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AbstractCeramic prosthesis made through additive and subtractive technologies, lead to superior esthetic and qualitative results towards metal-ceramic prosthesis. Material and Method: 30 IPS Empress ceramic discs were involved in this study. The samples were treated through two different methods for obtaining a superior adherent surface. The samples were devided into three groups. The first group was not conditioned. The other two groups were treated by (2) sandblasting, (3) sandblasting and then conditioned with HFA 9% (hidrofluoric acid), After conditioning, the surfaces were investigated by Scannig Electonic Microscopy technology (SEM) and Atomic Force Microscopy. Results: SEM and AFM images of conditioned specimens were investigated for evaluating surface’s texture in order to obtain an improved adhesion. Conclusions: The results has shown that new methods for conditioning the Empress ceramic core assure an adesion that give a good prognostic to the long term results. Keywords—SEM, AFM, ceramic core, sandblasting, etching I. INTRODUCTION Numerous attempts have been made to develop ceramic systems that eliminate metallic infrastructures in purpose to obtain superior esthetics. New ceramic systems like reinforced ceramic cores through dispersion with leucite, glass infiltration into sintered alumina (Al2O3) , high-purity alumina or Petrescu Emanuela Lidia , is with University of Medicine and Pharmacy Victor Babes Timisoara, Faculty of Dentistry (0040744616009, [email protected] ) Cosmin Sinescu is with University of Medicine and Pharmacy Victor Babes Timisoara, Faculty of Dentistry (0040744616009, [email protected] ) Meda Lavinia Negrutiu is with University of Medicine and Pharmacy Victor Babes Timisoara, Faculty of Dentistry (0040744616009, [email protected] ) Roxana Rominu is with University of Medicine and Pharmacy Victor Babes Timisoara, Faculty of Dentistry (0040744616009 [email protected] Florin Topala is with University of Medicine and Pharmacy Victor Babes Timisoara, Faculty of Dentistry (0040744616009 [email protected] Daniela Maria Pop is with University of Medicine and Pharmacy Victor Babes Timisoara, Faculty of Dentistry (0040744616009 [email protected] Mihai Rominu is with University of Medicine and Pharmacy Victor Babes Timisoara, Faculty of Dentistry (0040744616009 [email protected] zirconium dioxide (zirconia, ZrO2) are replacing metal- ceramic prostheses. But both metal-ceramic and all-ceramic prosthesis may lead to fracture of the esthetic component. Such accidents may be rehabilitating through direct methods in dental clinics after conditioning the ceramic infrastructure in order to improve the adhesion. Fracture of the esthetic component of all-ceramic prosthesys can be repaired with composite resin material. The core material must be conditioned through different methods for improving the adhesion of composite resin to ceramic core. This study intends to investigate IPS Empress e.max conditioned and not conditioned ceramic cores through AFM and SEM optical investigation methods. The investigation will assert the differencences and characteristics between the samples. II. MATERIAL AND METHOD In this study, 30 ceramic-cores were made, using IPS Empress e.max system. The wax-pattern had 1mm thickness, and 1x1cm. The probes and draw bar attached were positioned on the injection con with a special device, which assures an angle of 45-60º between the injection con and wax-pattern. The investment material Press Vest Speed was prepared after the manufacturer’s instructions in vaccum-blender. The kit, (wax- pattern, draw bar and pressing plunger) was invested using a proper ring, which was removed after the Press vest Speed setting. For obtaining the cast, the wax was evacuated and the kit was introduced in the preheating oven Sirio- Fire Light for 60 minutes at 850ºC. The injection plunger was isolated with Alox Plunger Separator and the ceramic cylinder e.max.press was introduced in the injection con. The pre-set parameters of the injection program rules at 920ºC, temperature at which the ceramic material is pressed in the cast. The pre-heated cast was introduced in the oven and the proper injection process took place. After ending the injection process and slow cooling, the kit was de-invested with low force. The residual investment material was removed by send blasting with particles of Al2O3 and 110μm in diameter al a pressure of 2 barr. The braw-bars were sectioned with burs. The probes were divided into three groups. The first group was conditioned by sandblasting with 110μm grain sized aluminium dioxide particles at a pressure of 3atm with Al2O3 grains from a distance of 10 mm for 13 s and hydrofluoric acid in 9% concentration for 90 s. Atomic Force Microscopy and Scanning Electronic Microscopy Investigations of Conditioned IPS Empress E.max Ceramic Core Emanuela Lidia Petrescu, Meda Lavinia Negrutiu, Cosmin Sinescu, Roxana Rominu, Florin Topala, Pop Daniela Maria, Mihai Rominu Advances in Communications, Computers, Systems, Circuits and Devices ISBN: 978-960-474-250-9 348

Atomic Force Microscopy and Scanning Electronic Microscopy ... · Petrescu Emanuela Lidia , is with University of Medicine and Pharmacy Victor Babes Timisoara, Faculty of Dentistry

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Abstract— Ceramic prosthesis made through additive and

subtractive technologies, lead to superior esthetic and qualitative

results towards metal-ceramic prosthesis. Material and Method: 30

IPS Empress ceramic discs were involved in this study. The samples

were treated through two different methods for obtaining a superior

adherent surface. The samples were devided into three groups. The

first group was not conditioned. The other two groups were treated

by (2) sandblasting, (3) sandblasting and then conditioned with HFA

9% (hidrofluoric acid), After conditioning, the surfaces were

investigated by Scannig Electonic Microscopy technology (SEM) and

Atomic Force Microscopy. Results: SEM and AFM images of

conditioned specimens were investigated for evaluating surface’s

texture in order to obtain an improved adhesion. Conclusions: The

results has shown that new methods for conditioning the Empress

ceramic core assure an adesion that give a good prognostic to the

long term results. Keywords—SEM, AFM, ceramic core, sandblasting, etching

I. INTRODUCTION

Numerous attempts have been made to develop ceramic

systems that eliminate metallic infrastructures in purpose to

obtain superior esthetics. New ceramic systems like reinforced

ceramic cores through dispersion with leucite, glass infiltration

into sintered alumina (Al2O3) , high-purity alumina or

Petrescu Emanuela Lidia , is with University of Medicine and Pharmacy

Victor Babes Timisoara, Faculty of Dentistry (0040744616009,

[email protected])

Cosmin Sinescu is with University of Medicine and Pharmacy Victor Babes

Timisoara, Faculty of Dentistry (0040744616009,

[email protected])

Meda Lavinia Negrutiu is with University of Medicine and Pharmacy Victor

Babes Timisoara, Faculty of Dentistry (0040744616009,

[email protected])

Roxana Rominu is with University of Medicine and Pharmacy Victor Babes

Timisoara, Faculty of Dentistry (0040744616009

[email protected]

Florin Topala is with University of Medicine and Pharmacy Victor Babes

Timisoara, Faculty of Dentistry (0040744616009

[email protected]

Daniela Maria Pop is with University of Medicine and Pharmacy Victor

Babes Timisoara, Faculty of Dentistry (0040744616009

[email protected]

Mihai Rominu is with University of Medicine and Pharmacy Victor Babes

Timisoara, Faculty of Dentistry (0040744616009

[email protected]

zirconium dioxide (zirconia, ZrO2) are replacing metal-

ceramic prostheses. But both metal-ceramic and all-ceramic

prosthesis may lead to fracture of the esthetic component. Such

accidents may be rehabilitating through direct methods in

dental clinics after conditioning the ceramic infrastructure in

order to improve the adhesion. Fracture of the esthetic

component of all-ceramic prosthesys can be repaired with

composite resin material. The core material must be

conditioned through different methods for improving the

adhesion of composite resin to ceramic core.

This study intends to investigate IPS Empress e.max

conditioned and not conditioned ceramic cores through AFM

and SEM optical investigation methods. The investigation will

assert the differencences and characteristics between the

samples.

II. MATERIAL AND METHOD

In this study, 30 ceramic-cores were made, using IPS Empress

e.max system. The wax-pattern had 1mm thickness, and 1x1cm.

The probes and draw bar attached were positioned on the

injection con with a special device, which assures an angle of

45-60º between the injection con and wax-pattern. The

investment material Press Vest Speed was prepared after the

manufacturer’s instructions in vaccum-blender. The kit, (wax-

pattern, draw bar and pressing plunger) was invested using a

proper ring, which was removed after the Press vest Speed

setting. For obtaining the cast, the wax was evacuated and the

kit was introduced in the preheating oven Sirio- Fire Light for

60 minutes at 850ºC. The injection plunger was isolated with

Alox Plunger Separator and the ceramic cylinder e.max.press

was introduced in the injection con. The pre-set parameters of

the injection program rules at 920ºC, temperature at which the

ceramic material is pressed in the cast. The pre-heated

cast was introduced in the oven and the proper injection process

took place. After ending the injection process and slow cooling,

the kit was de-invested with low force. The residual investment

material was removed by send blasting with particles of Al2O3

and 110µm in diameter al a pressure of 2 barr. The braw-bars

were sectioned with burs.

The probes were divided into three groups. The first

group was conditioned by sandblasting with 110µm grain sized

aluminium dioxide particles at a pressure of 3atm with Al2O3

grains from a distance of 10 mm for 13 s and hydrofluoric acid

in 9% concentration for 90 s.

Atomic Force Microscopy and Scanning

Electronic Microscopy Investigations of

Conditioned IPS Empress E.max Ceramic Core

Emanuela Lidia Petrescu, Meda Lavinia Negrutiu, Cosmin Sinescu, Roxana Rominu, Florin Topala,

Pop Daniela Maria, Mihai Rominu

Advances in Communications, Computers, Systems, Circuits and Devices

ISBN: 978-960-474-250-9 348

Samples from the second group were first sandblasted

in the same conditions and then acid conditioned with

hydrofluoric acid 9% for 90 seconds. The ceramic surfaces

were etched in the laboratory under ventilation, wearing acid-

resistant gloves and protective glasses. The etching gel was

rinsed in a polyethylene cup and the diluted solution was

neutralized using the neutralizing powder (calcium carbonate,

CaCO3) for 5 min and washed thoroughly for 20 s The etched

substrates were washed and rinsed thoroughly to remove the

residual acid after etching and air-dried.

The samples were investigated through Atomic Force

Microscopy and Scanning Electronic Microscopy investigation

methods.

Scanning Electron Microscope images the sample surface,

which is scanned with a high-energy beam of electrons. The

interaction between the electrons and the sample’s atoms

generate signals that contain information about the sample’s

surface topography. After conditioning the ceramic cores, the

surface topography has been changed and influenced by the

conditioning method. Atomic Force Microscopy or Scanning

Force Microscopy is a very high-resolution type of scanning

probe microscopy. The surface roughness is determined by a

cantilever’s sharp probe. The probe is attached at cantilever’s

end and it is extremely sensitive. When the tip is brought into

proximity of the sample’s surface, the forces between the tip

and the sample lead to a deflection of the cantilever. The

imaging modes are divided into static or contact mode or

dynamic or non-contact mode where the cantilever is vibrated.

The oscillation amplitude determined the surface roughness

providing information about the sample’s surface

characteristics.

III. RESULTS

The control group was not conditioned. The samples presented

a surface with a smooth negative relief.

Fig. 1. Control sample of IPS Empress ceramic core material.

The group conditioned through sandblasting and etching

presented a different surface texture. The samples have a

needle like aspect. This aspect was produced by selective

dissolution of glass from crystalline component of ceramic

material.

Fig. 2. Sand-blasted sample and conditioned with hydrofluoric acid 9%.

Fig. 3. Sandblasted and acid conditioning 9% sample of ceramic core

material

The sandblasted samples presented an irregular surface with a

disorderly character, a negative relief with gaps. The needle

like aspect could not be identified.

Advances in Communications, Computers, Systems, Circuits and Devices

ISBN: 978-960-474-250-9 349

Fig. 4. Sandblasted sample of IPS Empress e.max ceramic core

material.

Fig. 5. AFM investigation of ceramic material sample

sandblasted conditioned.

Fig. 6. The sample’s 3D topographic map. Sand-blasted and

etched conditioned ceramic core sample.

Fig. 7. Sand-blasted and acid conditioned sample.

Advances in Communications, Computers, Systems, Circuits and Devices

ISBN: 978-960-474-250-9 350

Fig. 8 Sand-blasted and acid conditioned ceramic core sample.

IV. DISCUSSIONS AND CONCLUSIONS

Texture’s surfaces depend by the conditioning method. The

evaluation of surface texture was performed through AFM and

SEM investigation methods. Significant improvement of

micro-retention could be observed in case of sandblasted and

acid conditioned samples. The negative relief of the

sandblasted samples was not as marked as the samples

conditioned through sandblasting and etching protocole. Also,

considerable differences could be observed after investigated

the samples that were not conditioned. Investigations of first

group (non-conditioned) evidenced a weak irregular relief not

appropriate for adhesion. The third group presented the most

suitable negative relief for adhesion of composite resin

material to IPS Empress e.max ceramic core.

ACKNOWLEDGMENT

The authors want to acknoldge the suport of CNCSIS

Research Project For Young Team Cod 101/2010.

V. REFERENCES

[1] Bo-Kyoung Kim, DDS, MSD, Hanna Eun-Eyung

Bae,BDS, June-Sung Shim, DDS, PhD, Keun-Woo Lee The

influence of ceramic surface treatments on the tensile bond

strength of composite resin to all-ceramic coping materials-

The Journal of Prosthetic Dentistry , vol 94, nr. 94

[2] X. -P. Luo, N. Silikas, M. Allaf, N. H. F. Wilson and D. C.

WattsAFM and SEM study of the effects of etching on IPS-

Empress 2TM dental ceramic-Surfac Science, vol 491, Issue 3,

oct. 2001

[3] D. Sen, G. Sunmazisik, E. Poyrazoglu, B. Tuncelli, B.

Ozkal, M.L. Ovecoglu- Effects of Different Acid treatments on

Dental Ceramic Surfaces –key Engineering Materials Vols.

264-268 (2004)

[4] Haluk baris kara, A. Nilgun Ozturk, Filiz Aykent, Ozlem

Koc, Bora Ozturk- The Effect of Different Surface Treatments

on Roughnessand Bond Strength in Low Fusing Ceramic-

Lasers in Medical Science DOI: 10.1007/s10103-010-08-6-9

Advances in Communications, Computers, Systems, Circuits and Devices

ISBN: 978-960-474-250-9 351