Effects of repeated processing on the

strength and microstructure of

a heat-pressed dental ceramic
Catherine M. Gorman, MSc,a Kate Horgan, BDentSc,b
Ruth P. Dollard, BSc, MSc,c and
Kenneth T. Stanton, BSc, MSc, PhD, CEngd
Dublin Dental University School and Hospital, Dublin, Ireland; University Dental School and Hospital, University College Cork, Wilton,
Cork, Ireland; University College Dublin, Dublin, Ireland
Statement of problem. The excess material produced after heat pressing a lithium disilicate glass ceramic restoration can
be either discarded or reused. The reuse of this material requires that any degradation of the material quality be
investigated.
Purpose. The purpose of this study was to investigate the number of times that leftover lithium disilicate material can be
re-pressed and to determine the effect that repeated use has on material properties.
Material and methods. A large (6.1 g) lithium disilicate ingot (A3.5) was heat pressed to yield a ceramic disk (15
1.5 mm)
for testing. The leftover material was reused to produce a further 3 disks, with the number of pressings increasing for each
specimen. An additional unpressed group was included to investigate the properties before pressing so that, in total, 5 groups
were established. Specimens were tested for biaxial exural strength, Vickers hardness, and fracture toughness. X-ray
diffraction was used to characterize the crystalline phase, scanning electron microscopy for the microstructure, and
differential scanning calorimetry for the thermal properties.
Results. No signicant difference was found in the biaxial exural strength of the groups. The hardness of the material
decreased, and no signicant difference was seen in fracture toughness with repeated pressings. An increase in grain size was
observed with increased pressings. By using x-ray diffraction analysis, lithium disilicate was identied as the main crystal
phase, and no difference in crystalline composition was found with repeated processing.
Conclusion. This material can be reused while maintaining good mechanical properties and without signicantly altering
the chemical or crystalline composition in an adverse manner. (J Prosthet Dent 2014;112:1370-1376)

Clinical Implications
This study showed that heat-pressed lithium disilicate can be reused up to 4
times. Routine mechanical strength tests revealed no adverse consequences
for lithium disilicate when it is reused and that dental laboratories may be
routinely and unnecessarily discarding excess material.
Heat pressing of glass ceramic materials for dental applications is a
proven method of fabricating xed
prosthodontic restorations.1-20 These
restorations are translucent because of
the absence of a metal substructure

and thus offer an excellent opportunity

for achieving life-like esthetic restorations. IPS Empress was the original
heat-pressed glass ceramic and leucite
(SiO2, Al2O3, 4K2O) is the main crystalline phase in this system.4,5 IPS

Empress 2 has lithium disilicate

(Li2O$2SiO2) as its main crystalline
phase and is 60% crystalline when
processed (Ivoclar Vivadent, IPS
Empress 2 Scientic Documentation,
1998). It offers higher strength, which

Assistant Professor, Division of Restorative Dentistry and Periodontology, Dublin Dental University School and Hospital.
Graduate student, Department of Restorative Dentistry, University Dental School and Hospital, University College Cork.
c
Graduate student, School of Mechanical and Materials Engineering, University College Dublin.
d
Senior Lecturer, School of Mechanical and Materials Engineering, University College Dublin.
b

The Journal of Prosthetic Dentistry

Gorman et al

December 2014
extends its recommended use to short
span partial xed dental prostheses. IPS
e.max Press material has now replaced
IPS Empress 2; it has improved mechanical properties and has signicantly higher translucency (Ivoclar
Vivadent, IPS e.max Press Scientic
Documentation, 2011). The microstructure consists of 70% lithium disilicate crystals embedded in a glassy
matrix. These crystals are acicular in
morphology and measure 3 to 6 mm in
length. Recommendations for its clinical use remain unchanged. IPS e.max
Press is available in 4 different levels of
opacity and/or translucency, the selection of which is determined by the requirements of the individual clinical
treatment. It is supplied for heat
pressing in 2 sizes, a small ingot that
weighs 3.2 g or a larger ingot that
weighs 6.1 g. It is more economical to
press several restorations from 1 ingot
at the same time. However, this often is
not possible and may result in a
considerable amount of leftover material. The issue is thereby raised whether
the leftover material should be discarded or reused. Concerns as to the
mechanical properties of the reused
material for clinical use are valid.
Extensive research into the mechanical properties and clinical performance
of heat-pressed glass ceramics has been
carried out over the past 2 decades.1-20
In spite of this, only 2 studies that
examined the mechanical and microstructural properties of re-pressed ceramics were identied by the present
authors.19,20 In the rst of these
studies, the re-pressing of both IPS
Empress and IPS Empress 2 was evaluated.19 The biaxial exural strength
(BFS) of the pressed and re-pressed
materials was unchanged, although a
higher scatter of the data was reported
for the re-pressed material. Weibull
analysis of the data indicated that there
was less reliability when the material
was re-pressed. X-ray diffraction (XRD)
revealed no differences in crystalline
phase assemblage or x-ray reection
intensities with re-pressing. Scanning
electron microscopy (SEM) revealed
larger crystals for the re-pressed IPS

Gorman et al

1371
Empress 2; this was attributed to Ostwald ripening, whereby larger crystals
grow at the expense of smaller ones.
The conclusion was that re-pressing the
material did not result in lower mechanical properties; however, the
greater scatter may predict a reduction
in reliability for the materials. In the
second study, a signicant difference in
BFS was observed for re-pressed IPS
Empress 2.20 These studies show
promising results and give good insight
into re-pressed materials. However,
studies have only tested a single reuse
of the material, whereas, in practice, it
could be reused several times, depending on the amount of material left over.
The null hypothesis of the present study
is that IPS e.max Press can be reused
without adversely affecting its mechanical properties.

MATERIAL AND METHODS

The aim of the current study was to
investigate the reuse of IPS e.max Press.
This was carried out by using the
maximum amount of pressings obtainable from the largest commercially
available ingot while preparing specimens suitable for biaxial exural
testing. Information regarding the exural strength, hardness, and indentation fracture toughness was evaluated.
The composition and microstructure of
the reused material also was studied to
evaluate changes that may have
occurred. One lithium disilicate ingot
(IPS e.max Press; Ivoclar Vivadent AG)
was selected for testing before pressing
(group 0). Ten ingots (6.1 g each) were
then pressed to give 10 disks (15
1.5
mm) for testing BFS (group 1). The
leftover material was recovered for
reuse to produce a further 3 disks
(groups 2, 3, and 4; the number corresponds to the number of pressings).
Thus, each ingot was pressed 4 times,
and 4 groups were established for
biaxial testing (n10), Vickers hardness
(n5), and fracture toughness (n5).
By using the Mead resource equation,21
a minimum sample size of 5 was
deemed adequate for the statistical
validity of all tests.

The specimens were ground at on

both sides by using 180-grit silicon
carbide (SiC) paper (Buehler-Met) and
were measured with a digital caliper
(Milomex Ltd) for parallelism to 0.05
mm, and the thickness (h) of each
specimen was recorded. A standard test
method was used for testing the BFS of
the disks.22 The disk was placed on the
support ring of the testing device, and
clear adhesive tape was placed on the
compressive surface before the loading
ring was applied. A thin piece of
nonrigid material (polyethylene lm)
was placed between the loading ring
and the disk. A force was applied to the
device with a tensometer (Tinius Olsen
H10KS; Tinius Olsen Ltd) at a rate of
0.75 mm/min in compressive mode
until the material failed. A 10-kN load
cell was used with a load range of 50%.
The load at failure was recorded for
each disk, and the fragments were
collected for further analysis. Ten
specimens were tested for each group.
The BFS was calculated for each specimen by using the following equation.22


3F
D2  D2
sf 2 1  v S 2 L
2ph
2D

DS
;
1 vln
DL
where sf is the maximum tensile stress
(MPa), F is the total load causing
fracture (N), h is the specimen thickness
at fracture origin (mm), v is the Poisson
ratio (taken here to be 0.23), DL is the
radius of the load ring (3 mm), DS is the
radius of the support ring (6 mm),
and D is the radius of the specimen
(7.5 mm).
Fragments of broken disks from
exural testing were retrieved and
further prepared for Vickers hardness
and indentation fracture toughness
testing. Specimens were cold mounted
in an acrylic resin and serially wet
ground with 300, 600, 1200, and 4000grade SiC paper. The specimens were
nally polished with 1-mm diamond
paste. A Vickers diamond indenter
(Mitutoyo AVK e C2 Hardness Tester;
Mitutoyo America Corp) was used to
create an indent under a load of 49 N.

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Volume 112 Issue 6

Table I.

Summary of mechanical properties for groups 0-4

BFS, MPa
Hardness, Hv/5
KIc, MPa.m

0.5a

Group 0

Group 1

Group 2

Group 3

Group 4

10

n/a

243.4 45.9

252.7 23.7

225.06 35.3

214.8 45.9

.137

585.2 6.42

548.8 28.68

559.4 8.68

526.4 49.13

547.6 13.39

.99

0.29 0

1.13 0.02

1.01 0.13

1.05 0.04

1.09 0.05

<.001

n/a, not available; BFS, biaxial exural strength; Hv, Vickers hardness; KIc, fracture toughness.
a
If group 0 is omitted, then there was no statistically signicant variation in fracture toughness (P>.05).

The 2 indentation diagonals d1 and d2

created in the material were measured
with the microscope on the hardness
tester, and a mean was calculated.23
The Vickers hardness value was determined according to the following:

250

Biaxial Flexural
Strength (MPa)

Hv

300

2F sin 136e
F
2
z1:854 2 ;
d
d2

where Hv is the Vickers hardness in

kgf.mm2, F the load applied in kg, and
d the arithmetic mean of the 2 diagonals, d1 and d2 in mm.
The length of radial cracks produced as a result of indents made in the
material were measured, and the
indentation fracture toughness (KIc)
was calculated by using the following
equation24:
!
P
KIc jb 3 ;
co2
where Jb 1/ (p3/2 tan J) and J is
the half angle of the Vickers indenter
(68 degrees), P is the indentation load
in MN, and co is the radial crack length
in meters.
XRD was carried out for each of the
specimen groups. Specimens were
placed in the holder of a diffractometer
(Diffraktometer D500; Siemens) and
scanned with Cu Ka x-rays between 10
and 70 degrees 2q with a step size of 0.02
degrees and a 2-second step interval.
JCPDS card no. 40-0376 was used to
identify the lithium disilicate phase.
In preparation for SEM, specimens
were cleaned, etched with 2% hydrouoric acid for 90 seconds, and then
dropped immediately into a water bath
for 15 seconds. Specimens were further
cleaned with isopropyl alcohol and
acetone. Finally, the specimens were

200
150
100
50
0

Press Number
1 Biaxial exural strength for IPS e.max Press groups 0-4
with 95% condence intervals.
dried and sputter coated with gold.
SEM (Quanta 3D FEG DualBeam) was
used to examine the surface topography
of the specimens; it also served as a
means of assessing a change in the
grain width or length within the specimens after re-pressing. Grains were
arbitrarily selected (n10) from 1
micrograph for each pressing, and the
width and length of each selected grain
was recorded.25 Optical microscopy
(Leica DFC320) also was performed to
assess indentations on the specimens.
Differential scanning calorimetry
(Stanton-Redcroft STA 1500; Rheometric Scientic) was carried out for
each group in a owing nitrogen atmosphere; the specimens were placed
in matched platinum-rhodium crucibles
and heated to 1200 C at 10 C/min
and cooled at 10 C/min until a temperature of 25 C was reached. Where
applicable, the results were statistically
analyzed with 1-way ANOVA (a.05).

RESULTS
The results of mechanical testing
are presented in Table I. No BFS

The Journal of Prosthetic Dentistry

measurements were available for group

0 because specimens could not be made
to the required specications for testing
without processing. BFS appears to
decrease slightly with an increased
number of pressings (Fig. 1). However,
this decrease was not found to be signicant (P.137). Quite a large scatter
in the data was found for group 1
(144.29-309.74 MPa) and for group 4
(114.41-260.79 MPa). The fracture
toughness data for each group are presented in Figure 2. The KIc of group 0 was
signicantly lower than the other groups,
with a measured value of 0.29 MPa.m0.5,
although the material was not engineered to be used in this condition. The
fracture toughness determined for all
other groups was between 1.13 and 1.01
MPa.m0.5 with no statistically signicant
variation. For group 0, the scatter in the
data was found to be remarkably low
compared with the pressed groups.
Hardness values were found to be in the
range of 550 to 600 Hv/5 (Fig. 3) and did
not change signicantly with the number
of pressings.
With XRD, lithium disilicate was
identied to be the main crystalline

Gorman et al

December 2014

1373
mm mean length and 0.19 mm mean

Fracture Toughness
(MPa.m0.5)

1.4

width were apparent for group 0,

whereas average grain sizes of 4.19 mm
mean length and 0.69 mm mean width
were apparent for group 4. Overall, a
systematic grain growth was evident
with an increased number of pressings
(see Fig. 5A-E). Also evident in the
microstructure were secondary crystals
that appeared to grow directly from the
primary crystals: a higher magnication
image of an etched group 2 specimen is
presented in Figure 5F. The results of
DSC showed an endotherm that
occurred at 960 C for all 5 groups (see
Fig. 6 for a representative curve). This
endotherm indicates melting of the
material and no difference in the traces
for any of the groups.

1.2
1
0.8
0.6
0.4
0.2
0

Press 1

Press 2

Press 3

Press 4

Press Number

Hardness (Hv/5)

2 Fracture toughness for IPS e.max Press groups 1-4

with 95% condence intervals.
700
600
500
400
300

DISCUSSION

200
100
0

Group Number

Intensity (arb.)

3 Hardness for IPS e.max Press groups 0-4 with 95%

condence intervals.

10

20

30

40

50

60

70

Degrees 2
4 X-ray diffraction data for groups 0-4 exhibiting peaks at
2q values of 24.19 degrees, 24.74 degrees and 46.54 degrees. Note difference between group 0 and that of other
groups.
phase. The dominant peaks present for
groups 1 to 4 are shown in Figure 4.
The major peaks for lithium disilicate
(Li2Si2O5) were observed at 2q values of
24.74 degrees, 24.19 degrees, and
46.54 degrees. The dominant peak was
at 24.74 degrees, which corresponds to
the (040) crystallographic plane of this
monoclinic phase. The XRD data

Gorman et al

showed that, after repeated pressings,

the crystalline phase assemblage did
not change. SEM images for all groups
are given in Figure 5. The complexity of
the grain structure made it difcult to
perform reliably accurate measurements of grain sizes or to otherwise
quantify aspects of the microstructure.
However, average grain sizes of 1.47

The null hypothesis that IPS e.max

Press can be reused without adversely
affecting its mechanical properties was
accepted. The results indicated the potential to re-press lithium disilicate
glass ceramic several times and was
only practically limited by the size of the
ingots. However, the handling characteristics of the material were observed
to decline somewhat by the denitive
pressing (group 4). This manifested itself with the material becoming more
brittle; for example, care was required
when cutting off sprues. To compare
the exural strengths with those in
the literature, group 1 results were
considered because this corresponds to
the manufacturers recommendations.
The mean  SD BFS for this group was
243.4 45.8 MPa, lower than those
values reported by the manufacturer or
in other studies.13,14 The surface nish
(180-grit SiC paper) may be responsible
for this because exural strength measurements have been shown to depend
on the surface nish.26-28 In addition,
residual stresses are normally present as
a result of manufacturing processes,
which can lead to the reporting of
articial mechanical properties. The
annealing of specimens can relieve
these residual stresses, which results in
more reliable mechanical data.28 The

1374

Volume 112 Issue 6

5 Scanning electron microscopy images for IPS e.max Press. A, Group 0. B, Group 1. C, Group 2. D, Group 3. E, Group 4.
Growth in grain size is evident from group 0 to group 4. F, Shows group 2 with increased magnication. Note increase in
secondary crystals present. This is due to partial dissolution of crystals at 960 C.

test method here (ASTM 1499-05) used

a ring-on-ring testing device.22 This requires specimens to be parallel to
within 0.05 mm for the test to produce
valid results. Accurate parallelism of the
ceramic disk was ensured in this study
with careful measurement of the height
at 3 intervals around the disk. A greater
specimen number would permit a
calculation of the probability of failure

(Weibull modulus), information that

could be valuable in further determining the clinical viability of reusing
this material several times over.
Flexural strength values were shown
to decrease slightly with an increased
number of pressings; however, the difference was not found to be signicant.
The specimen number (n10) may
have been too small to show

The Journal of Prosthetic Dentistry

signicance within the context of the

normal experimental variability that
would be expected with this technique.
The hardness of the material was not
shown to vary signicantly with
increased pressings (526.4-585.2 Hv/5,
equivalent of 5162-5739 MPa). Fracture toughness was not found to vary
signicantly with increased pressings,
and the values obtained here were for

Gorman et al

Heat Flow (mw/mg)

December 2014

1375

1.1
1.2
1.3
1.4
1.5
1.6
1.7
1.8
500

600

700

800

900

1000

Temperature (degrees C)
6 Representative differential scanning calorimetry for
IPS e.max Press group 3 showing dissolution at 960 C.
comparative purposes only. Because of
the indentation method selected to
measure this property, comparing the
results with absolute values determined
by other means in the literature is
inadvisable.
XRD revealed that lithium disilicate
was present in all the groups, and no
difference existed among the patterns for
each group. Observations of the scanning electron micrographs indicated an
increase in crystal grain growth at the
expense of smaller crystals. This nding
is in agreement with another study,
which found that Ostwald ripening
occurred when the material was reused
once.19 The current study indicated that
grain growth occurs and has an
approximately linear relationship with
an increased number of pressings.
SEM revealed not only the expected
primary lithium disilicate crystals (as
conrmed by XRD) but also secondary
crystals, which appeared in greater
numbers with an increased number of
press cycles. In other systems, such secondary crystals may be due to the
nucleation of polymorphs of the primary
crystal type.29 In the present study, no
additional phases were seen with
increased pressings from XRD, whereas
the number of secondary crystals did
appear to increase with the number of
pressings. Therefore, the secondary
crystals are likely to be due to recrystallization of the crystals after they either
partially melt or partially dissolve in the
residual glass phase during the process
cycle. The DSC trace (Fig. 6) showed
that the melting endotherm begins at

Gorman et al

approximately 850 C, and, when

considering that the processing temperature during pressing is 920 C, the likelihood that the secondary crystals are the
outcome of recrystallization is increased:
indeed, the initial melting is almost
certainly necessary to enable pressing in
the rst instance.

CONCLUSIONS
The optimum properties for IPS
e.max Press are probably obtained with
the rst pressing. However, no material
mechanical properties appear to vary
signicantly with subsequent pressings.
Although results of this study determined that reusing the material is
possible, the authors did notice some
qualitative differences in specimen
handling with increased reuse (up to 4
times). As such, conclusive support is
not possible for its reuse to this extent.

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2. Gorman CM, McDevitt WE, Hill RG. Comparison of two heat-pressed all-ceramic
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ceramic systems. J Dent 1999;27:183-96.
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6. Hland W, Schweiger M, Frank M,

Rheinberger V. A comparison of the microstructure and properties of the IPS Empress 2
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7. Kheradmandan S, Koutayas SO, Bernhard M,
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Sci Mater Med 1998;9:555-9.
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strength and indentation fracture toughness
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exural strength, elastic moduli, and x-ray
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Swain MV. Strength, fracture toughness and
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2004;20:441-8.
15. Stoll R, Cappel I, Jablonski-Momeni A,
Pieper K, Stachniss V. Survival of inlays and
partial crowns made of IPS empress after a
10-year observation period and in relation to
various treatment parameters. Oper Dent
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16. Etman MK, Woolford MJ. Three-year clinical
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Wolkewitz M, Stappert CF. All-ceramic partial coverage restorations: midterm results of
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of two recycled pressable glass ceramics.
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20. Chung KH, Liao JH, Duh JG, Chan DC. The
effects of repeated heat-pressing on properties of pressable glass-ceramics. J Oral
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21. Mead R, Gilmour SG, Mead A. Statistical
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22. ASTM. C1499-05 Standard test method for
monotonic equibiaxial exural strength of
advanced ceramic at ambient temperature.
West Conshohocken, PA: ASTM; 2005.
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Vickers indentation hardness of advanced
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International; 2009.
24. ASTM. E1820-11 Standard test method for
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Conshohocken, PA: ASTM International;
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processing with Imagej. Biophotonics Int
2004;11:36-42.

26. Cattell MJ, Palumbo RP, Knowles JC,

Clarke RL, Samarawickrama DY. The effect of
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amino acid additives on the crystallization
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593-7.
Corresponding author:
Ms Catherine M. Gorman
Division of Restorative Dentistry and Periodontology
Dublin Dental School and Hospital
Lincoln Place, Dublin 2
IRELAND
E-mail: catherine.gorman@dental.tcd.ie
Copyright 2014 by the Editorial Council for
The Journal of Prosthetic Dentistry.

Noteworthy Abstracts of the Current Literature

Peri-implantitis: A systematic review of recently published papers
Pesce P, Menini M, Tealdo T, Bevilacqua M, Pera F, Pera P.
Int J Prosthodont 2014;27:15-25.
Purpose. This systematic review considers possible etiologic factors and denitions of peri-implantitis as reported in the
recent literature.
Materials and Methods. An electronic search of databases plus a hand search of the most relevant journals published between January 2005 and September 2012 were performed.
Results. The electronic and manual searches yielded 640 and 14 titles, respectively. From the independent doublecheck of the
titles and abstracts, 24 full texts were downloaded (18 clinical studies and 6 animal studies). After reading the full texts, 10
articles (4 clinical studies and 6 animal studies) were included in this review. None of the human articles selected provided
sufcient evidence to address the research question, and no human clinical evidence is available to support a cause-effect
relationship between peri-implantitis and bacterial accumulation and/or occlusal overload. The animal literature is also not
unanimous regarding a specic peri-implantitis etiology. However, a correlation between periodontitis and smoking histories
was cited as contributing to a higher incidence of peri-implantitis.
Conclusion. The available scientic literature is characterized by an absence of a unanimous consensus regarding the etiology
of peri-implantitis and its specic relationship to periodontitis. Furthermore, both the choice of the term peri-implantitis and
its denition remain controversial.
Reprinted with permission of Quintessence Publishing.

The Journal of Prosthetic Dentistry

Gorman et al