2
FiltekTM LSIntroduction
Composite materials have been used in dental practices to restore teeth since the pioneering work of R. L. Bowen and the introduction of composites to the dental market by 3M in the early 1960s. Significant improvements have been made since then. Composites are an essential part of today’s dentistry due to their versatile clinical use and high esthetics that allow the creation of virtually invisible restorations. It is striking that, over the years, polymerization shrinkage has been only incrementally reduced, and remains as one of the major drawbacks of composite materials. Shrinkage during curing results in stress which challenges the tooth/composite interface.
Previously, the main strategy to reduce shrinkage focused on increasing the filler loading. Significant improvements in filler technology have been achieved using nanotechnology which was introduced in the 3M™ ESPE™ Filtek™ Supreme Universal Restorative product. However, shrinkage remains an intrinsic property of the methacrylate resin matrix which results in a dimensional change during polymerization.
We are very excited to introduce Filtek™ LS Low Shrink Posterior Restorative which uses a non-methacrylate resin matrix to realize a fundamental improvement in cure shrinkage.
Filtek LS resin is based on a new silorane chemistry comprised of ring-opening monomers that provide for low polymerization shrinkage. The new silorane system provides a direct solution to the long-standing customer need for low shrinkage.
During the development of the Filtek™ LS System researchers worldwide evaluated this break through technology in numerous studies. More than 40 high-quality studies have been performed proving Filtek LS’s excellent material properties, clinical performance and supporting its biocompatibility. Clinical studies continue to be carried out to investigate the long-term behavior.
Dr. Alfred Viehbeck Global Technical Director 3M ESPE
3
FiltekTM LSTable of Contents
Section Page
1. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
2. Shrinkage and Stress . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10
3. Tooth Deformation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
4. Adhesion and Marginal Quality . . . . . . . . . . . . . . . . . . . . . . . . 26
5. Mechanical/Physical Properties . . . . . . . . . . . . . . . . . . . . . . . . 32
6. Biocompatibility and Bacterial Adhesion . . . . . . . . . . . . . . . . 47
7. Clinical Studies . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55
4
FiltekTM LS
1
1. Introduction
Rationale
Polymerization shrinkage and the resulting shrinkage stress lead to microleakage, which is among the major factors for composite material failures in the oral environment. Moreover, shrinkage stress can lead to tooth deformation, enamel cracks and stress-induced post-operative sensitivity (Figure 1). Materials which remain dimensionally stable upon polymerization, coupled with an advanced bonding to the enamel and dentin, will markedly enhance the stability of the restoration under functional stress.
Filtek™ LS Low Shrink Posterior Restorative is designed to minimize shrinkage and polymerization stress.
Figure 1: Clinical challenges associated with high shrinkage and polymerization stress.
adaptation
post-operative
sensitivity
marginal staining
microleakage
secondary caries
enamel micro-cracks
5
FiltekTM LS
1
1. Introduction
Chemistry of the Resin System
The chemistry of dental restorative composites started in the late 1940s. Since then many technological developments have significantly improved the clinical performance of dental resin composites. However, the common chemical basis for all restorative composites remained the radical polymerization of methacrylates or acrylates and nowadays composites practically all employ dimethacrylates such as TEGDMA, UDMA or Bis-GMA. The low-shrinking Filtek LS Low Shrink Posterior Restorative is based on the new ring-opening silorane chemistry (Figure 2), which is a totally new class of compounds for use in dentistry.
Figure 2: Silorane chemistry.
Outlined in detail by Weinmann et al. (2005) in a study cited on page 11, the name Silorane derives from its chemical building blocks siloxanes and oxiranes. Siloxanes are well known in industrial applications for their distinct hydrophobicity. By incorporating the siloxanes into the dental silorane resin, this favorable property was transferred to the Filtek LS composite. Oxiranes have been used for a very long time in many technical fields, especially where high forces and a challenging physical environment are expected, such as in the manufacture of sports equipment like tennis rackets or skis, or in the automotive and aviation industries. The oxirane polymers are known for their low shrinkage and the outstanding stability toward many physical and chemophysical forces and influences. The combination of the two chemical building blocks of siloxanes and oxiranes provides the biocompatible, hydrophobic and low-shrinking silorane base of Filtek LS Low Shrink Posterior Restorative. This innovative resin matrix represents the major difference of Filtek LS restorative compared to conventional methacrylates. Also, the initiating system and the filler were adapted in order to provide the best performance of the new technology.
Siloxane
Oxirane
Silorane
6
FiltekTM LS
1
1. Introduction
The Filtek™ LS System (bond, primer, restorative) was thoroughly evaluated for its biocompatibility and was found to be safe for its intended use.We used industry standards and internationally- accepted guidelines to conduct our biocompatibility assessment on both the finished product and its ingredients. The assessment included a series of tests and a review of published toxicity literature on ingredients, in addition to characterization of product materials and performance. The biocompatibility of Filtek™ LS Low Shrink Posterior Restorative was confirmed by a variety of external studies. Some key studies you will find summarized in the section Biocompatibility and Bacterial Adhesion of this booklet.
Figure 3: Composition of Filtek™ LS Low Shrink Posterior Restorative.
Ring-Opening PolymerizationFigure 4 illustrates the reactive groups of the monomers for both methacrylates and siloranes.
The polymerization process of methacrylate-based resins occurs via radical addition reaction of their double bonds, which results in higher polymerization contraction compared to the cationic ring-opening polymerization of the siloranes.
The ring-opening step in the polymerization of the silorane resin compensates a significant amount of the polymerization shrinkage which occurs in the curing process. The reduced amount of shrinkage is illustrated schematically in Figure 4. During the polymerization process of methacrylates, molecules have to approach their “neighbors” to form chemical bonds. This process results in a loss of volume, namely polymerization shrinkage. In contrast to the linear-reactive groups of methacrylates, the ring-opening chemistry of the siloranes starts with the cleavage and opening of the ring systems. This process gains space
7
FiltekTM LS
1
1. Introduction
Figure 4: Reactive sites of Silorane and methacrylates and corresponding shrinkage reduction upon polymerization.
and counteracts the loss of volume which occurs in the subsequent step, when the chemical bonds are formed. In total, the ring-opening polymerization process yields a reduced volumetric shrinkage.
Besides shrinkage, another parameter of paramount importance to the performance of a restorative material is polymerization stress. Poly merization stress is generated when composites are cured in the bonded state and the polymerization shrinkage develops forces within the cavity walls. The rigid tooth structure will withstand these forces to a certain degree, however, these tensions can lead to marginal gaps or to damage of healthy tooth structure by its deformation. These forces or tensions are summarized under the term “polymerization stress.”
Silorane technology was developed to minimize shrinkage and for low stress development. The kinetics of the initiation and polymerization of the Filtek LS resin were optimized to provide very low polymerization stress. The minimal shrinkage and polymerization stress were evaluated extensively as reflected in the many studies on shrinkage and stress provided in this study booklet. The uniqueness of Filtek LS Low Shrink Posterior Restorative is nicely visualized, for example by Prof. Watts in the study “Correlation of Shrinkage and Shrinkage Stress” (page 10). Prof. Bouillaguet modeled the impact of shrinkage stress on the tooth
Oxirane
Methacrylate
Silorane – Volumetric Shrinkage < 1%1
Methacrylate – Volumetric Shrinkage
8
FiltekTM LS
1
1. Introduction
with a very sophisticated method that measures the movement of the cusps toward each other while the resin cures in the cavity (page 24).
At the same time, Filtek™ LS Low Shrink Posterior Restorative provides mechanical properties expected from a state-of-the-art compo site in terms of flexural strength or E-modulus. Moreover, based on the silorane network which is more hydrophobic than that of methacrylates, Filtek LS restorative exhibited a very low water uptake and proved to be very stable against chemical challenges representative of the diet. Many studies illustrating these favorable properties can be found in the chapter “Mechanical Properties” in this study booklet.
Initiator SystemOne component of the initiating system is the well-established camphor quinone, which matches the light spectrum of Halogen and LED dental polymerization light sources. Unique components of the Filtek LS initiating system are iodonium salts and electron donors, which generate the reactive cationic species that start the ring-opening poly merization process.
The initiating system of Filtek LS Low Shrink Posterior Restorative was tailored so that the resulting polymerization kinetics leads to a minimized polymeri zation stress, but provides another major advantage: it allows the practitioner to work longer under full operatory light than with any conventional methacrylate-based composite which is illustrated impressively by a study on page 46.
Filler TechnologyFiltek LS restorative is filled with a combination of fine quartz particle and radiopaque yttrium fluoride. From the filler side, Filtek LS restorative is classified as a microhybrid composite. The quartz surface is modified with a silane layer which was especially adopted to the Silorane technology in order to provide the proper interface of the filler to the resin for long-term, excellent mechanical properties.
Figure 5: Initiation chemistry for Siloranes.
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FiltekTM LS
1
1. Introduction
LS System Adhesive Self-Etch Primer and Bond – the one and only adhesive system for Filtek™ LS Low Shrink Posterior Restorative
LS System Adhesive has been specially designed to provide strong and long-lasting bonding of Filtek LS Low Shrink Posterior Restorative to enamel and dentin, providing the basis for excellent marginal integrity of the restorations.
Filtek LS restorative is more hydrophobic than conventional meth-acrylate resins. That means the LS System Adhesive has to bridge a larger gap between the hydrophilic tooth substrate and the hydro-phobic silorane material. Therefore, LS System Adhesive has been designed as a two-step adhesive:
• LS System Adhesive Self-Etch Primer is methacrylate-based and rather hydrophilic for good wetting of the tooth which provides the basis for strong and durable adhesion to the tooth.
• LS System Adhesive Self-Etch Bond is also methacrylate-based and optmized for wetting and adhering to the hydrophobic Filtek LS restorative.
Chemical bonding between LS System Adhesive and Filtek LS Low Shrink Posterior Restorative is ensured by hybrid molecules that can react with both methacrylates in the adhesive and the siloranes in the restorative. These hybrid molecules are crucial for achieving high bond strength with the silorane composite.
Due to the unique chemistry of Filtek LS restorative, it may only be used with its dedicated LS System Adhesive.
Figure 6: Mechanism of chemical bonding between LS System Adhesive Bond and Filtek™ LS Low Shrink Posterior Restorative.
Acidic Monomerof LS System
Adhesive Bond
Curingof Adhesive Application
and Curingof Filtek™ LSRestorative
Chemical BondBetween Adhesive
and Composite
OxiraneGroup
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FiltekTM LS
2
2. Shrinkage and Stress
Volumetric Shrinkage and Polymerization Stress
Title: Correlation of Volumetric Shrinkage and Shrinkage Stress for Dental Composites Executed by: D. C. Watts, University of Manchester, UK Unpublished data
Aim of the study: Shrinkage stress during polymerization of dental composites can lead to marginal gaps, tooth deformation, enamel cracks and even tooth hypersensitivity. The aim of this study was to characterize the development of volumetric shrinkage and shrinkage stress for Filtek™ LS Low Shrink Posterior Restorative in comparison to methacrylate-based composites.
Results: Filtek LS Low Shrink Posterior Restorative revealed significantly lower volumetric shrinkage and polymerization shrinkage stress values than the methacrylate-based composites tested.
Shrinkage Stress (Bioman method) and Polymerization Shrinkage (Bonded Disc Method)
0
1
2
3
4
5
6
7
8
9
0 0.5 1 1.5 2 2.5 3
Shrinkage [%]
Stre
ss [M
Pa]
Filtek™ LS
Venus™
TPH®3EsthetX®
CeramX™
Herculite XRV™EvoCeram®
Premise™ELS Filtek™ P60
Estelite®
QuiXfil™Grandio®
XtraFil™
11
FiltekTM LS
2
2. Shrinkage and Stress
Polymerization Shrinkage
Title: Siloranes in dental composites Published by: W. Weinmann, C. Thalacker and R. Guggenberger, 3M ESPE, Seefeld, Germany Published in: Dental Materials (2005) 21, 68-74
Aim of the study: The purpose of this study was to compare the product profile of a silorane-based composite which polymerizes by a cationic ring-opening process with the product profile of different methacrylate-based restoratives.
Results: The silorane composite revealed with 0.94 vol% (bonded-disc method) and 0.99 vol% (Archimedes method) the lowest polymerization shrinkage among all composites tested. Its reactivity was comparable to the reactivity of Tetric Ceram. However, the ambient light stability of >10 min for silorane was higher than the ambient light reactivity of the other tested methacrylates (55–90 s). The ring-opening chemistry of the siloranes enables for the first-time shrinkage values lower than 1 vol% and mechanical parameters as E-Modulus and flexural strength comparable to those of clinically well-accepted methacrylate- based composites.
Correlation of Polymerization Shrinkage (Bonded-Disc Method and Archimedes Method)
0.5
1
1.5
2
2.5
3
3.5
4
0.5 1 1.5 2 2.5 3
Bonded-disc shrinkage [%]
Arch
imed
es S
hrin
kage
[%]
Filtek™ LS
Filtek™ Z250
QuiXfil™
Aelite™ LS
Tetric® Ceram
Spectrum® TPH®
Solitaire® 2
Note: The study summarized on page 46 shows that Filtek™ LS Low Shrink Posterior Restorative provides up to 9 min working time under operatory light illumination (ISO 4049).
12
FiltekTM LS
2
2. Shrinkage and Stress
Polymerization Shrinkage
Title: Determination of Volumetric Shrinkage by means of a Video Imaging Method (AccuVol) Executed by: J. Burgess, U.S.A. Unpublished data
Aim of the study: This study compared the volumetric shrinkage of Filtek™ LS Low Shrink Posterior Restorative with methacrylate-based composites by means of a video imaging method (AccuVol).
Results: Filtek LS Low Shrink Posterior Restorative revealed significantly lower polymerization shrinkage values than the methacrylate-based composites.
Polymerization Shrinkage (AccuVol Method)
0
5
10
15
20
25
30
35
Nexus™ 2 PanaviaÙ F RelyXÙ Unicem VariolinkÙ II
0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
Filte
k™ L
S
Helio
mol
ar®
Filte
k™ Z
250
Sure
Fil®
Z100
™He
rcul
ite X
RV™
Venu
s™
Esth
etX
®
Rena
mel
®M
iris
® Den
tinPo
int 4
™
Shrin
kage
[Vol
%]
13
FiltekTM LS
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2. Shrinkage and Stress
Polymerization Shrinkage
Title: Parameters Influencing the Shrinkage Determination by Mercury Dilatometry Published by: G. Rackelmann, W. Weinmann, J. Hansen and A. Anderski, 3M ESPE AG, Seefeld, Germany Published at: IADR 2006, Brisbane, Australia, Abstract #2461
Aim of the study: Polymerization shrinkage can be measured by mercury dilatometry. This study investigates the influence of sample weight and recording time on the shrinkage values as determined by mercury dilatometry.
Results: Shrinkage determination by mercury dilato metry is highly dependent on sample weight and recording time. Lower sample sizes result in higher shrinkage values. Even the 500 mg samples are very likely too small, which results in unrealistic high shrinkage values. Recording time should be at least 12 h Filtek™ LS Low Shrink Posterior Restorative revealed the lowest shrinkage within all sample weights, whereas QuiXfil and Filtek™ Z250 showed the same higher shrinkage values. Filtek LS restorative revealed the lowest within all sample weights and reached its final shrinkage earlier than Filtek Z250.
Sample weight and shrinkage (Mercury Dilatometry)
0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
Silo
rane
Helio
mol
ar
Palfi
que
Z250
Sure
Fil
Z100
XRV
Herc
ulite
Venu
s
Esth
et X
Rena
mel
Miri
s De
ntin
Poin
t 4
Poly
mer
izatio
n Sh
rinka
ge [%
]
60
70
80
90
100
0 5 10 15 20 25 30time [h]
Rela
tive
shrin
kage
(24
h =
100%
) [%
]
Filtek™ Z250Filtek™ LS
Recording time and relative shrinkage (Mercury Dilatometry)
0
5
10
15
20
25
30
35
Nexus™ 2 Panaviaô F RelyXô Unicem Variolinkô II
0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
Abso
lute
Vol
umet
ric S
hrin
kage
[%]
Filtek™ LS Filtek™ Z250
100 mg300 mg500 mg
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FiltekTM LS
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2. Shrinkage and Stress
Polymerization Shrinkage
Title: Volumetric Shrinkage of “Low Shrinkage” Composite Resins Published by: T. M. Palmer, T. F. Gessel, C. C. Christensen, S. J. Melonakos and B. J. Ploeger, Clinical Research Associates, Provo, UT, U.S.A. Published at: IADR 2005, Baltimore, U.S.A., Abstract #0296
Aim of the study: Compare volumetric shrinkage of conventional composite resins and an experimental silorane resin using mercury dilatometry.
Results: Filtek™ LS Low Shrink Posterior Restorative exhibited the lowest shrinkage of all materials tested.
Volumetric Shrinkage (Mercury Dilatometry)
0
5
10
15
20
25
30
35
Nexus™ 2 PanaviaÙ F RelyXÙ Unicem VariolinkÙ II
0
0.5
1.0
1.5
2.0
2.5
3.0
Filte
k™ L
S
Nulit
e™He
liom
olar
®Es
telit
e® S
igm
a
Aelit
e™ ELS
Filte
k™ S
upre
me
Herc
ulite
XRV
™Sp
ectru
m® T
PH®
Tetri
c® C
eram
Shrin
kage
[%]
15
FiltekTM LS
2
2. Shrinkage and Stress
Polymerization Shrinkage
Title: Historical Evolution of Volumetric Polymerization Shrinkage of Restorative Composites Published by: R. Guggenberger, W. Weinmann, O. Kappler, J. Fundings land and C. Thalacker, 3M ESPE AG, Seefeld, Germany Published at: IADR 2007, New Orleans, U.S.A., Abstract #0403
Aim of the study: The purpose of this study was to determine the poly merization shrinkage of filling materials and analyze the importance of this shrinkage to dentistry. Therefore, volumetric shrinkage was determined (Archimedes method) for composites introduced since 1993.
Results: The development over the last decade reveals that the manufacturers are working on low shrink composites. However, only a slight decrease was achieved (average decrease 0.05 %/year), because methacrylates as the chemical basis for all available composites remained unchanged. In contrast, Filtek™ LS Low Shrink Posterior Restorative with its ring-opening poly merization monomer enables significant shrinkage reduction.
Material Manufacturer Shrinkage [%] (Deviation)* Year of Introduction
Herculite XRV™ Kerr 2.78(0.10)ef 1993
Tetric® Ceram Ivoclar-Vivadent 2.98(0.08)fg 1996
Spectrum® TPH® Dentsply 3.49(0.47)h 1996
Solitaire™ Heraeus-Kulzer 3.71(0.09)h 1997
SureFil® Dentsply 2.36(0.05)bcde 1998
Definite® Degussa/Dentsply 2.45(0.19)cde 1998
Alert Jeneric Pentron 2.48(0.16)cde 1998
Prodigy® Condensable™ Kerr 2.54(0.15)de 1998
Filtek™ P60 3M ESPE 2.13(0.13)abcd 1999
Filtek™ Z250 3M ESPE 2.14(0.04)abcd 1999
In-Ten-S® Ivoclar-Vivadent 2.14(0.02)abcd 2001
Aelite™ LS Bisco 2.29(0.23)bcd 2002
Filtek™ Supreme 3M ESPE 2.32(0.03)bcd 2002
Venus™ Heraeus-Kulzer 3.05(0.06)fg 2002
EsthetX® Dentsply 3.37(0.26)gh 2002
Grandio® VOCO 2.10(0.23)abc 2003
QuiXfil™ Dentsply 2.12(0.13)abcd 2003
ELS (Extra Low Shrinkage) Saremco 2.39(0.32)bcde 2003
Solitaire® 2 Heraeus-Kulzer 3.64(0.05)h 2003
Premise™ Kerr 1.80(0.22)a 2004
TPH®3 Kerr 3.48(0.32)h 2004
Tetric EvoCeram® Ivoclar-Vivadent 2.03(0.02)ab 2005
Filtek™ LS 3M ESPE 0.99(0.07) future
*Volumetric shrinkage as determined by the Archimedes method. Identical superscript letter indicates no statistical difference.
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FiltekTM LS
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2. Shrinkage and Stress
Polymerization Stress
Title: Polymerization Contraction Stress of Filtek LS and Metha crylate-based Composites. Executed by: T. DeGee and A. Feilzer, University of Amsterdam (ACTA), The Netherlands Unpublished data
Aim of the study: Contraction stress during polymerization of dental composites can lead to marginal gaps, tooth deformation, enamel cracks or even hypersensitivity. This study determined the polymerization shrinkage stress of Filtek™ LS Low Shrink Posterior Restorative and methacrylate-based composites by means of a tensilometer. In this device the composite samples are bonded between a glass and a metal plate. During polymerization the shrinkage stress is recorded over time by a load cell connected to the metal plate.
Results: Filtek LS Low Shrink Posterior Restorative revealed significantly lower polymerization shrinkage stress than the methacrylate composites tested.
Polymerization Stress (Tensilometer Method)
0
2
4
6
8
10
12
14
16
18
0 300 600 900 1200 1500 1800
Time [sec]
Stre
ss [
MPa
]
Quixfil™
Spectrum® TPH®
Tetric® Ceram
Filtek™ Z250Filtek™ SupremeFiltek™ LS
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FiltekTM LS
2
2. Shrinkage and Stress
Polymerization Stress
Title: Determination of polymerization shrinkage stress by means of a photoelastic investigation. Published by: C. P. Ernst, G. R. Meyer, K. Klöcker and B. Willershausen, University of Mainz, Germany Published in: Dent Mat 2004;20(4):313-21
Aim of the study: This study examined the polymerization stress of different established and experimental composite resins which have been claimed to exhibit less polymerization shrinkage by means of a photoelastic investigation.
Results: After 4 min and 24 h Filtek™ LS Low Shrink Posterior Restorative showed a significantly lower polymerization stress than the other materials tested. Except for Filtek LS restorative, all materials showed a statistically significant increase in polymerization force after 24 h compared to the results after 4 min.
Polymerization Stress (Photoelastic Method)
0
5
10
15
20
25
30
35
Nexus™ 2 PanaviaÙ F RelyXÙ Unicem VariolinkÙ II
0
1
2
3
4
5
6
Tetri
c® C
eram
Esth
etX
®
Filte
k™ Z
250
Clea
rfil®
AP-
X
Prod
igy
® Con
dens
able
™
Filte
k™ P
60Su
reFi
l®
Clea
rfil®
Pho
to P
oste
rior
Solit
aire
® 2In
Ten-
S®
Filte
k™ L
S
Poly
mer
izat
ion
Stre
ss [M
Pa] t = 4 min
t = 24 hr
18
FiltekTM LS
2
2. Shrinkage and Stress
Polymerization Stress
Title: Light-Source, Material and Measuring-Device Effects on Contraction Stress in Composites Published by: L. Musanje, R. L. Sakaguchi, J. L. Ferracane and C. F. Murchison, Oregon Health & Science University, Portland, U.S.A. Published at: IADR 2005, Baltimore, U.S.A., Abstract #0294
Aim of the study: The aim of this study was to evaluate contraction stress values of three methacrylate composites and Filtek LS Low Shrink Posterior Restorative as a function of the light-source and testing device (closed-loop-servo hydraulic testing system, Bioman, Low Compliance Device).
Results: Filtek LS Low Shrink Posterior Restorative showed significantly lower contraction stress values than the methacrylate- based composites independent of the light-source in the low compliance testing device.
Polymerization Stress (Low Compliance Device) as determined with different curing lights
0
5
10
15
20
25
30
35
Nexus™ 2 PanaviaŸ F RelyXŸ Unicem VariolinkŸ II
0
1
2
3
4
5
Stre
ss [M
Pa]
Tetric® Ceram Filtek™ Z250 Heliomolar® Filtek™ LS
VIP FreeLight 2 contin. FreeLight 2 ramp
19
FiltekTM LS
2
2. Shrinkage and Stress
Polymerization Stress and Mechanical Properties
Title: Polymerization contraction stress in light-cured composite restorative materials Executed by: K. Gonczowski1, A.Visvanathan2, N. ILIE2 and K.-H. Kunzelmann2: 1Jagiellonian University, Krakow, Poland; 2University of Munich, Germany Published at: CED 2005, Amsterdam, The Netherlands, Abstract #0346
Aim of the study: High contraction stress, as well as early start of stress build-up and rapid contraction force development in the composite materials, may be the reason for failures of bond to tooth structure. The purpose of the present study was assessment of the polymerization stress and the mechanical properties of different types of composites.
Results: The results of the study indicate that the polymerization stress and mechanical properties of the silorane composite are generally superior in maintaining the balance between the high mechanical resistance and good kinetic behavior compared to the other composite materials.
Polymerization Stress (Stress-Strain Analyzer)
0
5
10
15
20
25
30
35
Nexus™ 2 PanaviaÙ F RelyXÙ Unicem VariolinkÙ II
0
1
2
3
4
5
6
7
Stre
ss [M
Pa]
Filte
k™ L
STe
tric
EvoC
eram
®
Cera
mX
™
Filte
k™ S
upre
me
Filte
k™ Z
250
Dyra
ct® e
Xtra
QuiX
fil™
Gran
dio®
20
FiltekTM LS
2
2. Shrinkage and Stress
Polymerization Stress and Curing Lights
Title: Low shrinkage composite for dental application Published by: N. Ilie, E. Jelen and R. Hickel, University of Munich, Germany Published at: IADR 2007, New Orleans, U.S.A., Abstract #0398
Aim of the study: The purpose of this study was to analyze the shrinkage behavior of an innovative composite material for dental restoration based on a monomer with a new chemical formulation – silorane – with a focus on the influence of the irradiation regime.
Results: Filtek LS Low Shrink Posterior Restorative reveals low polymerization stress values in comparison to regular methacrylate composites; nevertheless stress due to thermal contraction after the end of the light exposure is not negligible and can be additionally reduced by applying the appropriate curing strategy.
Curing unit Regime Time [s] Energy density [J/cm²]
Polymerization stress [MPa]
Gradient m
Mini L.E.D. (Satelec) Serial No.:114-6064
Fast-cure
10 8.26 1.9abc(0.4)
1.0B(0.1) 20 1996 2.2bc(0.5)
40 1996 2.4c(0.2)
Pulse
12 1997 1.4a(0.2)
0.7A(0.2) 24 1998 1.8abc(0.2)
48 1998 2.3c(0.2)
Step-cure 20 1998 1.6ab(0.3) 0.7A(0.2)
Bluephase (Ivoclar Vivadent) Serial No.: 1547581
HIP (High Power)
10 1998 2.3c(0.5)
2.1C(0.3)* 20 1999 3.5d(0.4)
40 1999 4.4e(0.6)
*Identical superscript letter indicate no statistical difference, ANOVA (· = 0.05) and post-hoc Tukey’s test.
Polymerization Stress in relation to different curing strategies
21
FiltekTM LS
2
2. Shrinkage and Stress
Polymerization Stress
Title: Shrinkage stress of new experimental low shrinkage resin composites Published by: A. Schattenberg, G. R. Meyer, B. Willershausen and C. P. Ernst, University of Mainz, Germany Published at: IADR 2007, New Orleans, U.S.A., Abstract #0412
Aim of the study: Low-shrinkage resin composites are the focus of research in posterior resin composite restoratives. The aim of this study was to examine the polymerization shrinkage stress of experimental low-shrinkage resin composites (K0152/Dentsply, NEUN/Heraeus, Hermes/3M ESPE) in comparison to new and established low-shrinkage resin composites (Tetric EvoCeram/Ivoclar Vivadent, QuiXfil/ DENTSPLY, XtraFil/VOCO).
Results: New low-shrinkage resin composite formulations are able to show a significantly-reduced shrinkage stress compared to most of the conventional resin composites investigated. After 24 h, the experimental silorane restorative Hermes showed the lowest polymerization shrinkage stress.
Polymerization Stress (Photoelastic Investigation) of Low Shrinkage Composites
0
5
10
15
20
25
30
35
Nexus™ 2 Panaviaô F RelyXô Unicem Variolinkô II
0
1
2
3
4
5
Shrin
kage
Str
ess
[MPa
]
Tetric EvoCeram®
QuiXfil™ XtraFil™ K0152 NeuN Hermes
Note: The material Hermes corresponds to Filtek™ LS Low Shrink Posterior Restorative.
22
FiltekTM LS
2
2. Shrinkage and Stress
Polymerization Stress
Title: Shrinkage-Stress Kinetics of Silorane versus Dimethacrylate Resin-Composites Published by: D. C. Watts and M. A. Wahbi, University of Manchester, UK Published at: IADR 2005, Baltimore, U.S.A., Abstract #2680
Aim of the study: Silorane-based monomers have been developed as an alternative to dimethacrylate monomers as the matrix phase of composites. The aim was to characterize the kinetics of polymerization shrinkage-stress for this silorane composite system.
Results: Filtek LS Low Shrink Posterior Restorative had significantly-lower maximum-stress values (2.08 +/-0.03) than the methacrylate which ranged from 4.7 to 7.0 MPa. Maximum shrinkage-stress-rates for dimethacrylates were from 0.51 to 1.28 MPa s-1, but only 0.07 MPa s-1 for the silorane.
A considerable reduction in both shrinkage-stress magnitude and in peak-stress-rate was apparent with the silorane composite, as compared to established dimethacrylate materials. This class of material should be adequately irradiated – at or above, 500 mWcm-2 – to achieve optimum properties of, and stress-transfer by, the matrix.
23
FiltekTM LS
2
2. Shrinkage and Stress
Polymerization Stress
Title: Simulation of Spatial Distribution of Polymerization Stress Executed by: A. Versluis, University of Minnesota, U.S.A. Unpublished data
Aim of the study: The purpose of this study was to compare the spatial distribution of polymerization stress of QuiXfil and Filtek™ LS Low Shrink Porterior Restorative by Finite Element Analysis.
Results: The simulation shows absence of high stress “gray” areas where enamel cracks and leakage at the margin can occur.
MPa 50
0
Restoration: Filtek™ LS Restoration: QuiXfil™
Most stress
Least stress
Finite element analysis of Filtek™ LS Low Shrink Posterior Restorative and QuiXfil restorations
24
FiltekTM LS
3
3. Tooth Deformation
Cusp Movement during Polymerization
Title: ESPI Analysis of Tooth Deformation during Polymerization of Siloranes Published by: S. Bouillaguet1, J. Gamba2, J. Forchelet2, I. Krejci1 and J. C. Watanabe3: 1University of Geneva, Switzerland; 2School of Engineering, Yverdon, Switzerland; 3Medical College of Georgia, U.S.A. Published in: Dental Materials (2006) 22:896-902
Aim of the study: In the current study, electronic speckle pattern interferometry (ESPI) was used to measure tooth deformation in response to polymerization of five resin composites with a range of polymerization shrinkage. The hypothesis was that composites with higher polymerization shrinkage should cause more cuspal strain as measured by ESPI.
Results: The rate of polymerization shrinkage appeared to mediate the development of cuspal strain. Filtek™ LS Low Shrink Posterior Restorative showed the lowest shrinkage value and induced the least tooth deformation.
Cusp Displacement (ESPI)
7
6
5
4
3
2
1
0
Cus
p D
isp
lace
men
t (m
icro
ns)
Time (sec)0 50 100 150 200
Filtek™ LSTetric® FlowPremise™ Tetric® Ceram QuiXfil™
8
Cusp
Dis
plac
emen
t (m
icro
ns)
8
7
6
5
4
3
2
1
00 50 100 150 200
Time (sec)
7
6
5
4
3
2
1
0
Cus
p D
isp
lace
men
t (m
icro
ns)
Time (sec)0 50 100 150 200
Filtek™ LSTetric® FlowPremise™ Tetric® Ceram QuiXfil™
8
25
FiltekTM LS
3
3. Tooth Deformation
Cusp Movement
Title: Cusp Movement During Polymerization Using Experimental Low-Shrinkage Composites Published by: G. A. Laughlin and R. Sakaguchi, Oregon Health & Science University, Portland, U.S.A. Published at: IADR 2005, Baltimore, U.S.A., Abstract #0622
Aim of the study: One of the most significant adverse characteristics of currently-used composite restorative materials is polymerization shrinkage. Materials formulated from novel monomer systems have been suggested as alternatives, and have produced significantly lower shrinkage and stress in various in vitro experiments. The objective of this study was to determine if trends observed in these experiments would be seen in a more clinically relevant application, such as in restoring extracted teeth.
Results: The findings were consistent with previous shrinkage and stress results for these composites. The relatively high-shrinkage Bis-GMA composite caused more cusp deflection due to shrinkage than the experimental lower-shrinkage composites. This preliminary study suggests that the reduction in polymerization shrinkage of new composite systems could result in dramatic differences in their clinical performance.
Cusp movement as determined by microstrain (µε) ten minutes after polymerization
0
5
10
15
20
25
30
35
Nexus™ 2 Panaviaô F RelyXô Unicem Variolinkô II
–200
20406080
100120140160180200
Mic
rost
rain
Filtek™ Z250 Oxirane Filtek™ LS
Note: Oxirane is an experimental material not available on the market.
26
FiltekTM LS
4
4. Adhesion and Marginal Quality
Tensile Bond Strength
Title: Bond Strength of Filtek™ LS System to Tooth Structure Published by: R. Yapp and J. M. Powers, Dental Consultants, Inc., U.S.A. Published in: The Dental Advisor 12, August 2007
Aim of the study: The purpose of this study was to evaluate the in vitro bond strengths of Filtek™ LS Low Shrink Posterior Restorative in combination with its dedicated adhesive and other commercial resin composites with total-etch and self-etch bonding agents to human tooth structure.
Results: The Filtek LS System (Filtek LS Restorative LS System Adhesive) bonded equally well in vitro to both human cut enamel and superficial dentin, and had tensile bond strengths that were equal to or better than several commercial resin composites bonded with total-etch and self-etch bonding systems.
Strength of Adhesion (Tensile Bond Strength)
0
5
10
15
20
25
30
35
Nexus™ 2 Panavia™ F RelyX™ Unicem Variolink™ II
0
5
10
15
20
25
Clea
rfil®
SE
Bond
/Cle
arfil
® APX
Optib
ond
® All-
in-O
ne/P
rem
ise™
LS S
yste
m A
dhes
ive/F
iltek
™ L
S
Prim
e &
Bond
® NT™
/Est
hetX
®Ad
heSE
® /Tet
ric E
voCe
ram
®
Futu
rabo
nd N
R/Gr
andi
o®
Xeno
® III/Q
uixF
il™
Stre
ss [M
Pa]
Cut EnamelSuperficial Dentin
27
FiltekTM LS
4
4. Adhesion and Marginal Quality
Tensile Bond Strength
Title: Adhesion of LS System Adhesive to Enamel and Dentin Executed by: J. Fischer, B. Stawarczyk, University of Zurich, Switzerland Unpublished data
Aim of the study: The purpose of this study was to evaluate the adhesion of LS System Adhesive in combination with Filtek™ LS Low Shrink Posterior Restorative and methacrylate-based systems after water storage (H2O, 24 h) and thermocycling (TC, 1500 cycles, 5 °C / 55 °C).
Results: The adhesion of the Filtek LS Restorative system to enamel and dentin after water storage and thermocycling was in the range of clinically-proven restorative systems.
Reliability of adhesion (tensile bond strength after water storage [H2O] and thermocycling [TC])
0
5
10
15
20
25
30
35
Nexus™ 2 Panaviaô F RelyXô Unicem Variolinkô II
0
10
20
30
40
50
Bond
Str
engt
h [M
Pa]
Filtek™ LS/LS System Adhesive
Tetric EvoCeram®/AdheSE®
Clearfil® AP-X/Clearfil® SE
Enamel H2OEnamel TCDentin H2ODentin TC
28
FiltekTM LS
4
4. Adhesion and Marginal Quality
Film Thickness
Title: Film Thickness of Adhesives for Silorane and Methacrylate Restorative Composites Published by: C. Thalacker, K. Dede, W. Weinmann, R. Guggenberger, T. Luchterhandt and O. Kappler, 3M ESPE AG, Seefeld, Germany Published at: IADR 2007, New Orleans, #2003
Aim of the study: The goal of this study was to compare the film thickness of the filled two-step self-etch adhesive for a cationic curing silorane-based filling material with a polymerization shrinkage of <1% (Bonded Disc Method) to that obtained with filled adhesives for conventional methacrylate composites.
Results: LS System Adhesive Self-Etch Bond showed a comparable film thickness to Clearfil SE Bond, and a significantly-lower film thickness than Optibond FL.The filled adhesives investigated in this study provided relatively homogeneous films.
Film Thickness of LS System Adhesive and Marketed Materials
0
5
10
15
20
25
30
35
Nexus™ 2 Panaviaô F RelyXô Unicem Variolinkô II
0
10
20
30
40
50
60
Film
Thi
ckne
ss [M
Pa]
Filtek™ LS/LS Bond
Clearfil® AP-X/Clearfil® SE
Premise™ /Optibond® FL
29
FiltekTM LS
4
4. Adhesion and Marginal Quality
SEM Marginal Evaluation
Title: Chewing Simulation of Silorane and Methacrylate Restorations Published by: O. Kappler, H. Loll, W. Weinmann and C. Thalacker, 3M ESPE AG, Seefeld, Germany Published at: CED 2007, Thessaloniki, # 0537
Aim of the study: The goal of this study was to compare the marginal integrity of a cationic-curing silorane composite with a polymerization shrinkage of <1% (bonded-disc method) in combination with its self-etching system adhesive with conventional methacrylate systems before and after chewing simulation.
Results: The combination Filtek™ LS Low Shrink Posterior Restorative/LS System Adhesive resulted in a significantly-higher percentage of continuous margins before and after chewing simulation than the methacrylate systems tested.
Marginal integrity before and after chewing simulation (thermocycling with cyclic loading)
0
5
10
15
20
25
30
35
Nexus™ 2 PanaviaÙ F RelyXÙ Unicem VariolinkÙ II
0
20
40
60
80
100
% C
ontin
uous
Mar
gin
(ena
mel
and
den
tin)
Tetric EvoCeram®/AdheSE®
QuiXfil™/Xeno® III Filtek™ LS/LS System Adhesive
beforeafter
30
FiltekTM LS
4
4. Adhesion and Marginal Quality
SEM Marginal Evaluation
Title: Marginal Integrity of the Filtek LS System and self-etch adhesives in class I cavities Executed by: U. Blunck, Charité, Berlin, Germany Unpublished data
Aim of the study: Adhesive systems are used to improve the marginal seal of composite resin restorations at the interface to enamel and dentin. In the current study the marginal seal to enamel was tested in Class I cavities by SEM analysis of replicas. The Filtek™ LS System consisting of the self-etching LS System Adhesive, and Filtek™ LS Low Shrink Posterior Restorative was compared to several current self-etch adhesives in combination with methacrylate-based composites.
Results: Filtek LS System showed only little gap formation before and after thermocycling in comparison to the reference materials. It can be concluded that the tested two-step self-etch adhesive, LS System Adhesive, in combination with Filtek LS Restorative is effective in the marginal adaptation in enamel of Class I restorations.
Marginal Gaps before and after thermocycling (TC)
0
5
10
15
20
25
30
35
Nexus™ 2 Panaviaô F RelyXô Unicem Variolinkô II
0 0* 0* 0*
10
20
30
40
50
60
Mar
gina
l Gap
[%]
before TCafter TC
Filte
k™ L
S Sy
stem
G-Bo
nd® /G
radi
a® D
irect
Pos
terio
rAd
heSE
® /Tet
ric E
voCe
ram
®Fu
tura
bond
NR
/ Gra
ndio
®
Xeno
® III /
Qui
Xfil™
One-
Up B
ond
/ Est
elite
® Sig
ma
*A value of “0” indicates that no gaps were detected.
31
FiltekTM LS
4
4. Adhesion and Marginal Quality
Microleakage
Title: Microleakage Evaluation of a New Low-shrinkage Composite Restorative Material Executed by: PCV Yamazaki, AKB Bedran-Russo, PNR Pereira, EJ Swift Jr Published in: Operative Dentistry, 2006, 31-6, 670-676
Aim of the study: This study compared the microleakage of an experimental low-shrinkage resin composite (Hermes), a nanofilled resin composite material (Filtek™ Supreme Universal Restorative) and a hybrid resin composite (Tetric Ceram) using a dye penetration in Class I cavities.
Results: Incremental placement remains the preferred restorative technique for direct composites. To reduce the effects of polymerization shrinkage on marginal quality, the low-shrink Hermes system might become a good alternative in clinical practice.
Note: The material Hermes corresponds to Filtek LS Restorative which was applied with an experimental adhesive.
32
FiltekTM LS
5
5. Mechanical/Physical Properties
Degree of Conversion
Title: Silorane-based Dental Composite: Behavior and Abilities Executed by: N. Ilie and R. Hickel, University of Munich, Germany Published in: Dental Material Journal (2006) 25:445-454
Aim of the study: The purpose of this study was to examine the characteristics of an innovative composite material for dental restorations based on silorane. Degree of conversion was determined at 2 mm and 6 mm depth as a function of curing regimes.
Results: Siloranes exhibit good mechanical properties comparable to those of clinically-successful methacrylate-based composite materials. No differences in degree of cure were noted at 2 mm and 6 mm depth with the tested curing units.
Type Curing unit Regime Time [s] DC [2 mm] DC [6 mm] (layered in 3 increments)
LED
Mini L.E.D. (Satelec) Serial No.: 114-6064
Fast-cure102040
60.2cdef (2.7) 61.3fgh (2.1) 66.8lm (3.0)
57.3abc (4.4) 62.5fghij (2.2) 64.6ijklm (1.1)
Pulse122448
56.8ab (4.5) 64.3hijklm (2.7) 66.4lm (2.7)
55.3a (5.5) 61.6fgh (2.5) 64.0ghijklm (1.0)
Step-cure 20 64.4hijklm (6.2) 57.0ab (1.5)
Bluephase (Ivoclar Vivadent) Serial No.: 1547581
HIP102040
60.6ef (3.1) 61.9fghi (2.7) 64.9jklm (4.9)
57.6abcd (1.9) 58.2bcde (3.2) 60.5ef (3.2)
FreeLight 2 (3M ESPE) Serial No.: 939820013826
Standard102040
62.4fghij (1.4) 65.6klm (1.9) 66.5lm (2.8)
57.5abcd (2.8) 63.7ghijkl (1.9) 64.7ijklm (2.9)
HalogenAstralis 10 (Ivoclar Vivadent) Serial No.: 013336
HIP102040
60.5ef (4.5) 63.0fghijk (2.3) 64.9jklm (4.2)
55.8ab (3.4) 58.2bcde (1.1) 60.3def (1.1)
Superscript letters indicate statistically homogeneous subgroups “Tukey’s HSD test” 0.05.
Degree of Conversion of Filtek LS Low Shrink Posterior Restorative as determined by different curing regimes
33
FiltekTM LS
5
5. Mechanical/Physical Properties
0
5
10
15
20
25
30
35
Nexus™ 2 Panavia™ F RelyX™ Unicem Variolink™ II
56
58
60
62
64
66
68
70
72
Degr
ee o
f Con
vers
ion
[%]
Shrin
kage
Str
ess
[MPa
]
Filtek™ LS Prisme Aelite™ Filtek™ Z250
2.5
2
1.5
1
0.5
0
Degree of Conversion Shrinkage stress
Degree of Conversion and Shrinkage Stress
Title: Degree of Conversion and Shrinkage Stress of Silorane Composite Published by: H. M. EL-Damanhoury1, B. K. Moore1, A. N. Habib2, M. A. AL-Hassan2 and N. M. Aboul-Enein3: 1Indiana University, Indianapolis, U.S.A.; 2University of Cairo, Egypt; 3Suez Canal University, Ismalia, Egypt Published at: IADR 2007, New Orleans, Abstract #2682
Aim of the study: Silorane-based composite was introduced as a restorative material with lower polymerization shrinkage stress. The purpose of this study was to evaluate the effect of utilizing two different light sources on the degree of conversion (DC) and the polymerization shrinkage stress of the silorane-based composite Filtek LS Low Shrink Posterior Restorative and compare them to methacrylate-based composites.
Results: Silorane-based composites showed significantly-lower shrinkage stresses than any of the other tested materials, while the degree of conversion was not significantly different.
Degree of Conversion and Shrinkage Stress with Two Different Curing Systems
QTH (Halogen Light, 600 mW/cm2)
0
5
10
15
20
25
30
35
Nexus™ 2 Panavia™ F RelyX™ Unicem Variolink™ II
0
10
20
30
40
50
60
70
80
Degr
ee o
f Con
vers
ion
[%]
Shrin
kage
Str
ess
[MPa
]
Filtek™ LS Prisme Aelite™ Filtek™ Z250
2.5
2
1.5
1
0.5
0
Degree of Conversion Shrinkage stress
LED (1400 mW/cm2)
34
FiltekTM LS
5
5. Mechanical/Physical Properties
Flexural Strength
Title: Determination of the Flexural Strength of Filtek LS and Methacrylate-Based Composites Executed by: N. Ilie and K.-H. Kunzelmann, University of Munich, Germany Unpublished data
Aim of the study: The aim of the study was to determine the flexural strength of Filtek™ LS Low Shrink Posterior Restorative and methacrylate-based composites. The materials were fixed at two points and stress was applied to a third point until fracture. During the test, compressive forces built up on the upper side and tensile forces at the lower side.
Results: The flexural strength of Filtek LS restorative lies within the range of clinically proven composites and is substantially above the ISO 4049 limit of 80 MPa.
Flexural Strength (ISO 4049)
0
5
10
15
20
25
30
35
Nexus™ 2 PanaviaÙ F RelyXÙ Unicem VariolinkÙ II
020406080
100120140160180
200
Flex
ural
Str
engt
h [M
Pa]
Filtek™ LS Z100™ Filtek™
Z250Tetric® Ceram
Helio-molar®
Prodigy® InTen-S® QuiXfil™
35
FiltekTM LS
5
5. Mechanical/Physical Properties
Flexural Modulus and Hardness
Title: Silorane-based Dental Composite: Behavior and Abilities Executed by: N. Ilie and R. Hickel Published in: Dental Material Journal (2006) 25:445-454
Aim of the study: The purpose of this study was to examine the characteristics of an innovative composite material for dental restorations based on silorane – a monomer with a new chemical composition, and thereby compare the examined characteristics against those of well-known methacrylate-based composites.
Results: Siloranes exhibit good mechanical properties comparable to those of clinically successful methacrylate-based composite materials. No significant differences were observed for hardness and modulus of elasticity between 2 mm and 6 mm depth.
Curing unit Regime Time [s] HV – 2 mm [N/mm2]
HV – 6 mm [N/mm2]
E – 2 mm [GPa]
E – 6 mm [GPa]
Mini L.E.D.
Fast-cure102040
75.9 (4.1) 73.7 (1.0) 79.8 (4.6)
71.9 (4.6)72.6 (6.6)73.7 (6.2)
12.7 (0.1)12.4 (0.2)12.7 (0.6)
12.0 (0.4)11.8 (0.8)12.4 (0.6)
Pulse122448
73.4 (2.2)75.2 (0.1)82.2 (5.2)
70.1 (8.2)71.4 (5.1)74.4 (6.3)
12.8 (0.2)12.6 (0.2)13.4 (0.3)
11.9 (0.4)12.5 (0.2)12.4 (0.4)
Step-cure 20 76.0 (1.0) 74.2 (6.6) 12.5 (0.5) 12.8 (0.4)
Bluephase HIP102040
76.8 (4.0)78.8 (2.1)78.5 (4.4)
68.6 (5.5)72.1 (4.4)75.7 (6.1)
12.7 (0.6)12.5 (0.9)12.8 (0.4)
11.2 (0.8)11.9 (0.9)12.3 (0.3)
FreeLight 2 Standard102040
79.9 (3.4)82.5 (9.2)81.7 (5.7)
69.4 (6.7)76.6 (10)76.6 (10)
12.4 (0.7)12.8 (1.1)13.5 (0.1)
12.2 (0.9)12.7 (1.0)13.0 (1.2)
Astralis 10 HIP102040
80.8 (7.7)81.5 (2.9)80.8 (5.0)
68.2 (5.7)72.3 (8.0)73.9 (4.0)
12.6 (0.6)12.4 (0.5)12.5 (0.4)
11.6 (1.5)11.7 (2.1)12.5 (0.3)
Vickers Hardness and Modulus of Elasticity of Filtek LS
36
FiltekTM LS
5
5. Mechanical/Physical Properties
Compressive Strength and Flexural Strength
Title: Compressive Strength and Flexural Strength of Filtek LS and Methacrylate-Based Composites Executed by: W. Weinmann, A. Stippschild, 3M ESPE AG, Seefeld, Germany Unpublished data
Aim of the study: The aim of this study was to evaluate compressive strength and flexural strength of Filtek™ LS Low Shrink Posterior Restorative compared to methacrylate-based composites.
Results: Both the compressive strength and flexural strength of Filtek LS Low Shrink Posterior Restorative rank within the range of clinically proven composites and are substantially above the ISO 4049 limit of 80 MPa (flexural strength).
Compressive Strength and Flexural Strength (ISO 4049)
0
5
10
15
20
25
30
35
Nexus™ 2 PanaviaÙ F RelyXÙ Unicem VariolinkÙ II
050
100
150
200
250
300
350
400
450
Glac
ier
Aelit
e™ L
S Pa
ckab
leQu
iXfil
™
ELS
Cera
mX
™ D
uoTe
tric
EvoC
eram
®He
liom
olar
®
Gran
dio
®
Esth
etX
®
TPH
® 3Fi
ltek™
LS
Venu
s™Fi
ltek™
Sup
rem
ePr
emise
™
[MPa
]
Compressive StrengthFlexural Strength
37
FiltekTM LS
5
5. Mechanical/Physical Properties
Flexural Fatigue Limit
Title: Determination of the Flexural Fatigue Limit of Resin Based Composites and Filtek Silorane Executed by: M. Braem, University of Antwerp, Belgium Unpublished data
Aim of the study: Restoration fracture due to material fatigue is one of the main reasons for failure of direct restorations. To obtain insight into the fatigue behavior of Filtek™ LS Low Shrink Posterior Restorative its flexural fatigue limit was determined and compared with conventional methacrylate composites. In this test, 10,0000 cycles of 3-point loading were applied with the frequency of 2 Hz, which is the upper limit of chewing frequency, under wet conditions and a constant temperature of 35°C. Several tests were done for each material, increasing the stress compared to the previous test if a material did not fail, and decreasing the stress if the material broke under loading. This procedure is referred to as the staircase approach.
Results: The flexural fatigue limit of Filtek LS Low Shrink Posterior Restorative under wet conditions reaches top level, indicating that under clinical conditions Filtek LS restorative will likely withstand mastication forces without fracturing even after many years in service.
Flexural Fatigue Limit
0
5
10
15
20
25
30
35
Nexus™ 2 PanaviaÙ F RelyXÙ Unicem VariolinkÙ II
010
20
30
40
50
60
70
80
90
Shea
r Fle
xura
l Fat
igue
Lim
it [M
Pa]
Charisma™ Tetric® Ceram
Filtek™
Z250SureFil® Prodigy®
Condensable™Solitaire® 2 Filtek™ LS
38
FiltekTM LS
5
5. Mechanical/Physical Properties
Fracture Toughness (KIC
)
Title: Fracture Toughness of Filtek LS and Methacrylate-Based CompositesExecuted by: K.-H. Kunzelmann, University of Munich Unpublished data
Aim of the study: Fracture toughness is a measure of the resistance of a material to crack propagation. A high fracture toughness means clinically that a small crack needs more mechanical impact to cause a failure of the restoration.
Results: The fracture toughness of Filtek™ LS Low Shrink Posterior Restorative is in the range of clinically-proven methacrylate composites.
Fracture Toughness, resistance to crack propagation
0
5
10
15
20
25
30
35
Nexus™ 2 Panaviaô F RelyXô Unicem Variolinkô II
0
0.5
1.0
1.5
2.0
2.5
KIC
Filtek™
Z250Tetric® Ceram
Heliomolar® Prodigy® QuiXfil™ Filtek™ LS
39
FiltekTM LS
5
5. Mechanical/Physical Properties
Viscoelastic Stability
Title: Creep of solvent-aged silorane, Ormocer and dimethacrylate matrix composites Published by: D.C. Watts, and H. Y. Marghalani, University of Manchester, UK Published at: IADR 2007, New Orleans,U.S.A., Abstract #0235
Aim of the study: The purpose was to study time-dependent visco elastic deformation (creep and recovery) of new composite formulations with different matrix structures, under compressive load, after aging in food-simulating solvents of different solubility parameter. The hypo theses to be tested were that: (i) viscoelasticity would vary with solu bility parameter and that (ii) materials with the newer matrix chemistries would be more dimensionally stable under load.
Results: The materials all exhibited classic creep and recovery curves. Two new-matrix composite types: silorane and Ormocer, exhibited viscoelastic stability in food-simulating solvents. But this behavior was closely matched by one highly-filled dimethacrylate material.
40
FiltekTM LS
5
5. Mechanical/Physical Properties
Hydrolytic Stability
Title: Hydrolytical Stability of a Silorane and Three Methacrylate Composites Published by: R. Guggenberger, C. Thalacker, A. Syrek, A. Stippschild and W. Weinmann, 3M ESPE AG, Seefeld, Germany Published at: IADR 005, Baltimore, Maryland, U.S.A., Abstract #3093
Aim of the study: The goal of this study was to investigate the hydrolytical stability of an experimental silorane-based filling material in comparison to conventional methacrylate-based systems. Thus, their water sorption was correlated with their flexural strength (FS) after water storage and a boiling stress test.
Results: The silorane material exhibits statistically the lowest amount of water sorption. There was no statistical difference among all materials regarding the development of the flexural strength after 7d 36 °C. The boiling test for 10 h revealed that the silorane material and Prodigy Condensable showed the most robust hydrolytical stability.
Water sorption and FS according to ISO 4049. Standard deviations are given in parentheses. Means with the same letters are statistically the same.
Material Manu facturer Water sorption µg/mm3
FS ISO [MPa]
Ratio FS 7d 36 °C / ISO [%]
Ratio FS 10h 100 °C / ISO [%]
Silorane 3M ESPE 9.2 (0.6)a 124 (9)e 105 (9)f 89 (8)g
Tetric® Ceram Ivoclar Vivadent
19.6 (0.7)c 127 (14)e 99 (7)f 77 (5)i
QuiXfil™ Dentsply 11.7 (0.9)c 130 (29)e 104 (2)f 80 (7)hi
Prodigy® Condensable™
Kerr 15.2 (0.9)d 140 (24)e 101 (4)f 86 (5)gh
41
FiltekTM LS
5
5. Mechanical/Physical Properties
Hydrolytic Stability
Title: The influence of short- and medium-term water immersion on the hydrolytic stability of novel low-shrink dental composites Executed by: W. M. Palin1, G. J. P. Fleming1, F. J. T. Burke1, P. M. Marquis1, R. C. Randall2: 1University of Birmingham, UK; 23M ESPE, St. Paul, U.S.A. Published in: Dental Materials (2005) 21, 852–863
Aim of the study: The aim of the current study was to investigate the effect of water uptake characteristics and water solubility on the mechanical properties of two methacrylate (Z100™ and Filtek™ Z250), an experimental oxirane (OXI) and silorane (SIL) resin-based composites (RBC) following short- and medium-term immersion.
Results: Silorane exhibited the significantly-lowest water sorption, solubility and associated diffusion coefficient following each immersion period. This may potentially improve hydrolytic stability of composite restorations.
Immersion periods [weeks]
Material Water sorption [µg mm–3]
Water solubility [µg mm–3]
1
Z100™ 13.04 (0.5)b 0.92 (0.09)b
Z250 11.31 (0.3)c 0.36 (0.09)c
OXI 19.11 (1.0)a 2.28 (0.11)a
SIL 6.63 (0.5)d 0.26 (0.07)c
4
Z100™ 16.31 (0.5)b 0.92 (0.12)b
Z250 13.62 (0.5)c 0.49 (0.10)c
OXI 22.92 (1.0)a 2.94 (0.16)a
SIL 8.04 (0.6)d 0.28 (0.07)d
12 Z100™ 17.32 (0.9)b 0.89 (0.08)b
Z250 13.93 (0.6)c 0.49 (0.07)c
OXI 25.30 (0.7)a 2.90 (0.19)a
SIL 8.74 (1.1)d 0.29 (0.07)d
26
Z100™ 18.84 (1.4)b 0.95 (0.16)b
Z250 15.41 (0.8)c 0.54 (0.11)c
OXI 28.14 (1.2)a 2.95 (0.17)a
SIL 9.40 (0.8)d 0.26 (0.07)d
Water sorption and water solubility after storage in water (37°C)
Standard deviations are displayed in parentheses. Similar superscripts within each immersion period signify no significant difference between materials (P<0.05).
42
FiltekTM LS
5
5. Mechanical/Physical Properties
Oxygen Inhibition Layer
Title: Reducing the depth of oxygen inhibition in resin-based composites Published by: S. Mohammed, W. M. Palin and A. C. Shortall, University of Birmingham, UK Published at: IADR 2007, New Orleans, U.S.A., #2673
Aim of the study: To investigate the effect of monomer chemistry and filler content on oxygen diffusion and curing extent near to the irradiated surface of resin-based composites (RBCs).
Results: Silorane resin chemistry may eliminate oxygen inhibition near the cured surface. The depth of inhibition is complicated by filler content which may act as a diffusion barrier or adsorb oxygen onto the filler surface.
43
FiltekTM LS
5
5. Mechanical/Physical Properties
3-Body Wear
Title: 3-Body Wear of Filtek LS and Methacrylate based Composites Determined by Means of the ACTA Machine Executed by: T. DeGee, University of Amsterdam (ACTA), Netherlands Unpublished data
Aim of the study: Wear resistance is a critical factor especially for the survival of posterior restorations. In this study the wear resistance of Filtek™ LS Low Shrink Posterior Restorative and methacrylate-based composites was determined by means of the ACTA-wear machine. In this machine a structured steel wheel rotated against a composite sample wheel in a millet gruel suspension, causing a trace in the samples. The deeper the trace, the less wear resistant is the composite. Wear was determined after 200,000 revolutions and different storage times by measuring the depth of the trace that the steel wheel has caused on the composite samples.
Results: The wear resistance of Filtek LS Low Shrink Posterior Restorative was similar to clinically-proven resin composites.
Abrasion (ACTA, 3-body wear)
0
5
10
15
20
25
30
35
Nexus™ 2 Panaviaô F RelyXô Unicem Variolinkô II
0
10
20
30
40
50
60
70
80
Wea
r [µm
/200
,000
revo
lutio
ns]
Spectrum® TPH® Prodigy® Condensable™
InTen-S® Tetric® Ceram Filtek™ LS
1 day4 days1 week1 month2 months
44
FiltekTM LS
5
5. Mechanical/Physical Properties
3-Body Wear
Title: Wear of Filtek LS and methacrylate-based composites Executed by: A. Stippschild and Wolfgang Weinmann’ 3M ESPE, Seefeld, Germany Unpublished Data
Aim of the study: Wear resistance is a critical factor especially for the survival of posterior restorations. In this study the wear resistance of Filtek™ LS Low Shrink Posterior Restorative and methacrylate-based composites was determined by means of the ACTA-wear machine. Values are given in relation to Filtek™ Z250 Universal Restorative.
Results: The wear resistance of Filtek LS Low Shrink Posterior Restorative was equivalent to clinically-proven resin composites.
Abrasion (ACTA, 3-body wear)
0
5
10
15
20
25
30
35
Nexus™ 2 PanaviaÙ F RelyXÙ Unicem VariolinkÙ II
0
0.5
1.0
1.5
2.0
2.5
Filte
k™ Z
250
Char
isma
®
Poin
t 4™
Filte
k™ L
STe
tric
® Cer
am ELS
Cera
mX
™
Esth
etX
®Gr
adia
® Dire
ctTe
tric
EvoC
eram
®Fi
ltek™
Sup
rem
e
Wea
r in
rela
tion
to F
iltek
Z25
0
45
FiltekTM LS
5
5. Mechanical/Physical Properties
Ambient Light Stability and Flexural Modulus
Title: Comparative Testing of Ambient Light Stability and Reactivity of Silorane and Methacrylate Filling Materials Published by: W. Weinmann, C. Thalacker, R. Guggenberger, A. Stipp schild, K. Dede and A. Anderski, 3M ESPE AG, Seefeld, Germany Published at: IADR 2003, Göteborg, Sweden, #0733
Aim of the study: Light-curing dental composites already polymerize when exposed to daylight or operatory light. The sensitivity to ambient light reduces the time a practitioner has to properly shape the composite restoration. Especially for posterior applications, a long working time is desirable. This study compared the ambient light stability and the cor res ponding reactivity of Filtek™ LS Low Shrink Posterior Restorative with a resin composite (Tetric Ceram).
Results: The Filtek LS composite revealed a significantly higher ambient light stability than the resin composite, Tetric Ceram. The postcuring rate (reactivity), determined by the measurement of the E-modulus at different times, was not significantly different, although Filtek LS restorative showed a significantly-higher E-modulus at 5 min and 24 h than Tetric Ceram.
E-modulus in GPa
0
5
10
15
20
25
30
35
Nexus™ 2 PanaviaÙ F RelyXÙ Unicem VariolinkÙ II
0
2
4
6
8
10
12
GPa
Filtek™ LS Tetric® Ceram
5 min24 h
46
FiltekTM LS
5
5. Mechanical/Physical Properties
Ambient Light Stability
Title: Operatory Light Stability of Filtek LS and methacrylate-based composites Executed by: W. Weinmann, A. Stippschild, 3M ESPE AG, Seefeld, Germany Unpublished data
Aim of the study: The sensitivity to the operatory light of methacrylate-based composites often necessitates the practitioner to work without direct illumination if larger restorations need to be placed. This study evaluated the operatory light stability of Filtek LS™ Low Shrink Posterior Restorative with other resin composites according to ISO 4049.
Results: Filtek LS Low Shrink Posterior Restorative offers the dentist up to 9 minutes to place and shape the restoration under operatory light illumination.
Ambient Light Stability (ISO 4049)
0
5
10
15
20
25
30
35
Nexus™ 2 PanaviaŸ F RelyXŸ Unicem VariolinkŸ II
0
2
4
6
8
10
Tetri
c Ev
oCer
am®
Esth
etX
®
Filte
k™ Z
250
Filte
k™ P6
0
QuiX
fil™
Prem
ise™ P
acka
ble
Spec
trum
® TPH
®
Gran
dio
®
TPH
® 3
Filte
k™ L
S
Ambi
ent L
ight
Sta
bilit
y [m
in]
47
FiltekTM LS
6
6. Biocompatibility and Bacterial Adhesion
Stability in biological fluids
Title: Stability of silorane dental monomers in aqueous systems Executed by: Eick J. D.1, Smith R. E.1, Pinzino C. S.2 and Kostoryz E. L.1: 1University of Missouri Kansas City, U.S.A.; 2Midwest Research Institute, USA Published in: J Dent (2006) 34:405-410
Aim of the study: To test the stability of siloranes by measuring changes in the chemical structure of the oxirane group in biological fluids. Siloranes are extremely hydrophobic, perhaps making the oxirane groups inaccessible to attack by water or water-soluble species. The chemical stability of the silorane component can then be assessed by measuring changes in the chemical structure of the oxirane group. The stability of the component, in turn, will indicate the chemical stability of the composite in the oral environment.
Results: Siloranes were stable in all aqueous biological fluids tested.
48
FiltekTM LS
6
6. Biocompatibility and Bacterial Adhesion
Genotoxicity Testing
Title: The Induction of Gene Mutations and Micronuclei by Oxiranes and Siloranes in Mammalian Cells Executed by: H. Schweikl1, G. Schmalz1 and W. Weinmann2,: 1University of Regensburg, Germany;2 3M ESPE, Seefeld, Germany Published in: J Dent Res (2004) 83:17-2127
Aim of the study: Oxiranes and siloranes are candidate molecules for the development of composite materials with low shrinkage. Therefore, we analyzed the formation of micronuclei (chromosomal aberrations) and the induction of gene mutations (HPRT assay) in mammalian cells.
Results: No mutagenic effects were detected for the siloranes used in Filtek™ LS Low Shrink Posterior Restorative.
49
FiltekTM LS
6
6. Biocompatibility and Bacterial Adhesion
Mutagenicity Testing
Title: Evaluation of Siloranes for DNA Damage Using the Comet Assay Executed by: H. Zhao1, E. L. Kostoryz1, W. Weinmann2 and J. D. Eick1: 1University of Missouri, Kansas City, U.S.A.; 23M ESPE, Seefeld, Germany Published at: IADR 2005, Baltimore, #1196
Aim of the study: Dental monomers containing silicone and oxirane functional groups (siloranes) are potential components of new dental composites. The objective of this investigation was to evaluate the DNA damage potential of siloranes in L929 mouse fibroblast cells.
Results: None of the siloranes produced DNA damage in this evaluation. The non-DNA damaging effect exhibited by the siloranes supports their non-clastogenic properties as reported in the literature.
50
FiltekTM LS
6
6. Biocompatibility and Bacterial Adhesion
Mutagenicity Testing
Title: Mutagenic activity of structurally related oxiranes and siloranes in Salmonella typhimurium Executed by: H. Schweikl1, G. Schmalz1 and W. Weinmann2: 1University of Regensburg, Germany; 23M ESPE, Seefeld, Germany Published in: Mut Res Gen Toxicol Environ Mut (2002) 521:19-27
Aim of the study: Ring-opening molecules like oxiranes (epoxides) may be suitable for the development of non-shrinking dental com-posite materials. Since oxiranes are reactive molecules, they could cause adverse biological effects in living organisms. The introduction of siloranes, a merger of silane and oxirane, may solve this problem. Here, new oxiranes and siloranes were analyzed for the induction of mutations in Salmonella typhimurium.
Results: The Siloranes used in Filtek™ LS Low Shrink Posterior Restorative tested negative in all S. typhimurium strains which shows that the siloranes are non-mutagenic in S. typhimurium (Ames Test).
51
FiltekTM LS
6
6. Biocompatibility and Bacterial Adhesion
Cytotoxicity Testing
Title: Cytotoxicity of a Silorane-Based Composite in a Dentin Barrier Test Executed by: A. Sengun1, H. Schweikl2, K. A. Hiller2, F. Ozer1 and G. Schmalz2: 1Selcuk University Turkey; 2University of Regensburg, Germany Published at: CED 2005, Amsterdam, #0122
Aim of the study: The biocompatibility is an important requirement for a dental filling material. The objective of this study was to evaluate the cytotoxicity of a new silorane-based resin composite material with its corresponding adhesive in comparsion with a known material in a dentin barrier test simulating the in vivo situation.
Results: Cell survival rates for Hermes System and Tetric Ceram/Excite were statistically not different from the control. With residual dentin barriers of 200 µm and 500 µm the tested silorane-based composite/ adhesive may not alter biologically the dental pulp on a short-term basis.
Note: The Hermes System corresponds to Filtek™ LS Low Shrink Posterior Restorative which was applied with an experimental adhesive.
52
FiltekTM LS
6
6. Biocompatibility and Bacterial Adhesion
Histological Evaluation
Title: A Histological Evaluation of a New Adhesive/Composite Restorative System Published by: I. L. Dogon1, L. Murray2: 1Harvard University, Boston, MA, U.S.A.; 2Forsyth Institute, Boston, MA, U.S.A. Published at: IADR 2004, Honolulu, U.S.A., #4093
Aim of the study: Dental composites must not exhibit any adverse effects to the dental pulp. The purpose of this investigation was to evaluate the biological response of Filtek™ LS Low Shrink Posterior Restorative with the corresponding adhesive in comparison to a methacrylate-based composite in monkey teeth.
Results: No significant difference was observed between Filtek LS Low Shrink Posterior Restorative and the methacrylate-based composite with regards to pulp response.
Note: Filtek LS restorative was applied with an experimental adhesive.
53
FiltekTM LS
6
6. Biocompatibility and Bacterial Adhesion
Bacterial Adhesion
Title: Adhesion of S. mutans to dental restorations Published by: R. Lang, G. Groeger, M. Rosentritt and G. Handel, University of Regensburg, Germany Published at: CED 2005, #0426
Aim of the Study: The aim of this study was to rank commonly-used filling materials according to their susceptibility to bacterial adhesion.
Results: Due to the low bacterial adhesion rate in vitro, a low plaque susceptibility of Hermes, Enamel Plus and Grandio may be expected.
Medians and 25/75 percentiles were calculated; statistics: Mann-Whitney U-test.
Note: The material Hermes corresponds to Filtek™ LS Low Shrink Posterior Restorative.
Adhesion of S. mutnas (Resazurine Fluorescence)
0
5
10
15
20
25
30
35
Nexus™ 2 PanaviaŸ F RelyXŸ Unicem VariolinkŸ II
0
5000
10000
15000
20000
25000
Enam
el P
lus
Gran
dio
®Te
tric™
Cer
amGl
ass
Spec
trum
®Fi
ltek™
Sup
rem
eEs
thet
X®
Helio
mol
ar®
Filte
k™ Z
250
Adm
ira®
Venu
s™In
Ten-
S®
Com
pogl
ass
®Ar
abes
k® To
pFi
ltek™
LS
Rel.
Fluo
resc
ence
Inte
nsity
54
FiltekTM LS
6
6. Biocompatibility and Bacterial Adhesion
Bacterial Adhesion
Title: Adhesion potential of novel silorane-based restorative to oral streptococci Executed by: R. Bürgers, S. Hahnel, G. Handel, M. Rosentritt University of Regensburg, Germany Unpublished data
Aim of the study: To compare the susceptibility of one novel silorane-based and four conventional methacrylate-based resin composites to adhere oral streptococci. Bacterial suspensions of four streptococci were incubated on specimens of the test materials and bacterial adherence was determined with a fluorescence dye (Resazurine).
Results: The fluorescence intensities of the four methacrylate resin composites were comparable among each other. Significantly-lower fluorescence intensities were found on Filtek™ LS Low Shrink Posterior Restorative for all four strains of streptococci.
Medians and 25/75 percentiles were calculated; statistics: Mann-Whitney U-test.
Bacterial Adherence of Streptococci (Resazurine Fluorescence)
0
5
10
15
20
25
30
35
Nexus™ 2 Panaviaô F RelyXô Unicem Variolinkô II
0
5000
10000
15000
20000
25000
S. mutans S. oralis S. sanguinis S. gordonii
Filtek™ LS Filtek™ Z250 Tetric EvoCeram®
QuiXfil™ Spectrum® TPH® Glass (Reference)
55
FiltekTM LS
7
7. Clinical Studies
Title: One year performance of an innovative silorane posterior composite Published by: M. Brandenbusch, G. R. Meyer, K. Canbek, B. Willers hausen and C.-P. Ernst, Johannes Gutenberg University, Mainz, Germany Published at: IADR 2007, New Orleans, U.S.A., Abstract #1581
Aim of the study: The aim of the study was to evaluate the clinical performance of an experimental silorane restorative (Hermes/3M ESPE), in comparison to another low-shrinkage posterior resin composite (QuiXfil/DENTSPLY) in Class II cavities according to the Ryge/CDA-criteria. In accordance to a split mouth study design, 46 patients (36.9 SD±10.2a) received at least one pair of comparable Class II restorations (Total: 102 restorations).
Results: After one year, all restorations retained and showed clinically excellent and acceptable results. No Charlie or Delta scores were documented. This study was supported by 3M ESPE, Seefeld, Germany.
Note: The material Hermes corresponds to Filtek™ LS Low Shrink Posterior Restorative which was applied with an experimental adhesive.
56
FiltekTM LS
7
7. Clinical Studies
Title: Clinical performance of a Silorane restorative in combination with an experimental adhesive Executed by: Prof. Eliasson, University of Iceland Unpublished data
Aim of the study: In this study the clinical performance of Filtek™ LS Low Shrink Posterior Restorative is being tested with an experimental adhesive system and is compared to Tetric Ceram and a self-etching adhesive, AdheSE. At least one pair of restorations was placed in each patient according to research protocol. At one year, 53 restoration pairs in 31 patients were examined using the modified Ryge/CDA scale.
Results: All the restorations were retained. No Charlie and Delta scores were seen. Color match was unchanged and no secondary decay was observed. One Tetric Ceram restoration was removed because of sensitivity. No sensitivity was reported for Filtek LS restorative at one year, both the materials appear to be clinically acceptable and comparable.
Note: Filtek LS Low Shrink Posterior Restorative was applied with an experimental adhesive.
57
FiltekTM LS
7
7. Clinical Studies
Title: Clinical application of Filtek LS Posterior Restorative System Executed by: E. Mecher, 3M ESPE AG, Seefeld, Germany Unpublished data
Aim of the study: Filtek™ LS System was tested by 43 dentists in their offices during a six-week period. 1145 fillings were placed with an average of 27 fillings per dentist.
Results: The overall satisfaction of the Filtek LS System was rated as equivalent or better compared to their currently-used restorative system by 77% of the dentists. The Filtek LS System received very good ratings in many handling aspects and was rated as very easy/easy to use by 84% of the dentists. No post-operative sensitivities were reported.
Dental Products
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Based on the data contained in the publications 3M ESPE has prepared “Aim of the Study,” “Results” and graphs.
3M, ESPE, Filtek, Sinfony, Sof-Lex and Z100 are trademarks of 3M or 3M ESPE AG. Used under license in Canada.
All other trademarks are owned by other parties.
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