preparation and characterization of synthesized

28
Preparation and Characterization of Synthesized Hydroxyapatite, Poly Lactic Acid & Cotton (Gauze) Composite Film. Author Names: 1 Md. 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. GSJ: VOLUME 6, ISSUE 2, FEBRUARY 2018 330 GSJ© 2018 www.globalscientificjournal.com

Upload: others

Post on 18-Dec-2021

6 views

Category:

Documents


0 download

TRANSCRIPT

Page 1: Preparation and Characterization of Synthesized

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.

GSJ: VOLUME 6, ISSUE 2, FEBRUARY 2018 330

GSJ© 2018 www.globalscientificjournal.com

ashish
Typewritten Text
ashish
Typewritten Text
ashish
Typewritten Text
ashish
Typewritten Text
ashish
Typewritten Text
GSJ: Volume 6, Issue 2, February 2018, Online: ISSN 2320-9186 www.globalscientificjournal.com
ashish
Typewritten Text
ashish
Typewritten Text
ashish
Typewritten Text
ashish
Typewritten Text
ashish
Typewritten Text
ashish
Typewritten Text
ashish
Typewritten Text
ashish
Typewritten Text
ashish
Typewritten Text
ashish
Typewritten Text
ashish
Typewritten Text
ashish
Typewritten Text
Page 2: Preparation and Characterization of Synthesized

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.

GSJ: VOLUME 6, ISSUE 2, FEBRUARY 2018 331

GSJ© 2018 www.globalscientificjournal.com

Page 3: Preparation and Characterization of Synthesized

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

GSJ: VOLUME 6, ISSUE 2, FEBRUARY 2018 332

GSJ© 2018 www.globalscientificjournal.com

Page 4: Preparation and Characterization of Synthesized

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

GSJ: VOLUME 6, ISSUE 2, FEBRUARY 2018 333

GSJ© 2018 www.globalscientificjournal.com

Page 5: Preparation and Characterization of Synthesized

Chapter 1: Introduction

produce three dimensional bio mimicking scaffolds with layered configuration with

complex pore structures and controlled pore size[25]

GSJ: VOLUME 6, ISSUE 2, FEBRUARY 2018 334

GSJ© 2018 www.globalscientificjournal.com

Page 6: Preparation and Characterization of Synthesized

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

GSJ: VOLUME 6, ISSUE 2, FEBRUARY 2018 335

GSJ© 2018 www.globalscientificjournal.com

Page 7: Preparation and Characterization of Synthesized

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

GSJ: VOLUME 6, ISSUE 2, FEBRUARY 2018 336

GSJ© 2018 www.globalscientificjournal.com

Page 8: Preparation and Characterization of Synthesized

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.

GSJ: VOLUME 6, ISSUE 2, FEBRUARY 2018 337

GSJ© 2018 www.globalscientificjournal.com

Page 9: Preparation and Characterization of Synthesized

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%

GSJ: VOLUME 6, ISSUE 2, FEBRUARY 2018 338

GSJ© 2018 www.globalscientificjournal.com

Page 10: Preparation and Characterization of Synthesized

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%

GSJ: VOLUME 6, ISSUE 2, FEBRUARY 2018 339

GSJ© 2018 www.globalscientificjournal.com

Page 11: Preparation and Characterization of Synthesized

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

GSJ: VOLUME 6, ISSUE 2, FEBRUARY 2018 340

GSJ© 2018 www.globalscientificjournal.com

Page 12: Preparation and Characterization of Synthesized

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

GSJ: VOLUME 6, ISSUE 2, FEBRUARY 2018 341

GSJ© 2018 www.globalscientificjournal.com

Page 13: Preparation and Characterization of Synthesized

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

GSJ: VOLUME 6, ISSUE 2, FEBRUARY 2018 342

GSJ© 2018 www.globalscientificjournal.com

Page 14: Preparation and Characterization of Synthesized

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

GSJ: VOLUME 6, ISSUE 2, FEBRUARY 2018 343

GSJ© 2018 www.globalscientificjournal.com

Page 15: Preparation and Characterization of Synthesized

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

GSJ: VOLUME 6, ISSUE 2, FEBRUARY 2018 344

GSJ© 2018 www.globalscientificjournal.com

Page 16: Preparation and Characterization of Synthesized

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

GSJ: VOLUME 6, ISSUE 2, FEBRUARY 2018 345

GSJ© 2018 www.globalscientificjournal.com

Page 17: Preparation and Characterization of Synthesized

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%

GSJ: VOLUME 6, ISSUE 2, FEBRUARY 2018 346

GSJ© 2018 www.globalscientificjournal.com

Page 18: Preparation and Characterization of Synthesized

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%

GSJ: VOLUME 6, ISSUE 2, FEBRUARY 2018 347

GSJ© 2018 www.globalscientificjournal.com

Page 19: Preparation and Characterization of Synthesized

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%

GSJ: VOLUME 6, ISSUE 2, FEBRUARY 2018 348

GSJ© 2018 www.globalscientificjournal.com

Page 20: Preparation and Characterization of Synthesized

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%

GSJ: VOLUME 6, ISSUE 2, FEBRUARY 2018 349

GSJ© 2018 www.globalscientificjournal.com

Page 21: Preparation and Characterization of Synthesized

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%

GSJ: VOLUME 6, ISSUE 2, FEBRUARY 2018 350

GSJ© 2018 www.globalscientificjournal.com

Page 22: Preparation and Characterization of Synthesized

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)

GSJ: VOLUME 6, ISSUE 2, FEBRUARY 2018 351

GSJ© 2018 www.globalscientificjournal.com

Page 23: Preparation and Characterization of Synthesized

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)

GSJ: VOLUME 6, ISSUE 2, FEBRUARY 2018 352

GSJ© 2018 www.globalscientificjournal.com

Page 24: Preparation and Characterization of Synthesized

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)

GSJ: VOLUME 6, ISSUE 2, FEBRUARY 2018 353

GSJ© 2018 www.globalscientificjournal.com

Page 25: Preparation and Characterization of Synthesized

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.

GSJ: VOLUME 6, ISSUE 2, FEBRUARY 2018 354

GSJ© 2018 www.globalscientificjournal.com

Page 26: Preparation and Characterization of Synthesized

Chapter5: References

[1].D. Lahiri, S. Ghosh, A. Agarwal, A review Mater. Sci. Eng. C 32 (2012) 1727–1758.

[2]Molly M. Stevens, "Biomaterials for Bone Tissue Engineering"; Materials Today, May 2004,

vol. 11, number-5.

[3]Adele Boskey and Nancy Pleshko Camacho, "FT-IR imaging of Native and Tissue

Engineered Bone and Cartilage"; Biomaterials. 2007 May; 28(15): 2465-2478.

[4]Meijer, G.J., de Bruijn, J.D., Koole, R. and van Blitterswijk C. Cell-based bone tissue

engineering. PLoS Med 4, 260-264, 2007.

[5] LeGeros, R.Z. Propertiesof osteoconductive biomaterials: Calcium phosphates.

ClinOrthopRelat R 395, 81-98, 2002.

[6]Baksh, D., Davies, J.E. and Kim, S. Three-dimensional matrices of calcium

polyphosphates support bone growth in vitro and in vivo. J Mater Sci-Mater M9, 743-748, 1998.

[7]Vacanti, C.A., Bonassar, L.J., Vacanti, M.P., and Shufflebarger, J. Replacement of an avulsed

phalanx with tissue-engineered bone. New Eng J Med 344, 1511-1514, 2001. 43

[8]Dong, J.A., Uemura, T., Shirasaki, Y. and Tateishi, T. Promotion of bone formation using

highly pure porous beta-TCP combined with bone marrow-derived osteoprogenitor cells.

Biomaterials 23, 4493-4502, 2002.

[9]Yoshikawa, T., Ohgushi, H., Uemura, T., Nakajima, H., Ichijima, K., Tamai, S., and Tateisi,

T. Human marrow cells-derived cultured bone in porous ceramics. Bio-Med Mater Eng 8,

311-320, 1998.

[10]Y.W. Gu, K.A. Khor, P. Cheang, Biomaterials 25 (2004) 4127–4134.

[11]Rizzi SC, Heath DJ, Coombes AGA, Bock N, Textor M, Downes S. Biodegradable

polymer/hydroxyapatite composites: Surface analysis and initial attachment of human

osteoblasts. J Biomed Mater Res. 2001; 55:475-486.

[12]Skrtic D, Antonucci JM, Eanes ED. Amorphous calcium phosphate-based bioactive

polymeric composites for mineralized tissue regeneration. J Res Natl Inst Stand Technol 2003;

108:167-182.

GSJ: VOLUME 6, ISSUE 2, FEBRUARY 2018 355

GSJ© 2018 www.globalscientificjournal.com

Page 27: Preparation and Characterization of Synthesized

Chapter5: References

[13] Furukawa T, Matsusue Y, Yasunaga T, Shikinami Y, Okuno M, Nakamura T.

Biodegradation behavior of ultra-high-strength hydroxyapatite/poly (L-lactide) composite rods

for internal fixation of bone fractures. Biomaterials 2000; 21:889-98.

[14] Ducheyne P, QiuQ. Bioactive ceramics: The effect of surface reactivity on bone formation

and bone cell function. Biomaterials 1999; 20:2287-303.

[15] Mikos, A.G., Thorsen, A.J., Czerwonka, L.A., Bao, Y., Langer, R., Winslow, D.N. and

Vacanti, J.P. Preparation and characterization of poly(l-lactic acid) foams. Polymer 35, 1068-

1077, 1994.

[16] Holy, C.E., Shoichet, M.S. and Davies, J.E. Engineering three-dimensional bone tissue

in vitro using biodegradable scaffolds: Investigating initialcell-seeding density and culture

period. J Biomed Mater Res 51, 376-382, 2000.

[17] Salgado, A.J, Continho, O.P and Reis, R.L. Bone tissue engineering: state of the art and

future trends. MacromolBiosci 4, 743 -765, 2004.

[18] Mooney, D.J., Baldwin, D.F., Suh, N.P., Vacanti, L.P. and Langer, R. Novel approach

to fabricate porous sponges of poly(D,L-lactic-co-glycolic acid) without the use of organic

solvents. Biomaterials 17, 1417-1422, 1996.

[19]Lee, M., Dunn,J.C.Y. and Wu, B.M. Scaffold fabrication by indirect threedimensional

printing. Biomaterials 26, 4281-4289, 2005.

[20] Mao, J.S., Zhao, L.G., Yin, Y.J. and Yao, K.D. Structure and properties of bilayer

chitosan-gelatin scaffolds. Biomaterials 24, 1067-1074, 2003.

[21]Formhals, A. Process and Apparatus for Preparing Artificial Threads. US patent No.

1,975,504, 1934.

[22]Li, W.J., Laurencin, C.T., Caterson, E.J., Tuan, R.S. and Ko, F.K.

Electrospunnanofibrous structure: A novel scaffold for tissue engineering. J. Biomed. Mater.

Res. 60, 613-621, 2002.

[23]Li, M.Y., Mondrinos, M.J., Gandhi, M.R., Ko, F.K., Weiss, A.S., and Lelkes,

P.I.Electrospun protein fibers as matrices for tissue engineering. Biomaterials 26, 5999, 2005.

GSJ: VOLUME 6, ISSUE 2, FEBRUARY 2018 356

GSJ© 2018 www.globalscientificjournal.com

Page 28: Preparation and Characterization of Synthesized

Chapter5: References

[24]Han, D., and Gouma, P.I. Electrospunbioscaffolds that mimic the topology of

extracellular matrix. Nanomed-NanotechnolBiol Med 2, 37-41, 2006]

[25]Chen, L.J. and Wang, M. Production and evaluation of biodegradable composites

based on PHB-PHV copolymer. Biomaterials 23, 2631-2639, 2002.

[26] Shin, Y.M., Hohman, M.M., Brenner, M.P., Rutledge, G.C. Experimental

characterization of electrospinning: the electrically forced jet and instabilities. Polymer 42,

9955-9967, 2001.

GSJ: VOLUME 6, ISSUE 2, FEBRUARY 2018 357

GSJ© 2018 www.globalscientificjournal.com