CLINICAL RESEARCH

Bond strength of a self-adhesive

resin cement to enamel and dentin
Virglio Vilas Boas Fernandes, Jr, Prof, MSc
Pindamonhangaba Dental School, Pindamonhangaba College, Brazil

Jos Roberto Rodrigues, Prof, DDS

Department of Restorative Dentistry, So Jos dos Campos Dental School,
So Paulo State University, Brazil

Joo Maurcio Ferraz da Silva, Prof, DDS

Department of Restorative Dentistry, So Jos dos Campos Dental School,
So Paulo State University, Brazil

Clovis Pagani, Prof, PhD

Department of Restorative Dentistry, So Jos dos Campos Dental School,
So Paulo State University, Brazil

Rodrigo Othvio Assuno Souza, Prof, DDS

Department of Restorative Dentistry, Federal University of Paraba,
Joo Pessoa, PB, Brazil

Correspondence to: Virglio Vilas Boas Fernandes Jr, Master in Restorative Dentistry
Rua Enseada, 46 Cidade Jardim, So Jos dos Campos, 12230630 So Paulo, Brazil;
Tel: +55 12 988040749; E-mail: virgiliovilas@hotmail.com

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Abstract

The enameldentin resin cement blocks

were sectioned to produce non-trimmed

The purpose of this study was to evalu-

bar specimens, which were divided

ate the influence of surface treatments

into two storage conditions: dry, TBS

and thermocycling on the microtensile

immediately after cutting; TC (5,000 x;

bond strength (TBS) of self-adhesive

5C/55C). The samples were submit-

resin cement to human enamel and

ted to TBS, and data were statistically

dentin. Eighty human third molars were

analyzed by ANOVA and Tukeys test.

selected. The crowns of 40 teeth were

The results showed statistical differ-

transversally sectioned, exposing the

ences between UnicemC and the oth-

mid-coronal dentin. The buccal surfac-

ers. UnicemPA and VR showed better

es of the other 40 teeth were grinded to

bond strength to dentin during the pe-

mm2

flat enamel area. Eighty

riod before and after thermocycling,

resin blocks were produced and ce-

respectively. For the enamel, UnicemP

mented to the dental surfaces with Re-

showed better bond strength for both

lyX Unicem, then grouped according to

situations. Only for UnicemPA did the

the surface treatment (n = 10): UnicemC

thermocycling

with no conditioning, UnicemP with 37%

the bond strength values. Within the lim-

phosphoric acid/15 s, and UnicemPA

its of this study, it could be concluded

with 37% phosphoric acid/15s plus ad-

that the bond strength is influenced by

hesive bonding (Single Bond 2). There

the surface treatments, and that ther-

were two control groups, one for enamel

mocycling decreases the bond strength

and the other for dentin: VR with 37%

of all groups, but significantly only for

phosphoric

UnicemPA.

obtain a 5

acid/15 s

plus

adhesive

bonding (Single Bond 2) plus Variolink II.

significantly

decrease

(Int J Esthet Dent 2015;10:146156)

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CLINICAL RESEARCH

Introduction

with good results on ceramic, metal pins,

and indirect restorations.11-14

Restorative dentistry has been continu-

Previous investigations have provided

ously modified by the development of

the materials context for the introduction

new products, including modifications

of self-adhesive resin cements, of which

of adhesive procedures, such as resin

RelyX Unicem (3M ESPE) represents the

cements.1,2

first of this new class of materials.15

With the advent of dual-curing resin-

Despite the factors reported previ-

based cements, there has been signifi-

ously, the inorganic composition of these

cant improvement in the cementation

systems comprise weak acids, which

gap,3

can reduce their bonding to enamel

inadequate polymerization,4 secondary

and their conditioning capacity when

procedures relating to marginal

infiltration.5

In addi-

compared to conventional phosphoric

tion, these cements have shown impor-

acid-etching procedures.10 On the other

tant features, such as high mechanical

hand, the demineralization process and

resistance and excellent esthetic6 and

the bonding to dentin are improved.16

caries, and marginal

adhesive

properties.7

However, cemen-

To optimize the conditioning capacity

tation procedures require careful clinic-

and reduce possible adhesive failures,

al manipulation due to the high number

manufacturers have developed prod-

of operative steps involved, which make

ucts with low pH, leading to an increase

them a critical and sensitive technique.

in their acidity and the degree of condi-

Moreover, to increase the bonding to

tioning. However, they can be consid-

these cements, the acid etching of the

ered more biologically aggressive.17,18

dental surface is recommended, which

can result in dental sensitivity.8

Although self-conditioning cements

have certain advantages (mainly their

have

practicality and the reduced clinical

been recently introduced onto the mar-

time), further studies have been required

ket with the objective of combining the

to test their adhesive efficiency. This is

simple manipulation of glass-ionomer

what encouraged the present study to

cements with the mechanical, esthetic

assess one of these cements in terms

and adhesive properties of resin-based

of its bond strength to both enamel and

cements. This process is based on den-

dentin.

Self-adhesive

resin

cements

tal surface etching by a methacrylate

The hypotheses were: (1) that the

monomer, which contains groups of

bond strength is influenced by particular

phosphoric acids that can etch and dif-

surface treatments; and (2) that thermo-

fuse through the dental surface without

cycling decreases the bond strength to

the need of previous treatment,9 simplify-

both enamel and dentin.

ing adhesive procedures. This results in

a lower risk of dental sensitivity because
of the reduced possibility of non-impreg-

Material and methods

nated and demineralized dentin.10

Some authors have investigated the

The present study was approved by

bond strength of these cement agents,

the Ethical Committee in Research, No.

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FERNANDES JR ET AL

Table 1

Description of dental materials selected

Commercial name

Manufacturer

Variolink II

Ivoclar Vivadent

Adper Single Bond 2

3M ESPE

Composition

#JT(."6%."5&(%."%."CBSJVN
TVMGBUF
Ba-Al-F-Si-glass/silica, Benzoperoxiglycerol

#JT(."a, HEMAb, dimethacrylate, methacrylate

functional copolymer of polyacrylic and polytaconic
acid, water, alcohol, photoinitiator

Base paste: methacrylate monomers with phosphoric acid, methacrylate monomers, silanized fillers,
RelyX Unicem

3M ESPE

initiator, and stabilizers

Catalyst paste: methacrylate monomers, alkaline
fillers, silanized fillers, initiator components, and
stabilizers

067/2008 PH/CEP of the So Paulo

week later, the resin block surfaces were

State University UNESP, So Jos dos

airborne-particle abraded using 30-m

Campos, Brazil.

Al2O3 for 10 s under a pressure of 1 bar

The trade name and composition of

(MicroEtcher ERC, Danville).

dental materials selected for this research are presented in Table 1.

Dental preparation

Resin blocks manipulation

For the enamel groups, 40 extracted

human third molar teeth were cleaned

A silicone mold was used to prepare 80

and submitted to finishing and polish-

blocks (2 mm x 4 mm x 4 mm) of Z1OO

ing with 600-, 800- and 1,200-grit met-

direct composite resin (3M ESPE). The

allographic paper in a polishing ma-

resin was applied into the mold in 2 incre-

chine (DP-10, Panambra) in order to

ments (1 mm). Each increment was light

obtain a 5 mm2 enamel flat area on the

cured through a light-curing unit (Curing

buccal surface.

Light XL 3000, 3M ESPE) for 1 min at a

light intensity of 600

mW/cm2.

For the dentin groups, 40 teeth had

Before the

one third of their coronal part removed

polymerization of the last increment, a

with the aid of a diamond disc at low

polyester strip was placed onto the top

speed, and were then submitted to the

of the mold to achieve a flat and uniform

same protocol as described for the

surface. The final light curing was ob-

enamel groups.

tained by placing the resin blocks into

All surfaces were cleaned with 70%

a light oven for a period of 4 mins. One

alcohol solution prior to the cementation.

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CLINICAL RESEARCH

Cementation protocol

All specimens were stored in distilled

water at 37C for 24 h before sectioning.

The resin blocks and teeth were ran-

Following the storage period, the speci-

domly divided into 8 groups according

mens were sectioned into 6 mm-long mi-

to the dental surface treatment and the

crobars using the diamond-coated disc

luting material.

of a precision cutting machine (Labcut

UnicemC groups: two pastes of du-

1010, Extec), at 300 rpm in cold water.

(RelyX

The sections were performed from the

Unicem) were mixed using similar pro-

mesial to the distal sides and from the

portions and applied onto the previously

cervical to the occlusal surfaces in order

polished dental surface. A resin block

to obtain a 1 mm2 cross-section adhe-

was placed over the cement area and

sive area for each microbar.

al-cured

resin-based

cement

kept under a pressure of 20 N with the

About 9 specimens were obtained

arm of a prosthetic delineator. Five mins

from each resindental surface block.

later, the cement excess was removed

The

and the sample was light activated. The

chined (non-trimmed) bonding areas,

cement was then light cured for 40 s

with a bonded area measuring approxi-

through each side of the resin block.

mately 1.0 0.1 mm2.

UnicemP

groups:

the

dental

beam

specimens

had

non-ma-

sur-

The 9 specimens were then randomly

face was etched with 37% phosphoric

divided into 2 testing conditions. In the

acid (Vococid, Voco) for 30 s (enamel)

dry condition (Dry), the specimens were

and 15 s (dentin), rinsed for 60 s with

immediately submitted to microtensile

water, and dried prior to the cementa-

testing after sectioning. In the aged con-

tion. Thereafter, the luting agent (RelyX

dition (TC), the specimens were sub-

Unicem) was mixed and applied, as pre-

mitted to thermocycling (5,000 cycles;

viously described.

5C/55C, dwelling time: 30 s, transfer

UnicemPA groups: the dental surface was etched with 37% phosphoric

time: 2 s) (Nova Etica) and then submitted to testing.

acid (Vococid) for 30 s (enamel) and

15 s (dentin), rinsed for 60 s with water,

Microtensile bond strength test

and gently dried with the aid of a cotton pellet to maintain adequate humidity

The microbar specimens were attached

prior to the cementation. Two thin lay-

with cyanoacrylate gel (Super Bonder

ers of adhesive (Adper Single Bond 2,

(FM
-PDUJUF

UP
UIF
NJDSPUFOTJMF
EFWJDF

3M ESPE) were actively applied onto the

of a universal testing machine (DL1000,

conditioned surface of the enamel and

EMIC) (Figs 1a and 1b) and submitted

dentin with the aid of a microbrush and

to an axial tensile on the adhesion inter-

light cured for 10 s. Thereafter, the luting

face at a 0.5 mm/min crosshead speed.

agent (RelyX Unicem) was mixed and

The fracture surfaces were analyzed

applied, as previously described.

under light microscopy (x 40) (Olym-

The VR groups received the same

pus, CBB). The type of adhesive failure

cementation protocol as the UnicemPA

was classified into different categories:

groups.

adhesive failure at the enamelcement

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FERNANDES JR ET AL

interface; mixed adhesive and cohesive

failure of the cement; adhesive failure
at the cementresin interface, and adhesive failure at the dentincement interface.

Statistical analysis
Descriptive statistics were used to evaluate the results, including the three-way

Fig 1a

ANOVA (cements, thermal cycling, and

before the experiment.

Testing sample

dental substrate [enamel or dentin]) and

Tukeys post-hoc test. Significance for all
statistical tests was set at P 0.05 (95%
significance).

Results
The ANOVA results are shown in Table 2.
The mean (in MPa) and standard deviation values for all groups are shown in

Fig 1b

Table 3.

after the experiment.

Table 2

Testing sample

Results of three-way ANOVA for TBS data (P <0.05)

Source

DF

SS

MS

2721.68

907.228

47.27

0.0001

385.51

385.511

20.08

0.0001

C*T

517.67

172.566

8.00

0.0002

32

614.21

19.194

4.86

4.858

0.09

0.7628

C*S

808.77

269.588

5.14

0.0051

T*S

78.95

78.951

1.51

0.2287

C*T*S

44.05

14.682

0.28

0.8394

Residual II

32

1677.50

52.422

Total

79

6853.19

Residual I

C: cements; T: thermal cycling; S: dental substrate; * interaction between factors.

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CLINICAL RESEARCH

Table 3

Mean (in MPa) and standard deviation values for all groups

Mean
Group

Cement

Surface
treatment

Dental
surface

Before
thermocycling

After
thermocycling

UnicemC

RelyX Unicem

None

Enamel

11.94A 1.02

11.37A 1.04

UnicemC

RelyX Unicem

None

Dentin

9.65A 0.39

8.76A 0.53

UnicemP

RelyX Unicem

Acid etching

Enamel

29.85A 11.67

29.12A14.14

UnicemP

RelyX Unicem

Acid etching

Dentin

23.97A 4.17

15.53A3.30

UnicemPA

RelyX Unicem

Acid etching +
Single Bond 2

Enamel

25.93A7.19

16.29B 2.79

UnicemPA

RelyX Unicem

Acid etching +
Single Bond 2

Dentin

36.20A 10.65

20.64B 2.07

VR

Variolink II

Acid etching +
Single Bond2

Enamel

18.57A 3.11

19.91A 3.64

VR

Variolink II

Acid etching +
Single Bond 2

Dentin

22.46A 1.46

21.85A 1.91

Note:

and

refer to significant differences (Tukeys test: = 0.05).

According to ANOVA, it could be veri-

There was no significant difference

fied that the UnicemPA and the VR ce-

among the mean values of the enamel

ment groups showed the greatest mean

and dentin groups for all types of ce-

values for the bond strength in the dentin

ments (Fig 2).

groups, before and after thermocycling,

All groups presented mixed failure as-

respectively, while the UnicemP group

pects, except for the UnicemC group, in

showed the greatest mean values for the

which the main failure was the adhesive

enamel groups.

property between the cement and either

The UnicemP group showed smaller

the enamel or the dentin.

statistical bond strength values for all

groups.
There was a significant decrease in

Discussion

the bond strength values only for the

UnicemPA group due to the thermocy-

During the cementation process of an in-

cling procedure.

direct restoration, the cementing agent

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FERNANDES JR ET AL

needs to be placed between the tooth

and the restoration to form two distinct

30

interfaces: restorationcement and cementdental surfaces. The adhesion be-

25

tween resin-based cements and indirect

relevant problem for the clinical practice.19,20 However, the adhesion between

20
MPa

restorations is not considered to be a

R
RAC
RACAS

15

10

the dental substrate and resin-based

cements, which is necessary to increase
the durability of the system/tooth restor-

5
0

ation, has been difficult to achieve.21-23

d
Substrato

In order to obtain an adequate adhesion

between the dental substrate and resin-based cements, surface treatments,

Fig 2

Comparative

mean

values

among

the

enamel and dentin groups for each type of cement.

such as total acid etching24,10,25 and/or

the use of adhesive systems, have been
commonly performed.
The replacement of phosphoric acid

fore beginning the light curing increased

conditioning by the acidic monomers

the bond strength of self-adhesive res-

present in self-adhesive cements pro-

in-based cements. The increase in con-

motes low interprismatic hybridization,

tact time between cementenamel be-

and consequently weak adhesion.10,14,26

fore the light curing possibly increased

This may explain, in a simplified way, the

the substrate surface conditioning and

similarity between the results obtained for

impregnation with resin-cement mono-

the RelyX Unicem groups. De Munck21

mers, promoting a more effective union.

demonstrated that despite the low pH of

De Munck24 reports that previous acid

those cements, an apparent demineral-

conditioning can significantly increase

ization of tooth surface is hardly notice-

enamel adhesive resistance because

able. Yet, according to that author, this

of its high mineral content; however, it

may occur due to both the high viscosity

can decrease in the case of dentin. The

of those cements and poor penetration

increase in enamel adhesive resistance

due to insufficient time, as the immedi-

can be explained by the improvement

ate polymerization was carried out after

in the way the substrate is conditioned,

the application of the resin cement.

which makes it easier for impregnation to

Based on this statement, a prelimi-

occur. The resistance decrease can be

nary study was performed to test the in-

explained by the removal of the smear

fluence of the time period between the

layer, which should be incorporated into

application of the resin cement and the

the hybrid layer after polymerization.

beginning of the light curing on enamel

Further, the collagen fibrils of the den-

cement bond strength. The results ob-

tin exposed by the acid treatment are

tained in this first test demonstrated that

not filled by the resin cement because

a waiting period of more than 5 mins be-

of its high viscosity, thus creating a more

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CLINICAL RESEARCH

susceptible zone for degradation as a

the hydrolysis reaction and the adhesive

result of the activation of dentin colla-

resistance throughout the time, simulat-

genases (metalloproteinases), which in

ed in in vitro studies by thermocycling.

turn leads to postoperative sensitivity.

It should be noted that despite the in-

The present study showed a significant

crease in the bond strength of both the

increase in adhesive resistance, both

UnicemP and UnicemPA groups, the

for enamel and dentin, when the acid

cementation protocols used for these

conditioning (UnicemP) was carried out,

groups should not be used in clinical

which does not accord with what has

practice as they are not recommended

been noted by this author. However, for

by the manufacturers and do not act

UnicemP, a more marked decrease was

like self-etching resin-based cements.

seen on dentin after thermocycling.

The protocols used for these groups in

The thermocycling significantly de-

this study were undertaken to compare

creased the adhesion values for the

the procedures recommended by the

UnicemPA groups only. According to

manufacturers, without the intention of

Holderegger,16

proposing a new application technique.

this

occurs

because
the

Moreover, variables that affect ce-

quality of the hybridization layer. This

mentation, such as saliva, tongue, mu-

can be established by the pretreatment

cosa, and gingival fluid, are not present

of the surface of conventional cements.

in a laboratory study, which may have in-

If this is a porous layer, water molecules

creased the bond strength values of the

can penetrate and hydrolysis will occur.

UnicemPA, UnicemP, and VR groups,

Yet, according to this author, the primer

compared to the UnicemC groups. As

acid-base reaction of some adhesives

there are so few operative steps with

with the amines used in the initiation of

self-etching cements, they are less sus-

some cements leads to a smaller degree

ceptible to these variables, and more

of polymerization. It therefore allows the

advantageous over time. Further, ac-

hydrolysis of the hybrid layer and, sub-

cording to the manufacturers instruc-

sequently, a decrease in the adhesive

tions, the use of RelyX Unicem cement

resistance and an increase in nanoleak-

(UnicemC group) will provide a more

age.

practical handling and a lower risk of

composite

cements

depend

on

This did not occur in the case of the

hydrolysis degradation. This, together

cements from the UnicemC group, as

with a coronal preparation with satisfac-

there is no primer solution in the hybridi-

tory mechanical retention and a previ-

zation, which possibly explains the small

ous enamel etching with phosphoric

standard deviation for this group.

acid, makes this a material (as a luting

It is important to point out that, in the

agent for indirect restorations) with good

UnicemPA groups, even with a signifi-

clinical applicability and low risk of ad-

cant decrease in the adhesive resist-

hesive failure.

ance, after 5,000 cycles they showed

mean values above those of the UnicemC
groups. Future studies are required to
demonstrate the relationship between

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Conclusion

face for all groups, but it is indicated

only for RelyX Unicem in enamel with

RelyX Unicem proved to be more

practical than the conventional resin
cements.

phosphoric acid.
Thermocycling decreases the bond
strength to enamel and dentin, but

The bond strength is influenced by

previous treatment of the dental sur-

significantly only for the UnicemPA

groups.

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