Effects of Food-Simulating Solutions On The Surface Properties of Two CAD/CAM Resin Composites
Effects of Food-Simulating Solutions On The Surface Properties of Two CAD/CAM Resin Composites
Effects of Food-Simulating Solutions On The Surface Properties of Two CAD/CAM Resin Composites
1
Assistant Professor, Department of Dental Biomaterials, Faculty of Dentistry, Mansoura University, Mansoura, Egypt
2
Associate Professor, Department of Dental Biomaterials, Faculty of Dentistry, Mansoura University, Mansoura, Egypt
Correspondence:
Department of Dental Biomaterials
Faculty of Dentistry, Mansoura University
El-Gomhoria Street, Mansoura
El-Daqahlia, Egypt 35516
Dinasamy@mans.edu.eg Farahat DS, El-Wassefy NA. Effects of food-simulating solutions on the
surface properties of two CAD/CAM resin composites. J Clin Exp Dent.
2022;14(10):e782-90.
Received: 21/06/2022
Accepted: 16/08/2022 Article Number: 59822 http://www.medicinaoral.com/odo/indice.htm
© Medicina Oral S. L. C.I.F. B 96689336 - eISSN: 1989-5488
eMail: jced@jced.es
Indexed in:
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Abstract
Background: During clinical service, dental materials could experience chemical degradation due to exposure to
different diet components which could affect their functions and longevity. So, the objective of this study was to
investigate the effect of food simulating solutions on surface properties of two CAD/CAM dental resin composites.
Material and Methods: Two CAD/CAM composites; a nano-hybrid and a resin nano-ceramic were machined into 2
mm plates then assessed at baseline for their surface roughness and microhardness. Each group was immersed into
distilled water, ethanol and methyl ethyl ketone (MEK) for 15 days at 37oC. The surface properties were evaluated
after one day, 10 and 15 days of immersion by a surface profilometer and Vickers microhardness tester, and finally
the surface morphology was studied using scanning electron microscopy.
Results: At baseline, there was no significant difference in roughness between Teric CAD and Lava Ultimate,
however, Lava Ultimate was significantly harder than Tetric CAD. Aging in ethanol had no significant effect on
roughness and hardness of both the materials. Yet, Lava Ultimate showed significantly higher roughness and hard-
ness compared to Tetric CAD. Immersion in MEK resulted in a significant increase in roughness of Lava Ultimate
at 10 and 15 days. Neverthless, it caused a significant decrease in hardness of Tetric CAD at 10 and 15 days and
Lava Ultimate at 10 days. Finally, water immersion caused a significant increase of roughness Tetric CAD.
Conclusions: Exposure to different storage media variably affected the surface properties of CAD/CAM machina-
ble composites. Both materials showed greater stability in surface properties when being immersed in ethanol than
MEK. Hence, the surface deterioration suggests the advisability of more research involving increased immersion
periods and involvement of thermocycling changes.
Key words: Food simulating solutions, chemical degradation, nano-hybrid CAD/CAM composite, resin nano-
ceramic CAD/CAM material, surface roughness, micro-hardness, surface morphology.
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Table 1: Composition, manufacturer, batch no and shade of materials used in this study.
Bis-GMA = bisphenol A glycidyl methacrylate; UDMA = urethane dimethacrylate; Bis-EMA = ethoxylated bisphenol-A dimethacrylate; TEG-
DMA = triethylene glycol dimethacrylate; SiO2 = silicon dioxide; ZrO2 = zirconium dioxide
material specimens were first grinded by a medium rub- Precision Testing Equipment CO, Model HV-1000ltd,
ber wheel, and then a soft bristle brush with a polishing China) at room temperature. Three indentations were
agent applied slowly to the surface using a low speed made, each being 0.5 mm apart. The indenter was
handpiece. The baseline measurements of surface rou- applied against specimens with a load of 200 g for 15
ghness and microhardness were recorded. s dwell time.
-Storage agent immersions Vickers hardness number (VHN) was calculated using
60 specimens were divided into 2 groups of 30 speci- the following equation:
mens according to the type of materials, and then each HV = 2F sin (136/2) /d2
group was subdivided into three subgroups of 10 speci- Where F is the applied force, d is the average length of
mens according to the type of storage media; distilled the indentations’ diagonals and 136 is angle between the
water (served as a control), ethanol, methyl ethyl ketone face of the diagonal.
(MEK). The specimens were then randomly immersed -Surface morphology evaluation
in 10 ml of the storage media in individual glass vials in The surface morphology was studied using a scanning
an incubator at a 37±1ºC and kept under the same con- electron microscope (SEM, JSM-6510LV, JEOL, Tok-
ditions for 15 days. After the storage period specimens yo, Japan). First, a representative specimen was selected
were taken out of the storage media, rinsed with distilled from each group nad cleaned in an ultrasonic bath for 2
water and blot dried carefully against filter paper. The min and then air dried. Then, specimens were gold coa-
surface roughness and microhardness measurements ted (SPI-MODULETM, SPI Supplies, West Chester, PA,
were measured on day one, ten and 15 days, finally sur- USA) and examined by SEM to assess surface topogra-
face morphology of specimens was examined on day 15. phy using different magnifications.
Surface Roughness testing -Statistical analysis:
Surface roughness was measured by a stylus contact pro- Each experiment was repeated in triplicates. Data was
filometer (Surftest SJ-210, Mitutoyo, Corp, Kawasaki, presented as means ± standard deviations (SD). Sta-
Japan) in three directions according to ISO 4278-1997. tistical analyses were performed using SPSS software
Three measurements were done by placing the probe package for Windows (Version 20.0, SPSS Inc., Chica-
over the specimen’s surface. The tracing length was 0.8 go, IL). Based on data distribution, three-way analysis
mm, at a scanning speed of 0.5 mm/s and the resolu- of variance (ANOVA) and Tukey’s post hoc tests were
tion of the recorded data was 0.01 μm. The values of the used for statistical comparisons among groups. Diffe-
three readings of each specimen were recorded and the rences were considered significant when p< 0.05.
average roughness of each material (Ra) was calculated.
Surface microhardness testing Results
Surface microhardness was determined using a micro- The Shapiro-Wilk test revealed that all data followed a
hardness tester with a Vickers diamond indenter (Jinan normal distribution pattern in all research groups. There-
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fore, a parametric three-way analysis of variance (ANO- significantly from baseline for Lava Ultimate after 10
VA) was conducted first, followed by post-hoc tukey and 15 days (p=0.0001 and p=0.028 respectively), but
test. All tests were measured at baseline, after one day, there were no significant differences in surface rough-
10 days and after 15 days. The outcomes of ANOVA test ness for Tetric CAD at all timepoints from baseline. Yet,
revealed that “type of materials”, food simulating solu- surface roughness of Lava Ultimate was significantly
tions, “immersion period” significantly affected average higher than that of Tetric CAD after 15 days of MEK
roughness and Vickers microhardness results (p˂0.05). immersion (p<0.0001). Immersion in water significant-
1. Roughness results: ly increased surface roughness for Tetric CAD after 15
Surface roughness was significantly affected by mate- days compared to baseline (p=0.0018) . However, no
rial and immersion time (p<0.0001) and by food simu- significant effect was found for immersion in water on
lating solutions p=0.0043. Results of surface roughness surface roughness of Lava Ultimate at all aging times.
testing are shown in Tables 2,3. At baseline, there was 2. Hardness results:
no significant difference in surface roughness between Surface micro-hardness was significantly affected by
Tetric CAD and Lava Ultimate (p=0.15). After aging in material (p<0.0001), immersion time( p=0.0002) and
ethanol, there were no statistically significant differen- by food simulating solutions (0.0026) as shown by the
ces between surface roughness at baseline and surface results of the Three-way ANOVA test. Results of sur-
roughness after storage for one, 10 and 15 days for both face micro-hardness testing are shown in Tables 4,5.
Lava Ultimate and Tetric CAD. However, surface rou- At baseline, Tetric CAD had significantly lower hard-
ghness of Lava Ultimate was significantly higher than ness than Lava Ultimate (p<0.0001). After immersion
that of Tetric CAD after 15 days of immersion. in ethanol, hardness values recorded at all timepoints
After immersion in MEK, surface roughness increased were not significantly different from baseline for both
Table 2: Three way ANOVA showing the effect of Groups and Time on roughness measurements(um).
Table 3: The means and standard deviations of roughness values (um) of Tertric CAD and Lava Ultima materials at baseline, after immer-
sion in water, ethanol, methyl ethyl ketone groups, at one day, 10 days and 15 days of immersion.
Tetric CAD Group Lava Ultimate group
Baseline 0.322±0.056 aAC 0.346±0.057 aACF
Water Ethanol Methyl Ethyl Water Ethanol Methyl Ethyl
Ketone Ketone
1 day 0.340±0.052 aAB 0.371±0.075 aA 0.339±0.046 aA 0.355±0.057 bB 0.381±0.050 bcA 0.372±0.05 cFE
10 days 0.315±0.040 dA 0.293 ±0.049 dC 0.300±0.049 dA 0.388±0.067 eAB 0.293 ±0.076 fC 0.404±0.093 eDE
15 days 0.379±0.010 gB 0.293±0.082 kC 0.335±0.059 gkA 0.358±0.114 hAB 0.396±0.086 hiA 0.432±0.057 giD
Means with the same small letters have statistically non-significant difference in each row (separate materials)
Means with the same capital letters have statistically non-significant difference in each column
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Table 4: Three way ANOVA showing the Effect of Groups and Time on hardness measurements (kg.mm-2).
Table 5: The means and standard deviations of hardness values (kg.mm-2) of Tertric CAD and Lava Ultima materials at baseline, after
immersion in water, ethanol , methyl ethyl ketone groups, at one day, 10 days and 15 days of immersion.
Tetric CAD Group Lava Ultimate group
Baseline 87.66±8.13 aA
132.26±8.77 bAB
Water Ethanol Methyl Ethyl Water Ethanol Methyl Ethyl
Ketone Ketone
1 day 85.03±7.97 bA 94.49±11.82 aA 86.80±4.88 abA 124.02±11.84 cA 134.63±23.24 cA 126.72±9.71 cAB
15 days 81.43±8.45 hiA 86.53±3.48 hA 79.97±4.09 iB 130.12 ±4.91 jAB 132.55±8.00 jA 134.50±9.56 jA
Means with the same small letters have statistically non-significant difference in each row (separate materials)
Means with the same capital letters have statistically non-significant difference in each column
the materials. Following aging in MEK, micro-hardness 1A,2A’); photomicrographs of Tetric specimens immer-
significantly decreased from baseline for Tetric CAD at sed in ethanol show fewer polymer matrices with well
10 and 15 days (p<0.0001), and for Lava Ultimate at 10 prominent filler particles and very few narrow porosities
days. Immersion in water significantly increased surface (Figs. 1B,2B’); photomicrographs of Tetric specimens
hardness for Lava Ultimate after 10 days compared to immersed in methyl ethyl ketone show fewer polymer
baseline (p=0.0084). Nevertheless, no significant effect matrices with well prominent filler particles and few
was found for immersion in water on the surface hard- smaller sized porosities (Figs. 1C, 2C’).
ness of Tetric CAD at all immersion times (p=0.1617). Photomicrographs of Lava specimens immersed in disti-
At all periods of immersion in distilled water, ethanol, lled water show polymer matrices with multimodal filler
and methyl ethyl ketone, the Lava group had significant- particle size distribution and fewer pinpoint porosities
ly higher surface hardness values compared to the Tetric (Figs. 1D,2D’); photomicrographs of Lava specimens
group, p<0.0001. immersed in ethanol show less polymer matrices on the
-Surface morphology evaluation top surface with well prominent filler particles of hetero-
Figures 1 and 2 show scanning electron photomicrogra- geneous size distribution and large irregular size deepe-
phs of Tetric and Lava Groups for specimens immer- ned porosities (Figs. 1E,2E’); photomicrographs of Lava
sed for 15 days in storage solutions (X 1000, 3000 and specimens immersed in methyl ethyl ketone show fewer
5000). Photomicrograph of Tetric specimens immersed polymer matrices on the top surface with well prominent
in distilled water show a well condensed polymer ma- filler particles of heterogeneous size distribution and lar-
trix with filler particles and negligible porosity (Figs. ge sized porosity (Figs. 1F,2F’).
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Fig. 1: Scanning electron photomicrograph of Tetric CAD (left column) and Lava Ultimate (right
column) specimens immersed for 15 days in storage solutions at X 3000 and X 1000 (smaller im-
age). A,B,C photomicrographs of Tetric specimens after immersion for 15 days in distilled water,
ethanol, and methyl ethyl ketone respectively. D,E,F photomicrographs of Lava Ultimate speci-
mens after immersion for 15 days in distilled water, ethanol, methyl ethyl ketone respectively.
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Fig. 2: Scanning electron photomicrographs of Tetric CAD (left column) and Lava Ultimate
(right column) specimens immersed for 15 days in storage solutions at X 5000. A’,B’,C’ photomi-
crographs of Tetric specimens after immersion for 15 days in distilled water, ethanol, methyl ethyl
ketone respectively. D’,E’,F’ photomicrographs of Lava Ultimate specimens after immersion for
15 days in distilled water, ethanol, methyl ethyl ketone respectively.
after 7 days then significantly decreased after 30 and lling and plasticization of the material. The plasticizing
60 days (12). effect of ethanol on dental composites was reported in
Surface roughness is an important characteristic that several investigations (17-20). It was suggested that the
could impact the aesthetics and longevity of tooth colo- increased plasticization could render surface flaws less
red restorations. Chemical degradation in the oral cavity severe (21,22).
can increase surface roughness thus promoting plaque However, the dimensional changes due to swelling of
adhesion with subsequent discoloration, gingival in- resin based polymers can cause stresses on the bond
flammation, and secondary caries (16). In this study, a between the matrix and filler leading to its failure and
contact profilometer was used to assess surface rough- the formation microcracks within the matrix. The sub-
ness of both types of resin composite CAD/CAM blocks sequent debonding of the inorganic filler particles will
after immersion in three different food simulating fluids. result in porosities that would be expected to increase
There were no significant differences in roughness va- surface roughness (23). Ferracane and Marker observed
lues for both types of materials from baseline after im- cracking in resin composite matrix and resin filler inter-
mersion in ethanol at all timepoints, yet the recorded face after immersion in ethanol using SEM (24). This
roughness of LAVA ultimate was significantly higher could explain the significantly higher roughness of Lava
than that of Tetric CAD. On storage in fluids, resin based Ultimate compared to Tetric CAD blocks after immer-
matrices tend to absorb the fluids whose molecules per- sion in ethanol. Both the materials utilize nanohybrid
colate the network and diffuse between polymer chains. filler technology. Tetric CAD contains silica nanoparti-
An increase in distance between chains results in swe- cles (<20 nm) and barium glass particles with a size < 1
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μm, whereas Lava Ultimate comprises silica and zirco- it resists surface penetration and indentations, increasing
nia nanomers (6-20 nm) and silica and zirconia aggrega- the surface hardness, indicates the higher the mechanical
ted nanoclusters (6-10 μm). It could be postulated that properties. Chemical degradation of these CAD/CAM
the loss of larger sized nanoclusters in Lava Ultimate composites after immersion in food simulating fluids, as
(Figs. 1E,2E’), due to filler debonding, would lead to an evidenced by a decrease in hardness, is due to diffusion
increase in surface roughness compared to the loss of of solvent molecules between filler particles and matrix.
smaller barium and silica that might occur in Tetric CAD This resulted in fillers dislodgement from the polymer
as observed in Figs. 1B,2B’. Furthermore, Tetric CAD matrix. Diffusion of solvent molecules within the ma-
comprises a higher percentage of resin matrix (28.4%) trix structure also made it softer and less wear-resistant
than Lava Ultimate (20%), so it would be expected to (30). The average surface hardness of Lava Ultimate
be more prone to plasticization caused by ethanol (25). was significantly higher than Tetric CAD at baseline le-
The sorption and solubility properties of polydimetha- vel; this might be attributed to its higher percentage of
crylate based polymers is affected by several factors filler loading, type of filler (zirconia) and their intimate
such as the presence of reinforcing fillers, the resin frac- compaction due to their nanocluster composition aggre-
tion, the hydrophilicity of the polymer, the cross-linking gation (31). The increase in filler content was shown to
of the polymer network and most importantly the diffe- result in lower water absorption, and consequently redu-
rence between the solubility parameters of the polymer ced surface degradation (31). Water absorption and hy-
and that of the solvent (26). The square root of the cohe- drolytic degradation of the filler surface can predispose
sive energy density of a solvent is used to calculate its to filler/matrix cracking which has been shown to ad-
solubility parameter (25). The smaller the difference in versely affect the mechanical properties of composites
solubility parameters of the polymer and the solvent, the (32). In this study, the surface microhardness of Tetric
greater the solvent uptake and polymer solubility. The CAD decreased in-significantly than the baseline when
solubility parameters of ethanol and MEK are close to being immersed in distilled water and ethanol solutions
that of the dimethacrylate monomers commonly used in for 15 days, while significantly decreased in MEK solu-
dental resin composites. After immersion in MEK, both tion. The decrease in hardness in MEK solution can be
the materials in this study showed an increase in sur- attributed to its solubility parameter that is closer to the
face roughness compared to the baseline being signifi- resin and thus more resin degradation occurred, as noted
cant only for Lava Ultimate. The solubility parameter in Figs. 1C,2C’).
of dimethacrylate based resins (18.6 δ/MPa1/2) is closer On the other hand, the surface microhardness of Lava
to that of MEK (19.3 δ/MPa1/2) than ethanol (26.2 δ/ Ultimate group decreased in-significantly than the base-
MPa1/2) and more different than water (48 δ/MPa1/2). line when being immersed in distilled water and ethanol
Accordingly, the resin degradation would be expected to for 15 days. However, it increased in-significantly after
be more evident with MEK than with ethanol (27,28). being immersed in MEK, this might be due to the higher
The scanning electron micrographs of Tetric CAD spe- fillers loading and their nanoclusters distributions, that
cimens (Figs. 1C,2C’) showed a surface with exposed was maintained and highly compacted as seen in Figs.
inorganic fillers with increased resin degradation which 1F,2F’), the little effect of resin matrix dissolution as the
could be due to the increased solubility of resin in MEK. Lava ultimate has 20% resin content.
On the other hand, Lava Ultimate showed an increase in
roughness at all recorded timepoints after MEK immer- Conclusions
sion and the highest roughness value among the speci- The surface properties of CAD/CAM machinable com-
mens after immersion in the three liquids for 15 days. posites were variably impacted by the exposure to di-
Immersion in water affected the surface roughness of fferent aging media. Both materials showed greater
Tetric CAD in which roughness values increased signi- stability in surface properties when being immersed in
ficantly from the baseline. Sideridou et al. described the ethanol than MEK. Hence, the surface degradation im-
degradation of direct composite surfaces due to water plies the advisability of more research involving increa-
absorption. Water uptake can lead to softening of the sed immersion periods and involvement of thermocy-
resin matrix, hydrolysis of the silane coupling agent, cling changes.
microcrack formation, resin degradation and filler de-
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