Long-term Resin Bond Strength to

Zirconia Ceramic
Stefan M. Wegnera/Matthias Kern^

Purpose: The airr of this in vitro study was to evaluate the iong-term bond strength of adhesive bonding
systems to yttrium-oxide-partiaily-stabiiized zirconia ceramic (YPSZ).
Materials and Methods: Piexiglas tubes fdled with resin composite ware bonded to industrially manufac-
tured zirconia ceramic disks (96% ZrO2 stabiiized by 4% VïOa). After air abrading the ceramic and ultra-
sonic cleansing, groups of 15 samples were bonded in an aiignment apparatus using 7 different bonding
methods. Subgroups of S bonded sampies were tested for tensiie strength foiiowing storage in distiiied
water at 37^C either for 3 days or 2 years. In addition, the 2-year samples were thermccycled 37,500
times. The statistical anaiyses were conducted with the Kruskai-Wallis test followed by muitipie pair-wise
comparison of the groups using the Wilcoxon rank sum test
Results: A moderate to relatively high initial bond strength was achieved by air abrasion alone, the addi-
tional use of a siiane, or acryiizing the YPSZ surface in combination with a conventional bis-GMA resin
oomposite. However, these methods failed spontaneously over storage time. The use of the bis-GMA resin
oomposite after tribochemicai siiica coating of YPSZ and the use of a poiyacid-modified resin composite
after air abrasion of VPSZ resuited in a high initiai bond strength which decreased significantly over stor-
age time, A durable resin bond strength to YPSZ was achieved only after air abrasion of YPSZ and using
one of two resin composites containing a speciai phosphate monomer.
Conclusion: A durable bond strength to YPSZ was achieved oniy by using resin composites containing a
special adhesive monomer.
J Adhesive Dent 2000:2:139-147. Submitted for publication:05.08.99: accepted for pubiication: 14.01.00.

Inrial,recent years, a new high-strength ceramic mate-

yttrium-oxide-partiaiiy-stabiiized zirconia
impiant abutments,^5 ail-ceramic crowns and
bridges,^'iS'^s and various aii-ceramic core and post
(YPSZ) ceramic, has been introduced in restorative systems,^'' for which a first 5-year follow-up study
dentistry. This ceramic has optimized physical prop- shows successful clinicai results.^'^ Considering the
erties'''^^ and exhibits much higher fracturai advantages of this new material, now truly esthetic,
strength and toughness than aiumina ceramic.i^'^s metal-free, stabie restorations are available for
Clinical applications of YPSZ inciude implants,^'^ restorations in prosthetic dentistry.
Although bonding with resin to YPSZ ceramic
would be advantageous for many clinical appiioa-
^ Assistant PrD^ssor, Department of Prosthodontics. Propaedeutics, tions, only very limited information on this is con-
and Dentai Materiais. School of Dentistry, Christian-Aibrechts Uni- tained in the literature. In a recent iaboratory
versity, Kiel, Germany.
study,^3 the resin bond strength to YPSZ was evaiu-
Professor and Chairman. Department of Prosthodontics, Pro- ated after 1 week water storage, and an acceptable
paedeutics, and Dentai Materiais, Schooi of Dentistry, Christian-AI-
brechts University, Kiel, Germany. resin bond strength to siianized YPSZ ceramic was
found. Based on these results, the authors con-
cluded that with air abrasion and silanization, a
Reprint requests: Dr. Stefan M. Wegner. Department of Prosthodon-good and hydrolyticaiiy stabie bond to YPSZ ce-
tics, Propaedeutics, and Dentai Materiais, School of Dentistry. Chris- ramic can be obtained. In another in vitro study,
tian-Aibrechts University, Arnoid-Heiler-Str. 16. D-24105 Kiel, several methods of bonding to YPSZ ceramic have
Germany. Fax: +49-431-597-2860, e-mail: swegner@proth.uni-kiel.de

Vol 2, No 2, 2000 139

Wegner/Kern

Table 1 List of materials used

System Component Batch No Manufacturer

Clearfil F2 Base paste 0233 Kuraray, Osaka, Japan

Catalyst paste 0133
Dyract Cem Base powder 9510181 DeTrey/Dentsply,
Cataiyst liquid 9510133 Konstanz, Germany
Atrbiock 9505111
Kevioc Kevioc Primer 28 Heraeus Kuizer,
Kevioc Bond 23 Wehrheim, Germany
Panavia Base povjder PN I l l s Kuraray, Osaka, Japan
Catalyst liquid 2220
Oxyguard 0541
Panavia 21 Base paste 0208 Kurgray Osaka, Japan
Catalyst paste 0180
Oxyguard i i 0118
Rocatec Roca tec Pre 0055 Espe, Seefeld, Germany
Rocatec Plus 0176
Espe-Sii 0063
Twiniook Estiseal LC 56 Heraeus Kuizer,
Base paste 42 Wehrheim, Germany
Catalyst paste 42

aiso been tested,^^ After water storage of up to 150
days with thermocyciing, some bonding methods
faiied completeiy, while others showed only a de-
creased or even an unchanged bond strength. How-
ever, the siianization of YPSZ ceramic resulted in a
resin bond which faiied during water storage of 150
days. This result questions the conclusion men-
tioned above, which was based on only 1 week of
water storage. To the knowiedge of the authors,
however, there are no longer-term data currently
available on the durability ofthe resin bond to YPSZ
ceramic exceeding 150 days of water storage.
Therefore, the purpose of this study was to evaiu-
ate the long-term bond durabiiity to YPSZ ceramic
with a storage time of two years and to investigate
the bond failure modes by SEM characterization.
MATERIALS AND METHODS
Industrially manufactured yttrium-oxide-partially-
stabilized zirconia ceramic disks (94,9% ZrO2Stabi-
iized by 5 , 1 % Y2O3, BCE Special Ceramics,
Karlsruhe, Germany) with a diameter of 7.0 mm and
a thickness of 3,4 mm were used for this study. Ail
samples were air abraded with 110-pm AI2O3 at 2,5
bars pressure (13 s) at a distance of 10 mm and
then ultrasonically cleaned in isopropanol for 3
min.
Seven different bonding systems were used. The
materiais utilized and their characteristics are
listed in Table 1, In group T, a dual-curing conven-
t i o n a l bis-GMA l u t i n g composite (Adhesive
Bond/Twinlook) was applied directly to the air-
abraded ceramic surface. In group ST, the ceramic
surface was silanized (Espe-Si!, 3-methacryloy-
loxypropyi trimethoxysiiane in isopropanol) prior to
the application o f t h e conventional bis-GMA com-
posite. In group RT, the ceramic surface was tribo-
chemically silica coated (Rocatec system) prior to
the application of the silane (Espe-Sii] and the bis-
GMA composite, in group KT, an acrylonitrile iayer
was fused to the ceramic surface (Kevioc oven
method] prior to the application of the bis-GMA
composite. In group P, a chemicaliy cured resin
composite modified with phosphate monomer {10-
methacryloyloxydecyi dihydrogenphosphate, MDP)
(Panavia EX) was appiied directly to the air-abraded
ceramic surface. In group P21, another chemically
cured resin composite modified with MDP (Panavia

140 The Journal of Adhesive Dentistry


2 1 EX) was applied directly to the air-abraded ce-
ramic surface. In group D, a chemicaily cured poly-
acid-modified resin composite (Dyract Cem) was
used directly on the air-abraded ceramic surface.
Plexiglas tubes (inner diameter 3.3 mm) were
fiiled with self-curing resin composite Clearfil F2.
After 8 min, these tubes were bonded with the cho-
sen resin to the YPSZ samples using an alignment
apparatus. The alignment apparatus consists of
parallel guides, the tube holder, a siiicone pad, and
an added weight of 750 g. The apparatus ensured
that the tube axis was perpendicular to the sample
surface. The bonding method has been described
in detaii previously.^^
Excess resin was removed from the bonding mar-
gin using cotton pellets, and an oxygen-blocking gel
was applied (Airblock, DeTrey, with Twinlook and
Dyract Cem; Oxyguard, Kuraray, with Panavia and
Panavia 21). After 7 min, ail sampies were light
cured from two sides, 180 degrees apart, for 30 s
with a dental curing light (Heliomat, Vivadent,
Schaan, Lichtenstein), then further cured in a
xenon strobe light-curing unit (Dentacolor XS, Her-
aeus-Kulzer, Wehrheim, Germany) for an additional
90 s. Samples employing the chemically cured resin
were also subjected to the light-curing step, as this
applies some heat to the samples. In this manner,
all samples were subjected to similar curing condi-
tions.
Each bonding group with a total of 16 samples
was divided into two subgroups (each with eight
samples] with the foiiowing storage times and ther-
mal cycles (TC) between 5°C and 55°C: 3 days with
nc TC, and 2 years with 37,500 TC. Sampies were
stored in distilled water at 37"C,
The tensile bond strength test was performed at
a crosshead speed of 2 mm per min in a tensiie
tester (Zwick, Ulm, Germany) using a speciai test
configuration, which provides a moment-free axial
force application. A coilet held the tube while an
alignment jig allowed self-centering of the sample.
The jig was attached to the load cell and crosshead
by upper and lower chains, allowing the whole sys-
tem to self-align.
Statistical analyses of the test results were con-
ducted with the Kruskal-Wallis test followed by mul-
tiple pair-wise comparisons of the means using the
Wilcoxon rank sum test for independent sampies.i^
Significance ievels were adjusted with the Bonfer-
roni-Holm correction for multiple testing.^ Nonpara-
metric statisticai test procedures were used for
group comparisons, because Bartiett's test showed
Vol2,No2, 2000
Wegner/Kern
inhomogeneity of variances between groups, and
the data were found to be non-normaliy
distributed.19
The fractured interfaces on the YPSZ samples
were examined under a light microscope at 30X
magnification to calcuiate the debonded area as-
signed to adhesive and cohesive failure modes.
Representative sampies were examined using a
scanning electron microscope (Phiilips XL30,
Einthoven, Netherlands) with an acceieration voit-
age of 15 keV and a working distance of 10 mm,
after sputtering using a goid-alloy conductive layer
of approximateiy 30 nm.
RESULTS
The tensile bond strength vaiues are summarized in
Fig 1 for all seven bonding groups and the two stor-
age conditions. Statistically significant differences
between the bonding groups are shown in Tabie 2,
while the statisticaiiy significant differences be-
tween the storage times are shown in Table 3.
The bond strength of the bis-GMA resin compos-
ite to air-abraded or air-abraded and siianized YPSZ
(groups T, ST) was initiaiiy relatively low with means
of 14.2 MPa and 13.9 MPa, respectiveiy. During the
2-year storage time with 37,500 thermal cycles, ail
samples of these two groups debonded sponta-
neously.
Tribochemical silica coating of the air-abraded
ceramic (group RT) increased the bond strength of
bis-GMA resin composite significantly to 29.0 MPa,
However, the bond strength decreased significantly
duringthe storage time to 15.8 MPa.
Acrylizing the air-abraded ceramic (group KT) re-
suited in an initially higher bond strength (mean
37,9 MPa) than did silica coating. However, during
the 2-year storage time with 37,500 thermal cycles,
all samples of group KT debonded spontaneously.
The use cf phosphate-modified bis-GMA resin
composite with air-abraded ceramic (groups P and
P21) resulted in the highest bond strength values to
YPSZ after 3 days (means: 49,7 and 46.0 for P and
P21, resp.) and 2 years (means: 39,8 and 44,2 for
P and P21, resp.). Aithough the bond strength of
groups P and P21 decreased siightly over 2 years,
this decrease was not statistically significant. Fur-
ther, there was no statistically significant difference
between the bond strength of groups P and P21.
Using the chemically cured poiyacid-modified
composite on air-abraded ceramic (group D), a rela-
141
Wegner/Kern

Fig 1 Mean bond strength

values of the test bonding
systems and the two stor-
age conditions ( X / l " 3 days
no thermal cycling; X/2 = 2
years with 37,500 thermal
cycles).

Table 2 Statistically significant differences between bonding groups

at te5ted storage times

STATiSTiCAL COMPARISON STORAGE TIME

3 days 2 years
lOTCj (37,500 TC¡

T-ST N,S, fJ,S.

T-RT
T-KT " N.S.
T-R **
T-P21
T-D
ST-RT " ..
ST-KT n M,S,
ST-P tt t»

ST - P21 »* •*

ST-D «*

RT-KT *

RT-P ••

RT - P21 *«

RT-D N.S, **

KT-P *
KT-P21 N.S. **

KT-D N.S. **

P-P21 N.S. N,S,

P-D **
P21-D ** **

Global KRUSKAL.WALLIS rest followed by pairwise comparison using tlie WILCOXON test modified by BON-
FEfiONI-HOLM;
-p<0,05;N,S,:p>O05
- • psO.Ol

142 The Journal of Adhesive Dentistry

 Wegner/Kern

Table 3 Statistically significant differences between the bond

strength at different storage times within the same bonding group

3 days vs 2 years

T
ST
RT
KT
P N,S,
P21 N,S,
D

GloCial KRUSKAL-WALLIS test followed by comoarison usmg tlie WILCOXOM test modified By BON-
FERONI-HOLM.
• D50.05;N.S.: p> 0.05,
" p s 0.01.

90%

80%

70% -

60% -
• adhesive
50%
Ö cohesive
40% -

30%

20% - —

10% -
.--Í
D/2
D/1
P/2
RT/2

P/1
KT/1
RT/1

KT/2

P21/1
ST/2

P21/2
T/1

ST/1
T/2

Fig 2 Mean percentages of areas assigned to the failure modes obsewed in the seven bonding groups after different storage
times.

tively high bond strength to YPSZ was noted after 3
days, but it decreased statisticaily significantiy over
2 years of storage with 37,500 thermai cycles to
merely 3.1 MPa,
The distribution of two types of failure modes for
all samples is shown in Fig 2. After 2 years of stor-
age with thermocyciing, the failure mode was purely
adhesive for all samples in the bonding groups T,
ST, KT, and D. The failure mode was exciusively co-
hesive for the groups P and P21, However, after the
2-year storage period with thermocycling, the failure
mode was mixed for samples of group RT, where a
mean of 80% of the bonding area failed adhesively.
Figures 3 to 6 show representative SEM pho-
tographs of the fracture interfaces after the tensile
test following 3 days or 2 years storage time with
37,500 thermai cycles.

143
Vol 2, No 2, 2000
Wegner/Kern

Fig 3 SEM photograph of air-abraded YPSZ disk (onginai Fig 4a Sample of group RT after 3 days' water storage show-
magnification lOOOX, white bar = 20 Mm). ing a mixed faiiure mode (SEM photograph, original magnifi-
cation 75X, white bar = 200 um).

Fig 4b Sampie of group RT after 3 days' watei stotage show- Fig 4c Sample of group RT after 2 years/37,500 thermal cy-
ing a mainly adhosiveiy debonded area of the specimen with cies, sdhesiveiy debonded area of the specimen (SEM photo-
remains of the resin composite (SEM photograph, original graph, originai magnification lOOOX, white bar = 20 pm).
magnification lOOOX, white bar = 20 um).

Fig 5a Sair.iîic of group KT after 3 d¿ys '.víilür storage show- Fig 5b Sample of group KT after 2 yesrs/37,500 thermai cy-
ing a totally cohesive failure mode. Note that the ceramic sur- cles demonstrating a change in failure mode during storage
face is covered with a relatively smooth acryi coating from totaiiy cohesive (compare Fig 5a) to totaiiy adhesive
indicating a faiiure between the bonding interface (SEM pho- (SEM photograph, original magnification lOOOX, white bar =
tograph, original magnifioation lOOOX, white bar = 20 ) 20 Mm).

144 The Journal of Adhesive Dentistry

 Fig 6a Sampie or grojp w:. ji:.ci 2 years/37,5C0 thermal
cycles sliovjing cohesive failure of the resin composite (SEM
photograph, original magnification 75X, white bar = 200 ym).
DISCUSSION
As the resuits of this study have shown, it was not
possibie to achieve a stabie, iong-term bond using a
conventional bis-GMA resin composite. Groups T
and ST showed mid-range bond strengths initially,
and group KT high initial bond strengths. However,
the samples of all three groups debonded during
long-term storage, indicating an unstabie physicai
and chemicai bond o f t h e conventional bis-GMA
resin composite to YPSZ ceramic. It is possibie that,
although air abrading the YPSZ ceramic produces a
certain roughness, it creates only limited or even no
undercuts compared to air-abraded metal. This may
be the explanation for the differences of reported
bond strengths to dental alloys, where the bond
strength decreased over time, but remained at a
level of severai MPa.iO'i^.i? However, these results
are simiiar to those of previous studies on bonding
to glass-infiltrated alumina ceramic and pure alu-
mina ceramic, which also found unstable bonds of
bis-GMA resin composite to air-abraded alumina ce-
ra m ic.^i
Further, as already shown in a previous study,^^
silane improved neither the durability nor the stabii-
ity of the bond to YPSZ ceramic. This indicates that
silane cannot bond to YPSZ due to the missing sii-
ica phase of this oxide ceramic, in conventional
dental ceramics, it is thought that silane bonding is
mediated t h r o u g h the silica at the ceramic
surface,^1 These results differ from those of an ear-
Voi 2, No 2, 2000
Fig 6b Sair,pie Ù1 group P21 af;ei 2 je«.^, j,,üOi.' t,-.crmal
cycies at high magnification showing biank squares indicating
torn filler particies of the resin composite (SEM photograph,
original magnification lOOOX, white bar - 20 pm).
iier study in which the combination of siiane and a
bis-GMA resin composite was suggested to achieve
a proper bond to YPSZ,23 However, this study inves-
tigated the influence of water storage for a period
not exceeding 1 week and inciuded an additional
storage period of 24 h in boiiing water,
Acrylizstion of the YPSZ surfaces did enhance
the bond strength of the conventionai bis-GMA
resin composite, but it, too, did not prove to be sta-
bie over the 2 years' storage with 37,500 thermai
cycies. This mirrors results with acrylized nickel-
chromium alioy,^ The breakdown in bond strength
of group KT after 2 years of storage was associated
with the change in fracture mode from cohesive
within the acrylonitriie layer to compieteiy adhesive
at the ceramic surface. This indicates that the bond
of the acryionitrile layer to YPSZ is dissolved by
long-term water ingress.
Unlike groups T, ST, and KT, where the samples
debonded spontaneousiy over storage time, the tri-
bochemical silica coating of samples in group RT re-
suited in a significant increase in the initiai bond
strength ofthe conventionai bis-GMA resin compos-
ite to YPSZ ceramic. Nevertheless, the resin bond
strength decreased statisticaiiy significantly to 15,8
MPa over 2 years of storage time. This is in contrast
to the high and durable resin bond strength ob-
tained to tribochemically silica-coated glass-infil-
trated alumina ceramic, which was 50 MPa after
150 days of water storage with thermocycling,ii
However, compared to another study over 150 days
145
Wean er/Kern
of water storage,^^ the iong-term water storage over
2 years did not cause any further decrease in bond
strength to siiica-coated and siianized YPSZ ce-
ramic.
In contrast to the conventional bis-GMA resin
composite, the bond strengths of the MDP-contain-
ing resin composites (group P and P21) were statis-
ticaiiy significantly higher, due to this active
monomer. Although a slight decrease in bond
strength over the 2-year storage period was ob-
served, it was not statistically significant. Since a
compieteiy cohesive failure mode was found for
both the 3-day and 2-year samples, this decrease in
bond strength is related to the degradation of the
resin itseif, which has been shown previously in
other resins.2o As already shown for glass-infiltrated
aiumina ceramic,"'•^i the resuits of this study
demonstrate that MDP promotes a water-resistant
chemicai bond to YPSZ ceramic. The phosphate
ester group of the monomer is reported to bond di-
rectly to metai oxides,^'i and the data of the current
and cited studies suggest that MDP bonds chemi-
cally to both aluminum and zirconium oxides. Com-
pared to the earlier study,i3 there is also no
obvious change in bond strength between storage
times of 150 days and 2 years, each with 37,500
thermal cycles.
As was the case with the conventional bis-GMA
composite resin, the chemicaiiy cured poiyacid-
modified resin composite (group D) initially showed
a relatively high bond strength to air-abraded YPSZ
which decreased statistically significantly over 2
years' storage time with 37,500 thermal cycles to
only 3 , 1 MPa. This dramatic change in bond
strength was accompanied by a change In the faii-
ure mode from mainly cohesive to compieteiy adhe-
sive. According to the manufacturer's description,
the poiyacid-modified composite contains two adhe-
sive monomers (macromonomer M-IA-BSA and
aminopenta). This study shows, however, that the
addition of these adhesive monomers did not result
in a water-resistant chemical bond to YPSZ ceramic.
Given the present results, the need for long-term
investigations regarding the bond strength of dental
composite resins to restorative materials is evident.
In summary, after 2 years' storage with thermocy-
ciing, only the two resin composites containing
phosphate monomers did not exhibit a statistically
significant decrease in bond strength to air-abraded
YPSZ as compared with the initial values after 3
days. Therefore, only these methods can currently
be recommended for clinical use.
146
CONCLUSION
This study implicates that only the use of bonding
systems which contain the adhesive monomer MDP
results in acceptably high-strength, stable bonds to
air-abraded YPSZ. Siiane, siiica coating, acrylization
in combination with a conventionai bis-GMA resin,
and the modified resin Dyract Cem did not result in
a durable resin bond to YPSZ.
ACKNOWLEDGMENTS
The authors wish to thank Espe {Seefeld, Germany). Hcracus Kulzcr
(Wehrheiin, Germany), Dciitsply/DeTrey (Konstanz, Germany), and
Kuraray (Osaka, Japan) for providing materials and equipment.
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Proceedings of the International Symposium on Adhesive it requires a mixture of scientific and artistic
Prosthodontics, 24 June 1986, Amsterdam, Netherlands, skills. In this book the author offers one pathway
Chicago; Academy of Dental M ate rials, 1986 ;9-18, based on scientific principles to master the art of
25, Wohlwend A, Studer S , Schärer P, Das Zirkondioxidabutment constructing a complete denture.
- ein neues Konzept zur ästhetischen Verbesserung der
SupraStruktur in der Implantoiogie. Quintessenz Zahntech
1996;22:364-381.
1, Identifying the Problem
26, Vanagida H, Kawamoto K, Miyayama M, Chemistry of Ceram-
2, Impressions for Study Casts
ics, Chichester; Wiley, 1996:225-228,247-249,
3, Master Casts
4, Selecting Maxillary Anterior Teeth
5, Recording the Maxiilomandibular Relationship
and Arranging the Maxillary Anterior Teeth
6, Arranging the Mandibular Anterior Teeth and All
of the Posterior Teeth
7, Clinical Evaluation of cheTeeth in Wax
8, Processing Acr/lic Resin
9, Adjustment and Insertion of the Dentures
10, Relining a Complete Denture
11, Immediate Dentures
12, Implant Overdenture
Appendix I, The Complete Denture;
A Step-by-Step Summary
Appendix II, Living with Your Complete Dentures

i36 pp (¡piral binding]; 320 illus: ISBN 0-367 '5-ÍÍ0-4; US $48/£30

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