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Selective enamel etching reconsidered: Better than etch-and-rinse and self-

etch?

Article  in  The journal of adhesive dentistry · November 2008

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Selective Enamel Etching Reconsidered: rP

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Better than Etch-and-Rinse and Self-etch? te
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Roland Frankenbergera/Ulrich Lohbauerb/Matthias J. Roggendorfc/Michael Naumannd/
Michael Taschnerc

Purpose: This study evaluated the marginal quality of differently bonded direct resin composite restorations in
enamel and dentin, before and after thermomechanical loading (TML). Special attention was focussed on the perfor-
mance of selective enamel etching, etch-and-rinse, and self-etching adhesives.

Materials and Methods: Eighty MO cavities with proximal margins beneath the cementoenamel junction were pre-
pared in extracted human third molars. Direct resin composite restorations (Tetric EvoCeram, n = 8) were placed with
4-step selective enamel etching (Syntac SE), 4-step etch-and-rinse (Syntac ER), 2-step etch-and-rinse (XP Bond,
Scotchbond 1 XT/Single Bond Plus), 2-step self-etching (AdheSE, Clearfil SE Bond), 2-step self-etching with selective
enamel etching (AdheSE SE, Clearfil SE Bond SE), and 2-step self-etching with etch-and-rinse (AdheSE TE, Clearfil SE
Bond TE). Marginal gaps were analyzed using epoxy resin replicas under a scanning electron microscope at 200X
magnification.

Results: Initially, high percentages of gap-free margins were identified for all adhesives. After TML, the results were
as follows: A) Enamel margins: When phosphoric acid was used on enamel, results were constantly higher (~90%)
compared with two-step self-etchin adhesives (~70%; p < 0.05). B) Dentin margins: No statistical differences were
found when etch-and-rinse and selective etch approaches were compared (59% to 64%; p > 0.05). When self-etching
adhesives were used as per manufacturers’ directions, dentin margins exhibited the best marginal quality (74% to
82%; p < 0.05). When self-etching adhesives were used under etch-and-rinse conditions, marginal quality in dentin
was significantly reduced to 35% to 42% (p < 0.05).

Conclusion: Enamel bonding was generally more effective with phosphoric-acid etching. Enamel bonding perfor-
mance of 2-step self-etching adhesives was improved when phosphoric acid was applied on enamel selectively.

Keywords: marginal integrity, gap, etch-and-rinse, self-etch, selective etch.

J Adhes Dent 2008; 10: 339-344. Submitted for publication: 22.03.07; accepted for publication: 02.08.07.

T ooth-colored materials are widely used in dentistry all

over the world.22,27 There is clear evidence that adhesion
to dental hard tissues functions on a high level when pit and
age of resin-based composites still requires durable adhe-
sion to enamel and dentin as a fundamental prerequisite,
and without successful adhesion, gap formation potentially
fissure sealants, resin composites, and bonded ceramics hinders clinical success.3,11,22,25
are applied.19,22,28,29 Nevertheless, polymerization shrink- Enamel bonding to phosphoric-acid–etched enamel is
clinically durable;2,10,14,16,36,37 the durability of the self-etch-
a Associate Professor, Dental Clinic 1, Operative Dentistry and Periodontology, ing approach in stress-bearing Classes I and II is still not
University Medical Center, University of Erlangen-Nuremberg, Germany. clinically proven, whereas in cervical lesions the results
b Materials Science Lab Supervisor, Dental Clinic 1, Operative Dentistry and are promising.26,28,32,34,38 In dentin it is quite the opposite:
Periodontology, University Medical Center, University of Erlangen-Nuremberg, here, the self-etching approach, at least with two steps,
Germany. seems to be the most promising way to obtain durable
c Assistant Professor, Dental Clinic 1, Operative Dentistry and Periodontology,
bonds.7,8,34,36,38
University Medical Center, University of Erlangen-Nuremberg, Germany.
Of course, clinical trials remain the final instrument in ad-
d Associate Professor, Department of Prosthodontics and Geriatric Dentistry,
hesive dentistry; however, the main problem with clinical tri-
Charité, Humboldt University, Berlin, Germany.
als is that when they give valuable results after several years
Correspondence: Prof. Dr. Roland Frankenberger, Dental Clinic 1 - Operative
Dentistry and Periodontology, University of Erlangen-Nuremberg, Glueckstrasse
of clinical service, the adhesive and/or resin composite may
11, D-91054 Erlangen, Germany. Tel: +49-9131-8533693, Fax: +49-9131- no longer be on the market.5,19-22 Nevertheless, ultimate
8533603 . e-mail: frankbg@dent.uni-erlangen.de judgements are possible, for instance, in the case of truly

Vol 10, No 5, 2008 339

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Table 1 Chemical compositions, batch numbers, dentin pretreatment, bonding procedures, and manufacturers r P of the

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Adhesive Components Batch # Composition Application protocol Manufacturer tio
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Syntac Etchant F51814 36% phosphoric acid Etch enamel and dentin for Ivoclar Vivadent;
(4-step selective 15 s, rinse, dry. Schaan, Liechten-
etch) (etch-and- Primer E52572 Maleic acid, TEG-DMA, Apply Primer, leave undis- stein
rinse) water, acetone turbed for 15 s, air dry.
Adhesive (2. E08386 PEG-DMA, glutaraldehyde, Apply Adhesive, leave
Primer) water undisturbed for 10 s, air
dry.
Heliobond E10061 Bis-GMA, TEG-DMA, UDMA Apply Bond, air thin, light
cure.

XP Bond Etchant 0506000765 36% phosphoric acid Etch for 15 s, rinse, dry Dentsply DeTrey;
(2-step etch-and- gently. Konstanz,
rinse) Primer+Bond 0503004020 TCB resin, PENTA, UDMA, Scrub for 30 s, air thin, light Germany
TEG-DMA, BHT, CQ, amor- cure.
phous silica

Single Bond Etchant 7EJ 35% phosphoric acid Etch for 15 s, rinse, dry 3M ESPE;
Plus gently. Seefeld, Germany
(2-step etch-and- Primer+Bond 1FW Bis-GMA, HEMA, Scrub for 30 s, air thin, light
rinse) dimethacrylates, cure.
polyalkenoic acid copolymer,
initiator, 3-8% water, ethanol

AdheSE Primer E35881 Dimethacrylate, phosphonic Apply Primer, leave undis- Ivoclar Vivadent
(2-step self-etch- acid acrylate, water, stabiliz- turbed for 30 s, air dry.
ing) ers
(3-step etch-and- Bond E35881 Dimethacrylate, HEMA, sil- Apply Bond, air thin, light
rinse) ica, initiators and stabilizers cure.

Clearfil SE Bond Self-etching 00191A HEMA, hydrophilic Apply Primer, leave undis- Kuraray; Tokyo,
(2-step self-etch- primer dimethacrylate, 10-MDP, turbed for 20 s. Japan
ing) toluidine, camphorquinone,
water
(3-step etch-and- Adhesive 00186A Silanated silica, bis-GMA, Apply Bond, light cure.
rinse) HEMA, hydrophilic
dimethacrylate, 10-MDP,
toluidine, camphorquionone

catastrophic outcomes when adhesive performance is ne- MATERIALS AND METHODS

glected.5,12,20
Therefore, preclinical in vitro investigations are still need- Eighty intact, noncarious, unrestored human third molars,
ed, especially when experimental questions have to be ad- extracted for therapeutic reasons, were stored in an aque-
dressed.1,6,9,23,24 It was shown that selective enamel etch- ous solution of 0.5% chloramine T at 4°C for up to 30 days.
ing may have some beneficial effects on marginal adapta- The teeth were debrided of residual plaque and calculus,
tion in cervical lesions,34 and may cause less detrimental and examined under a light microscope at 20X magnifica-
stress in minimally invasive box-only cavities.4 However, no tion to ensure that they were free of defects.
evidence is provided in the literature about extended Class Standardized Class II cavity preparations (OD, 4 mm in
II cavities in vitro. width buccolingually, 2 mm in depth at the bottom of the
Therefore, the aim of this in vitro study was to investigate proximal box) with proximal margins located 1 to 2 mm be-
different application protocols of well-proven and recent ad- low the cementoenamel junction were performed. The cavi-
hesives of different classes. The null hypothesis tested was ties were cut using coarse diamond burs under profuse wa-
that there is no difference between selective enamel etch- ter cooling (80-μm diamond, Brasseler; Lemgo, Germany),
ing and total etching in (1) enamel and (2) dentin margins. and finished with a 25-μm finishing diamond (one pair of

340 The Journal of Adhesive Dentistry

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Table 2 Methodological setup of the study for

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Group Adhesive Enamel Dentin Self-etch SEM TML
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SEM ati
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etched etched
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Syntac SE Syntac X X
Syntac ER Syntac X X
XP Bond XP Bond X X
Single Bond Plus Single Bond Plus X X
AdheSE AdheSE X
AdheSE SE AdheSE X X
AdheSE ER AdheSE X X
Clearfil SE Bond Clearfil SE Bond X
Clearfil SE Bond SE Clearfil SE Bond X X
Clearfil SE Bond ER Clearfil SE Bond X X

diamonds per four cavities). Inner angles of the cavities were eral ridges were occluded against a steatite (a multi-compo-
rounded and the margins were not bevelled to deliver com- nent semi-porous crystalline ceramic material) antagonist (6
parable results to previous experiments. The cavities were mm in diameter) for 100,000 cycles at 50 N at a frequency
restored using different adhesives (Table 1) with different ap- of 0.5 Hz. The specimens were simultaneously subjected to
plication protocols (Table 2). 2500 thermal cycles between +5°C and +55°C by filling the
The prepared cavities (n = 8) were treated with different chambers with water of each temperature for 30 s. The me-
classes of adhesives according to the manufacturers’ in- chanical action and the water temperature within the chew-
structions (Table 1). Eight teeth were randomly selected for ing chambers were checked periodically to ensure a reliable
each adhesive. The dentin adhesives and resin composite thermomechanical loading (TML) effect.
were polymerized with a Translux CL light-curing unit (Her- After the completion of the 100,000 mechanical loading
aeus Kulzer; Dormagen, Germany). The intensity of the light and the 2500 thermal cycles, impressions of the teeth were
was checked periodically with a radiometer (Demetron; Dan- made again and another set of replicas was made for each
bury, CT, USA) to ensure that 650 mW/cm2 was always de- restoration. The replicas were mounted on aluminum stubs,
livered during the experiments. The adhesive was polymer- sputtercoated with gold, and examined under an SEM (Leitz
ized for 40 s prior to application of the resin composite in all ISI 50, Akashi; Tokyo, Japan) as before at 200X magnifica-
cases. The resin composite Tetric EvoCeram (Ivoclar Vi- tion.
vadent; Schaan, Liechtenstein; shade A3; batch no. J13609) SEM examination was performed by one operator having
was used for all experimental restorations. experience with quantitative margin analysis who was blind-
Each cavity preparation was surrounded with a metal ma- ed to the restorative procedures. The marginal integrity be-
trix band, bonded with the respective adhesives, and re- tween resin composite and dentin was expressed as a per-
stored incrementally with the resin composite in layers up to centage of the entire margin length in enamel and dentin.
2 mm thick. The increments were separately light cured for Marginal qualities were classified according to the criteria
40 s each with the light source in contact with the coronal “continuous margin”, “gap/irregularity” and “not judge-
edge of the matrix band. After removal of the matrix band, able/artefact”. Afterwards, the percentage of “continuous
the restorations were light cured from their buccal and lin- margin” in relation to the individual judgeable margin was
gual aspects for an additional 20 s on each side. Prior to the calculated as marginal integrity.
finishing process, visible overhangs were removed using a Statistical analysis was performed using SPSS/PC+, Ver-
posterior scaler (A8 S204S, Hu-Friedy; Leimen, Germany). sion 14.0 (SPSS; Chicago, IL, USA) for Windows. As the ma-
Proximal margins were finished with flexible disks (SofLex jority of groups in each of the two investigations (ie, enamel
Pop-on, 3M ESPE; St Paul, MN, USA). or dentin marginal integrity) did not exhibit normal data dis-
After storage in distilled water at 37°C for 21 days, im- tribution (Kolmogorov-Smirnov test), nonparametric tests
pressions (Provil Novo; Heraeus Kulzer, Hanau, Germany) of were used (Wilcoxon matched-pairs signed-ranks test,
the teeth were taken and a first set of epoxy resin replicas Mann-Whitney U-test) for pairwise comparisons at the 95%
(Alpha Die, Schuetz Dental; Rosbach, Germany) was made significance level.
for SEM evaluation.
Thermomechanical loading of specimens was then per-
formed in an artificial oral environment. Two specimens RESULTS
were arranged in one simulator chamber in proximal con-
tact, similar to the oral situation with the two restored mar- Results for marginal quality in enamel are presented in Table
ginal ridges in a normal intercuspation. The two adjacent lat- 3. Prior to TML, high percentages of gap-free margins were

Vol 10, No 5, 2008 341

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Table 3 Results of the SEM analysis of enamel margins An overview of marginal quality results inodentin
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before and after thermomechanical loading (TML) played in Table 4. Before TML, all groups exhibiteduab100%

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perfect adhesive performance to dentin. After thermome- tio
Adhesive Gap-free margins in enamel [%] (SD) chanical loading, marginal quality was significantly
te lower n
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(p < 0.05; Wilcoxon test), but the results were further e
ss e n cchar-
prior to TML after TML acterized by the following findings: Syntac revealed a signif-
icantly better performance when used under etch-and-rinse
Syntac SEE 100A 91.4 (6.7)A* conditions compared to the selective etch approach (p < 0.05;
Syntac ER 100A 88.7 (8.4)A* Mann-Whitney U-test). When AdheSE and Clearfil SE Bond
XP Bond 100A 89.4 (8.3)A* were used according to their directions for use, the percent-
Single Bond Plus 99.0 (1.9)A 87.5 (11.9)A* ages of gap-free margins in dentin were the highest in the
AdheSE 100A 70.3 (11.7)B* field (p < 0.05; Mann-Whitney U-test). Under a modified etch-
AdheSE SEE 100A 89.2 (15.3)A* and-rinse protocol, the results were significantly worse (p < 0.05;
AdheSE ER 100A 88.9 (17.7)A* Mann-Whitney U-test).
Clearfil SE Bond 100A 68.6 (15.3)B*
Clearfil SE Bond SEE 100A 88.8 (13.4)A*
Clearfil SE Bond ER 100A 90.6 (12.1)A* DISCUSSION
Same letters within column indicate no statistically significant difference Since resin composites must be adhesively bonded to obtain
(p > 0.05, Mann-Whitney U-test). Asterisks stand for p < 0.05; Wilcoxon test. an acceptable clinical performance, many approaches to
SEE = selective enamel etch; ER = etch-and-rinse.
reach optimum performances have been made. Focussing
on the main tendencies, ie, etch-and-rinse and self-etching
adhesives, the main problem is that the clinician has to deal
with two completely different adhesion substrates in the
vast majority of cavities being adhesively restored.27,36 The
Table 4 Results of the SEM analysis of dentin margins aim of the present study was to acquire clinically relevant re-
before and after TML sults in order to optimize bonding performance. Since the
modern all-in-one adhesives exhibited several shortcomings
Adhesive Gap-free margins in enamel [%] (SD) primarily in bonding equally to enamel and dentin,15,18,27,29-
31,36 this particular class of adhesives was not included in
prior to TML after TML the present study design.
For bonding of resin composites, it would be easier to fo-
Syntac SEE 100A 40.5 (13.7)C* cus on each of the hard tissues separately. Almost everyone
Syntac ER 100A 62.7 (18.7)B* would then use the etch-and-rinse approach on enamel (eg,
XP Bond 100A 60.0 (18.3)B* for laminate veneers) and the 2-step self-etching approach
Single Bond Plus 100A 58.9 (16.9)B* on dentin (eg, in a completely dentin-bordered Class V cavi-
AdheSE 100A 74.1 (15.3)AB* ty). This was confirmed by a clinical trial in noncarious Class
AdheSE SEE 100A 61.6 (13.4)B* V cavities which demonstrated a good clinical performance
AdheSE ER 100A 41.8 (12.2)C* of Clearfil SE Bond as represented by high retention
Clearfil SE Bond 100A 82.0 (12.3)A* rates.28,35 However, when enamel margins were selectively
Clearfil SE Bond SEE 100A 63.9 (14.0)B* etched with phosphoric acid prior to the application of the
Clearfil SE Bond ER 100A 35.4 (16.4)C* self-etching primer, margins remained more stable and stain
free over time.28,35
Same letters within one column indicate no statistically significant differ- On the other hand, preclinical and clinical results of cer-
ence (p>0.05, Mann-Whitney U-test). Asterisks stand for p < 0.05; Wilcoxon vical lesions do not necessarily have to be transferable to oc-
test. SEE= selective enamel etch; ER = etch-and-rinse.
clusally loaded posterior cavities. Here, the results in the lit-
erature are not all in agreement: Clinical results in Class I
cavities indicated that the etch-and-rinse approach may be
beneficial in order to prevent marginal gap formation and
marginal discoloration over time, whereas all self-etching ad-
found (p > 0.05; Mann-Whitney U-test). After thermome- hesives including Clearfil SE Bond performed considerably
chanical loading, the percentages of gap-free margins worse.13 A preclinical investigation by Bortolotto et al repor-
dropped statistically significantly (p < 0.05; Wilcoxon test); ted advantages for the self-etching approach again using
however, a consistently high level of perfect margins re- Clearfil SE Bond in minimally invasive box-only preparations,
mained when phosphoric acid was used (p > 0.05; Mann- assuming that a slightly inferior enamel bonding perfor-
Whitney U-test). AdheSE and Clearfil SE Bond showed sig- mance may produce less stress at the margins, resulting in
nificantly lower percentages of gap-free margins than the fewer gaps and paramarginal enamel fractures.4 It was con-
other groups (p < 0.05; Mann-Whitney U-test), but were not cluded that the etch-and-rinse approach does not neces-
significantly different among themselves (p > 0.05; Mann- sarily have to be the optimum for durable resin composite
Whitney U-test). restorations over the long run.4 However, some method-

342 The Journal of Adhesive Dentistry

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Fig 1 Continuous margin in enamel in the Syntac SE group after Fig 2 Severe gap formation at the bottom of the proximal box in
thermomechanical loading. Paramarginal fractures were not the Clearfil SE Bond ER group after thermomechanical loading
found. E: enamel. RC: resin composite. with osmotic blistering in dentin (D: dentin; RC: resin composite).

ological differences are obvious, such as longer TML and marginal quality values in vitro, it is predicable that its clini-
minimum-intervention type cavities. This may be the reason cal behavior regarding margial quality will be not problem-
that in the present study paramarginal fractures played no atic; however, it must be considered that some of the adhe-
role (Fig 1), although also in the present study enamel mar- sives under investigation have already proven to be clinical-
gins were not bevelled. ly effective.13 On the other hand, it is nearly impossible from
It has been previously published that any unintentional laboratory results to exactly define the critical lower limit of
etching of dentin with phosphoric acid results in an insuffi- marginal quality that is still able to predict acceptable clini-
cient hybrid layer morphology when Clearfil SE Bond is cal behavior. For stress-bearing Class II cavities, it is clear not
used.33 This micromorphological finding was clearly con- only from the present results that etch-and-rinse adhesives
firmed by the present results with severe gap formation (Fig – irrespective of their number of application steps – are a
2). It is noteworthy that after TML, marginal quality in dentin truly promising way of bonding direct resin compos-
is reduced about 50% when phosphoric acid is used on ites.2,9,12,22 Yet the present study is not able to predict
dentin prior to the use of both 2-step self-etching adhesives whether Class II restorations bonded with the 2-step self-
under investigation, AdheSE and Clearfil SE Bond. etching approach alone will fail earlier compared to restora-
In an in vitro study, Frankenberger and Tay investigated all tions bonded with etch-and-rinse adhesives. Nevertheless,
available bonding tactics regarding gap formation in enam- this study is well able to predict that (1) an additionally per-
el and dentin before and after thermomechanical fatiguing, formed selective enamel etching step improves margins in
with the comparable groups AdheSE and Clearfil SE Bond enamel and that (2) phosphoric acid etching of dentin prior
not demonstrating a superior performance in dentin mar- to the use of AdheSE and Clearfil SE Bond is a hazard for
gins as shown during the present investigation.18 This may long-term bonding performance to dentin.
be related to the fact that the present investigation utilized Therefore, both parts of the null hypothesis had to be re-
a restorative resin composite providing less shrinkage and jected because there was (1) a beneficial effect of enamel
shrinkage stress compared to Tetric Ceram, which was used etching on enamel margins and (2) a detrimental effect of
by Frankenberger and Tay.39 Finally, it was shown again that dentin etching when 2-step self-etching adhesives were
the conventional multistep adhesive Syntac exhibited sig- used for bonding of direct Class II resin composite restora-
nificantly better findings in bonding to dentin when dentin tions.
was etched with phosphoric acid, ie, in this case, the self-
etching approach on dentin is less promising compared to
the 2-step self-etching adhesives AdheSE and Clearfil SE CONCLUSIONS
Bond.15,17,18 It is remarkable that with these adhesives, re-
sults after TML were better in dentin than in enamel (Tables • Enamel bonding in extended Class II cavities is more ef-
3 and 4). fective with phosphoric acid etching.
Nevertheless, one problem with any preclinical prediction • The enamel bonding performance of the tested 2-step
of adhesive performance remains. When an adhesive self-etching adhesives is improved when phosphoric acid
restoration (eg, a resin composite restoration) achieves good is applied on enamel selectively.

Vol 10, No 5, 2008 343

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• On dentin, two-step self-etching adhesives perform better 19. Krämer N, Ebert J, Petschelt A, Frankenberger R. Ceramic
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344 The Journal of Adhesive Dentistry

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