Clinical Oral Investigations

https://doi.org/10.1007/s00784-019-03101-w

ORIGINAL ARTICLE

Influence of accelerated ageing on the physical properties

of CAD/CAM restorative materials
Thomas Niem 1 & Nivin Youssef 1 & Bernd Wöstmann 1

Received: 8 May 2019 / Accepted: 26 September 2019

# Springer-Verlag GmbH Germany, part of Springer Nature 2019

Abstract
Objectives This study aims to investigate the influence of thermocycling on the physical properties of different CAD/CAM
restorative materials and assess their ability to maintain energy dissipation capacities and damping effects.
Materials and methods The results of a 3-point bending test were used to calculate flexural strength (FS), modulus of elasticity
(ME), modulus of toughness (MT) and elastic recovery (ER) for three ceramic, twelve composite and five polymer-based
materials. Specimens (n = 10, 4.0 × 1.5 × 17.0 mm3) were loaded until rupture after water storage (24 h; 37.0 ± 1.0 °C) or
thermocycling (5000 cycles; 5–55 °C). Statistical data analysis was performed using parametric statistics (p = 0.05).
Results Thermocycling had no significant influence on any investigated properties of ceramic materials (p > 0.05). Hybrid
composites showed significant differences between water storage and thermocycling (p < 0.05), with the exception of FS of
Tetric CAD. Similarly, ME with AMBARINO High-Class, CERASMART, Tetric CAD and Vita Enamic and MT and ER with
Paradigm and Tetric CAD were not affected. For polymer-based materials, significant differences were found with the exceptions
of FS (PEEK-OPTIMA, Telio CAD), ME (M-PM Disc, PEEK-OPTIMA, Telio CAD, Vita CAD-Temp), MT (Telio CAD) and
ER (Telio CAD).
Conclusions The material properties of composite and polymer-based CAD/CAM materials were susceptible to degradation
processes induced by thermocycling. Only Telio CAD and Tetric CAD showed no significant effects like all ceramic materials,
thus preserving their inherent ability to elastically and plastically dissipate energy.
Clinical relevance A careful material selection is advisable when planning CAD/CAM restorations as remarkable differences
may exist in the durability of physical characteristics through the impact of water.

Keywords CAD/CAM material . Thermocycling . Modulus of toughness . Elastic recovery . Resiliency . Energy dissipation

Introduction preserved during the lifetime of a restoration without being

Longevity of biomimetic restorative materials is a crucial factor
when restoring natural tooth structures. It is highly desirable
that the physical properties of restorative materials match the
original materials as closely as possible, and that they will be
Nivin Youssef is deceased. This paper is dedicated to her memory.
* Thomas Niem
thomas.niem@dentist.med.uni-giessen.de
Bernd Wöstmann
bernd.woestmann@dentist.med.uni-giessen.de
1 properties and the durability of dental restorative materials
Dental Clinic - Department of Prosthodontics,
Justus-Liebig-University, Schlangenzahl 14,
35392 Giessen, Germany
susceptible to degradation processes. In particular, durable elas-
tic and plastic material properties seem to be important for
dissipating energy and preserving material integrity [1]. These
particular characteristics are achieved for natural enamel and
dentine structures by means of a definite water content that
appears to be mandatory for maintaining resilient and tough
biomechanical behaviour in addition to providing stability and
robustness [2, 3]. Similarly, other natural composites show su-
perior fracture resistance as a result of well-defined volumes of
embedded water in their material structure [4–7].
In contrast, water uptake, swelling processes, plasticization
and thus a higher risk of molecular structure decomposition on
the microscale, are considered to significantly alter physical
[8–12]. Because of these findings, the question arises as to
the impact water has on the physical characteristics of novel

computer-aided design/computer-aided manufacturing (CAD/
CAM) restorative materials being recently available on the
market. In particular, the influence on the ability to elastically
and plastically dissipate energy via damping effects and on
long-term stability is not currently well understood. Until
now, in vitro studies merely investigated water’s influence
on Martens hardness and indention modulus [13], flexural
strength [14, 15], flexural strength and Weibull modulus
[16], flexural strength and modulus of elasticity [17–20] and
fracture toughness [15, 21] for a few materials using a 3-point
bending test or a biaxial flexural strength test [22]. Only one
investigation considered water’s influence on the modulus of
resilience to more precisely describe the impact on elastic
material behaviour [19]. However, elastic and plastic material
properties, such as those previously characterized via the
modulus of toughness (MT) [23–26] and elastic recovery
(ER) [26, 27], were not yet investigated for their susceptibility
to water degradation and ageing.
Therefore, the aim of this in vitro study was to investigate
the resiliency and toughness of CAD/CAM restorative mate-
rials that are commonly used in dental practices following
water storage and thermocycling and to compare their flexural
strength (FS), modulus of elasticity (ME), modulus of tough-
ness (MT) and elastic recovery (ER). We hypothesised that
material properties are influenced by the water-ageing pro-
cess. The null hypothesis to be tested was that FS, ME, MT
and ER are independent of the thermocycling process used.
Materials and methods
The purpose of this investigation was to assess the influence
of accelerated ageing on the resistance of different CAD/CAM
restorative materials to fracture and to simultaneously evaluate
their elastic and plastic deformation energy before rupture
occurs. The terms ‘resilience’ and ‘toughness’ are used in
the concept of strain energy density [23, 26–28] to assess the
relationship between forces and material deformation and not
to describe material behaviour in linear elastic fracture me-
chanics (LEFM) or elastic-plastic fracture mechanics where
the crack propagation of pre-existing microcracks and flaws
are observed [29–31]. In this context, the modulus of tough-
ness (MT) which is related to material ductility describes the
total amount of elastic and plastic deformation energy re-
quired to fracture a material. It is represented by the area under
the characteristic stress-strain curve [23, 26]. On the contrary,
in a typical ‘work-of-fracture’ evaluation, total energy is de-
fined as energy that is consumed to produce a unit area of
fracture surface during the fracture process of a pre-existing
crack [32]. Furthermore, elastic recovery (ER) is also used in
the concept of strain energy density and describes the recov-
erable amount of elastic deformation energy occurring during
Clin Oral Invest
plastic deformation of a material and is calculated in case of
material rupture [26, 27].
Materials
Three types of commercially available CAD/CAM restor-
ative materials were used: three ceramic materials (Cerec
Blocs, IPS e.max CAD, VITABLOCS Mark II), twelve
hybrid composites (AMBARINO High - Class;
BRILLIANT Crios, CERASMART, DS Block, Grandio
blocs, Katana Avencia, Lava Ultimate, Paradigm
MZ100, Shofu Block HC, Shofu Block HC hard, Tetric
CAD, Vita Enamic) and five polymer-based materials (M-
PM Disc, PEEK-OPTIMA, Telio CAD, Tizian Blank, Vita
CAD-Temp) (Table 1).
Specimen preparation
Because of limited milling block dimensions and to allow
comparisons, bar-shaped material specimens (4.0 × 1.5 ×
17.0 mm, n = 20) were prepared for each investigated material
in accordance with ISO 6872 [33] using a water-cooled pre-
cision saw (IsoMet1000, Buehler, Esslingen, Germany) in
combination with a diamond-coated saw blade (127-mm di-
ameter, No. 11-4255, Buehler). Milling block mounts were cut
off, and blocks or discs were sliced and cut to the desired
dimensions. Final specimen sizes were adjusted by grinding
on wet SiC paper (800 grit, Leco Corp, Michigan, USA), and
specimens of IPS e.max CAD were additionally sintered ac-
cording to the recommended sintering programs (Programat
EP 3000, Ivoclar Vivadent, Schaan, Liechtenstein). All mate-
rials were used under ambient laboratory conditions (23 ±
1 °C; 50 ± 5% relative humidity) [34] according to the manu-
facturer’s instructions.
Water-ageing conditions
Water storage
Ten specimens from each material were stored in plastic ves-
sels with distilled water and placed in an incubator (Ehret,
Emmendingen, Germany) at 37 °C for 24 h. This group was
assigned a ‘W’.
Thermal cycling
Ten specimens for each material were subjected to a
thermocycling process of 5000 cycles (group ‘TC’) in a 5–
55 °C distilled water bath (SD Mechatronik, Feldkirchen-
Westernham, Germany). Each cycle lasted 120 s: 45 s in a
5 °C bath, 15 s to drain and transfer the samples to the second
bath, 45 s in a 55 °C bath and 15 s to transfer the samples back
to the 5 °C bath.
Clin Oral Invest

Table 1 Tested materials

Material type Brand Code Manufacturer Lot No.

Ceramic Cerec Blocs S3 PC CB Dentsply Sirona 35850 (b)

IPS e.max CAD LT A2 IPS Ivoclar Vivadent AG U10458 (b)
VITABLOCS Mark II A2C VB VITA Zahnfabrik 37480 (b)
Composite AMBARINO High-Class A2 AHC Creamed GmbH 041114 (b)
BRILLIANT Crios A2 HT BC Coltène Whaledent AG I43077 (b)
CERASMART A2 HT CS GC Dental Products 1412041 (b)
DS Block (experimental) DSB Dentsply Sirona ECG 08-275 (b)
Grandio blocs A3 HT GB VOCO GmbH 1715234 (b)
Katana Avencia A2 LT KA Kuraray Noritake Dental 000368 (b)
Lava Ultimate A2 HT LU 3 M ESPE N472545 (b)
Paradigm A2 P 3 M ESPE N573663 (b)
Shofu Block HC A2 LT SB SHOFU Inc. 021501 (b)
Shofu Block HC hard A3 LT SBH SHOFU Inc. 0818223 (b)
Tetric CAD A2 HT TC Ivoclar Vivadent AG X09399 (b)
Vita Enamic 2M2HT VE VITA Zahnfabrik 38910 (b)
Polymer M-PM Disc A2 MPM Merz Dental GmbH 10417 (d)
PEEK-OPTIMA PO Juvora Ltd. J000025 (d)
Telio CAD LT A3 T Ivoclar Vivadent AG VW9680 (b)
Tizian Blank A1 TB Schuetz Dental 2015007272 (d)
Vita CAD-Temp 1M2T VCT VITA Zahnfabrik 23170 (d)

b, block; d, disc
Three-point bending test
After drying specimens in air, they were loaded until rupture
in a 3-point bending test using a newly calibrated universal
testing machine (1454, Zwick/Roell, Ulm, Germany) and a
0.5-kN load cell to minimize the effect of the system compli-
ance [35]. The span width was 15.0 mm, and the crosshead
speed was 1 mm/min [33]. Specimen deflection was detected
via the crosshead motion of the testing machine as recently
described [24, 25, 36–38] (incremental linear encoder; repeat-
ability fw: 0.006 μm), and likewise engineering stress-strain
curves were used for the modulus of toughness calculation
without correction for true stress-strain material behaviour. If
specimen deflection surpassed 2.5 mm without sample frac-
ture, loading was discontinued and the results for MT and ER
were noted as ‘not available’.
Calculation of results
(FS) [34, 38], (ME) [34, 38] and (MT) [3, 26] were calculated
using Eqs. (1), (2) and (3):
3 F max L
FS ¼ ; ð1Þ
2wh2
F lin L3
ME ¼ ; ð2Þ
4d lin wh3
9A
MT ¼ ; ð3Þ
whL
where Fmax (N) is the maximum load, L (mm) is the span
width between the two support bars and w (mm) and h (mm)
are the width and height of the specimen. Flin (N) is the force
in the linear part of the stress-strain curve and dlin (mm) is the
corresponding deflection at Flin. A (J) is the total area under
the load-deformation curve (work performed by the applied
load to deflect and fracture the specimen) obtained with the
software (TestXpert; release 10.11, Zwick/Roell, Ulm,
Germany) used for the testing machine.
(ER) at rupture was calculated using Eq. (4) [19, 26,
39–42]:
FS2
ER ¼ ; ð4Þ
2ME
where FS (MPa) represents the flexural strength of the speci-
men and ME (MPa) is equivalent to the respective modulus of
elasticity.
For each material property, the relative percentage loss PL
(%) was calculated for ten separate values of TC using Eq. (5):
ðW−TCÞ  100
PL ¼ ð5Þ
W
where W is the determined mean of the considered material
property after water storage (24 h, 37 °C) (Table 2) and used as
a constant parameter in this particular calculation. TC repre-
sents one of the ten respective values after thermocycling.

Statistical analysis
Means and standard deviations of the different material
properties were calculated. All data sets were subjected
to the Kolmogorov-Smirnov test to check for a normal
distribution and to the Levene test to check for homoge-
neity of variance. As the test results revealed, there was
no significant deviation for any group from a normal dis-
tribution and homogeneity of variance. Parametric statis-
tics were applied to identify significant differences be-
tween the two water-ageing conditions for each CAD/
CAM restorative material (Student’s t test for independent
samples) and between the calculated percentage losses
(PL) and zero as the reference value (Student’s t test for
one-sample). Percentage losses of different CAD/CAM
materials belonging to one material property were not
compared as only the relation to the reference value of
zero was of interest in this study to identify materials with
no significant property degradation. Cohen’s effect size ds
was calculated to further assess the differences between
the two water-ageing conditions [43]. All statistical anal-
yses were performed using SPSS for Windows (release
23.0.0.2, IBM Corp., Armonk, NY, USA).
Results
Means and standard deviations obtained from the universal
testing machine software are listed in Table 2. Referring the
material properties of PO, no results for MT and ER were
obtained as the respective specimens demonstrated no rupture
during the bending test. Instead, signs of crazing on the spec-
imen surfaces, indicating the formation of micro-cracks, were
detected [44]. All the other materials revealed specimen rup-
ture at Fmax. While the results and statistical parameters of the
pairwise comparisons of the two water-ageing conditions are
listed in Table 3, the calculated PL values are shown in Figs. 1,
2, 3 and 4.
Ceramic materials
For all investigated properties of the ceramic materials,
independent-sample t tests revealed no statistically significant
differences between the two water-ageing conditions
(p > 0.05). The respective effect sizes (−0.029 ≤ ds ≤ −0.753)
for this analysis (Table 3) did not exceed Cohen’s convention
[45] for a large effect (ds = 0.80), thus suggesting low to me-
dium practical significance. A one-sample t test showed that
all calculated PL values of the investigated material properties
were not statistically significantly different from the test value
of zero (Figs. 1, 2, 3 and 4).
Clin Oral Invest
Hybrid composites
The independent-sample t tests indicated significant differ-
ences between both water-ageing conditions for most of the
hybrid composites (p < 0.05) (Table 3). Only a few exceptions
were found where the original material properties were par-
tially retained. This partial retention was true for FS where
both TC means were not significantly different and was sim-
ilarly detected for ME, where the respective results for AHC,
CS, TC and VE were assigned not to be different (Table 3).
The pairwise comparisons for MT and ER revealed no detect-
able differences for P and again for TC. In addition, the effect
sizes for this analysis (− 0.858 ≤ ds ≤ −5.797) (Table 3) were
found to markedly exceed Cohen’s convention for a large
effect (ds = 0.80); this suggests, in the respective cases, a very
high practical significance except for afore-mentioned com-
parisons where the independent-sample t test indicated no
difference (p > 0.05) (Table 3). Furthermore, a one-sample t
test comparing the PL values of the investigated material prop-
erties to the test value of zero revealed no significant differ-
ences for FS (TC), for ME (CS, TC and VE) or for MT and ER
(P and TC) (Figs. 1, 2, 3 and 4). Among the tested hybrid
materials, TC was the only composite where no significant
influence of thermocyling was detected for any investigated
properties.
Polymer-based materials
For the polymer-based materials, significant differences be-
tween water-ageing conditions were found (p < 0.05)
(Table 3). Exceptions were detected for FS with PO and T
(p > 0.05) and for ME with MPM, PO, T and VCT
(p > 0.05). Comparisons of MT and ER revealed no significant
differences only for T (p > 0.05) (Table 3). For this analysis,
effect sizes (− 1.139 ≤ ds ≤ − 2.645) were found to exceed
Cohen’s convention for a large effect (ds = 0.80); this suggests
that in the respective cases there is high practical significance
except for those comparisons where the independent-sample t
test indicated no difference (p > 0.05) (Table 3). A one-sample
t test comparing the calculated PL values of the investigated
material properties with the test value of zero showed no sig-
nificant differences (p > 0.05) for FS (T and PO), for ME
(VCT, T, MPM and PO) or for MT and ER (each with T).
Finally, in the polymer-based material group, only T showed
no influence of thermocycling on all investigated material
properties.
Discussion
Dissipation of energy via elastic and plastic material deforma-
tion and damping effects are considered an important factor to
impart long-term material stability in natural composites [1,
Clin Oral Invest

Table 2 Mean ± (SD) of data obtained from the 3-point bending test

MM FS (MPa) ME (MPa) MT (MJ/m3) ER (MJ/m3)

W TC W TC W TC W TC

CB 114.9 (7.5) 111.9 (6.9) 56,131.9 (1949.1) 54,442.8 (3109.2) 0.10 (0.01) 0.10 (0.01) 0.11 (0.01) 0.11 (0.01)
IPS 348.5 (39.8) 340.1 (35.5) 77,562.2 (3600.9) 74,382.7 (4761.5) 0.79 (0.17) 0.78 (0.17) 0.79 (0.17) 0.79 (0.16)
VB 110.9 (3.4) 109.8 (5.7) 53,642.5 (2297.6) 52,702.0 (1495.9) 0.10 (0.01) 0.10 (0.01) 0.11 (0.01) 0.11 (0.01)
AHC 162.5 (7.3) 145.7 (10.1) 10,537.6 (609.4) 10,048.5 (527.9) 1.53 (0.15) 1.31 (0.23) 1.26 (0.11) 1.06 (0.16)
BC 213.3 (5.1) 192.0 (5.0) 11,190.5 (322.3) 10,493.8 (171.0) 3.41 (0.31) 2.78 (0.19) 2.03 (0.10) 1.76 (0.09)
CS 174.2 (10.6) 151.9 (14.2) 8517.6 (797.1) 8384.5 (588.9) 2.31 (0.26) 1.68 (0.40) 1.79 (0.12) 1.40 (0.29)
DSB 227.6 (8.6) 207.8 (9.3) 12,724.8 (317.7) 11,994.4 (659.7) 2.79 (0.28) 2.52 (0.22) 2.04 (0.15) 1.80 (0.11)
GB 244.9 (10.7) 216.7 (21.3) 18,094.0 (1023.8) 16,864.4 (1126.5) 2.03 (0.20) 1.65 (0.37) 1.66 (0.14) 1.41 (0.30)
KA 198.2 (7.4) 158.8 (6.1) 9144.6 (212.4) 8438.8 (433.8) 3.22 (0.34) 2.02 (0.16) 2.15 (0.16) 1.50 (0.09)
LU 197.7 (10.9) 161.8 (10.4) 12,074.2 (451.3) 11,604.6 (495.1) 1.98 (0.25) 1.34 (0.20) 1.62 (0.17) 1.13 (0.15)
P 167.9 (6.8) 155.4 (8.7) 16,020.0 (575.7) 14,223.0 (800.9) 1.00 (0.11) 0.97 (0.12) 0.88 (0.06) 0.85 (0.09)
SB 132.3 (5.6) 104.4 (9.0) 8216.4 (477.4) 7671.2 (366.0) 1.24 (0.11) 0.80 (0.15) 1.07 (0.08) 0.72 (0.13)
SBH 227.5 (7.4) 196.3 (5.2) 14,440.8 (521.2) 13,122.8 (424.1) 2.49 (0.25) 2.09 (0.12) 1.80 (0.13) 1.47 (0.07)
TC 185.0 (12.8) 181.9 (8.2) 10,928.8 (183.0) 10,735.0 (385.9) 2.17 (0.41) 2.24 (0.32) 1.57 (0.21) 1.54 (0.13)
VE 141.1 (5.8) 129.6 (4.3) 28,784.8 (1657.2) 27,969.1 (1718.3) 0.33 (0.03) 0.29 (0.02) 0.33 (0.03) 0.29 (0.03)
MPM 116.8 (6.3) 102.7 (6.2) 2821.6 (129.2) 2814.8 (100.2) 3.85 (0.74) 2.71 (0.50) 2.42 (0.22) 1.88 (0.21)
PO 202.1 (3.1) 202.8 (5.8) 4145.5 (109.2) 4145.9 (152.6) n.a. n.a. n.a. n.a.
T 115.6 (8.2) 115.2 (7.2) 2870.7 (162.3) 2823.7 (77.2) 5.35 (2.02) 5.36 (1.50) 2.34 (0.34) 2.36 (0.31)
TB 90.8 (3.9) 83.8 (2.6) 3177.6 (77.9) 2997.7 (73.4) 1.59 (0.19) 1.40 (0.15) 1.30 (0.11) 1.17 (0.09)
VCT 88.5 (2.9) 81.9 (2.0) 3637.5 (263.5) 3544.6 (284.1) 1.11 (0.08) 0.97 (0.05) 1.08 (0.08) 0.95 (0.06)

ER, elastic recovery; FS, flexural strength; ME, modulus of elasticity; MM, milling material; MT, modulus of toughness; SD, standard deviation; TC,
thermocycling 5/55 °C; W, water storage 37 °C 24 h; n.a., not available

46, 47] and dental restorative materials [26, 48]. Therefore, the
present investigation studied the influence of water storage
and thermocycling on FS, ME, MT and ER to assess the im-
pact on resilience and toughness properties of novel CAD/
CAM restorative materials. While thermocycling induced a
significant degradation in the mechanical properties of the
majority of the hybrid composite and polymer-based materials
in this study, ceramic materials were not impaired, revealing
that they have higher potential to preserve their original ca-
pacity to elastically and plastically dissipate energy. The re-
sults of the independent-sample t test (Table 3) and substan-
tially lower PL values for all ceramic materials, which were
not significantly different from zero (Figs. 1, 2, 3 and 4),
confirmed this observation and supported the null hypothesis
for ceramic materials. The received results are in good accor-
dance with previously reported findings where the fracture
toughness [15, 21], Martens hardness [13] and flexural
strength [15, 18, 19] of CAD/CAM materials were investigat-
ed, and thermocycling showed no statistically significant ef-
fect on ceramic material properties. On the contrary, the re-
spective data for polymer-based materials significantly de-
creased. Similarly, the biaxial flexural strength test by Okada
et al. [22] showed significantly lower flexural strength values
after water degradation testing (90 °C, 28 days) for hybrid
composite CAD/CAM materials when compared with sam-
ples without degradation testing; while in the same conditions,
the ceramic material IPS revealed no detectable influence of
the water-ageing test. This was likewise found in the present
investigation after thermocycling. All results showed that ce-
ramic CAD/CAM materials appeared to be much less prone to
hydrolytic degradation processes than hybrid composite and
polymer-based materials. In contrast, Porto et al. [21] found a
significant increase in fracture toughness for wet specimens of
ceramic CAD/CAM materials (7 days; 37 °C; distilled water)
when compared with samples stored in a desiccator. A similar
stability increase caused by a hydration effect was recently
found by Kruzic et al. in natural dentin [7] and by Yan et al.
in bovine bone [5], both demonstrating the important role of
water in toughening mechanisms of natural composites.
When analysing the received results for hybrid CAD/CAM
materials, a distinct influence of the thermocycling process on
the examined material properties for most CAD/CAM com-
posites was observed, leading to a partial rejection of the null
hypothesis. In this material group, a considerable degradation
in mechanical properties was detected, which was unequivo-
cally demonstrated by the results of the independent-sample t
test (Table 3) and was corroborated by the negative signs of
the high Cohen’s ds values (Table 3). Furthermore, the highest
 Clin Oral Invest

Table 3 Statistical parameters of the pairwise comparisons of both Table 3 (continued)

water-ageing conditions
MM Value FS ME MT ER
MM Value FS ME MT ER W/TC W/TC W/TC W/TC
W/TC W/TC W/TC W/TC
ds − 2.262 − 0.059 − 1.794 − 2.539
CB t(18) 0.94 1.46 0.60 0.56 PO t(18) − 0.35 − 0.01 n.a. n.a.
p .358 .163 .556 .582 p .729 .994 n.a. n.a.
ds − 0.422 − 0.651 − 0.268 − 0.250 ds 0.157 0.003 n.a. n.a.
IPS t(18) 0.49 1.68 0.08 0.07 T t(18) 0.10 0.83 − 0.01 − 0.15
p .627 .109 .935 .949 p .926 .419 .995 .884
ds − 0.221 − 0.753 − 0.037 − 0.029 ds − 0.042 − 0.370 0.003 0.066
VB t(18) 0.54 1.09 − 0.23 0.12 TB t(18) 4.70 5.31 2.55 2.77
p .595 .292 .824 .908 p .000 .000 .020 .013
ds − 0.242 − 0.485 0.101 − 0.053 ds − 2.103 − 2.376 − 1.139 − 1.241
AHC t(18) 4.28 1.92 2.58 3.21 VCT t(18) 5.92 0.76 4.67 4.02
p .000 .071 .019 .005 p .000 .458 .000 .001
ds − 1.915 − 0.858 − 1.155 − 1.435 ds − 2.645 − 0.339 − 2.090 − 1.799
BC t(18) 9.43 6.04 5.48 6.52
p .001 .000 .000 .000 ER, elastic recovery; FS, flexural strength; ME, modulus of elasticity;
MM, milling material; MT, modulus of toughness; TC, thermocycling;
ds − 4.217 − 2.700 − 2.450 − 2.916
W, water storage 37 °C 24 h; n.a., not available; ds, Cohen’s ds; p, statis-
CS t(18) 3.98 0.43 4.22 3.95 tical significance; t(18), t-statistic (degrees of freedom)
p .001 .676 .001 .001
ds − 1.778 − 0.190 − 1.888 − 1.766
DSB t(18) 4.97 3.15 2.45 4.05 PL values detected in the present study were observed in this
p .000 .005 .025 .001 material group. In detail, for MT, a maximum loss of 37.3%
ds − 2.221 − 1.411 − 1.097 − 1.812 (KA) was measured (Fig. 3). For ER, the highest value was
GB t(18) 3.72 2.55 2.84 2.36 found for SB with 33.0% (Fig. 4), FS had a maximum loss of
p .002 .020 .011 .030 21.1% for SB (Fig. 1); finally, in the ME group, the largest loss
ds − 1.664 − 1.142 − 1.271 − 1.056 of 11.2% was found for P (Fig. 2). Nevertheless, among the
KA t(18) 12.96 4.62 10.07 11.17 tested materials, there was one exception, TC, where all inves-
p .000 .000 .000 .000 tigated properties, especially the MT and ER, had no detected
ds − 5.797 − 2.067 − 4.504 − 4.094 influence of thermocycling, which was the same as ceramic
LU t(18) 7.53 2.22 6.34 6.89 materials. This observation was supported for all results by
p .000 .040 .000 .000 low PL values that were not significantly different from zero
ds − 3.368 − 0.991 − 2.836 − 3.081
(Figs. 1, 2, 3 and 4), thus showing less influence of
P t(18) 3.59 5.76 0.58 0.86
thermocycling on the resilient and tough material behaviour
p .002 .000 .567 .401
and that implied a high chance to preserve the original capac-
ity of the TC to elastically and plastically dissipate energy. The
ds − 1.607 − 2.577 − 0.261 − 0.385
findings for the other composites in this material group were
SB t(18) 8.28 2.87 7.27 7.45
in line with recently reported outcomes where hybrid compos-
p .000 .010 .000 .000
ite CAD/CAM materials generally showed degradation in
ds − 3.701 − 1.282 − 3.252 − 3.331
their material properties after water exposure. In detail,
SBH t(18) 10.91 6.20 4.62 7.06
Tsujimoto et al. [17], whose test conditions were closest to
p .000 .000 .000 .000
the conditions of the present study, found that all FS and
ds − 4.878 − 2.774 − 2.064 − 3.156
ME values for LU, PM, CS, SB and KA were significantly
TC t(18) 0.65 1.44 − 0.41 0.36
lower after thermocycling (5 °C/60 °C 10,000 cycles) com-
p .526 .169 .689 .724
pared with simple water storage (24 h; 37 °C), which was
ds − 0.290 − 0.642 0.182 − 0.161
equally shown in the present investigation. In the same way,
VE t(18) 5.06 1.08 3.86 3.56
the studies by Egilmez et al. [16], who solely investigated
p .000 .294 .001 .002
hybrid materials (CS, LU and VE), showed that for CS and
ds − 2.263 − 0.483 − 1.726 − 1.590
LU, there was a significant degradation in FS after
MPM t(18) 5.06 0.13 4.01 5.68 thermocycling (5 °C/55 °C 5000 cycles) when compared with
p .000 .896 .001 .000 ‘no-treatment specimens’ (no further details available). This
Clin Oral Invest

Fig. 1 Percentage loss of flexural

strength (PL(FS)) after
thermocycling for ceramic, hybrid
composite and polymer-based
CAD/CAM restorative materials;
each bar represents the mean and
the 95% confidence interval of ten
measurements; asterisks indicate
groups with means not signifi-
cantly different from zero
(p > 0.05); PL(FS), relative per-
centage loss of flexural strength

result was also found for CS and LU by Lauvahutanon et al.
[18], who instead used 10,000 cycles (5 °C/55 °C) directly
after previous application of 7 days water storage (37 °C) and
who further examined dry (23 ± 2 °C) and water storage
(7 days, 37 °C) conditions. As a result of that investigation,
only the comparison with the dry condition revealed signifi-
cant differences, while the water storage itself showed no ef-
fect when compared with thermocycling. In addition, in the
same study, VB was likewise investigated as a reference ma-
terial for ceramics, and no effect of the thermocycling process
on FS was detected. This outcome is perfectly in line with the
present results and was recently confirmed by Al-Harbi et al.
[14], Sonmez et al. [15], Awada and Nathanson [39] and
Blackburn et al. [19], who further investigated ME and ER
for the first time to more precisely characterize elastic material
properties and resilient behaviour of CAD/CAM materials in
an elaborated way. Unfortunately, ER was erroneously termed
modulus of resilience in that report [19, 39] because of con-
fusion with yield strength and flexural strength in the respec-
tive calculations [26]. Nevertheless, a significant influence of
thermocycling (5 °C/55 °C; 5000 and 10,000 cycles) was
found on FS and the modulus of resilience (Ur in that study)
for all investigated composite materials (LU, P and VE) when
compared with water storage conditions (24 h, 20 °C) [19],
which is in line with the results received in the present study
for FS and ER.
However, all results showed that common material proper-
ties such as FS and ME of hybrid composite CAD/CAM ma-
terials appeared to be susceptible to degradation processes
induced by water contact during thermocycling. Moreover,
equally resilient behaviour characterized by ER (Ur in [19])
and tough material characteristics that were previously quan-
tified as MT [26] showed notable degradation effects from the
thermocycling process. In particular, SB, KA, LU and CS

Fig. 2 Percentage loss of

modulus of elasticity (PL(ME))
after thermocycling for ceramic,
hybrid composite and polymer-
based CAD/CAM restorative
materials; each bar represents the
mean and the 95% confidence in-
terval of ten measurements; aster-
isks indicate groups with means
not significantly different from
zero (p > 0.05); PL(ME), relative
percentage loss of modulus of
elasticity
 Clin Oral Invest

Fig. 3 Percentage loss of

modulus of toughness (PL(MT))
after thermocycling for ceramic,
hybrid composite and polymer-
based CAD/CAM restorative
materials; each bar represents the
mean and the 95% confidence in-
terval of ten measurements; aster-
isks indicate groups with means
not significantly different from
zero (p > 0.05); n.a., not available;
PL(MT), relative percentage loss of
modulus of toughness

revealed that both properties had a very large influence,
reflected by the highest PL values determined in this study
(Figs. 3 and 4), ranging from 20 to 30%. Hence, these results
concurrently imply a reduction in the respective material’s
capacity to elastically and plastically dissipate energy that
may negatively affect the long-term material stability.
Recently determined water sorption values showed that SB
had the highest water uptake, and VB had the lowest uptake
(SB, 39.7 μg/mm3; LU, 30.7 μg/mm3; CS, 22.0 μg/mm3; VE,
7.0 μg/mm3; VB, 0.1 μg/mm3) [49], which is in agreement
with the findings of the present study, as the results in de-
scending order exactly reflect the observed orders for PL(FS)
(Fig. 1), PL(MT) (Fig. 3) and PL(ER) (Fig. 4). Consequently, a
previously discussed plasticizing and softening effect on poly-
mer networks caused by solvent uptake [8, 50, 51] could thus
be substantiated by the present investigation for hybrid
composite CAD/CAM materials with the only exception of
TC where this effect was not ascertainable.
When analysing the results for polymer-based CAD/CAM
restorative materials, a considerable influence of the
thermocycling process on most examined material properties
was observed, leading to a partial rejection of the null hypoth-
esis. In this material group, a noticeable degradation in the
mechanical properties was detected, which was proven by
the results of the independent-sample t test (Table 3) and the
negative signs of the Cohen’s ds values (Table 3). There was
again one exception among the tested materials with T, where
for all investigated properties, no influence of thermocycling
was detected like those found for the ceramic materials and
TC. This finding equally implies that for T, there was a high
chance of preserving its original capacity to elastically and
plastically dissipate energy, which might help explain the

Fig. 4 Percentage loss of elastic

recovery (PL(ER)) after
thermocycling for ceramic, hybrid
composite and polymer-based
CAD/CAM restorative materials;
each bar represents the mean and
the 95% confidence interval of ten
measurements; asterisks indicate
groups with means not signifi-
cantly different from zero
(p > 0.05); n.a., not available;
PL(ER), relative percentage loss of
elastic recovery
Clin Oral Invest
notable performance of T when being used in fracture load
tests of three-unit fixed dental prostheses with the same [52,
53] or different connector cross-sectional areas [54].
Furthermore, it was possibly responsible for finding no detect-
able impact of thermocycling on Martens hardness when com-
pared with VCT [13].
Finally, the results showed that most hybrid and polymer-
based CAD/CAM materials, with only a few exceptions, ap-
peared to be highly susceptible to physical property degrada-
tion after thermocycling when compared with ceramics. To
date, such impairment in mechanical properties by water-
ageing tests are mainly attributed to water sorption of polymer
networks resulting in resin plasticizing and softening effects
[8, 50, 51, 55], as well as stress corrosion on filler surfaces
[56]. Furthermore, a speculated hydrolysis of the interfacial
silane coupling agent was discussed [18, 21]. Nevertheless,
meaningful investigations are necessary to get deeper insight
and better understanding of this complex silane coupling
agent interface such as that initiated by Schrader and Block
[57], Söderholm [56], Ishida and Miller [58] and Mohsen et al.
[55] and to unequivocally clarify whether irreversible hydro-
lysis effects, possibly caused by bond cleavage scenarios on a
microscale, may be substantiated with experimental data. In
contrast, a well-defined amount of water inside a polymer-
mineral interface, composed of silane coupling agents, was
associated with bond cleavage and bond formation equilibria
having the potential to self-healing in sense of stress relaxation
and stability improvement [59].
Although TC, and especially T, had a high polymeric
resin content (TC, < 30.8%; T, < 99.9%),1 which has pre-
viously discussed water-induced destabilizing effects on
the polymer network, such as swelling and plasticization
processes [8] that did not markedly affect their material
properties in the present study. This result is so far diffi-
cult to explain as both materials revealed noticeable water
uptake according to the manufacturer specifications (TC,
22.5 μg/mm3 [60]; T, < 28.0 μg/mm3 [61], 23.2 μg/mm3
[49]) when compared with ceramics (VE, 5.7 μg/mm3
[62], 7.0 μg/mm 3 [49]; VB, 0.1 μg/mm 3 [49]).
However, for SB and LU, much greater water uptake
was previously observed (SB, 39.7 μg/mm 3 ; LU,
30.7 μg/mm3) [49], which may help explain their very
high PL(FS) (Fig. 1), PL(MT) (Fig. 3) and PL(ER) (Fig. 4)
values observed in the present investigation compared
with TC and T. This finding is logical, especially in light
of possible lower cross-linking density in their respective
polymer networks that facilitates water sorption and plas-
ticizing effects such as previously discussed [8] and due
to their unique resin compositions and the particular
manufacturing processes of their CAD/CAM blocks under
ideal industrial conditions. A more profound
1
Ashing in air (1 h, 700 ± 20 °C)
interpretation of the results for TC and T may be
discussed when considering the outcome of an investiga-
tion where the dielectric relaxation of a urethane
dimethacrylate polymer was examined [55]. In the respec-
tive publication, it was shown that a small moisture con-
tent (≤ 0.69 wt%) in the polymer network had a stiffening
effect on the molecular structures as demonstrated by a
distinct shift in the β-relaxation peak at higher tempera-
tures. Conversely, increased moisture content (0.69–
3.0 wt%) caused a plasticizing effect on the same polymer
network as proved by a shift in the β-relaxation peak at
lower temperatures. These deviating results for different
moisture content were explained by various hydrogen
bonding effects arising between carbonyl groups of the
polymer chain and absorbed water molecules [55] that
generate ‘firmly’ (stiffening effect) and ‘loosely’ (plasti-
cizing effect) bound water being responsible for different
spacing between polymer chains and their resulting devi-
ant mobility. An identical behaviour was observed in the
respective study for the same polymer if a silanised
zirconia-silica filler was admixed. Hence, these observa-
tions allow a more precise explanation of the different
behaviours of TC and T when compared with LU and
SB. Accordingly, the water uptake of TC and T seems to
be small enough to provoke the discussed stiffening effect
and negligible plasticisation, while the uptake for LU and
SB appeared to be comparatively large, causing a
plasticisation effect resulting in the drop in physical prop-
erties. Nevertheless, this plausible interpretation should be
handled with care; the effect should not be overestimated
as the specific compositions of different CAD/CAM ma-
terials are often not available to the public, and multiple
resin mixtures are used instead of just the single urethane
dimethacrylate monomer. Further investigations in this
field of activity are strongly recommended to produce
better understanding of different material behaviours of
CAD/CAM materials during water uptake and ageing
processes.
Conclusion
Mechanical properties of ceramic CAD/CAM materials were
not affected by thermocycling. In contrast, most hybrid com-
posite and polymer-based materials showed significant degra-
dation. Only TC and T revealed no influence of the
thermocycling process on investigated material characteristics
and consequently on resilience and toughness properties.
Dental practitioners should be aware of careful material selec-
tion when planning CAD/CAM restorations because remark-
able differences may exist in the durability of physical char-
acteristics through the impact of water. Only a few materials
appear to maintain their properties during ageing, and thus

their damping effects and their capacity to elastically and plas-
tically dissipate energy to ensure long-term material stability.
Acknowledgements The authors thank Antje Hübner for her technical
assistance in sample preparation and data acquisition. We also thank
Juvora Ltd. for donating PEEK-Optima. In addition, we gratefully ac-
knowledge the support of our biostatistician Dr. Johannes Herrmann.
Funding information This research did not receive any specific grant
from funding agencies in the public, commercial or not-for-profit sectors.
No external funding; the study is solely based on the department budgets
of the authors.
Compliance with ethical standards
Conflict of interest The authors declare that they have no conflict of
interest.
Ethical approval This article does not contain any studies with human
participants or animals performed by any of the authors.
Informed consent For this type of study, formal consent is not required.
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