UNIVERSIDADE ESTADUAL PAULISTA
JÚLIO DE MESQUITA FILHO”
Instituto de Ciência e Tecnologia
Campus de São José dos Campos
ORIGINAL ARTICLE DOI: https://doi.org/10.4322/bds.2024.e4433
1
Braz Dent Sci 2024 Oct/Dec;27 (4): e4433
This is an Open Access article distributed under the terms of the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in
any medium, provided the original work is properly cited.
Evaluation of monomer conversion, Vickers hardness, compressive
strength & water sorption of commercial dental composite resins
Avaliação da conversão de monômeros, dureza Vickers, resistência à compressão e sorção de água de resinas compostas
dentárias comerciais
Saadia Bano LONE1 , Usama SIDDIQUI2 , Nayab AMIN2 , Munazzah EJAZ3 , Saad LIAQAT4 , Anila ASIF5 ,
Zohaib KHURSHID6,7
1 - Rashid Latif Medical and Dental College, Department of Dental Materials. Lahore, Pakistan.
2 - Rehman College of Dentistry, Department of Dental Materials. Peshawar, Pakistan.
3 - Sardar Begum Dental College, Department of Dental Materials. Peshawar, Pakistan.
4 - Khyber Medical University, Institute of Basic Medical Sciences, Department of Dental Materials. Peshawar, Pakistan.
5 - COMSATS University Islamabad, Interdisciplinary Research Center in Biomedical Materials. Lahore, Pakistan.
6 - King Faisal University, College of Dentistry, Department of Prosthodontics and Dental Implantology. Al-Ahsa, Saudi Arabia.
7 - Chulalongkorn University, Center of Excellence for Regenerative Dentistry, Faculty of Dentistry, Department of Anatomy. Bangkok,
Thailand.
How to cite: Lone SB, Siddiqui U, Amin N, Ejaz M, Liaqat S, Asif A, et al.] Evaluation of monomer conversion,
Vickers hardness, compressive strength & water sorption of commercial dental composite resins. Braz Dent Sci. 2024;27(4):e4433.
https://doi.org/10.4322/bds.2024.e4433
ABSTRACT
Objective: The objective was to compare four commercially available resin-based composites so that clinicians
can select an economic material that has better monomer conversion and improved mechanical properties with
lower water sorption. Material and Methods: Four commercially available resin-based composites were used.
These included “Z350” and “Z250” by 3M, “Charisma” by Heraeus, and “All Purpose” by Dentex. Fourier transform
infrared spectroscopy was done in attenuated total reluctance mode before curing and after curing to evaluate
the degree of conversion. For hardness and compressive strength, specimens (n=5) were cured from both sides
followed by storing them in distilled water. Then they were placed in an oven at 37 °C for 24 h, and tests were
performed. The water sorption study was done for 7 days. Results: One-way ANOVA and then post hoc Tukey’s
test (p 0.05) were done to analyze the data. The pattern of degree of conversion was Z250>Z350>Charisma>All
Purpose. The mean hardness value of Z250 was the highest followed by Charisma, Z350, and All Purpose. In
the case of compressive strength, the pattern was Charisma>Z350>Z250>All Purpose. Z250 had less water
sorption followed by All Purpose, Z350, and Charisma. Conclusion: According to the obtained results of this
in-vitro
study Z250 can be a resin resin-based composite of choice for clinicians as it has all the acceptable results
and is a mid-range in price.
KEYWORDS
Compressive strength; Degree of conversion; Hardness; Resin-based composites; Water sorption.
RESUMO
Objetivo: O objetivo foi comparar quatro compósitos à base de resina disponíveis no mercado para que os clínicos
possam selecionar um material económico que tenha uma melhor conversão de monômeros e propriedades
mecânicas melhoradas com menor sorção de água. Material e Métodos: Foram utilizados quatro compósitos à
base de resina disponíveis no mercado. Estes incluíam a “Z350” e a “Z250” da 3M, a “Charisma” da Heraeus e a
“All Purpose” da Dentex. A espetroscopia de infravermelhos transformada de Fourier foi efectuada no modo de
relutância total atenuada antes da cura e após a cura para avaliar o grau de conversão. Para a dureza e a resistência
à compressão, os espécimes (n=5) foram curados de ambos os lados e depois armazenados em água destilada.
Em seguida, foram colocados numa estufa a 37 °C durante 24 h e foram efectuados testes. O estudo da absorção
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Braz Dent Sci 2024 Oct/Dec;27 (4): e4433
Lone SB et al.
Evaluation of monomer conversion, Vickers hardness, compressive strength & water sorption of commercial dental composite resins
Lone SB et al. Evaluation of monomer conversion, Vickers hardness,
compressive strength & water sorption of commercial dental
composite resins
INTRODUCTION
Dental caries is well-known as tooth decay,
and it is a predominant disease that has an impact
on the human population globally [1]. These
defects may be rehabilitated by specially designed
dental materials called dental restorative materials
or lling materials which are manufactured to
restore the function, integrity, and structure of the
missing structure [2]. Previously, several novel
restorative materials have been manufactured
that have superior predictability and reliability
for dental clinicians [3]. Commonly used
dental restorative materials include resin-based
composites (RBCs), glass ionomer cement,
amalgams, compomers, and ceramics. Among
these, RBCs have the advantage of esthetics
as they are available in different shades and
can resemble natural tooth color [4,5]. RBCs
are primarily composed of dimethacrylate
resin, fillers, and silane coupling agents to
enhance the bond between non-organic llers
and organic matrix. Moreover, agents such
as camphorquinone, diethyl amino benzoate,
benzoyl peroxide, butylated hydroxy toluene, etc.
are added which promote, enhance, or control
polymerization reaction [6].
RBCs are now essential materials of
contemporary restorative dentistry [7]. They are
customized based on need as restorative, sealants,
cement, or provisional materials because of their
practical adaptability and aesthetic benets [8].
There are many clinical situations such as closing
of diastema, carious lesions in anterior regions,
treatment of discoloration, and dental trauma of
anterior teeth in which only RBCs can be used
due to aesthetic reasons [9]. The main concern
of RBCs is sensitivity due to monomer elution
because of incomplete polymerization [10].
Besides this, the prime cause of restoration failure
is the breakage of RBCs [11].
Although clinical outcomes have improved
due to ongoing advancements in formulations
of RBCs, choosing the best material remains a
challenge for practitioners [12]. The performance
and long-term success of these materials are
greatly inuenced by factors such as monomer
conversion, mechanical properties, and water
sorption [13].
Various in-vitro tests are done to analyze
the properties of RBCs to evaluate their
longevity and to judge the problems in present
RBCs. These include water sorption, degree of
conversion [14,15], hardness, and compressive
strength [16]. The mechanical strength and
durability of the composite are greatly inuenced
by monomer conversion, which is the degree to
which resin monomers are polymerized during
curing [17]. Low conversion rates may have
detrimental effects on patient safety and the
longevity of the restoration by causing less-
than-ideal mechanical properties, increased
wear, and the possible release of unreacted
monomers [18]. Moreover, mechanical properties
such as compressive strength, and hardness are
crucial for withstanding harsh oral environments
as variable chewing forces, food of various
hardness, temperature and pH may contribute
to further deterioration [19]. Additionally, water
sorption is also crucial since too much moisture
absorption can cause hydrolytic deterioration,
dimensional instability, and discoloration,
which will ultimately impair the appearance and
functionality of RBCs [20].
Therefore, for long-term promising clinical
applications of the materials, a high degree of
conversion and superior mechanical properties
are very important. Various companies have
developed different RBCs which are available
in the market under different brand names
and different price ranges claiming all have
de água foi efectuado durante 7 dias. Resultados: ANOVA de uma fator e, em seguida, teste post hoc de Tukey
(p 0,05) foram feitos para analisar os dados. O padrão do grau de conversão foi Z250>Z350>Charisma>All
Purpose. O valor médio de dureza do Z250 foi o mais elevado, seguido do Charisma, do Z350 e do All Purpose.
No caso da resistência à compressão, o padrão foi Charisma>Z350>Z250>All Purpose. A Z250 teve menos
sorção de água, seguida pela All Purpose, Z350 e Charisma. Conclusão: De acordo com os resultados obtidos
neste estudo in vitro, a Z250 pode ser um compósito à base de resina de escolha para os clínicos, pois apresenta
todos os resultados aceitáveis e tem um preço médio.
PALAVRAS-CHAVE
Resistência à Compressão; Grau de conversão; Dureza; Compósitos resinosos; Sorção de água.
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Braz Dent Sci 2024 Oct/Dec;27 (4): e4433
Lone SB et al.
Evaluation of monomer conversion, Vickers hardness, compressive strength & water sorption of commercial dental composite resins
Lone SB et al. Evaluation of monomer conversion, Vickers hardness,
compressive strength & water sorption of commercial dental
composite resins
optimal results and markets them with attractive
strategies to catch the interest of clinicians. In this
era of ination for cost cutting many clinicians
opt for cheaper available dental composite.
The aim of the study was to compare different
properties of various commercially available RBCs
in the market. With the help of evidence-based
data, we hope to help clinicians choose the best
restorative materials that maximize long-term
success while considering the price in this state
of ination.
MATERIAL AND METHODS
Materials
Four commercially available RBCs are
available in the market were analyzed. “Z350”
and “Z250” by 3M, “Charisma” by Heraeus,
and “All Purpose” by Dentex were tested. The
composition of all the types of RBCs provided by
the manufacturers used in this experiment are
explained in Table I.
Sample preparation
The mold was placed on a glass slab and
the material was poured into the mold carefully.
A single increment layer was placed, and to
prevent oxygen inhibition layer samples were
covered with mylar strip. Then, the light curing
unit having a wavelength of 470nm (LED,
Woodpecker) was used to cure both sides of the
samples. After curing, the samples were carefully
retrieved from the mold followed by polishing
with various grit papers (600, 800, and 1200)
under a steady ow of water. Five samples for
every test were made and subjected to testing.
The sample size was calculated as per the
following equation keeping the power of study
equal to 90% and level of signicance equal to
5% by the given formula below:
()
( )
2
22
1 12
12
2
12
ZZ
n
βα
σσ
µµ


++


=
(1)
1
Z score for power of study at 90% 1.28Z
β
= =
;
12
Z score for level of significance at 5% 1.96Z
α
= =
;
1
µ
-
(176.45- 54.20) = mean difference
(compressive strength) = 122.5;
2
1
σ
+
2
2
σ
[(50.59)2 + (8.62)2] = standard
deviations of the groups = 2633.64 [21];
Calculated sample size for each test = 2;
Sample Size is taken for each test = 5.
Characterizations
Degree of conversion (DOC)
Fourier Transform Infrared Spectroscopy
(FTIR) was used to investigate DOC. It was done
before as well as after the curing of samples.
FTIR (Thermo Nicolet 6700, USA) with ATR
cell (MTEC, USA) was used as a detector. The
detector is placed on the sample and the scan is
started. 256 scans were performed at a resolution
of 8 cm-1 and spectra were collected over the
region 4000–400 cm-1. OMINIC software (8.1.11,
Driver version 8.1, Firmware version 2.10) was
utilized to analyze the data peaks which were
matched from the software library. DOC was
computed by the given formula below:
( )
100 1 / DC R polymerized R unpolymerized


= ×−
(2)
where DC represents the degree of conversion, R
denotes the ratio of the peak height of polymerized
and unpolymerized samples [22,23].
Vickers hardness (VHN)
VHN was evaluated for samples which were
disc-shaped samples having dimensions of 2 mm
× 8 mm (height x diameter). A total of 5 samples
Table I - Information on the composition of dental materials is
provided by the manufacturer
Composite
Resin Classification Filler Resin
Z350 Conventional
Nanoparticle
Zirconia /
silica 75wt.
% or 59.5
vol%
bis-
GMA,
UDMA,
TEGDMA,
BISEMA
Z250 Nanohybrid
Zirconia/
silica 60
vol%
bis
-GMA,
UDMA,
bis
-EMA
Charisma Universal
hybrid
barium
aluminum
fluoride
glass, pre-
polymerized
filler 61 vol.%
bis
-GMA matrix
All Purpose Nanohybrid
Barium Glass
Nano Silica
34wt.%
bis
-GMA matrix
Where
bis
-GMA: stands for Bisphenol A glycidal methacrylate;
UDMA: Urethane dimeth acrylate;
bis
-EMA: ethoxylated bisphenol A
glycol dimethacrylate; TEGDMA: Triethylene glycol dimethacrylate.
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Lone SB et al.
Evaluation of monomer conversion, Vickers hardness, compressive strength & water sorption of commercial dental composite resins
Lone SB et al. Evaluation of monomer conversion, Vickers hardness,
compressive strength & water sorption of commercial dental
composite resins
were made in Teon mold. After keeping samples
in deionized water for 24 h and then in a desiccator
for 1 hour, the hardness was determined according
to ASTM E384-11 [24] when a 300 g load was
applied for 10 seconds on each sample site via
hardness tester (HVS 1000). The mean value was
calculated to determine VHN for samples as three
indentations were produced on each sample [25].
Compressive strength (CS)
CS was assessed for samples that were
cylindrical shaped having dimensions of 4 mm x
6 mm (diameter x height). A total of 5 samples
were made in Teon mold. The mold was placed
on a glass slab and the material was poured into
the mold carefully. A single increment layer was
placed, and to prevent oxygen inhibition layer
samples were covered with mylar strip. Then, the
light curing unit having a wavelength of 470nm
(LED, Woodpecker) was used to cure both sides
of the samples. After curing, the samples were
carefully retrieved from the mold followed by
polishing with various grit papers (600, 800, and
1200) under a steady ow of water. The samples
were kept in deionized water for 24 h then in a
dessicator for 1 hour and then subjected to testing.
The CS was determined via a Universal Testing
Machine having 0.5 mm.min-1 of cross-head speed,
according to ISO 4049-49. Peak compressive stress
(σc) was calculated after the peak compressive load
(P) withstood by each sample was noted [26].
Water sorption
Water sorption samples (n=5) were made
disc-shaped and it was determined in accordance
with the procedure mentioned in ANSI/ADA
Specication No. 27-1993 (ISO 4049). Samples
were placed at 37 °C in an oven for 24 h. Then,
they were taken out, placed for 1 h in a desiccator,
and weighed using a balance having an accuracy
of 0.1 mg. The weight of the sample was measured
[Analytical Balance, SHIMADZU, JAPAN (10mg)]
and recorded in dry and standard conditions.
Then, the samples were submerged for 7 days in
water at 37 °C. After 7 days they were removed
followed by blotted drying and weighing. The
percentage weight increase for each sample was
computed by using by the given formula:
( )
/
fii
W W WW


=
where Wf denotes the water saturation after
7 days of immersion (final weight) while Wi
denotes the initial weight [25].
Statistical analysis
Data were statistically analyzed by IBM SPSS
23 (Armonk, NY, USA) with mean ± standard
deviation. As the data was normally distributed
One-way ANOVA followed by Post Hoc Tukey’s
test was used for analysis while keeping the
signicance 0.05.
RESULTS
Fourier Transform Infrared (FTIR)
Spectroscopy
Z250 showed the highest DOC (69%)
followed by Z350 (55.2%), and Charisma (32.6%)
while the least degree of conversion was shown
by All Purpose (15%) as shown in Table II. There
was a statistically signicant difference between
DOC of all the RBCs compared. The DOC was
calculated by graphs shown in Figures 1 and 2.
Vickers hardness (VHN)
The mean VHN of Z250 was highest (97.57
VHN) followed by All Purpose (93.55 VHN),
Z350 (89.73 VHN), and Charisma (59.36 VHN)
respectively. The mean hardness along with
standard deviation is shown in Table II. There
was a signicant difference statistically between
Charisma and all other commercial composites
while no signicant difference amongst the other
three when compared between each other.
Table II - Mean Degree of Conversion, Hardness. Compressive strength and water sorption of commercial composite
Commercial
Composite
Degree of conversion
(%) ± SD
Hardness
(VHN) ± SD
Compressive Strength
(MPa) ± SD
Water sorption
(µg/mm3) ± SD
All Purpose 15 ± 3.2 59.36 ± 8.1 122 ±10.2 0.45 ± 0.28
Z250 69± 1.7 97.57 ± 7.5 184 ± 9.3 0.33 ± 0.28
Charisma 32.6 ± 2.4 93.55 ± 10.7 192 ± 12 0.82 ± 0.29
Z350 55.2 ± 1.4 89.73 ± 7.7 187 ± 7.7 0.53 ± 0.30
SD: Standard Deviation.
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Braz Dent Sci 2024 Oct/Dec;27 (4): e4433
Lone SB et al.
Evaluation of monomer conversion, Vickers hardness, compressive strength & water sorption of commercial dental composite resins
Lone SB et al. Evaluation of monomer conversion, Vickers hardness,
compressive strength & water sorption of commercial dental
composite resins
Compressive strength (CS)
The mean CS values of Charisma were
highest followed by Z350, Z250, and All Purpose.
The highest compressive strength was seen in
charisma which was 192± 12 MPa followed by
Z350 (187 ± 7.7 MPa), Z250 (184 ± 9.3 MPa),
and the least compressive value was observed
in All Purpose (122±10.2 MPa). There was a
signicant difference statistically between All
Purpose and all other commercial RBCs while
no signicant difference among the other three
when compared between each other.
Water sorption
Z250 had the least water sorption (0.33
± 0.28 µg/mm3) followed by All Purpose (0.45
± 0.28 µg/mm3), Z350 (0.53 ± 0.30 µg/mm3)
while Charisma had the highest water sorption
(0.82 ± 0.29 µg/mm3) as shown in Table II. There
was a signicant difference statistically between
Charisma and all other commercial composites
while no signicant difference amongst the other
three when compared between each other. The
mean water sorption of samples along with the
standard deviation after 7 days is shown in Table II.
Figure 1 - Degree of conversion of All purpose and Charisma.
Figure 2 - Degree of conversion of Z250 and Z350.
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Braz Dent Sci 2024 Oct/Dec;27 (4): e4433
Lone SB et al.
Evaluation of monomer conversion, Vickers hardness, compressive strength & water sorption of commercial dental composite resins
Lone SB et al. Evaluation of monomer conversion, Vickers hardness,
compressive strength & water sorption of commercial dental
composite resins
DISCUSSION
In dentistry, RBCs have been used by
dental clinicians for many years. Data related
to the properties of every product of RBCs is
not available in black and white. As well as
the ranking of various products in accordance
with their laboratory ndings does not indicate
their clinical performance [27,28]. This
in-vitro
study was conducted to analyze the mechanical
properties of different composites that are present
in the market with different price range and are
used in dental practices by our common dentist.
Both mechanical and physical properties
of RBCs are directly proportional to the DOC in
a polymerized sample. DOC depends upon the
amount of double bonds present after curing in
comparison to the double bonds present before
curing [29]. A higher degree of monomer conversion
means that there is a less unreacted monomer in
the mixture which may reduce the chances of
monomer leaching into the oral cavity, which in
turn enhances the longevity of restoration [30].
Dental materials when placed in oral cavity
absorb water and leach out unreacted monomer.
Moisture in the restoration acts as a plasticizer
resulting in detrimental mechanical properties and
compromised biocompatibility [31]. A minimal
degree of conversion for a dental restorative
material has not been clearly recognized till now
but the acceptable range is above 55% [32]. The
FTIR results showed that DOC is the maximum
for Z250 followed by Z350 and the relatively low
value was shown by Charisma and All Purpose.
Both Charisma and All Purpose had DOC less than
the acceptable value. Kim et al. [33] also showed
in their study that the conversion of Z250 is better
than Z350.
Teeth are continuously being subjected to
masticatory load and stresses in the oral cavity.
So, when a restoration or a prosthetic material is
placed it also shares the load applied. Continuously
load and stresses sometimes result in restoration
failure [34]. Vickers hardness test was done to
measure the surface hardness of the selected dental
composites. Surface hardness is an important
virtue because the relationship between surface
hardness and the physical properties of a material
is well known for good longevity of restoration
[35]. The mean hardness was maximum for Z250,
“All purpose” value was comparable to Z250.
Mota et al. [36] in their article evaluated Vickers
hardness of Z250 and results as comparable with
our study. Okulus and Voelkel [37] in their article
compare Charisma with nanocomposites which
gave good hardness results, but when compared
with hybrid composite in our study the results
were not comparable.
Compressive strength is the resistance to
fracture under compression and shows the potential
of a material to withstand vertical stresses. It is
important in extreme stress-bearing areas such
as the posterior region. Measuring compressive
strength is very benecial for determining materials
such as RBCs as they are generally weak and brittle
in tension. Compressive strength is deemed a key
index of success as a greater compressive strength
is essential to resist masticatory forces, though the
accurate value is unknown. The composition of
ller and ller load may have a substantial effect
on the mechanical properties. The mechanical
properties mostly increase with filler load for
the similar type of materials [38]. “All purpose”
showed relatively low compressive strength as
compared to Z250, Z350, and Charisma. The low
compressive strength of “All Purpose” may be
due to low degree of monomer conversion. In a
study where the compressive strength of Z250 was
evaluated, the results were similar to the results in
our study [36]. Saleem et al. [39], also evaluated
the compressive strength of Z350, although the
results were better comparable to our study. In
another study, Sonwane and Ramachandran [40]
evaluated the compressive strength of Z350 and
Charisma and the mean values obtained were less
than the mean values found in our study.
Water sorption to a specific degree is
unavoidable in the oral cavity as restorative
materials are in constant contact with saliva.
Moreover, they are exposed to masticatory load,
beverages, and food, thus changes in pH are
also present. The sorption phenomenon of RBCs
in an oral environment has adverse effects on
them [41]. As, the bond between the resin matrix
and ller particles is broken by the process of
hydrolysis when water molecules inltrate the
resin/ller interface through the process of dif-
fusion, therefore resulting in the deterioration of
ller particles and resin matrix [42] and initiating
adverse effects on the mechanical properties of
RBCs, which consequently impacts the longevity
of the RBCs. Moreover, allergic reactions may
occur in the patients due to eluted monomers and
additives in the oral cavity [43]. In RBCs, water
uptake is a diffusion-controlled mechanism and
mostly takes place in a resin matrix. The diffusion
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Braz Dent Sci 2024 Oct/Dec;27 (4): e4433
Lone SB et al.
Evaluation of monomer conversion, Vickers hardness, compressive strength & water sorption of commercial dental composite resins
Lone SB et al. Evaluation of monomer conversion, Vickers hardness,
compressive strength & water sorption of commercial dental
composite resins
coefcient is inversely proportional to the amount
of water in the resin matrix [44]. Thus, a decrease
in the amount of water uptake is to be anticipated
with an increase in storage time. Regarding
sorption, just Z250 had a value which was in
accordance with ISO 4049, i.e., water sorption
was below 40 µg/mm3 [45]. “Charisma” showed
the highest water sorption followed by Z350,
All Purpose and Z250. Kumar and Sangi [46]
evaluated the water sorption of Z250 which was
much more than the results obtained in our study.
Similarly, in another study, Syed et. al assessed
the water sorption of Z350 and the results were
comparable to our study [25].
CONCLUSION
Z250 showed a better degree of conversion,
hardness, and less water sorption. All Purpose
showed comparable hardness to Z250, but its
degree of conversion and compressive strength
was low. Charisma has the maximum compressive
strength, but its mean hardness value was very
low and water sorption value was high. Z350
showed a comparable degree of conversion and
mean hardness, compressive strength, and water
sorption values. Thus, according to this study, Z250
can be the RBC of choice for clinicians as it has all
the acceptable results and is a mid-range in price.
Author’s Contributions
SBL: Methodology, Formal Analysis. US:
Conceptualization, Methodology, Formal Analysis.
NA: Writing – Original Draft Preparation. ME:
Writing – Review & Editing. SL: Methodology,
Validation. AA: Supervision. ZK: Resources.
Conict of Interest
The authors declare no conict of interest
concerning the publication of this article.
Funding
There was no funding received from any
organization and it was self funded project.
Regulatory Statement
This was an in-vitro study which was
conducted according protocols mentioned in ISO
4049:2021 for Resin based Dental Composites.
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9
Braz Dent Sci 2024 Oct/Dec;27 (4): e4433
Evaluation of monomer conversion, Vickers hardness,
compressive strength & water sorption of commercial dental
composite resins
Lone SB et al.
Evaluation of monomer conversion, Vickers hardness, compressive strength & water sorption of commercial dental composite resins
Lone SB et al. Evaluation of monomer conversion, Vickers hardness,
compressive strength & water sorption of commercial dental
composite resins
Date submitted: 2024 June 30
Accept submission: 2024 Nov 06
Usama Siddiqui
(Corresponding address)
Rehman College of Dentistry, Department of Dental Materials, Peshawar, Pakistan
Email: siddiquiusama01@gmail.com