RETENTION OF CAD/CAM CROWNS LUTED WITH RESIN CEMENTS AND RMGI by SHRUTI SUSHILKUMAR SONAVANE DR. JOHN O. BURGESS (COMMITTEE CHAIR) DR. AMJAD JAVED DR. JACK E. LEMONS DR. LANCE RAMP DR. NATHANIEL C. LAWSON A THESIS Submitted to the graduate faculty of The University of Alabama at Birmingham, in partial fulfillment of the requirements for the degree of MS in Clinical Dentistry BIRMINGHAM, ALABAMA 2015 i Copyright by Shruti Sushilkumar Sonavane 2015 RETENTION OF CAD/CAM CROWNS LUTED WITH RESIN CEMENTS AND RMGI SHRUTI SUSHILKUMAR SONAVANE MS IN CLINICAL DENTISTRY ABSTRACT Objectives: To measure retention of lithium disilicate (IPS e.max CAD, Ivoclar Vivadent) and zirconia reinforced lithium disilicate (CELTRA™ DUO, Dentsply) copings luted using resin cements and resin-modified glass ionomer cement. Methods: 110 Extracted human, non-carious mandibular 2nd premolars (n=10) were embedded in PVC cylinders with acrylic resin and placed into a lathe to produce a uniform crown preparation (22°-convergence & 3mm-height). Following the orientation groove placement (69L bur), preparations were scanned and milled using a CEREC 3D/Sirona machine to produce e.max and CELTRA™ DUO crowns. Preparations were imaged with a digital microscope (Keyence/VHX-600-20X) and the surface area of each crown was calculated. IPS e.max crowns and CELTRA™ DUO crowns were cemented using the cements as in Tables 1 & 2. Specimens were stored (distilled water/37°C/24h) and thermocycled (10,000cycles/5-50°C/30secs) before debonding in tension at crosshead speed-5mm/min (INSTRON Model/5565). The bond strength was calculated by dividing the failure load with preparation surface area. The CELTRA™ DUO and e.max data were compared separately with 1-way ANOVA and Tukey post-hoc analysis (alpha=0.05). Results: The simulated crown strength test results for e.max were: Calibra=4.89±2.35a; ExpE(TE)=3.70±2.08a,b; ExpSE=3.18±2.03a,b RelyXLP=3.11±1.99a,b; ExpE(SelfEtch)=2.74±1.23a,b; Multilink=2.66±1.72a,b; RelyXU=2.65±1.46a,b; Reiii lyXLP/HF=1.91±0.70b. For CELTRA™: Exp/S=4.73±2.45a; Exp/S/E=4.40±1.76a,b; RelyXLP/HF=3.34±1.65a,b, c; Exp=1.79±0.70b,c; and RelyXLP=0.95±0.58c. The ANOVA showed some significant differences between groups (p=0.01) where the same letter denotes similar groups. Conclusions: The Calibra material resulted in significantly higher retention with the than RelyXLP/HF for the coping fabricated from e.max. The experimental resin cement with silane when compared to Exp and RelyXLP resulted in significantly higher test retention strength for the CELTRA™ DUO. KEYWORDS: Adhesion, CAD/CAM, Biomaterials, Cements, Ceramics. iv DEDICATION This thesis is dedicated to my husband, Sushil and my son, Dhruv for their continuous support throughout my masters program. This thesis is also dedicated to my parents for teaching me the value of knowledge, persistence and hard work, without which I would have never been where I am today. v ACKNOWLEDGMENTS This project would not have been possible without the support of many people. I would like to thank my mentor, Dr. John Burgess, for his outstanding guidance, patience, support and trust that he put in me throughout my masters. I would also like to thank Dr. Lemons for making me think about the details and made me realize that “Devil lies in the details” I would like to thank Dr. Nathaniel Lawson for his smart ideas. I really appreciate him for being good at everything he does. I thank Dr. Lance C. Ramp for providing his statistical expertise and his timely Responses. I thank Dr. Amjad Javed, for their invaluable student friendly advices over the period of my masters. I would like to thank Mr. Preston Beck for his patience and his readiness to help everyone around him. His expertise in engineering has saved my day many times. A special thanks to Ms. Rhonda Scott, for helping in all the paper work since my admission process till date. vi I would like to thank Kanchan Sawlani, Chinkai Lin, Latara Rogers, Rashmi Radhakrishanan, Ritika Bansal and Nan Xiang for wonderful company. I would like to thank my husband, Sushil for constant encouragement, patience and support he has shown since we met. Special thanks to my son, Dhruv for willingly or unwillingly supporting me. Special thanks to my family and my in-laws for their blessings and having faith in me that I can balance family life with studies. vii TABLE OF CONTENTS Page Abstract...............................................................................................................................iii Dedication............................................................................................................................ v Acknowledgments .............................................................................................................. vi List of Tables ....................................................................................................................... x List of Figures..................................................................................................................... xi List of Abbreviations ........................................................................................................xiii INTRODUCTION ............................................................................................................... 1 Ceramics .............................................................................................................................. 3 Luting Agent ........................................................................................................................ 3 Various methods of bond strength testing ........................................................................... 4 Previous Crown-Tensile testing .......................................................................................... 5 OBJECTIVES AND HYPOTHESIS .................................................................................. 7 MATERIALS AND METHODS ........................................................................................ 8 Teeth Selection .................................................................................................................. 15 Teeth Mounting ................................................................................................................. 15 Standardized Tooth Preparation ........................................................................................ 18 Total Bonding Surface area Calculation............................................................................ 19 viii Designing, Milling and Crystallization of Copings ........................................................... 21 Cementation of Copings .................................................................................................... 25 Storage, Thermocycle and Tensile Testing ....................................................................... 30 Statistical Analysis ............................................................................................................ 33 RESULTS .......................................................................................................................... 34 DISCUSSION.................................................................................................................... 38 LIMITATIONS ................................................................................................................. 44 CONCLUSIONS ............................................................................................................... 45 FUTURE DIRECTIONS ................................................................................................... 46 REFERENCES .................................................................................................................. 47 APPENDICES A. IRB Approval .......................................................................................................... 51 ix LIST OF TABLES Table Page 1. Materials 8 2. Groups for e.max 9 3. Groups for Celtra 12 4. Parameters for CAD/CAM Design and Milling Crystallization 22 5. Directions for Use of Resin Cement 25 6. Mode of failure 31 7. e.max Retention in MPa 34 8. Celtra Retention in MPa 35 9. SEM of Celtra 43 x LIST OF FIGURES Figure Page 1. Flattening the cusps on model trimmer 15 2. Slow-speed handpiece with abrasive disc 16 3. Notching the roots with abrasive disc 16 4. Mandibular 1st Premolar with flattened and notched roots 16 5. Surveyor for mounting teeth 17 6. Centering the tooth using caliper 17 7. Centered tooth embedded in auto-polymerizing clear acrylic resin 17 8. Tooth preparation on lathe 18 9. Keyence- to calculate the total bonding surface area of the prepared tooth 19 10. Measurement of radii ‘r’ of top circle & ‘R’ of base circle 19 11. Measurement of areas of irregular shaped whole base 20 12. Truncated Cone 21 13. Spraying the prepared tooth with titanium dioxide powder for scanning 22 14. Cerec 3 23 15. e.max block inserted in Cerec 3 23 16. Inserting object fix putty in milled coping to stabilize the coping on the firing stand 23 17. Programmat CS 24 18. Firing e.max copings 24 19. Etching with 5% HF 28 20. Application of bonding agent 29 xi 21. Silane application 29 22. Insertion of mixed cement 29 23. Cemented specimen under load of 2.5Kgs 30 24. Fixture for holding the specimen for testing 31 25. Specimen placed in fixture wrapped in rubber dam sheet 32 26. Specimen during tensile testing in Instron 32 27. e.max Retention 34 28. Celtra Retention 35 29. Failure Mode (%) for e.max 36 30. Failure Mode (%) for Celtra 37 31. Fractured Celtra crown during testing 42 xii LIST OF ABBREVIATIONS CAD/CAM Computer Assisted Designing/ Computer Assisted Machining Celtra Celtra™ Duo e.max IPS e.max (CAD) HF Hydrofluoric acid RMGI Resin Modified Glass Ionomer Cement ZLS Zirconia Reinforced Lithium Silicate xiii INTRODUCTION Recent advancements in dentistry have been driven by a demand for esthetic and natural appearing restorations. Improvements in the formulation and fabrication of dental ceramics have resulted in escalated applications of these esthetic materials.1, 2 During the same time, demand for metal-ceramic restorations has dropped significantly, due to esthetic limitations and reactions or sensitivity to various metals.3-5These drawbacks, along with the high material and labor costs associated with metal substrate fabrication (particularly noble metals), have prompted the development of new ceramic systems with a high strength, precision fit and superior esthetic and optical properties not found for metalceramics systems.6-8 One of the most prolific dental ceramics is IPS e.max CAD, a lithium disilicate material that exhibits superior esthetics and durability, combined with clinically satisfactory physical properties. When fabricated to full-contour, the monolithic structure is one of the most robust ceramic systems tested to-date.7 The opalescence, translucency and light diffusion properties of IPS e.max were all designed to replicate natural tooth structure for beauty and undetectable restorations. Massive casting on a continuous manufacturing process (based on glass technology) is used to produce the blocks. This new technology uses optimized processing parameters, which prevent the formation of defects (pores, 1 accumulation of pigments, etc.) in the bulk of the ingot.9 Partial crystallization ensures that the blocks can be processed in a crystalline intermediate phase, which enables fast machining with CAD/CAM systems (blue, translucent state).10 The partial crystallization process leads to a formation of lithium metasilicate crystals Li2 SiO3, which are responsible for the material's processing properties, relatively high strength and edge stability. Following the milling procedure, the restorations are tempered and thus reach the fully crystallized state. In the course of this process, lithium disilicate crystals (Li 2Si2O5) are formed, which impart the ceramic restoration with the desired high strength9. The crystallization process of IPS e.max CAD, however, requires about 21-30 minutes. Due to a demand for reduced chair-side time without compromising esthetics, Caulk Dentsply patented a zirconia reinforced lithium silicate (ZLS)-based ceramic (CELTRA™ Duo). Unlike IPS e.max CAD, this material possesses sufficient strength to withstand intra-oral forces and acceptable esthetics without heat treatment. Ceramic restorations also benefit from technologies that automate aspects of their fabrication11. In other words, these materials are fabricated by machines rather than relying on the hand-layered fabrication method used for dental porcelain. Automation allows less reliance on the skill of the individual ceramist as well as greater homogeneity and lower probability of defects within the material itself.12 In addition, ceramic restorations demonstrate optical properties superior to metal-ceramic restorations.13 Ceramic materials are also the major type of material used with in-office digital dentistry. The evolution of digital technology and computer-aided 2 design/computer-aided manufacture (CAD/CAM) systems now offer the opportunity to avoid traditional, analog impressions, including the time, expense, and handling limitations associated with them.14 Intraoral scanners have the potential to offer excellent accuracy with a more comfortable experience for the patient and more efficient workflow for the office.15 Ceramics In dentistry, ceramics are widely used due to their ability to imitate the optical characteristics of enamel and dentin and their biocompatibility and chemical durability.16 There are three main types of dental ceramics: (1) predominantly glassy materials, (2) particlefilled glasses, and (3) polycrystalline ceramics.16 Highly esthetic dental ceramics are predominantly glassy, and higher strength substructure ceramics are generally crystalline. Hybrid combinations have also been developed. The history of development of substructure ceramics involves an increase in crystalline content to fully polycrystalline. IPS e.max CAD is a type of particle-filled glass, while CELTRA™ Duo is a hybrid zirconiareinforced lithium silicate. Luting Agents The luting agents used for indirect restorations mainly have to fulfill three requirements: (1) to fill the space between the indirect material and the prepared tooth; (2) to keep the restoration in place (retention) and prevent dislodging; and (3) to provide adequate aesthetical conditions for the indirect restoration.17 Bonding of ceramic to dental tissue is 3 based on the adhesion of luting cement to the ceramic substrate, together with the adhesion of luting cement to enamel and/or dentin. Adhesive cementation is recommended for ceramic restorations 18, 19 particularly for over-tapered or short preparations. It has been reported that a long-term durable bond to the ceramics is imperative for a long-term successful restoration.20, 21 For bonding to silica-based ceramics, hydrofluoric acid has been used to etch the restoration and silane applied to serve as a chemical link between the ceramic and the resin cement.22, 23 Methods for bonding to zirconia, on the other hand, include the use of phosphate monomer-containing (MDP) composite resins, or silica coating and silane application24. Inokoshi et al 25 recommended techniques which combine mechanical and chemical surface pre-treatments for zirconia. The introduction of Celtra Duo presented a unique bonding challenge. An effective method of bonding to novel zirconia reinforced- lithium silicate needs to be established. Various Methods Of Bond Strength Testing Bond strength testing methods used in dentistry can be broadly classified as shear and micro-tensile testing. A disadvantage reported for shear and micro-tensile bond strength tests is that they do not take into account the complex geometry of a tooth preparation as the luting agent is only bonded to flat surfaces. The ratio of bonded to non-bonded surfaces (Configuration factor or C-factor)26 is much higher in crowns luted onto abutments or dies than in composite or ceramic cylinders luted onto flat surfaces. A laboratory study has shown that the C-factor influences the bond strength of the adhesive significantly27. 4 This might explain why bond strength data of 1–10 MPa are found in crown retention strength investigations compared to 20–40 MPa in shear bond strength tests.28 Previous Crown-Tensile testing Influence of tooth preparation characteristics Retention of the single-unit crowns is influenced by the taper angle-–the angle of convergence between the opposing axial walls. The retention of bonded crowns has been shown to depend on the taper angle: the lower the taper angle, the higher the retention29-33. The maximum retention is obtained between 60 and 120 taper29. In practice, ideal axial wall convergence may not be routinely obtained. Studies have reported mean taper angles ranging from 30 to 260 34. Influence of type of cement Several factors have been shown to influence the retention of metal-ceramic restorations, including the preparation convergence and height, and the type of cement. A recent study confirmed that neither the surface conditioning type, nor the taper angle affected the retentive strength of IPS e.max Press single-unit crowns when bonded adhesively35. Metalceramic crowns cemented with resin cements, showed higher retention than conventional cements.3, 36-43 Dental adhesives and cements are a complex mixture of ingredients designed to provide retention for a variety of materials to tooth structure. These materials must interact with enamel, dentin, and the restorative material. The development of 4META system has led to a wide variety of adhesives and cements over the past dec- 5 ades—all of which have consisted of the same essential ingredients and have provided outstanding consistency and predictability of bonding to dentin44, 45 6 OBJECTIVES AND HYPOTHESIS The objectives of this dissertation are 1. To measure retention of lithium disilicate (IPS e.max CAD, Ivoclar Vivadent) copings luted using resin cements and resin-modified glass ionomer cement with various surface treatments. 2. To measure retention of zirconia reinforced lithium disilicate (CELTRA™ DUO, Dentsply) copings luted using resin cements and resin-modified glass ionomer cement with various surface treatments. The null hypotheses of the study are: 1. Retention of lithium disilicate (IPS e.max CAD, Ivoclar Vivadent) copings is not influenced by the type of cement and various surface treatments. 2. Retention of copings of zirconia reinforced lithium disilicate (CELTRA™ DUO, Dentsply) is not influenced by the type of cement and various surface treatments. 7 MATERIALS AND METHODS The materials, groups and methods for this study are summarized in the following Tables and associated descriptions. Table 1: Materials Material Manufacturer e.max Ivoclar Celtra Duo Caulk Dentsply Adhesive resin cement experimental Caulk Dentsply 130916 03/2014 Prime & Bond Elect Caulk Dentsply 130811 08/2016 Calibra Resin cement Caulk Dentsply 130417 10/2014 Caulk Dentsply 130603 06/2015 Caulk Dentsply Adhesive -121031 Activator – 130805 08/2014 08/2015 Scotchbond Universal 3M ESPE 521198 06/2015 RelyX Ultimate 3M ESPE 521894 09/2014 Monobond Plus Ivoclar 626221 04/2015 Multilink Automix Ivoclar Primer – S02167 Adhesive – S06441 07/2014 08/2014 RelyX Luting Plus Ivoclar N484102 01/2015 Calibra Silane coupling agent XP Bond/Self-cure Activator Lot No 8 S37918, S33811, S53671 TWA#61, TWA#58, 18016483 Expiration 2028 Table 2: Groups for e.max Group Intaglio Surface Etch Multilink Silane 5%HF Tooth Treatment Bond Monobond Plus Multilink Primer A/B (Self-Etch) RelyXU 5%HF Scotch Bond Universal Scotch Bond Universal (Self-Etch) Calibra 5%HF Silane XP Bond/ Self Cure acti- XP Bond/Self Cure acti- vator vator (Total-Etch) ExpSE 5%HF ExpE 5%HF P&B Elect (Self-Etch) ExpE (TE) 5%HF P&B Elect (Total-Etch) RelyXLP/Etch 5%HF RelyXLP Multilink: Silane P&B Elect (Self-Etch) a. Tooth preparation. Apply Multilink Primer A/B for 20 seconds. Air dry. b. Etch e.max coping with 5% HF for 20 seconds, rinse and ultrasonically clean. Air dry. Apply Monobond Plus for 60 seconds and air dry. Deliver Multilink Automix to e.max coping. Allow to self-cure under seating force of 2.5Kgs. Debond after thermocycling for 10,000 times, between 5° C and 50°C with 30 seconds dwell time. 9 RelyXU: a. Tooth preparation. Apply Scotchbond Universal, agitate for 20 seconds. Air dry. b. Etch e. max coping with 5% HF for 20 seconds, rinse and ultrasonically clean. Air dry. Apply Scotchbond Universal for 20 seconds agitate and air dry. Deliver RelyX Ultimate to e. max coping. Allow to self-cure under seating force of 2.5Kgs. Debond after thermocycling for 10000 cycles (between 5° C and 50° C with 30 seconds dwell time). Calibra: a. Tooth preparation. Etch with Caulk Etching Gel for 15 seconds. Rinse well and blot dry. Apply XP Bond/Self-cure Activator (1:1) for 20 seconds. Air dry. b. Etch e.max coping with 5% HF for 20 seconds, rinse and ultrasonically clean. Air dry. Apply Caulk Silane coupling agent for 60 seconds. Air dry. Apply XP Bond/Self-cure Activator (1:1) for 20 seconds. Air dry. Insert mixed Calibra resin cement into e.max coping. Allow to self-cure under seating force of 2.5Kgs. Debond after thermocycling for 10,000 cycles (between 5° C and 50°C with a 30 seconds dwell time) ExpSE: a. Tooth prep. Apply Prime & Bond Elect and agitate for 20 seconds. Air dry for 5 seconds. Light cure for 20 seconds with 3M ESPE Elipar S10 with output of 878.5mW/cm2. 10 b. Etch e.max coping with 5% HF for 20 seconds, rinse and ultrasonically clean in distilled water. Air dry. Apply Caulk Silane coupling agent for 60 seconds. Air dry. Insert mixed Experimental Adhesive Resin Cement R1096 to e.max coping. Allow to self-cure under seating force of 2.5Kgs. Debond after thermocycling for 10000 times (between 5° C and 50° C with 30 seconds dwell time) ExpE: a. Tooth Preparation: Apply Prim & Bond Elect and agitate for 20 seconds, air dry for 5 seconds and light cure for 20 seconds with 3M ESPE Elipar S10 with output of 878.5mW/cm2. b. Etch e.max coping with 5% HF for 20 seconds, rinse and ultrasonically clean in distilled water. Air dry. Deliver Experimental Adhesive Resin Cement R1096 to e.max coping. Allow to self-cure under seating force of 2.5Kgs. Debond after thermocycling for 10000 times (between 5° C and 50° C with 30 seconds dwell time) ExpE(TE) a. Tooth preparation. Etch with Caulk Etching Gel for 15 seconds with agitation. Rinse well and blot dry. Apply Prime & Bond Elect; agitate for 20 seconds and air dry for 5 seconds. Light cure 20 seconds with 3M ESPE Elipar S10 with output of 878.5mW/cm2. b. Etch e. max coping with 5% HF for 20 seconds, rinse and ultrasonically clean in distilled water. Air dry, insert mixed (Experimental Adhesive Resin Cement R1096) to e. Max coping. Allow the cement to self-cure under a seating force of 2.5Kgs and debond after thermo- 11 cycling for 10,000 cycles (between 5° C and 50° C with 30 seconds dwell time) RelyXLP/Etch: a. Tooth preparation. Dry the tooth surface while keeping it moist. b. Etch e.max coping with 5% HF for 20 seconds, rinse and ultrasonically clean in distilled water for 10 mins. Air dry. Deliver mixed RelyX luting plus to e.max coping. Allow to self-cure under seating force of 2.5Kgs. Debond after thermocycling for 10000 times (between 5° C and 50° C with 30 seconds dwell time) RelyXLP: a. Tooth preparation. Dry the tooth surface while keeping it moist. b. Air dry e.max copings. Deliver mixed RelyX luting plus to e.max coping. Allow to self-cure under seating force of 2.5Kgs. Debond after thermocycling for 10000 times (between 5° C and 50° C with 30 seconds dwell time) Table 3: Groups for Celtra Group Intaglio Surface Etch Silane Tooth Treatment Bond Exp 5%HF ExpS 5%HF Silane ExpSE 5%HF Silane P&B Elect P&B Elect (Self-Etch) RelyXLP/Etch 5%HF RelyXLP P&B Elect (Self-Etch) P&B Elect (Self-Etch) 12 Exp: a. Tooth prep. Apply Prime & Bond Elect and agitate for 20 seconds. Air dry for 5 seconds. Light cure for 20 seconds with 3M ESPE Elipar S10 with output of 878.5mW/cm2. b. Etch Celtra coping with 5% HF for 20 seconds, rinse well for 20 seconds and ultrasonically clean for 10 minutes. Air dry for 10 seconds. Insert mixed Experimental Adhesive Resin Cement R1096 to Celtra coping. Allow to self-cure under seating force of 2.5kgs. Debond after thermocycling between 5°C and 50°C with dwell time of 30 seconds for 10000 cycles. ExpS: a. Tooth prep. Apply Prime & Bond Elect and agitate for 20 seconds. Air dry for 5 seconds. Light cure for 20 seconds with 3M ESPE Elipar S10 with output of 878.5mW/cm2. b. Etch Celtra coping with 5% HF for 20 seconds, rinse well for 20 seconds and ultrasonically clean for 10 minutes in distilled water. Air dry for 10 seconds. Apply Caulk Silane coupling agent for 60 seconds and air dry for 5seconds. Insert mixed Experimental Adhesive Resin Cement R1096 to Celtra coping. Allow to self-cure under seating force of 2.5 Kgs. Debond after thermocycling for 10000 times (between 5° C and 50° C with 30 seconds dwell time) ExpSE: a. Tooth prep. Apply Prime & Bond Elect and agitate for 20 seconds. Air dry for 5 seconds. Light cure for 20 seconds with 3M ESPE Elipar S10 with output of 878.5mW/cm2. 13 b. Etch Celtra coping with 5% HF for 20 seconds, rinse well for 20 seconds and ultrasonically clean for 10 minutes. Air dry for 10 seconds. Apply Caulk Silane coupling agent for 60 seconds. Air dry for 5seconds. Apply Prime & Bond Elect and agitate for 20 seconds. Air dry for 10 seconds. Light cure for 20 seconds with 3M ESPE Elipar S10 with output of 878.5mW/cm2. Deliver Experimental Adhesive Resin Cement R1096 to Celtra coping. Allow to self-cure under seating force of 2.5 Kgs. Debond after thermocycling for 10000 times (between 5° C and 50° C with 30 seconds dwell time) RelyXLP/Etch: a. Tooth preparation. Dry the tooth surface while keeping it moist. b. Etch Celtra coping with 5% HF for 20 seconds, rinse and ultrasonically clean in distilled water for 10 mins. Air dry. Deliver mixed RelyX luting plus to e.max coping. Allow to self-cure under seating force of 2.5Kgs. Debond after thermocycling for 10000 times (between 5° C and 50° C with 30 seconds dwell time) RelyXLP: a. Tooth preparation. Dry the tooth surface while keeping it moist. b. Air dry Celtra coping. Deliver mixed RelyX luting plus to e.max coping. Allow to self-cure under seating force of 2.5Kgs. Debond after thermocycling for 10000 times (between 5° C and 50° C with 30 seconds dwell time) 14 Teeth Selection Mandibular second premolar teeth, freshly extracted for orthodontic reasons, were collected from the Oral and Maxillofacial Surgery Department of the UAB School of Dentistry. One hundred and ten (110) mature teeth without caries, non-carious cervical lesions and cracks were selected. Teeth were examined for cracks under 2.5X loupes. Teeth Mounting The roots of the selected teeth were notched with a rotating disc on a slow-speed handpiece and the occlusal surfaces were ground flat on the model trimmer. For mounting, the teeth were centered in Teflon cylinders with the help of a surveyor and digital caliper and then embedded in clear auto-polymerizing acrylic resin (Yates Motloid, USA). The methods are shown in Figures 1-8. Figure 1: Flattening the cusps on model trimmer 15 Figure 2: Slow-speed handpiece with abrasive disc Figure 3: Notching the roots with abrasive disc Figure 4: Mandibular 1st Premolar with flattened and notched roots 16 Figure 5: Surveyor for mounting teeth Figure 6: Centering the tooth using caliper Figure 7: Centered tooth embedded in auto-polymerizing clear acrylic resin 17 Standardized Tooth Preparation After complete curing of the acrylic resin, the sample was fixed into a lathe for precise uniform reduction with diamond cutting tools to produce a uniform coping preparation with exact taper, diameter and fit. The teeth were prepared to uniform dimensions (22° total taper using 846.11.025 HP medium flat end taper diamond bur (Brasseler, USA), 3 mm preparation height using X 889 diamond bur). An orientation groove was placed into the occlusal surface of preparation by hand using a 69 L bur and high-speed handpiece. Teeth were kept moist prior to bonding. Figure 8: Tooth preparation on lathe 18 Total Bonding Surface Area Calculation The bonding surface area of the prepared surface was calculated under 20X in Keyence as shown in Figures 9-12. Figure 9: Keyence- to calculate the total bonding surface area of the prepared tooth Figure 10: Measurement of radii ‘r’ of top circle & ‘R’ of base circle 19 Figure 11: Measurement of areas of irregular shaped whole base In order to calculate the bonding surface area, the lateral walls, occlusal table, and margin width were all measured separately. The bonding area was calculated using the formula: Bonding area = lateral surface area of truncate cone + area of top circle of truncated cone + (Difference between area of base and bottom circle of truncated cone) Each of these areas were calculated as described below: 1. Lateral surface area of the truncated cone is calculated by formula= π(R + r) S sq. units 2. The area of top circle of truncated cone was measured as πr2. This area represents the occlusal table of the preparation. 20 3. The base of the preparation was measured with a function on the Keyance microscope. The bottom circle of the truncated cone was measured as πR2. The difference between these values represents the width of the preparation margin. Figure 12: Truncated Cone Where r=radius (of top circle) and R (of base circle), h=height and s=slant height and π= 3.14. This area represents the lateral wall of the preparation. An excel sheet was prepared for the calculations. Designing, Milling and Crystallization of Copings Seventy (70) e.max and forty (40) Celtra copings were milled using the Cerec 3 (Sirona) CAD-CAM machine as shown in Figures 15-18. The parameters for CAD/CAM design and milling are given in Table 4. 21 Table 4: Parameters for CAD/CAM Design And Milling Proximal contacts strength 75µm Occlusal contacts strength 25 µm Occlusal offset 0 µm Margin thickness 0 µm Minimal thickness (occlusal) 1000 µm Minimal thickness (radial 700 µm Minimal thickness (Veneer) 500 µm Adhesive gap 20 µm Spacer 0 µm Scan step width 3 µm Figure 13: Spraying the prepared tooth with titanium dioxide powder For scanning 22 Figure 14: Cerec 3 Figure 15: e.max block inserted in Cerec 3 The e.max copings were crystallized using Programmat CS (Ivoclar, Vivadent, Schaan), with the following parameters. Before crystallization the e.max copings were filled with Object Fix putty (Ivoclar) for stabilization on the stand during crystallization. The parameters for program P1 of Programmat CS were used. 23 Figure 16: Inserting object fix putty in milled coping to stabilize the coping on the firing stand Figure 17: Programmat CS Figure 18: Firing e.max copings 24 Cementation of Copings The e.max and Celtra copings were then individually tried on the tooth preparations and an explorer was used to ensure there were no marginal defects. The copings were cemented with the appropriate primers and cements as was listed inTable1. The cements were mixed following the manufacturers’ directions listed in Table 6 for the groups listed in Tables 2 and 3. A 2.5Kgs weight placed on the cemented coping until the cement set. Table 5: Directions for Use of Resin Cement 3M ESPE RelyX™ Ulti- Clean the interior surface of the coping with 5% hydroflumate oric acid for 20secs, rinse thoroughly with water for 15secs and air dry. Apply Scotchbond Universal Adhesive; allow it to react for 20secs, air dry for 5secs. Attach the mixing tip, squeeze out and discard a peppercorn-size quantity of RelyX Ultimate until evenly mixed paste in a homogeneous color flows out of the tip. Wet the entire internal surface of restoration evenly with RelyX Ultimate. Seat the restoration and stabilize long enough for the cement to fully set. Remove excess. Ivoclar Vivadent tilink® Automix Mul- Etch the interior surface of coping with 5% hydrofluoric acid for 20 seconds. Thoroughly rinse the restoration with water spray and dry with oil-free air. Apply Monobond-S to the surfaces with a microbrush and let react for 60 se- 25 conds. Disperse it with a strong stream of air. Mix the two Multilink Primer liquids A and B in a 1:1 mixing ratio. The mixed Primer A/B is solely self-curing and does not need to be protected against light, but it must be applied within 10 minutes. Apply the mixed Multilink Primer A/B to the prepared tooth surface using a microbrush – starting from the enamel and scrubbing with slight pressure for 15 seconds. A reaction time of 30 seconds is recommended on the enamel and 15 seconds on the dentin. The applied primer is subsequently dried with water- and oil-free air. As the Primer is solely self-curing, no light curing is necessary. Place a new automix tip on the syringe. Dispense Multilink from the automix syringe and apply Multilink Automix directly to the inner surface of the restoration. Seat the restoration in place and fix/hold. Remove the excess material. Experimental adhesive Clean the internal surface of the restoration with Caulk® resin cement R1096 34% Tooth Conditioner Gel (34% phosphoric acid) for 30 seconds, rinse thoroughly with water for 20 seconds and air-dry. Directly apply the silane to the clean internal surface of the coping and air-dry. Remove syringe cap. Dispense and discard a small amount of material from the dual-barreled syringe. Be sure material is flowing freely 26 from both ports. Holding syringe vertically, carefully wipe away excess so base and catalyst do not cross contaminate and cause obstruction of the ports. Save syringe cap for replacement following use. Install a mixing tip on the cartridge by lining up the v-shaped notch on the outside of the mixing tip with the V-shape notch on the syringe flange. Turn colored mixing tip cap 90 degrees in a clockwise direction to lock in place on syringe. Gently depress syringe plungers to begin the flow of material. DO NOT USE EXCESSIVE FORCE. Dispense a small amount through the mixing tip onto a mixing pad and discard. Apply a uniform layer of cement on the entire internal surface of the restoration directly from the mixing tip. At room temperature, R1096 Esthetic Resin Cement, in either viscosity, offers a minimum work time of 2 minutes. A gentle rocking or vibratory motion was used to insure optimal seating. Protect restoration from contamination and movement until the final set of the cement (till completion of light curing). Remove excess cement. Dentsply Caulk Calibra® Microetching (sandblasting) with 50µ alumina (or hyEsthetic Resin Cement drofluoric acid chemical etching of the internal surfaces of a ceramic restoration) is recommended. Clean the internal surface of the restoration with Caulk® 34% Tooth Condi- 27 tioner Gel (34% phosphoric acid). Apply for 30 seconds, rinse thoroughly with water for 20 seconds and air-dry. Clean the prepared tooth surface with water and apply adhesive, light cure. Attach supplied needle tip to end of the Calibra® Silane Coupler syringe. Silane agent should express easily, one drop at a time. Apply the silane to the etched, clean internal surface of the restoration and airdry. Dispense Calibra® Esthetic Resin Cement base paste from the syringe onto a clean mixing pad. Dispense an equal amount of the desired viscosity of catalyst paste; mix the cement for 20-30 seconds. Apply a uniform layer of cement on the entire internal surface of the restoration. Seat the restoration with gradual pressure. Remove excess cement. The procedures for cementation are shown in Figures 19-23. Figure 19: Etching with 5% HF 28 Figure 20: Application of bonding agent Figure 21: Silane application Figure 22: Insertion of mixed cement 29 Figure 23: Cemented specimen under load of 2.5Kgs Storage, Thermocycle And Tensile Testing Excess cement was carefully removed and the copings stored in a moist zip lock bag for 24 hours at 37°C, thermocycled for 10,000 cycles between 5-500C with dwell time of 30 seconds before debonding. The specimens were placed in a special fixture (INSTRON Model no: 5565) and loaded in tension at a crosshead speed of 5 mm/min until debonding. The force (N) of debonding was recorded. The retention force was calculated in MPa by the formula: Retention (MPa)= Debonding Force (N) Total Bonding Surface area of Preparation (mm2) Note—Pascal= N/m2 Examination of the failure site was made optically with Keyance at 100 X and categorized according to 41Table 7. The test apparatus is shown in Figures 24-26. 30 Table 6: Mode of failure Category Description Category 1 Cement mainly on prepared tooth (over 75%) Category 2 Cement on both crown and tooth (between 25 and 75%) Category 3 Cement mainly on crown (over 75%) Category 4 Fracture of tooth without crown separation Category 5 Fracture of Crown Figure 24: Fixture for holding the specimen for testing 31 Figure 25:Specimen placed in fixture wrapped in rubber dam sheet Figure 26: Specimen during tensile testing in Instron 32 Statistical Analysis A Levine’s test of homogeneity was used to determine that all groups demonstrated a normal distribution of variance. A 1-way ANOVA performed to compare differences between bonding procedures for e.max was significant. A Tukey HSD post-hoc analysis was used to compare groups. A separate 1-way ANOVA performed to compare differences between bonding procedures for Celtra was also significant. A Tukey HSD posthoc analysis was used to compare groups. 33 RESULTS The test results for the simulated crown removal tests are summarized in Tables 8 and 9 and Figures 27 and 28. The mean values of crown retention ranged from 0.95 (RelyXLP with Celtra) to 4.89 MPa (Calibra with e.max) 10000 thermal cycles (5°C and 50°C). The IPS e.max when cemented with Calibra showed the highest bond strength, however it was not significantly different from other groups except for RelyX Luting without etchant. CELTRA™ Duo showed highest bond strength when used with Experimental Resin cement with silane, however it was not significantly different from other groups except for RelyX Luting with etchant or when using Experimental resin cement alone. Table 7: e.max Retention in MPa 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. Av SD Multilink RelyXU Calibra ExpSE ExpE ExpE(TE) RelyXLP/ Etch RelyXLP 0.98 2.30 1.26 4.78 4.34 5.04 0.50 4.49 2.17 0.79 2.66 1.72 4.28 2.57 4.42 3.03 0.64 3.00 0.80 1.34 4.85 1.60 2.65 1.46 7.88 6.59 3.94 4.60 7.08 2.11 8.57 2.95 3.59 1.59 4.89 2.35 5.08 7.49 1.78 1.80 4.54 0.83 3.63 4.02 1.27 1.38 3.18 2.03 4.62 2.05 2.10 4.49 4.26 2.84 1.20 2.03 1.21 2.63 2.74 1.23 1.49 1.86 3.89 4.18 7.05 6.80 5.08 4.01 0.82 1.84 3.70 2.08 2.75 0.98 1.72 1.65 2.46 1.86 5.49 4.83 2.63 0.76 1.91 0.70 3.11 1.99 34 e.max Retention 8.00 7.00 6.00 4.89 MPa 5.00 3.70 4.00 3.00 3.18 2.66 3.11 2.74 2.65 1.91 2.00 1.00 0.00 Figure 27: e.max Retention Table 8: Celtra Retention in MPa 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. Av SD Exp ExpS ExpSE RelyXLP/Etch RelyXLP 0.99 1.07 1.71 0.91 2.31 1.54 1.92 3.21 2.56 1.66 1.79 0.70 3.87 6.67 1.38 8.64 5.77 1.40 2.00 4.26 5.65 7.65 4.73 2.45 4.93 7.21 5.62 2.25 6.77 2.62 2.02 3.29 3.98 5.35 4.40 1.76 3.77 3.79 1.08 5.52 2.53 1.21 0.82 1.48 1.24 0.00 3.34 1.65 0.95 0.58 35 Celtra Retention 8.00 7.00 6.00 4.73 MPa 5.00 4.40 4.00 3.00 2.00 3.34 1.79 0.95 1.00 0.00 Exp ExpS ExpSE RelyXLP/Etch RelyXLP Figure 28: Celtra Retention 100% 90% 80% 70% 60% 50% 40% 30% 20% 10% 0% Multilink 1-on tooth RelyXU 2-Mixed Calibra ExpSE 3-on Coping ExpE ExpE(TE) RelyXLP/Etch 4-Tooth Fracture Figure 30: Failure Mode (%) for e.max 36 RElyXLP 5-Coping Fracture 100% 90% 80% 70% 60% 50% 40% 30% 20% 10% 0% Exp 1-on tooth ExpS 2-Mixed ExpSE 3-on Coping RelyXLP/Etch 4-Tooth Fracture Figure 31: Failure Mode (%) for Celtra 37 RElyXLP 5-Coping Fracture DISCUSSION Crown retention is known to be influenced by a number of different parameters: the abutment size and surface roughness46, 47, the total convergence angle of the walls of the abutment33, and the cements33 used for luting contribute significantly to the performance of the restorations.47 As new cements and ceramic materials develop, it is important to measure and compare the crown retention produced by these cements compared to other more clinically established materials. The most common laboratory tests which assess the adhesive properties of a luting agent are shear, tensile, microtensile or push-out 28 bond strength tests. The advantages of bond strength tests are reproducibility and ease of conducting the test. The drawbacks is that the bond strength testing does not reflect the clinical situation where the thixotropic cement applied under pressure during crown insertion exhibits flow and lower viscosity permitting it to bond differently than a passive bonding test to a flat prepared tooth. Therefore, crown tensile testing procedures were developed to more closely simulate the clinical procedure.28 Dental luting cements play a vital role in the success of indirect restorations. The primary function of the luting cement is to fill the space between the prepared tooth and indirect restoration, in addition to mechanically or chemically bonding the restoration to the preparation to prevent dislodgement during function. A final property is to enhance the color 38 of the esthetic all ceramic restoration 17, 48, 49. Resin cements have gained popularity in the dental market during recent years due to high compressive and tensile strengths, low solubility and favorable esthetic qualities. In addition, in vitro and in vivo studies suggest that resin bonding helps diffuse stress and limit crack propagation on the internal aspect of porcelain restorations20. However, they are expensive and have the disadvantages of being technique sensitive, easily contaminated during multiple step application procedures and difficult and time consuming during clean-up50. They can be categorized based on the bonding process as: (a) Total etch adhesive resin cements (b) Self-etch adhesive resin cements and (c) Self-adhesive resin cements. Restoration retention has been shown to depend on many factors. Macromechanical retention is mainly determined by the configuration of the crown preparation: (1) convergence angle; (2) surface area; (3) apical-coronal height; (4) and auxiliary retention devices such as pinhole, grooves or notches17, 32. In addition, some properties of the luting agents which may prevent restoration dislodgement are: higher flexural strength51; lower shrinkage, increased water uptake and cement expansion can improve retention52-54 In the present study, the influence of different surface treatments and luting agents were studied. The mean values of crown retention ranged from 0.95 MPa (RelyXLP with Celtra) to 4.89 MPa (Calibra with e.max) after 10,000 thermal cycles (5°C and 50°C). 39 The groups can be arranged in descending order as below For e.max: Calibraa=4.89±2.35>ExpE(TE)=3.70±2.08>ExpSE=3.18±2.03>RelyXLP=3.11±1.99 >ExpE=2.74±1.23>Multilink=2.66±1.72>RelyXU=2.65±1.46>RelyXLP/Etchb= 1.91±0.70. For Celtra: ExpSa=4.73±2.45>ExpSE=4.40±1.76>RelyXLP/Etch=3.34±1.65> c Expb, =1.79±0.70>RelyXLPc=0.95±0.58. The retention values in this study are in agreement with those of other studies on cement luting and zirconia ceramic.33, 55 Retention strength in the present study had lower values than the previous studies.43, 56-58 The use of a different ceramic, the treatment of the ceramic crown intaglio surface, the aging conditions, the degree of convergence, the surface area measurement, and the type of cement were all different from previous studies. Palacios 43 et al and Ernst 56, 57 et al used a lower degree of total occlusal convergence (5 and 10 degrees) than the 22 degrees in the present study. As the pull-off test of crowns is supposed to be a clinically relevant test, clinically relevant preparation parameters should be chosen. A convergence angle that reflects the clinical situation should be chosen. Studies, which evaluated the convergence angle of casts produced of clinical cases, concluded that the mean angle was about 20◦59. 40 The lower angle of draw may increase the retention resistance, regardless of the type of cement.60 The current study, with a greater angle of prepared total occlusal convergence, may better assess the contribution of the cement and surface treatment to the retention of crowns.41, 42 Also, zirconia was used in the previous studies, while in present study lithium disilicate and zirconia reinforced lithium silicate were used; this may have contributed to differences in retention. The ceramic composition and intaglio surfaces are specific for each ceramic; thus, conclusions drawn for one ceramic type may not apply to others. In addition, in the previously mentioned studies,43, 56, 57 the axial walls were used to calculate the surface area, and the occlusal surface was excluded because of different surface roughness. However, in this study, the surface area of the occlusal and axial walls was measured as surface area because they were both prepared with a medium-grit diamond rotary cutting instrument and had similar roughness. Therefore, the higher angle of total occlusal convergence, different ceramics, and a larger surface area may have contributed to the lower crown retention values observed in the present study. Furthermore, the physical properties of the cement may influence the retentive qualities. In the present study, although there was no difference in surface area and axial wall height of the preparations between tested groups, standard deviations were rather high for crown retention. Previous studies56-58also show high standard deviation, which may be due to the variability inherent with using natural teeth. Studies based on tooth structure show that dentinal bonding may be influenced by dentinal depth preparation, tubule orientation, and age of tooth and proximity of dentin to pulp tissue. It is very important to control dentin depth because the adhesive strength is 1.6 to 10.7 times greater in the superficial layer than in the deep layer61 Other important factors which influence the dentin 41 bonding is tooth age, location and sclerosis. The factors affecting the bonding of resin to tooth structure cannot be completely controlled due to use of natural teeth. In order to control these variables, an in-vitro prefabricated artificial tooth can be used. In this study, data shows failure mode of Category 1. 27.27%- Cement mainly on prepared tooth Category 2. 10%- Cement on both crown and tooth Category 3. 20.9%- Cement mainly on crown (over 75%) Category 4. 30.90%-Fracture of tooth root without crown separation Category 5. 10%- Fracture of Crown The 10% of crown fracture (category 5) was noticed only with Celtra. Some of the Celtra coping fractured during testing, as shown in Figure 29 and to evaluate the cause of fracture SEM of Celtra disc was performed, SEM pictures are presented in Table 10.. Figure 29: Fractured Celtra crown during testing 42 Table 9: SEM of Celtra HF Polished Fired 3000 No Yes Yes No Yes Yes Unfired 30,000 3000 Back Scattered No No Back Scattered 43 30,000 LIMITATIONS 1. This in–vitro study may not completely simulate in-vivo performance for example crowns were luted at room temperature. 2. All the cements were allowed to self-cure, studies have shown that light activation of the resin cements improved their shear bond strengths. 62 3. Fracture of 34 teeth and fracture of 11 crowns out 110 also might have some confounding effect on the result. 44 CONCLUSION Within the limits of this study, when e.max is used for restoration of single tooth dual cure resin cement shows a good retention strength. When luting e.max with RMGI, hydrofluoric etching is not necessary as it lowers the retention. When Celtra is bonded with the Experimental resin cement, etching the intaglio with 5%HF for 20 secs and application of Silane seems to improve the bond strength, while the use of Prime & Bond Elect is optional. However, when Celtra is luted with RMGI, etching the intaglio with 5% HF is advisable to improve its retention 45 FUTURE DIRECTIONS 1. Polishing or firing the Celtra copings. 2. Incorporating fatigue testing. 46 REFERENCES 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 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