan
,
M. G.
Kutty
, and
A.
Niakan
,
Ceramics International
42
,
17620
17625
(
2016
).
56.
S.
Ramesh
,
W. J. K.
Chew
,
H. A.
Chee
, and
C. Y.
Tan
, "
Sintering behaviour and properties of flyash-doped zirconia
," in
Materials Science Forum
894
, (Trans Tech Publications Ltd,
2017
), pp.
85
88
.
57.
B. N.
Matcha
,
S.
Sivanesan
, and
K. C.
Ng
, “
Modelling road traffic congestion at urban merge section under mixed traffic conditions
,” in
Proceedings of the Institution of Civil Engineers-Transport
, edited by Thomas Telford Ltd. (
2021
), pp.
1
17
.
58.
S.
Sivakumar
,
C. H. C.
Alexander
,
H. L.
Teow
,
M. Y.
Ali
, and
S.
Ramesh
, "
Two-Stage Sintering of Zirconia Toughened Alumina Composite (ZTA) Doped with Copper Oxide
," in
Proceeding of 5th International Conference on Advances in Manufacturing and Materials Engineering: ICAMME 2022
, (
Springer Nature Singapore
,
2023
), pp.
661
667
.
59.
S.
Sivakumar
,
C. H. C.
Alexander
,
H. L.
Teow
,
M. Y.
Ali
, and
S.
Ramesh
, "
Effect of Zirconia Doping on the Sintering and Mechanical Properties of Hydroxyapatite Bioceramic
," in
Proceeding of 5th International Conference on Advances in Manufacturing and Materials Engineering: ICAMME 2022
, (
Springer Nature Singapore
,
2023
), pp.
147
153
60.
V.
Sekar
,
S. Y. E.
Noum
,
A.
Putra
,
S.
Sivanesan
,
K. C.
Chin
,
Y. S.
Wong
, and
D. H.
Kassim
,
Sound Vib
55
,
4
(
2021
).
61.
H. L.
Teow
,
S. K.
Sivanesan
, and
S. Y. E.
Noum
, “
Effect of Fe2O3 on the densification behaviour and mechanical properties of zirconia-toughened alumina (ZTA) composites prepared by two-stage sintering
,” in
AIP Conference Proceedings
2233
(
2020
). -
62.
A.
Soosai
,
S.
Sivanesan
,
S.
Muniandy
, and
T. H.
Loong
, “
Influence of Zirconia Content to the Mechanical Behaviour of Alumina Zirconia Composite Prepared via Colloidal Method
,” in
International Conference and Exhibition on Sustainable Energy and Advanced Materials
, edited by Springer Nature Singapore (
Springer Nature Singapore
,
Singapore
,
2021
), pp.
124
132
.
63.
S.
Muniandy
,
A.
Soosai
,
T. H.
Loong
, and
S. K.
Sivanesan
, “
Effect of Sintering Temperature and Low Weight Percentage of Zirconia in Hydroxyapatite-Zirconia Composite on Mechccical Properties for Biomedical Application
,” in
International Conference and Exhibition on Sustainable Energy and Advanced Materials
, edited by Springer Nature Singapore (
Springer Nature Singapore
,
Singapore
,
2021
), pp.
133
140
.
64.
O. G.
Agbabiaka
,
I. O.
Oladele
,
A. D.
Akinwekomi
and
A. A.
Adediran
,
Sci. Afr.
8
,
e00452
(
2020
).
65.
M. Amiri
Roudan
,
S.
Ramesh
,
A.
Niakan
,
Y.H.
Wong
,
M. Akhtari
Zavareh
,
H.
Chandran
,
W.D.
Teng
,
N.
Lwin
and
U.
Sutharsini
,
J. Ceram. Process. Res.
18
,
69
72
(
2017
).
66.
A.
Shavandi
,
A. E. D. A.
Bekhit
,
A.
Ali
and
Z.
Sun
.
Mater. Chem. Phys.
149
,
607
616
(
2015
).
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