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 Procedia Materials Science 11 ( 2015) 588 – 593  Av ailable o nline at www .sciencedire ct.com 2211-8128 © 2015 Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/ ). Peer-review under responsibility of the organizing committee of UFGNSM15 doi:10.1016/j.mspro.2015.11.083 ScienceDirect 5th International Biennial Conference on Ultrafine Grained and Nanostructured Materials, UFGNSM15 Preparation and Characterization A Novel Nano Composite Barrier For Gtr / Gbr  N. Alikhanifard a , A. Zargar a, *, S. Karbasi a a  Biomaterials,Nanotechnology and Tissue Enginee ring Group,Department of Advanced Medical Techno logy,Isfahan university of Medi cal sciences,Isfahan,Iran Abstract Lack of bone tissue and its regeneration has been one of the important challenges of dentistry. Periodontitis is a chronic inflammatory disorder such factors can lead to periodontal tissue destruction, loss of bone tissue and eventually cause tooth loss. Currently, to repair and replace lost bone tissue, membranes are used. In this research, the Nanocomposit barrier was made by poly (3-hydroxybutyrate) (P3HB) as matrix with different percentage Diopside nanoparticles as reinforcement were prepared by Electrospining process. Scanning electron microscope (SEM) image showed uniform fibers with diameter less than 200 nanometres and the image processing by MATLAB software shown 85% porosity with interconnected porous architecture. The FTIR results demonstrated the proper interaction between the polymer and Nono powder Diopside. Thin sheeting, as well as, confirmed optimal strength as a barrier to stability in the affected area by applying compressive forces during chewing. In conclusion, this Nano composite could be used as a admissible nomination for Guided tissue regeneration and Guided bone regeneration (GTR/GBR) applications. © 2015 The Authors. Published by Elsevier Ltd. Peer-review under responsibility of the organizing committee of UFGNSM15. Keywords:Barrier; Nanocomposite; Guided tissue regeneration; Guided bone regeneration . *Corresponding author. Tel.: 098-31-3266-6138; fax: 098-31-95016490 E-mail address:[email protected] © 2015 Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/ ). Peer-review under responsibility of the organizing committee of UFGNSM15
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 Procedia Materials Science 11 (2015) 588 – 593

 Available online at www.sciencedirect.com

2211-8128 © 2015 Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license

(http://creativecommons.org/licenses/by-nc-nd/4.0/ ).

Peer-review under responsibility of the organizing committee of UFGNSM15

doi:10.1016/j.mspro.2015.11.083

ScienceDirect 

5th International Biennial Conference on Ultrafine Grained and Nanostructured Materials,UFGNSM15

Preparation and Characterization A Novel Nano Composite Barrier

For Gtr / Gbr

 N. Alikhanifard a, A. Zargar a,*, S. Karbasia

a Biomaterials,Nanotechnology and Tissue Engineering Group,Department of Advanced Medical Technology,Isfahan university of Medical

sciences,Isfahan,Iran

Abstract

Lack of bone tissue and its regeneration has been one of the important challenges of dentistry. Periodontitis is a chronic

inflammatory disorder such factors can lead to periodontal tissue destruction, loss of bone tissue and eventually cause tooth loss.

Currently, to repair and replace lost bone tissue, membranes are used. In this research, the Nanocomposit barrier was made by poly

(3-hydroxybutyrate) (P3HB) as matrix with different percentage Diopside nanoparticles as reinforcement were prepared by

Electrospining process. Scanning electron microscope (SEM) image showed uniform fibers with diameter less than 200 nanometres

and the image processing by MATLAB software shown 85% porosity with interconnected porous architecture. The FTIR results

demonstrated the proper interaction between the polymer and Nono powder Diopside. Thin sheeting, as well as, confirmed optimal

strength as a barrier to stability in the affected area by applying compressive forces during chewing. In conclusion, this Nano

composite could be used as a admissible nomination for Guided tissue regeneration and Guided bone regeneration (GTR/GBR)

applications.© 2015 The Authors. Published by Elsevier Ltd.

Peer-review under responsibility of the organizing committee of UFGNSM15.

Keywords:Barrier; Nanocomposite; Guided tissue regeneration; Guided bone regeneration.

*Corresponding author. Tel.: 098-31-3266-6138; fax: 098-31-95016490

E-mail address:[email protected]

© 2015 Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license

(http://creativecommons.org/licenses/by-nc-nd/4.0/ ).

Peer-review under responsibility of the organizing committee of UFGNSM15

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589 N. Alikhanifard et al. / Procedia Materials Science 11 (2015) 588 – 593

1. 

Introduction

Aging population and unpredictable events of the main reasons for the development of dental biomaterials. This

causes a significant increase in the number and reconstructive surgery, dental implants and crowns with a ceramic or

 prostheses are to rebuild gums, this often leads to the use of membranes for guided tissue regeneration or bone (GTR

/ GBR) with or without the hybrid materials. Apart from the above, periodontitis is also one of the most devastating

injuries that affect periodontal integrity system and periodontal tissue damage and ultimately tooth loss, Pihlstrom et

al. (2005). To repair and replace lost bone graft materials, membranes, or both are used Membranes as a physical

 barrier to prevent penetration of fibroblasts into the connective tissue and create space and help to regenerate the

 periodontal tissues used. In order to connect need membranes and biocompatibility with the host tissue without

causing inflammatory responses, Profile destruction in order to comply with the new tissue formation, physical and

mechanical properties are suitable for inclusion in body and sufficient strength to prevent collapse of the membrane

and spontaneous performance are as a barrier, Rakhmatia et al. (2013). But is important that, membrane absorption

time to comply with the restoration of the affected area and stabilize the site of injury by applying compressive forces

during chewing. Commercially available membranes has many structural constraints, mechanical and biological

functions. Among the variety of methods used for fabricating the membranes, electrospinning is promising for

applications such as GTR / GBR, Dimitriou et al. (2012). Essentially, the three-dimensional structure obtained by the

electrospun membranes with a high level of structural, mechanical strength and performance tuning guide the newcells into the bone defect offers. Electrospinning has attracted much attention because it is a unique technique to obtain

the scaffolds with micro or nanofibrous structure which are similar to extracellular matrix (ECM). due to the high

surface area, the functional groups associated pore size at the nanoscale, the scaffold-based nanofibers more favorable

micro-fiber scaffolds or other morphological forms, Venugopal et al. (2008), Ayres et al. (2010).

Polymer/bioceramicnanocomposites have indicated improved mechanical and structural properties, optimum

degradation kinetics, bioactivity and tissue interaction. P3HB as a member of the Polyhydroxyalkanoates (PHA)

family, has attracted much attention for a variety of medical applications because of its biodegradation, excellent

cytocompatibility to various cell including osteoblasts, fibroblasts, chondrocytes, endothelium and epithelium cells

and Compared with polymers of poly-alpha-hydroxy acids (e.g., poly-lactic acid or poly lactic glycolic acid) have a

longer degradation time, Misra et al. (2006), Yang, et al. (2009). In recent years, diopside ceramics, biomaterials

applications are considered. Allowing the formation of apatite in simulated body fluid and will connect seamlessly to

the bone. In addition, studies, Hase et al. (2011), indicate a much higher mechanical strength of hydroxyapatite andWollastonite was much slower degradation rate. Haes et al. (2011), has been recommended diopside in the treatment

of dentinal caries due to rapid deposition of apatite on the surface. Another bioactive diopsideceramics, provides

desirable properties in the human mouth. So, dental applications such as bone repair in periodontal disease can be a

good option. Generally, the purpose of adding nanoparticles to the polymer material used in bio-mimicking

compounds are to improve the response of biological tissue such as cell adhesion, cell proliferation or destruction and

mainly improve the mechanical properties of nanocomposite structures. 

Nomenclature

 ND NanoDiopside

PHB Polyhydroxybutyrate

D Distance

V Voltage

2. 

Experimental procedure 

2.1. 

Fabrication and sample preparation

Poly (3hydroxybutyrate) powder was purchased from Sigma-Aldrich USA (CAS=26063-00-3, Mw=3000,000g

mol-1,LOT NUMBER: S68924-099). Chloroform (CF) and Dimethylformamid (DMF) were bought from MERCK,

Germany. Diopsid nanoparticles, were synthesized as described by(Iwata, Lee et al. 2004) with following precursors:

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590  N. Alikhanifard et al. / Procedia Materials Science 11 (2015) 588 – 593

analytical grade Ca(NO3)2.4H2O,MgCl2.6H2O, Ethanol and Si(OC2H5)4(Merck). Transmission electron

microscope, TEM (CM120 PHLIPS), was utilized to study the morphology and to determine the size of diopside

nanoparticles. X-ray diffraction (XRD) analysis of samples was performed using (Bruker. DB ADVANCE. Germany)

diffract meter. For preparation of polymer solution with 6% Wtconcentration, P3HB dissolved in a mixture of

CF/DMF solvents. The solution was stirred for 30 min at 50 ºC. Then nD with different (5, 10, 15%Wt) were added

to the solution and stirred for 30 min. Homogenizer was used for improving homogenization and preventing of

nanoparticles agglomeration. Finally, electrospinning was done with applying different voltage and distance betweenthe nozzle and the webs collector .

3. 

Results and Discussion

3.1. Characterization of NanoDiopside powder

Figure 1 shows the TEM image (a) and XRD (b) pattern of diopside nanoparticles. According to Fig. 1a, the

diopside nanoparticles are in the range of 50 – 100 nm and exhibit agglomerative morphologies with irregular shapes.

The XRD analysis of the prepared powder indicated the peaks associated with the diopside phase according to JCPDS

standard. (Fig. 1b).

Fig. 1. (a) TEM image; (b) XRD pattern of diopside Nanoparticles.

3.2. FT-IR analysis

To characterize the surface of modified samples, attenuated total The Fourier transform infrared (FTIR)

spectroscopy analysis was performed using FT Infrared Spectroscope, JASCO, FT/IR-6300 (400-4000 cm-1), Japan.

FTIR spectroscopy of the P3HB /nD nanocomposite revealed proper interaction between PHB and nD. In Fig.2, the

 peak of carbonyl groups was shifted from 1725.98 to 1721.16 cm¹ and the intensity is shorter than the same peak for

 pure PHB. These changes could be related to the formation of hydrogen bonds between the carbonyl groups of the

nD.

Fig. 2. FT Infrared Spectroscope of PHB/ NanoDiopside.

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591 N. Alikhanifard et al. / Procedia Materials Science 11 (2015) 588 – 593

3.3. 

Scanning electron microscopy (SEM)

The results of Scanning electron microscope (SEM) kyky- EM3200, images show that the fibers in the composite

with ND (10% wt) in comparison with other amount is more uniform (Fig. 3b). Also fibers diameter compared with

 pure polymer significantly from average about 600 nm to lesser than 200 nm dropped (Fig. 3 (h and k)) .The reduced

diameter of the fibers makes the composite produced closer to ECM of natural texture. This is a positive factor which

is expected to lead to cell growth. On the other hand, due to a decrease in fiber diameter Pores size may be reduced.

As a result, the average pore size is reduced, interconnectivity of porosity increases. Also, SEM images (Fig. 3 (d and

f)) of Nanocomposite membranes demonstrate at ND conconcentration above 10% Wt, and voltage upper than 10 Kv,

they tend to agglomerate. Pursuant to demonstrate that nanofibers are uniformly. Finally, electrospinning was done

with applying voltage of 10KV. The distance between the nozzle and the webs collector was 20 Cm. SEM images in

Fig. 2 (d and e), show that the other amounts of voltage and distance fibers morphology is not uniform and in some

circumstances has occurred agglomeration.

Fig. 3. SEM image (a) ND=5%, V=10kv ,D=20 cm; (b) ND=10, v=10 ,D=20; (c) ND=15, V=10 ,D=20; (d) ND=15, V=15 ,D=10; (e) ND=10,

V=15 ,D=10; (f) ND=15, V=15 ,D=20; (g) ND=10,V=15, D=20; (h) ND=0,V=10, D=20; (k) ND=10,V=10,D=20 .

b

1000× 10 m×

c

1000× 10 m

×

f d

×1000× 10 m 

e

k

1000× 10μm 1000× 10μm 

h

1000× 10μm 

g

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592  N. Alikhanifard et al. / Procedia Materials Science 11 (2015) 588 – 593

3.4. 

 Determination of porosity

This method revealed that image analysis can easily be exerted to the porosity measurement of various layers,

Ghasemi et al. (2007). It can be seen from SEM images samples that3-b has an open porosity. Using MATLAB

software 85% of porosity sample were confirmed. The porosity of each right nutrients to penetrate the cell and

cellular metabolism are required .

Fig. 4. Porous membrane images processed by MATLAB software.

3.5.  Mechanical properties

Tensile properties done according to ASTM D882-02.When the membrane is placed UNDER PRESSURE, the

load is transmitted from matrix to nanoparticles that could result in improved mechanical properties. As can be seen

with the percentage of Nano-powder diopside significant change in strength of composites in comparison with

 polymer cannot be seen. But By comparing the average modulus of elasticity, it can be reviled that composites

containing with (10% wt) nD Compared with the rest of the percentages have Lower modulus of components. That ,It is very suitable for clinical applications due to its easily forming manner at the site of the defect, Stamatialis et al.

2008, Rakhmatia, et al. 2013). 

Fig. 5. (a) Tensile stress; (b) Modulus of Nano composite. 

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593 N. Alikhanifard et al. / Procedia Materials Science 11 (2015) 588 – 593

4. Conclusion

In this study, the novel nanocomposite membrane was prepared with 10 wt% NanoDiopside, and the SEM images

demonstrated that the membrane possesses less agglomeration and have uniform fibers with diameter less than 200

nanometers and the image processing of the optimum sample by MATLAB software shown 85% porosity with

interconnected porous architecture, that may improve cell attachment. In addition, the FTIR results showed that it

seems there is a favourable interaction between polymer and diopside nanoparticles which improves connection in theinterface of nanocomposite’s phases. Finally, this membrane has acceptable porosity and morphologic character that

warrants further studies to be conducted on the perspective for Guided tissue regeneration and Guided bone

regeneration (GTR/GBR) applications.

Acknowledgements

The authors especially thanks to the members of fatuity of medical sciences of new technologies, and the department

of biomaterials.

References

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structure and function." Wiley Interdisciplinary Reviews: Nanomedicine and Nanobiotechnology 2(1): 20-34.

Dimitriou, R., Mataliotakis, G.I., Calori, G.M., Giannoudis, P.V., 2012. "The role of barrier membranes for guided bone regeneration and

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Stamatialis, D.F., Papenburg, B.J., Gironés, M., Saiful, S., Bettahalli, S.N., Schmitmeier, S., Wessling, M., 2008. "Medical applications of

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