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Resin - Resin Bonding - A New Adhesive - Technology
Resin - Resin Bonding - A New Adhesive - Technology
Technology
Ralf Jandaa/Jean-François Rouletb/Michael Wulfc/Hans-Jürgen Tillerd
Purpose: Evaluation of a new surface treatment method to obtain a good bond strength between a luting
composite and (1) a light-cured, (2) a heat-cured and (3) a thermoplastic resin.
Materials and Methods: Specimens were prepared and tests conducted according to ISO 10477,
Amend. 1. The surfaces of Targis (light cured), SR Isosit (heat cured), and Dental D (thermoplastic) were
ground under water cooling with 400-grit grinding paper, polished with 800-grit paper and air dried. Each
resin material was divided into 3 groups of 10 specimens each. Group 1 was flame treated with a Py-
rosilPen for 5 s/2 cm2, group 2 for 10 s/2 cm2, and group 3 for 20 s/2 cm2. Subsequently, a methacryl
silane was applied, followed by a luting composite. Prior to measuring shear bond strength, the speci-
mens were thermocycled 5000 times in a water bath between 5°C and 55°C. SEM, FTIR investigations,
and fracture analysis were also done. Etched and silanized Empress II – the gold standard – was used
as a control.
Results: The following shear bond strengths were found: treatment time 5 s/2 cm2, Targis 25 (±12)
MPa, SR Isosit 17 (±11) MPa; treatment time 10 s/2 cm2, Targis 23 (±12) MPa, SR Isosit 26 (±8) MPa;
treatment time 20 s/2 cm2, Targis 29 (±5) MPa, SR Isosit 26 (±9) MPa. All Dental D specimens failed
completely so that shear bond strength could not be measured. The control achieved 27 (±6) MPa. No
significant differences were found between the materials or the flaming times. On all flamed surfaces,
Si was detected by FTIR. SEM showed that no heat destruction occurred at a flaming time of 5 s/2 cm2,
a slight change at 10 s/2 cm2, and a significant change at 20 s/2 cm2.
Conclusion: This new bonding technology is an effective method for surface-treating polymerized com-
posite resin materials to obtain good bonding to luting composites. The method fails on thermoplastic
resins.
J Adhes Dent 2002; 4: 299–308. Submitted for publication: 27.08.01; accepted for publication: 06.09.02.
rate might negatively affect the bond strength to The present study investigates a new surface
the luting composite. Recently, new fiber-rein- treatment method called the PyrosilPen technique
forced composite materials for manufacturing (SurA Instruments, Jena, Germany). The PyrosilPen
crowns and bridges have been introduced and in- (Fig 1) is a very special, small hand-held lighter con-
vestigated. It is recommended that these restora- taining a mixture of butane gas and a silane (tetra-
tions also be luted with an appropriate luting com- ethoxy silane). The flame is lit by a piezo element.
posite.7,21,28,30,41,49 The substrate surfaces are flame treated for only a
To obtain an acceptable bond strength between few seconds. Then SurALink (SurA Instruments), a
the luting composite and the cured composite res- proprietary solution of 3-methacryloyl oxypropyl tri-
toration, various surface pretreatment methods methoxy silane in an organic solvent, is brushed on
have been tested in vitro, such as sandblasting, the surface. Finally, the composite material is ap-
hydrofluoric acid etching, phosphoric acid etching, plied.
roughening with burs, silicating and silanizing, or The PyrosilPen technique is based on the Sili-
combinations thereof.1,6,16,29,33,36,43,44,50 Howev- coater technique (Heraeus-Kulzer, Hanau, Germa-
er, the reported results are not uniform and some- ny) developed in 1984.17,18,20,22,32,35,37-39,45 For
times even contradictory. Stokes et al43 reported the first time, this system allowed a very strong and
shear bond strength values of 19 MPa, Haller et long-lasting adhesive bond to be created between
al12 10 to 50 MPa, and Ludwig33 21 to 24 MPa. resins and precious as well as nonprecious met-
Krämer et al,29 who used a different test method, als.10,23-25,48 More recently, this technique has
obtained bond strength values of approximately also been used to bond luting composites to zirco-
48 MPa. The reported in vitro tests are complicat- nia and alumina ceramics.9,13 The Silicoater is a
ed. Moreover, it is also very difficult to compare lab device for flame-treating metal or ceramic. The
the results of the in vitro tests mentioned, since fuel gas is butane, which is burned with atmospher-
each one of the authors used a different test pro- ic oxygen. Prior to lighting the gas, it is guided over
cedure. a container filled with tetraethoxy silane. After light-
In addition, clinical investigations have been ing, this silane decomposes in the flame, and
conducted comparing composite inlays that had SiOx-C fragments are created. Objects put in the
undergone different pretreatments prior to inser- flame are covered by a layer of these SiOx-C frag-
tion with adhesively (etched and silanized) insert- ments that bond adhesively (van der Waals forces)
ed ceramic inlays.3,16,34,47 These tests proved onto the substrate surfaces.38,45 This extremely
that marginal integrity of composite inlays was not thin layer (ca 0.1 µm)38,45 has glasslike properties
as good as the adhesively inserted ceramic inlays. and can be silanized with 3-methacryloyl oxypropyl
Based on these results, it seems to be appropriate trimethoxy silane, which polymerizes with acrylic or
to look for a more reliable, simpler technique to methacrylic groups. Figure 2 schematically shows
bond already cured composite inlays to a luting the single layers created by the Silicoater tech-
composite. nique. However, the Silicoater technique was rather
ns ns ns
ns = not significant
change after being flamed for 10 s/2 cm2 and a se- Furthermore, a fracture analysis to determine
vere destruction after 20 s/2 cm2. Therefore, flam- cohesive and adhesive failures was conducted. In
ing times longer than 5 s/2 cm2 were done step- reference to the control, only cohesive failures
wise in periods of 2 s. SEM revealed that this pro- could be observed in the Empress II ceramic. Con-
cedure did not damage composite surfaces. The be- cerning Targis and SR Isosit, the following failure
havior of the thermoplastic resin Dental D was again characteristics were observed: At a treatment time
different. The resin tags projecting from the surface of 5 s/2 cm2, Targis showed 10% adhesive failure
after polishing were molten after flaming, and loose- and 90% cohesive in the Targis material; SR Isosit
ly cover the surface in an overlapping manner. displayed 30% adhesive failure and 70% cohesive
5s
20s
(10×2s)
20s
(continuously)
Fig 6 SEM images of the specimens after different flaming times (1000X).
were not sandblasted or roughened to avoid the in- times in water between 5°C and 55°C), in addition
fluence of microretentions on the bond strength. to a significantly better performance by the
The only intention of this study was to investigate light-cured composites (approximately 50 MPa).
the performance of the Pyrosil technique. Sandblasting did not significantly influence shear
Furthermore, Empress II frame ceramic was used bond strength of the tested materials. Without sand-
as the control. This is justified by the fact that nu- blasting, the heat-cured composite did not bond at
merous clinical investigations16,36,44 have shown all (shear bond strength ca 0.4 MPa). The sand-
that there is no completely optimal bond between a blasted samples achieved approximately 10 MPa.
polymerized composite and luting composite. How- Ludwig33 measured shear bond strength of a
ever, the procedure of etched and silanized ceram- heat-cured microfilled composite to a dual-curing
ic/luting composite is clinically well known, proven, luting composite. The microfilled composite speci-
and established, and is considered to be the gold mens were conditioned by different methods. After
standard. To guarantee that optimal conditions thermocycling (1000 cycles between 15°C and
were available for this system, the manufacturer’s 65°C), lower values were obtained as compared to
instructions for use were followed. A further reason the 24 h values. The conditioning methods sand-
why none of the methods described by other blasting and cleaning with hydrofluoric acid etching
authors1,6,16,29,33,36,43,44,50 was used in this gel, sandblasting and cleaning with hydrofluoric
study, was that sandblasting – commonly the first acid etching gel followed by an application of a spe-
step of surface conditioning – had to be avoided in cial MMA-containing bonder, and sandblasting and
the present study for the reasons mentioned above. cleaning with hydrofluoric acid etching gel followed
If the PyrosilPen is expected to compete, it by 5 min of etching in an ultrasound bath with 10%
needs to be seen as a truly innovative and promis- hydrofluoric acid, showed the best results with
ing technique. Composite inlays and onlays are of shear bond strength values between approximately
increasing interest in restorative dentistry. There- 21 and 24 MPa. The conditioning method sand-
fore, the question of how to adhesively bond al- blasting and cleaning with hydrofluoric acid etching
ready cured composite restorations to hard dental gel followed by 5 min of etching in an ultrasound
tissues has been discussed by several investiga- bath with 40% hydrofluoric acid achieved a signifi-
tors.1,7,12,16,29,31,33,36,43,44,50 cantly lower bond strength of ca 15 MPa.
With respect to the present investigation, the Krämer et al29 investigated bond strength be-
most important literature shall be reviewed in more tween a light-cured hybrid composite and a dual-cur-
detail, since it shows the difficulties of achieving a ing luting composite. A completely different test
good bond between a cured composite and a luting method was used by preparing standardized cavi-
composite. ties in light-cured hybrid composite specimens in
Stokes et al43 investigated shear bond strength such a way that they formed holes. The inlays were
between a heat-cured hybrid composite and a du- directly shaped and cured in these cavities. After
al-curing luting composite. The specimens were removing the inlays of the cavities, the inner surfac-
conditioned by sandblasting, hydrofluoric acid etch- es of the cavities were sandblasted by a standard-
ing, and/or silanizing. Next, the dual-curing luting ized process. The inlay surfaces were conditioned
composite was applied in the form of cylinders. Pri- by the following methods:
or to measuring shear bond strength, the speci-
mens were stored in water at 37°C for 7 days. For 1. no conditioning
all conditioning methods, shear bond strength val- 2. silanizing
ues around 19 MPa were measured. Stokes et al 3. etching and silanizing
considered these values as sufficient for an accept- 4. sandblasting
able clinical performance. 5. roughening with rotating instruments
Haller et al12 tested the shear bond strength of 6. roughening with rotating instruments, etching
three light-cured inlay composite materials as well and silanizing
as one heat cured and the respective dual-curing lut- 7. using Rocatector -Intraoral
ing composite. The surfaces were pretreated by sev-
eral methods. As a general conclusion, the results Then the hybrid composite inlays were inserted
showed a significant difference between the non- into the hybrid composite cavities after the respec-
thermocycled and the thermocycled group (1440 tive surface treatment by using the dual-curing lut-
ing composite. Bond strength was measured by tem works according to almost the same principle
pushing the inlays through the cavities after 24 h as the PyrosilPen. By a blasting process, a silicon
storage in water followed by 1440 thermocycles in dioxide is fixed on the composite surface. In a fol-
water between 5°C and 55°C. Bond strength values lowing step, a silane coupling agent is applied, cre-
increased from conditioning method No. 1 (ca ating the bond to the luting composite. However, the
28 MPa) to method No. 7 (ca 48 MPa). Condition- first step of this system, too, is a sandblasting pro-
ing method No. 7 significantly achieved the best cedure.
performance. As already stated above, none of the results pro-
Shear bond strength was also investigated by vided by the literature can be compared directly
Latta et al31 between a cured composite inlay ma- with ours, since each author used a different test
terial and a luting composite. The surface of the procedure. Only the test by Stokes et al22 is similar
composite inlay material was treated by several to the one used in the present study. He recorded
methods. Microabrasion achieved the best results. bonding values in optimal cases of 19 MPa, which
Mehl et al,36 Hannig,16 and Zuellig-Singer et al50 he considered to be sufficiently high. The present
investigated marginal gap formation of adhesively in- investigation proves that the PyrosilPen technique
serted composite and ceramic inlays after in vitro is a further method which enables light- and
and in vivo service of the inlays. After testing adhe- heat-cured composites to bond to luting compos-
sively restored extracted teeth in a chewing simula- ites with very good shear bond strength. However,
tion device, Mehl et al36 proved that the marginal the flaming time needs to be considered, since
quality of ceramic inlays was superior to that of flaming periods longer than 10 s/2 cm2 will destroy
light-cured hybrid composite. Zuellig-Singer et al50 the resin surfaces. This time seems to be optimal,
investigated marginal integrity of light-cured hybrid and values of approximately 23 to 26 MPa were
composite inlays and ceramic inlays. The inlays man- achieved with SR Isosit and Targis, which are iden-
ufactured of each material were inserted adhesively. tical to the bond strength of the clinically well-prov-
The restored teeth were exposed to a chewing sim- en system of etched and silanized ceramic/luting
ulation test. Zuellig-Singer et al reported no change composite. It was also observed that the majority
in the marginal quality after the chewing simulation of the fractures occurred in the polymerized com-
was conducted. In contrast to this study, Thordrup posite material, which is a further indication of the
et al44 found a tendency of less microleakage for ce- strength of the bond.
ramic inlays compared to composite inlays. Nevertheless, bonding to the thermoplastic res-
Clinical tests proved that marginal integrity of in Dental D (polyacetale) seems to be problematic.
composite inlays was not as good as that of adhe- Pretesting of this material has shown that a shear
sively inserted ceramic inlays. Hannig16 has report- bond strength of ca 10 MPa could be achieved with
ed 67.6% marginal imperfections of heat-cured nonthermocycled specimens. After thermocycling,
composite inlays in Class I and 54.9% in Class II all specimens failed totally, suggesting that the lut-
cavities after a clinical service of seven years. ing composite and the polyacetale separated in the
As described above, the literature reports numer- thermocycling bath. When the nonthermocycled
ous, sometimes very complicated procedures for specimens were examined with SEM after conduct-
adhesively bonding polymerized composite restora- ing the shear bond test, it was observed that the
tions.1,7,12,16,29,31,33,35,43,44,50 The general state- polyacetale resin showed a flaky surface. These
ment can be made that light-cured composites bond scales are considered to be the residues of the
significantly better to luting composites than do tags that had been observed after the polishing
heat-cured.12 Heat-cured composite restorations process and prior to flaming (Fig 5). It is assumed
achieve an acceptable shear bond strength after that the luting composite only bonds to these tags
sandblasting and etching with hydrofluoric acid.33 It and not to the “actual” surface. This indicates that
is very interesting that without sandblasting, no the luting composite had bonded to a loose surface
bond at all could be achieved with heat-cured com- that separated during thermocycling under the in-
posites.12 However, Rocatector-Intraoral (3M Espe, fluence of water from the firm, “actual” surface.
Seefeld, Germany) seems to be a very innovative Whether or not this is true can only be confirmed
and effective bonding technology, which Krämer et by a further investigation using a surface treatment
al29 have reported as achieving the best perfor- method other than polishing, that does not destroy
mance among all other tested methods. This sys- the surface of the polyacetale resin.
37. Musil R, Tiller, HJ. Das Silicoater Verfahren nach fünfjähriger 45. US Patent 4,600,390. Apparatus and method for applying a
klinischer Bewährung. Zahnärztl Praxis 1989;4:124-128. silicon oxide-containing adhesion-promoting layer on metallic
38. Musil R, Tiller, HJ. Der Kunststoff-Metall-Verbund Silicoater- dental prostheses, Kulzer, Wehrheim, Germany.
verfahren. Heidelberg: Hüthig, 1989. 46. Vojvodic D, Predanic-Gasparac H, Brkic H, Celebic A. The
39. Nord RS. Kulzer’s Silicoater: a new technique for bonding bond strength of polymers and metal surfaces using the sil-
methacrylates to metal. Trends Tech Contemp Dent Lab icoater technique. J Oral Rehabil 1995;22:493-499.
1986;3:32-46. 47. Wendt SL, Leinfelder KF. Clinical evaluation of a heat-treated
40. Reinhardt 18KJ. Seitenzahnrestauration mit Composite-Fül- resin composite inlay: 3-year results. Am J dent 1992;5;258-
lung oder Inlay. Phillip J 1994;11:465-472. 262.
41. Rosenthal L, Trinkner T, Pescatore C. A new system for pos- 48. Wirz J, Schmidli F. Neue Kunststoff-Metall-Verbundsysteme
terior restorations: a combination of ceramic optimized poly- und ihre legierungsabhängige Haftqualität. Quintessenz
mer and fiber-reinforced composite. Pract Periodontics Aes- 1996;47:1231-1240.
thet Dent 1997;9:6-10. 49. Zanghellini G. Fiber-reinforced framework and Ceromer res-
42. Sindel J, Ebert J. Einfluß von Befestigungskompositen und torations: a technical review. Signature 1997;4:1-5.
Haftvermittler auf die biaxiale Biegefestigkeit sandgestrahl- 50. Zuellig-Singer R, Krejci I, Lutz F. Effects of cement-curing
ter Komposite. Dtsch Zahnärztl Z 1995;50:459-462. modes on dentin bonding of inlays. J Dent Res 1992;71:
43. Stokes AN, Tay WM, Pereira P B. Shear bond of resin cement 1842-1846.
to post-cured hybrid composites. Dent Mat 1993;9:370-374.
44. Thordrup M, Isidor F, Horsted-Bindslev P. Comparison of mar-
ginal fit and microleakage of ceramic and composite inlays:
an in vitro study. J Dent 1994;22:147-153.