PLA and HAp

1. STUDENT INDUSTRIALWORK EXPERIENCESCHEME (SIWES)
FEBRUARY, 2022
MULTIFUNCTIONAL MATERIAL LABORATORY,SHELL CHAIR OFFICE,
MECHANICAL ENGINEERING, A.B.U ZARIA
Presentation
BY
KUTA MUSA UMAR (U16PT1065)
ON
PRESENTED TO
DEVELOPMENT AND CHARACTERIZATION OF HYDROXYAPATITE (HAp)/ POLY
LACTIC ACID (PLA) BIOCOMPOSITE FOR BIOMEDICAL APPLICATION
UNDERTAKEN AT
DEPARTMENT OF POLYMER AND TEXTILE ENGINEERING, A.B.U ZARIA

2. PRESENTATION
OUTLINE
2
 Introduction
 Development of Hydroxyapatite (HAp)
 HAp/PLA Composite production
 Characterization tests
 Challenges and Solution
 Conclusion
 Recommendation
 References

3. 3
INTRODUCTION
Multifunctional Materials Laboratory is a research laboratory was established by Dr. David Obada after
winning the National Research Fund in 2020. There research focus includes the development,
characterization, and testing of multifunctional materials that are naturally existing and specifically
engineered.
Hydroxyapatite (HAp) is a naturally occurring form of Calcium phosphate, widely used in biomedical
areas, but its deficiency in mechanical properties calls for the development of bio composites.
Polylactic acid (PLA) on the other hand, is a biodegradable thermoplastic polymer, with excellent
mechanical strength as established by previous studies, hence it suitability as a reinforcement to HAp.
Characterization of the properties of these materials helps in understanding the suitability of the
materials in biomedical or other areas of application.

4. 4
DEVELOPMENT OF
HAp
Calcination at
 Pre synthesis treatments
Plate 1: Carbonized
bovine
Plate 2: Calcined
bovine
Sourcing of
bovine
Washing &
Deproteiniza
tion
Carbonizat
ion
Calcination at
900oC
Crushing &
sieving
the bone to
100um
 Sol Gel synthesis of HAp
Plate 5: Fine HAp powder Nano
particle size
Plate 3: Set-up of Sol gel
synthesis
Plate 4: Dying the gel in
Microwave oven

5. 5
HAp/PLA COMPOSITE
PRODUCTION
Plate 6: Melt-Mixing using the Two-roll mill
machine
Plate 8: Compounding using the compression
moulding Machine
Plate 10: Filament formation using Felfill
evo machine.
Plate 7: Melt mixed PLA/HAp Plate 9: Compressed PLA/HAp composite Plate 11: PLA filaments for 3D printing

6. 6
 CAD design modelling of the scaffold using Solid works
 Slicing using the Ultimaker cura software
Plate 13 : Creality 3 pro 3D Printer
3D PRINTING
Plate 12 : FDM layer by layer 3D Printing

7. CHARACTERIZATION
TESTS
7
Plate 14 & 15: Pelletization using Universal Testing Machine
 Hardness Test
 Mechanical characterization test
Plate 16: Micro Vickers Hardness Tester
C100 B100 B50 C50
0.00
0.05
0.10
0.15
0.20
0.25
0.30
0.35
0.40
Hardness
(Gpa)
HAp Sample codes
Fig. 1: Hardness values of 3 HAp samples

8. 8
CHARACTERIZATION TESTS CONT.
 Fracture toughness  Brittleness index
C100 B100 B50 C50
0
1
2
3
4
5
6
7
Brittleness
Index
(-)
HAp Sample Codes
C100 B100 B50 C50
0.00
0.01
0.02
0.03
0.04
0.05
0.06
0.07
Fracture
Tougness
(Kic)
HAp Sample codes
Kic
BI =
Hv (Gpa)
Fig. 2: Fracture toughness of 3 HAp samples Fig. 3: Brittleness index of 3 HAp samples
Kic = 0.016 x ( )-1.5 x Hv x (a)0.5
a
c

9. 9
CHARACTERIZATION TESTS
CONT.
0 2 4 6 8 10 12 14 16 18 20
8.7
8.6
8.5
8.4
8.3
8.2
8.1
Weight
(g)
Days
BC 50/50
C100
B100
 In vitro test
C100 B100 BC 50/50
30
40
50
Porosity
Sample codes
 Porosity test
Fig. 4: Porosity of 3 HAp samples
Fig. 5: Weight loss in 21days period of 3 HAp samples
 Physical characterization test

10. CHARACTERIZATION TESTS
CONT.
10
 Chemical characterization  Other characterization tests carried out
 X-Ray Fluorescence Analysis (XRF)
2.3792
3.10068
2.85919
C100 B100 BC 50/50
0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
Ca/p
ratio
Sample Codes
Fig. 6: Calcium/phosphate ratio of 3 HAp samples
SEM, FTIR, XRD
 Softwares used to carry out calculations,
analysis and making plots
 Ms Excel
 PowDll converter software
 Origin Pro software
 Match 3! software

11. CHALLENGES &
SOLUTION
12
 Inadequate power supply (affects 3Dprinting, prolong experiment time & incubation)
 Rerunning test due to contamination of test sample
 Unavailability of some important machines and equipment
 Importation PLA filaments
 Alternative power source e.g solar energy
 Proper handling/ packaging of test samples
 Purchase of essential equipment and machineries
 Finding alternative source of Synthesizing of PLA locally
Challenges:
Solution:

12. 13
At the end of my internship at MFML, I was exposed to the
basics of materials characterization and analysis, software
operations (Excel, origin Pro, Match 3!), polymer processing,
theoretical and practical researches, articles review/writing, CAD
design modelling (Solidworks), 3D printing/ additive
manufacturing, project defense and presentation etc.
CONCLUSION

13. REFERENCES
14
Destefano, V., Khan, S., & Tabada, A. (2020). Applications of PLA in modern medicine. 1(April), 76–87.
Lin, K., & Chang, J. (2015). Structure and properties of hydroxyapatite for biomedical applications. In
Hydroxyapatite (Hap) for Biomedical Applications (Vol. 4214, Issue 8). Elsevier Ltd. https://doi.org/10.1016/b978-1-
78242-033-0.00001-8
Ma, G. (2019). Three common preparation methods of hydroxyapatite. IOP Conference Series: Materials Science
and Engineering. https://doi.org/10.1088/1757-899X/688/3/033057
Vyas, D., & Udyawar, D. (2019). A review on current state of art of bioprinting. In 3D Printing
and Additive Manufacturing Technologies (pp. 195-201). Springer, Singapore.
Zimina, A., Senatov, F., Choudhary, R., Kolesnikov, E., Anisimova, N., Kiselevskiy, M., ... &
Karyagina, A. (2020). Biocompatibility and physico-chemical properties of highly porous PLA/HA scaffolds for
bone reconstruction. Polymers, 12(12), 2938.

14. THANK YOU