preparation and characterization of synthesized
TRANSCRIPT
Preparation and Characterization of Synthesized Hydroxyapatite, Poly Lactic
Acid & Cotton (Gauze) Composite Film.
Author Names:
1Md. Amir Hamza Dider; Email:[email protected]
Student, Department of Applied Chemistry& Chemical Engineering, Noakhali
Science and Technology University,Sonapur,Noakhali-3814,Bangladesh.
2 Shujit Chandra Paul: Email:[email protected]
Lecturer, Department of Applied Chemistry& Chemical Engineering, Noakhali
Science and Technology University,Sonapur,Noakhali-3814,Bangladesh
*3 Md.Shafiul Islam;Email:[email protected](Corresponding Author)
Assistant Professor,Department of Applied Chemistry& Chemical Engineering,
Noakhali Science and Technology University,Sonapur,Noakhali-3814,Bangladesh
4 Md. Gulam Sumdani;Email:[email protected]
Student, Department of Chemical Engineering & Polymer Science, Shahjalal
University of Science and Technology, Kumargaon, Sylhet-3114, Bangladesh.
5 Md.Shamim Akter;Email:[email protected]
Student,Department of Applied Chemistry& Chemical Engineering, University of
Dhaka,Dhaka-1000,Bangladesh.
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2
Abstract
In biomedical research, fabrication of porous scaffolds from advanced biomaterial for
healing bone defects represents a new approach for tissue engineering.
Hydroxyapatite (HAp) is a biologically active ceramics have been recognized as
substitute material for bone and teeth in orthopedic and dentistry field due to their
chemical and biological similarity to human hard tissue. It is biocompatible and
bioactive material that can be used to restore damaged human calcified tissue.
Hydroxyapatite, Poly Lactic Acid & Cotton (Gauze) Composite Scaffold film were
produced by natural drying in-situ synthesized hybrid suspension. Matrix mediated
precipitation of hydroxyapatite particles in the polymer, controlled the particle size in
nanometer range. The chemical and thermal properties of composite were investigated
by Simultaneous Thermal Analyzer (STA)/ (TGDTA). Crystallographic
characterization by X-Ray Diffraction and Mechanical properties by tensile testing are
calculated as tensile strength.
This systematic study was carried out to assess the possibility of developing
Hydroxyapatite, Poly Lactic Acid & Cotton (Gauze) Composite film as a new
approach for tissue engineering and improved understanding of its characteristics.
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Chapter 1: Introduction
1. Introduction
Biomaterials is a most rising discipline, due to its direct relation with the healthcare and
impact on human health related issues. [1].So development and improvement of
orthopedic related biomaterials is a very active and growing research field.
Tissue engineering is an interdisciplinary and multidisciplinary field that aims at the
development of biological substitutes that restore, maintain, or improve tissue function
[2]. From the viewpoint of tissue engineering, tissue formation in three dimensions (3D),
a considerable approach to make porous scaffold that provides the microenvironment
(synthetic temporary extracellular matrix) for regenerative cells, supporting cell
attachment,proliferation, differentiation, and neo tissue genesis [3]. Therefore, the
chemical composition, physical structure, and biologically functional moieties are all
important attributes to biomaterials for tissue engineering.Biodegradability being one of
the most important requirements, limits the choice of materials to a few ceramics and
polymers.[4] Ceramics are considered as ideal materials because of their osteoinductive
properties, the ability to induce bone formation. Synthetic ceramics such as β-tricalcium
phosphate and synthetic hydroxyapatite (HAp) have been used[5-9].That’s why; research
on bioceramics (ceramics, carbon, glass and glass-ceramics) has attracted significant
attention because of their potential for biocompatibility and bioactivity with the human
body. An important research on different forms of biocompatible calcium phosphate,
hydroxyapatite [Ca10(PO4)6(OH)2,HAp] is one of the most well-known phases studied for
a number of biomedical applications, due to its similar chemical composition and crystal
structure to apatite in the human skeletal system. The bioactivity and osteoconductivity of
HAp offer a suitable surface for new bone growth and integration as well as
reinforcement to polymer scaffold material for tissue regeneration [1,10]
Use of calcium phosphate polymer composites creates a highly biocompatible product by
increasing cell-material interactions compared to the polymer alone.[11]. Furthermore,
the sustained release of calcium and phosphate from those composites, where the two
ions serve as substrates in the remodeling reactions of mineralized tissues is an added
benefit.[12] Due to the extensive use of PLAs in the biomedical field, their composites
with HAp improved the bending strength of the composite but also had an active role in
new bone formation.[13]. The HAp surface was found to be highly reactive and led to
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Chapter 1: Introduction
favorable attachment to tissue and bioactivity in bone repair.[14] Solvent casting was first
described by Mikos et al.[15] to prepare highly porous biodegradable polymer
membranes used as scaffolds with tunable porosity and desired crystallinity. Phase
Inversion is similar to solvent casting technique is not useful because of the low
mechanical properties.[16] Besides, Melt Molding is not viable because of highly porous
scaffolds inhibit in controlling pore distribution .Fiber bonding method produces
scaffolds variable pore size. That’s why; it is not beneficial due to immiscibility might
harm cells and organs.[17] High pressure processing is a novel technique suggested for
fabricating macro porous sponges of biodegradable polymers without the use of organic
solvents. Mooney et al.[18] have employed this technique to fabricate poly (D,L-lactic-
co-glycolic acid) by saturating them with high pressure CO2 and then by rapidly reducing
the gas pressure to atmospheric levels. These porous sponges have been suggested as
ideal candidates for tissue engineering. The process has a few disadvantages such as, low
mechanical properties and closed pore structure.Three-dimensional printing (3DP) is a
technique to produce scaffolds[19] have limited layer thickness is one of the major
disadvantages of this technique.Freeze-drying process has been used to prepare hybrid
collagen-gelatin polymer networks by Mao et al.[20] by utilizing ice micro particles as
pyrogen. This process depends on thermally induced phase separation. Precise control of
parameters is required to fabricate the scaffolds. Electrospinning, invented by
Formhals[21] in 1934 to fabricate fibrous structures of polymers by the application of a
high voltage to a viscous polymeric based solution, has recently emerged as a leading
technique to fabricate fibrous structures for tissue engineering[22-24]
as the process has the unique capability to fabricate three-dimensional scaffolds that can
mimic the extracellular matrix (ECM) with tunable porosity and morphology [25].
Electro spun fibers have various diameters ranging downward from 5 µm to 0.05 µm.
The small diameter of the fibers provides high surface area to volume ratio making it
suitable for scaffolds for biomedical applications.[26] Electrospinning has emerged as a
promising one-step technique to fabricate scaffolds for bone tissue engineering.
Most of these techniques described do not have the capability to produce three
dimensional scaffolds with controlled amount of porosity and pore size in a single step.
Electrospinning, however a remarkable Nano manufacturing technique has the ability to
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Chapter 1: Introduction
produce three dimensional bio mimicking scaffolds with layered configuration with
complex pore structures and controlled pore size[25]
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Chapter 2: Materials and Method
.
2. Experimental
2.1. Synthesis of Nanohydroxy Apatite
nHAp powders are produced via wet chemical precipitation technique.
Figure 2.1.1: Schematic drawing of the synthesis apparatus for nHAp powders using
precipitation technique.
nHAp powders were prepared via, precipitation technique. In brief, 50 ml aqueous
suspension of 0.5 M calcium hydroxide [Ca (OH) 2] was prepared and vigorously
stirred for 30 minutes. Then 50 ml of 0.3M Orthophosphoric acid [H3PO4] was slowly
added drop wise (0.5 ml/min) into the Ca (OH) 2 suspension. And
simultaneouslytemperature and pH are measured and the pH (10.5) is adjusted by
adding drop wise 1 M ammonium hydroxide [NH4(OH)] solution. The suspension
were well stirred (1000 rpm) using magnetic stirrer for 2 hour and aged for overnight
at room temperature (as shown in figure 3.5. In the second day the suspension is
heated at 1500C for 2 hour and stirred at 1000 rpm then cooled at room temperature.
After that the suspension is sonicated at ultra-sonication bath with 30 minutes period
for 6 times for dispersion and finally high-speed stirring at 1500 rpm for 6 hour, and
then aging for 24 hour. On the fourth day the precipitates were subjected vacuum
filtrating using Buchner funnel, repeatedly washed to obtain pH 7 with deionized
water and filtered again. The precipitates were dried at 800C for 48 hours. Dried
lumps of powders were ground by clean pestles and mortars.
Temperature
Meter pH
Meter
Magnetic Stirrer
0.3 M H3PO4(75%) NH4OH (25%)
0.5 M Ca (OH)2
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Chapter 2: Materials and Method
2.2. Preparation of HAp/PLA/Cotton scaffold
The materials are weighted as follows.
Table 2.2.1: Sample weighting for the hot press scaffold preparation.
Sample Name HAp (gm.) PLA (gm.) Cotton (gm.) 1,4-Dioxane
(ml)
5%nHAP/PLA 0.107 2.043 0.362 20
10%nHAP/PLA 0.207 2.080 0.360 20
15%nHAP/PLA 0.303 2.118 0.380 20
20%nHAP/PLA 0.409 2.031 0.388 20
Table 2.2.2: Sample weighting for the cold press scaffold preparation.
Sample Name HAp (gm.) PLA (gm.) Cotton (gm.) 1,4-Dioxane
(ml)
5%nHAP/PLA 0.105 2.049 0.367 20
10%nHAP/PLA 0.211 2.046 0.363 20
15%nHAP/PLA 0.311 2.016 0.366 20
20%nHAP/PLA 0.403 2.010 0.365 20
The required quantity (given at the table) of HAp powder was dispersed in 1,4-
Dioxane by sonication, then following the table required amount of PLA was added to
the mixtures, and stirred at 500C until complete dissolution. Four solutions with
different content in HAp were prepared, 5%, 10%, 15%, 20% particle by weight with
respect to PLA. TheHAp/PLA solution was poured in petri dish containing Gauze
film. Then the scaffolds were placed in a vacuum dryer at 400C in order to remove the
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Chapter 2: Materials and Method
1, 4-Dioxane. After extraction of Dioxane, scaffolds were dried in atmospheric
temperature. These samples were then stored in desiccator.
For Hot Press sample, after removing from the vacuum dryer it scaffold kept in mold
of Hot Press machine at 400C temperature and 20 bar Pressure for 15min. Then it is
stored in desiccator.
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Chapter 3: Result & Discussion
3.1 Measurement of Water Absorption:
Water absorption, % by mass, after 24 hours immersion in water is given by the formula:
W =M2−M1
M1× 100
Where M1 = Initial weight & M2 = Final weight
Cold press:
Table 3.1.1: Measurement of Water Absorption (Cold Press)
Sample ID Initial Weight Water Absorption, %
% gm. Day 1 Day 2 Day 3
SM 0% 0.098 3.06 5.10 5.10
SM 5% 0.106 1.89 3.77 3.77
SM 10% 0.080 3.75 7.50 7.50
SM 15% 0.089 6.74 10.11 10.11
SM 20% 0.068 5.88 11.76 11.76
Figure 3.1.1(a): Measurement of Water Absorption of Composite (Cold Press)
0
2
4
6
8
10
12
14
0 0.5 1 1.5 2 2.5 3 3.5
% W
ATE
R A
BSO
RP
TIO
N
NUMBER OF DAYS
SM 0% SM 5% SM 10% SM 15% SM 20%
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Chapter 3: Result & Discussion
Hot press:
Table 3.1.1(b): Measurement of Water Absorption (Hot Press)
Sample ID Initial Weight Water Absorption, %
% gm. Day 1 Day 2 Day 3
SM 0% 0.049 2.04 4.08 4.08
SM 5% 0.081 3.70 6.17 6.17
SM 10% 0.056 1.78 3.57 3.57
SM 15% 0.084 2.38 4.76 4.76
SM 20% 0.105 1.90 3.81 3.81
Figure 3.1.1(c): Measurement of Water Absorption of Composite (Hot Press)
It reveals that the water absorption depends on filler content and immersion time. Result shows
that the rate of water absorption is very low with time. This is due to the fact that degree of
cross-linking reaction, which diminishes the void spaces i.e. with the increase of degree of
polymerization, the composite becomes more dense or reinforced materials are distributed
properly eliminating all voids. The water absorption is positively co-related with the porosity of
sample. That means the higher the porosity the higher the water absorption. For 20% composite
the absorption is higher because of its higher porosity.
0
1
2
3
4
5
6
7
0 0.5 1 1.5 2 2.5 3 3.5
% W
ATE
R A
BSO
RP
TIO
N
NUMBER OF DAYS
SM 0% SM 5% SM 10% SM 15% SM20%
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Chapter 3: Result & Discussion
3.2 Measurement of Tensile Properties:
3.2.1 Measurement of Tensile Strength:
Tensile Strength is the maximum stress that a material can withstand while being stretched or
pulled before failing or breaking. It measure the force required to pull something such as rope,
wire or a structural beam to the point where it breaks.
Tensile Strength is measured by the formula:
𝑇𝑒𝑛𝑠𝑖𝑙𝑒 𝑠𝑡𝑟𝑒𝑛𝑔𝑡ℎ = 𝐹𝐴 ⁄ (𝑁/𝑚𝑚2)
The 0% composition has a high tensile strength value due to its high elasticity. With the
addition of filler tensile strength value show a downward inclination due to its rigidity and non-
elastic property.
Figure 3.2.1(a): Tensile strength of % Sample composite (Cold Press)
Figure 3.2.1(b): Tensile strength of % Sample composite (Hot Press)
5.215.4
9.8
5.864.35
0
5
10
15
0 5 10 15 20 25
Ten
sile
Str
engt
h (
MP
a)
% of Sample
Cold Press
4.113 3.181
6.19
9.07
4.507
0
2
4
6
8
10
0 5 10 15 20 25
Ten
sile
Str
engt
h (
MP
a)
% of Sample
Hot Press
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Chapter 3: Result & Discussion
3.2.2 Measurement of% of Elongation
The elongation of the test specimen expressed as a percentage of the gage length.
% of Elongation =( 𝐹𝑖𝑛𝑎𝑙 𝑙𝑒𝑛𝑔𝑡ℎ−𝑂𝑟𝑖𝑔𝑖𝑛𝑎𝑙 𝑙𝑒𝑛𝑔𝑡ℎ)
𝑂𝑟𝑖𝑔𝑖𝑛𝑎𝑙 𝑙𝑒𝑛𝑔𝑡ℎ × 100
Figure 3.2.2(a): % of Elongation of composite (Cold Press)
Figure 3.2.2(b): % of Elongation of composite (Hot Press)
179.4
22.7 20.55 18.26 12.83
0
50
100
150
200
0 5 10 15 20 25
% o
f El
on
gati
on
% of Sample
Cold Press
9.95
19.3321.23 19.88
10.01
0
5
10
15
20
25
0 5 10 15 20 25
% o
f El
on
gati
on
% of Sample
Hot Press
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Chapter 3: Result & Discussion
3.2.3 Measurement of Ductility:
Ductility is the ability to deform before braking. It is the opposite of brittleness. Ductility can be
given either as percent maximum elongation Emaxor maximum area reduction.
%EL = E max * 100%
Figure 3.2.3(a): Ductility of composite (Cold Press)
Figure 3.2.3(b): Ductility of composite (Hot Press)
144.6
22.18 20.5 18.18 10.95
0
50
100
150
200
0 5 10 15 20 25
Du
ctili
ty
% of Sample
Cold Press
9.94
16.9314
18.84
9.51
0
5
10
15
20
0 5 10 15 20 25
Du
ctili
ty
% of Sample
Hot Press
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Chapter 3: Result & Discussion
3.2.4 Measurement of E-modulus:
The E-modulus is a measure of stiffness of materials. It was calculated from the tangent of
stress-strain curve. It is related to the second derivative of the interatomic potential, or the first
derivative of the force vs. intern clear distance.
Due to thermal vibrations the elastic modulus decreases with temperature. E is large for ceramics
(stronger ionic bond) and small for polymers (weak covalent bond).
In case of tensile modulus the higher the elongation the lower will be the modulus for the same
stress. In case of 0% of the sample the elongation is higher therefore possessing the lowest E-
modulus. On the other hand the E-modulus continuously increases with the addition of filler in it
due to its reduction in elongation at yield
Figure 3.2.4(a): Comparison of E-Modulus of composite (Cold Press)
Figure 3.2.4(b): Comparison of E-Modulus of composite (Hot Press)
8.64
63.1
155.3 154.5138.6
0
50
100
150
200
0 5 10 15 20 25
E-M
od
ulu
s (M
Pa)
% of Sample
Cold Press
131.6144.8 146.8
194.1151.2
0
50
100
150
200
250
0 5 10 15 20 25
E-M
od
ulu
s (M
Pa)
% of Sample
Hot Press
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Chapter 3: Result & Discussion
3.2.5 Measurement of Maximum Force required at yield point:
With the increase in elongation at yield for a composite the maximum force required will be
higher and vice-versa. For this reason, the maximum force required to bring yield point is highest
for 0% sample with lowest value for 50% sample
Figure 3.2.5(a): Maximum Force required at yield point for Composite (Cold Press)
Figure 3.2.5(b): Maximum Force required at yield point for Composite (Hot Press)
36.44 34.32
50.7
31.28
21.93
0
10
20
30
40
50
60
0 5 10 15 20 25
Max
imu
m F
orc
e (N
)
% of Sample
Cold Press
15.4622.48
27.96
65
25.56
0
10
20
30
40
50
60
70
0 5 10 15 20 25
Max
imu
m F
orc
e (N
)
% of Sample
Hot Press
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Chapter 3: Result & Discussion
3.3 TG/DTA Analysis
Cold press
Figure 3.3.1: TG/DTG/DTA/ curve of 0% Sample (Cold Press)
Figure shows the TG, DTA and DTG curves for 0% sample.The blue curve for % TG, the green
one for DTA and the red one for DTG. TG shows for initial loss 2.1% due to moisture. The onset
temperature, 50% of major degradation and the maximum slope are at 318.50C, 344.00C and
369.50C. The total degradation is 89.1%. The maximum peak is at 346.80C where the
degradation is 56.7%.
The DTA curve shows two endothermic peaks at 166.40C and 347.00C are due to moisture and
thermal degradation respectively.
The DTG curve shows one peak at 347.10C means that there is one-step degradation. The
maximum degradation occurs at a rate of 3.61mg/min.
Temp Cel
500.0400.0300.0200.0100.0
DT
A u
V
300.0
250.0
200.0
150.0
100.0
50.0
0.0
-50.0
-100.0
-150.0
TG
%
150.0
100.0
50.0
0.0
-50.0
-100.0
-150.0
-200.0
-250.0
-300.0
-350.0
-400.0
DT
G m
g/m
in
25.00
20.00
15.00
10.00
5.00
0.00
318.7Cel21.6uV
347.0Cel-7.8uV
347.1Cel3.61mg/min
283.7Cel95.0%
318.5Cel92.9%
369.5Cel3.8%
459.1Cel1.4%
344.0Cel48.3%
89.1%
346.8Cel43.3%
95.4Cel98.6% 156.6Cel
96.5%
2.1%
166.4Cel10.3uV
155.9Cel21.3uV
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Chapter 3: Result & Discussion
Figure 3.3.2: TG/DTG/DTA/ curve of 15% Sample (Cold Press)
Figure shows the TG, DTA and DTG curves for 15% sample.The blue curve for % TG, the green
one for DTA and the red one for DTG. TG shows for initial loss 1.8% due to moisture. The onset
temperature, 50% of major degradation and the maximum slope are at 340.90C, 363.80C and
386.70C. The total degradation is 87.5%. The maximum peak is at 364.00C where the
degradation is 54.4%.
The DTA curve shows two endothermic peaks at 166.50C and 364.50C are due to moisture and
thermal degradation respectively.
The DTG curve shows one peak at 364.50C means that there is one-step degradation. The
maximum degradation occurs at a rate of 3.01mg/min.
Temp Cel
500.0400.0300.0200.0100.0
DT
A u
V
250.0
200.0
150.0
100.0
50.0
0.0
-50.0
-100.0
-150.0
TG
%
100.0
50.0
0.0
-50.0
-100.0
-150.0
-200.0
-250.0
DT
G m
g/m
in
16.00
14.00
12.00
10.00
8.00
6.00
4.00
2.00
0.00
156.3Cel25.1uV
166.5Cel17.4uV
245.9Cel28.8uV
337.0Cel35.2uV
364.5Cel-4.7uV
364.5Cel3.01mg/min
310.2Cel92.5%
340.9Cel89.7%
386.7Cel2.2%
482.4Cel-1.4%
363.8Cel45.9%
87.5%
364.0Cel45.6%
96.8Cel98.2%
154.6Cel96.4%
1.8%
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Chapter 3: Result & Discussion
Figure 3.3.3: TG/DTG/DTA/ curve of 20% Sample (Cold Press)
Figure shows the TG, DTA and DTG curves for 20% sample.The blue curve for % TG, the green
one for DTA and the red one for DTG. TG shows for initial loss 1.6% due to moisture. The onset
temperature, 50% of major degradation and the maximum slope are at 331.40C, 357.80C and
384.30C. The total degradation is 85.7%. The maximum peak is at 358.90C where the
degradation is 55.3%.
The DTA curve shows two endothermic peaks at 164.70C and 359.70C are due to moisture and
thermal degradation respectively.
The DTG curve shows one peak at 360.30C means that there is one-step degradation. The
maximum degradation occurs at a rate of 1.709mg/min
Temp Cel
500.0400.0300.0200.0100.0
DT
A u
V140.0
120.0
100.0
80.0
60.0
40.0
20.0
0.0
-20.0
-40.0
-60.0
TG
%
100.0
50.0
0.0
-50.0
-100.0
-150.0
-200.0
DT
G m
g/m
in
9.000
8.000
7.000
6.000
5.000
4.000
3.000
2.000
1.000
0.000
164.7Cel21.6uV
245.0Cel31.8uV
359.7Cel21.1uV
155.5Cel28.1uV
326.4Cel36.4uV
360.3Cel1.709mg/min
284.8Cel93.5%
331.4Cel89.3%
384.3Cel3.6%
473.7Cel0.2%
357.8Cel46.5%
85.7%
358.9Cel44.7%
109.3Cel97.7%
164.6Cel96.1%
1.6%
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Chapter 3: Result & Discussion
Hot press
Figure 3.3.4: TG/DTG/DTA/ curve of 0% Sample (Hot Press)
Figure shows the TG, DTA and DTG curves for 0% sample.The blue curve for % TG, the green
one for DTA and the red one for DTG. TG shows for initial loss 1.7% due to moisture. The onset
temperature, 50% of major degradation and the maximum slope are at 322.10C, 349.80C and
377.50C. The total degradation is 94.5%. The maximum peak is at 353.60C where the
degradation is 64.8%.
The DTA curve shows two endothermic peaks at 164.20C and 344.90C are due to moisture and
thermal degradation respectively.
The DTG curve shows one peak at 353.60C means that there is one-step degradation. The
maximum degradation occurs at a rate of 1.356mg/min.
Temp Cel
500.0400.0300.0200.0100.0
DT
A u
V
160.0
140.0
120.0
100.0
80.0
60.0
40.0
20.0
0.0
-20.0
-40.0
TG
%
100.0
50.0
0.0
-50.0
-100.0
-150.0
-200.0
-250.0
-300.0
DT
G m
g/m
in
8.000
7.000
6.000
5.000
4.000
3.000
2.000
1.000
0.000
155.7Cel28.9uV
164.2Cel24.3uV
245.9Cel32.2uV
344.9Cel31.2uV
306.4Cel37.0uV
353.6Cel1.356mg/min
279.6Cel92.2%
322.1Cel88.9%
377.5Cel-5.6% 467.2Cel
-11.8%
349.8Cel41.7%
94.5%
353.6Cel35.2%
93.8Cel97.0%
147.0Cel95.3%
1.7%
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Chapter 3: Result & Discussion
Figure 3.3.5: TG/DTG/DTA/ curve of 15% Sample (Hot Press)
Figure shows the TG, DTA and DTG curves for 15% sample.The blue curve for % TG, the green
one for DTA and the red one for DTG. TG shows for initial loss 1.3% due to moisture. The onset
temperature, 50% of major degradation and the maximum slope are at 341.80C, 363.10C and
384.60C. The total degradation is 77.9%. The maximum peak is at 364.30C where the
degradation is 51.3%.
The DTA curve shows two endothermic peaks at 166.10C and 363.90C are due to moisture and
thermal degradation respectively.
The DTG curve shows one peak at 365.00C means that there is one-step degradation. The
maximum degradation occurs at a rate of 2.47mg/min
Temp Cel
500.0400.0300.0200.0100.0
DT
A u
V150.0
100.0
50.0
0.0
-50.0
TG
%
100.0
50.0
0.0
-50.0
-100.0
-150.0
-200.0
DT
G m
g/m
in
14.00
12.00
10.00
8.00
6.00
4.00
2.00
0.00
166.1Cel21.8uV
245.5Cel32.7uV
363.9Cel7.0uV
156.8Cel28.4uV
331.8Cel36.6uV
365.0Cel2.47mg/min
309.8Cel92.9% 341.8Cel
89.8%
384.6Cel12.0%
500.2Cel7.5%
363.1Cel51.0%
77.9%
364.3Cel48.7%
111.7Cel97.9%
169.0Cel96.6%
1.3%
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Chapter 3: Result & Discussion
Figure 3.3.6: TG/DTG/DTA/ curve of 20% Sample (Hot Press)
Figure shows the TG, DTA and DTG curves for 20% sample.The blue curve for % TG, the green
one for DTA and the red one for DTG. TG shows for initial loss 1.9% due to moisture. The onset
temperature, 50% of major degradation and the maximum slope are at 346.30C, 364.30C and
382.50C. The total degradation is 72.3%. The maximum peak is at 365.80C where the
degradation is 52.9%.
The DTA curve shows two endothermic peaks at 165.10C and 365.80C are due to moisture and
thermal degradation respectively.
The DTG curve shows one peak at 366.30C means that there is one-step degradation. The
maximum degradation occurs at a rate of 2.63mg/min.
Temp Cel
500.0400.0300.0200.0100.0
DT
A u
V200.0
150.0
100.0
50.0
0.0
-50.0
TG
%
150.0
100.0
50.0
0.0
-50.0
-100.0
-150.0
-200.0
-250.0
DT
G m
g/m
in
14.00
12.00
10.00
8.00
6.00
4.00
2.00
0.00
331.4Cel38.4uV
365.8Cel6.6uV
165.1Cel22.2uV
155.8Cel27.9uV
366.3Cel2.63mg/min
324.1Cel89.8%
346.3Cel86.3%
382.5Cel14.0%
470.9Cel11.6%
364.3Cel50.3%72.3%
365.8Cel47.1%
111.2Cel97.5%
192.6Cel95.6%
1.9%
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Chapter 3: Result & Discussion
3.4 X-ray diffraction (XRD) Analysis
Figure 3.4.1: XRD pattern of Hydroxyapatite particle showing characteristic peak
Figure 3.4.2: XRD pattern of 0% Sample showing characteristic peak
0
200
400
600
800
1000
1200
1400
1600
1800
20 25 30 35 40 45 50 55 60 65 70
Inte
nsi
ty (
Counts
)
2 Theta
XRD analysis of HAp Powder
0
200
400
600
800
1000
1200
1400
10 15 20 25 30 35 40 45 50
Inte
nsi
ty C
ou
nts
2 theta
0% Sample (Cold Press)
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Chapter 3: Result & Discussion
Figure 3.4.3: XRD pattern of 0% Sample showing characteristic peak
Figure 3.4.4: XRD pattern of 20% Sample showing characteristic peak
0
500
1000
1500
2000
2500
3000
3500
4000
4500
10 15 20 25 30 35 40 45 50
Inte
nsi
ty C
ou
nts
2 theta
0% Sample (Hot Press)
0
200
400
600
800
1000
1200
1400
10 15 20 25 30 35 40 45 50
Inte
nsi
ty C
ou
nts
2 theta
20% Sample (Cold Press)
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Chapter 3: Result & Discussion
Figure 3.4.5: XRD pattern of 20% Sample showing characteristic peak
From the above figures it can be said that, the Synthesized HAp sample exhibit almost same
diffraction pattern with the characteristic peaks of Hap. The prepared samples are amorphous
structure with some crystalline structure found due to percentage of Hydroxyapatites.
0
500
1000
1500
2000
2500
3000
10 15 20 25 30 35 40 45 50
Inte
nsi
ty C
ou
nts
2 theta
20% Sample (Hot Press)
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CONCLUSION
Lack of osteoinductivity and the problem of inherent brittleness are the two major
challenges associated with hydroxyapatite (HAp), the main mineral component of
bone. This imposes a limitation in its application as a load bearing orthopedic implant
material. The present work aims to overcome the problem of inherent brittleness of
HAp by incorporating HAp/PLA/Cotton composite matrix. This work focused on the
investigation of composites in two main areas: (1) the production and characterization
of composite and (2) the evaluation of mechanical properties and thermal properties.
In this work we try to present some mechanical properties of composite such as
tensile strength, E-modulus, %elongation.TG/DTA analysis, X-ray diffraction (XRD).
The study was involved to prepare composites containing HAp, Poly Lactic Acid and
Cotton by natural drying processafter proper mixing in 1,4 Dioxine at about500C and
also the effect of percentage of PLA and HAp on the composite. The composite are
used to replacement of bone. From this study the following can be conclude that-
The tensile properties of the composite are reduced with increasing HAp.
10% HAp composite shows better tensile properties for Cold Press.
15% HAp composite shows better tensile properties for Hot Press.
From the TG/DTA data it is observed that sample is highly stable.
The prepared samples are amorphous structure with some crystalline structure
found due to percentage of Hydroxyapatites.
Though HAp has good biocompatibility it lacks the strength. The composites are
found to complement each other and improve the required properties. This study
indicates that, HAp, PLA and Cotton can be used as a bone replacement material.
Therefore this is an attempt to bring out the ideas in this emerging field, to kindle the
research in this line, to modify the composition of the composite and to explore the
highly potential applications
Recommendations for Future Research:
1. Cytotoxicity test can be done to analyze cytotoxicity effects.
2. Cell Culture test can be done to investigate acute biocompatibilityof materials
and solutions used in the composite synthesis for the prediction of toxicity
potential.
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