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Scientific

Documentation

Table of Content

1. Introduction ................................... ................................................................................... 2


1.1

The succcess of gla


ass ceramiccs ................................................................................ 2

1.2
2

The bra
and Monobo
ond ............ ................................................................................... 3

1.3
3

Etching
g with hydro
ofluoric acid ................................................................................... 4

1.4
4

Monobo
ond Etch & Prime ....... ................................................................................... 5

1.5
5

The me
echanism ..................... ................................................................................... 6

2. T
Technical Data
D
for Mon
nobond Etch
h & Prime ................................................................... 8
3. M
Materials sccience and physical
p
invvestigations ................................................................ 9
3.1

Adhesio
on to restorrative materrials ............................................................................. 9

3.1.1

Tensile strength on variouss substrates ................................................................ 9

3.1.2

Tensile strength of various adhesives and


a primers
s on IPS e.m
max CAD ........... 11

3.1.3

ar bond strength of variious adhesives and primers on IPS


AD .... 12
Shea
S e.max CA

3.1.4

Shea
ar bond strength on IPS
S e.max CA
AD ........................................................... 13

3.1.5

Concclusion: ........................ ................................................................................. 14

3.2
2

Etching
g effect of Monobond
M
E
Etch & Prime
e versus hy
ydrofluoric aacid ..................... 14

3.2
2.1

Scan
nning electro
on microsco
ope investig
gation ...................................................... 14

3.2
2.2

Mech
hanical prop
perties (flex ural strengtth) ........................................................... 16

3.3
3

Toleran
nce to conta
amination ... ................................................................................. 17

3.4
4

User tolerance ....................... ................................................................................. 18

4. B
Biocompatib
bility............................. ................................................................................. 19
4.1

Introducction............................ ................................................................................. 19

4.2
2

Cytotoxxicity ............................ ................................................................................. 19

4.3
3

Genoto
oxicity........................... ................................................................................. 19

4.4
4

Skin irriitation and skin


s
damag
ge .............................................................................. 19

4.5
5

Sensitizzation .......................... ................................................................................. 20

4.6
6

Conclussions: .......................... ................................................................................. 20

4.7
7

Toxicolo
ogical data.................. ................................................................................. 20

5. R
References ................................... ................................................................................. 21

Scientific Documen
ntation Mon
nobond Etch
h & Prime

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e 1 of 22

1. Inttroductio
on
1.1 The
e success
s of glass ceramics
Glass cceramics be
ecame a su
uccessful allternative to
o amalgam or metal innlays and onlays
o
in
the postterior filling therapy sin
nce IPS Em
mpress was launched in
n the 1990ss. Long-term
m clinical
trials co
onfirm the success rate
e [1,2,3] Thiis outcome was not a matter
m
of coourse. Form
mer glass
ceramicc inlays, fo
or example Dicor (De
entsply) sho
owed a hig
gh numberr of fracturres after
cementing with gla
ass ionome
er cements [4]. With the impleme
entation of an adhesiv
ve luting
procedu
ure the su
urvival of IPS Empre
ess and other
o
glass
s ceramic brands ha
as been
dramatically improvved [5].

nt of teeth 16
1 and 17 w
with
Fig. 1: Treatmen
amallgam

Fig
g. 2: Treatm
ment of teethh 16 and 17
7 with
gla
ass ceramic
c onlays

ng procedure is based
d on a com
mposite ma
aterial and aan adhesiv
ve which
The adhesive lutin
a
ename
el. This ca
an be done
e in an ettch-and-rinsse mode including
bonds to dentin and
oric acid etching
e
or with
w
self-ettching adhe
esives. The
e bond to the glass ceramic
phospho
surface is achieved
d by etching
g and silaniization. Glass ceramic can be etcched by hyd
drofluoric
ve etching pattern. The
T
bulky glass
g
is moore suscep
ptible by
acid forrming a micro-retentiv
dissoluttion by the acid
a
than the crystal pa
arts. A rough ceramic surface
s
is o btained.
In a se
econd step
p a chemic
cal bond iss formed by
b silanization. In geeneral a fu
unctional
methacrylate is use
ed with a trimethoxysila
ane endgro
oup.
procedure allows
a
These p
a perfect se
ealing of the
e dentin and
d enamel in
nterface
a strong bo
ond to the re
estoration
a high stre
ength of the cement, which min
nimizes tensile loads within the ceramic
sstructure
Adhesivvely luted ceramic
c
inla
ays and on
nlays in the posteriorr region proovide a number of
advanta
ages to othe
er restorativ
ve alternativves, i.e. ama
algam, glas
ss ionomerss or compos
sites.
Scientific Documen
ntation Mon
nobond Etch
h & Prime

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C
Ceramic is known as bioinert
b
C
d discolorattion
Ceramic is less prone to wear and
Due to its stiffness and
a
its harrdness sim
milar to ena
amel, ceram
mic shows a good
a
adaptation to the rema
aining tooth walls

1.2 The
e brand Monobond
M
to glass cceramic surfaces is achieved
The bo
onding of composites
c
a
byy silanization. The
reactive
e agent is a silane me
ethacrylate which form
ms a strong
g chemical bond to the
e silicon
dioxide surface (ssee fig.2). The
T
remain
ning methac
crylate grou
up reacts w
with the co
omposite
matrix d
during curing. Beside
es the che mical bond
ding, the silanization also impro
oves the
wettability of the hydrophilic
c ceramic surface fo
or an easie
er adaptatioon of the organic
compossite.

O
HO
H3C
H2C

OC
CH3

C C O
O

Si OCH3

HO

OC
CH3

Silane methacrylate
m

Si
Si
O

Sillicate surface
e (schematic)
c)

O
H3C

OH Sii
O
H2C C C O R Si
O
O
O
Sii
O
Methacryla te silicate co
ompound

Fig. 3: S
Schematic representat
r
ion of the s ilanization reaction
r
me
echanism

Scientific Documen
ntation Mon
nobond Etch
h & Prime

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e 3 of 22

Ivoclar V
Vivadent la
aunched Mo
onobond S as silanizin
ng product composed of trimethoxypropyl
methacrylate and solvent
s
in 1991.
1
It pro
oved its clin
nical efficien
ncy in a nu mber of stu
udies [1]
pported the
e success of
o glass cerramic restorrations in combination with Variolink II or
and sup
Dual Ce
ement.
In 2009
9 Monobon
nd Plus wa
as launched
d by Ivocla
ar Vivadentt. Monobonnd Plus allows the
priming and conditioning of different re
estorative substrates.
s
It containss the silane
e plus a
phospho
oric acid methacrylate
m
e and a sulp
phide in one bottle. Its
s efficiency could be proved
p
in
several studies [6]

1.3 Etc
ching with
h hydrofluoric acid
The combination of
o silanization and etcching of glass ceramic surfacess showed the most
effective
e bonding of luting co
omposites tto glass ce
eramics [7]. The appliication of a diluted
hydroflu
uoric acid forms
f
a rete
entive etch
hing pattern
n by dissolv
ving silicon ions in the
e glassy
state. S
Silicon has a high ch
hemical afffinity to flu
uoride ions.. The form
med silicon fluoride
derivativves are soluble and can be rapid
dly washed off with wa
ater. Etchinng of glass ceramic
with HF
F gel is an established
e
method co
ommonly ca
arried out in the techniccian laborattory. But
also den
ntists know the techniq
que.
Unfortunately hydrrofluoric acid is a very strong pois
son [8] even in the disssolute state. It is a
weak accid and can
n burn the skin.
s
After p
penetrating it moves qu
uickly into ddeeper tissu
ue layers
and releases the freely dissociable fluo
oride anion
n. Fluoride is very toxxic due to its high
reactivitty. It reacts with cellula
ar calcium a
and magnes
sium to form
m insoluble salts. This induces
cellular deaths and
d necrosis. Skin
S
contacct with HF (e
even in dilute solutionss) can cause
e painful
hat heal ve
ery slowly. Latent dam
mages can also
a
be obs
served sincce the fluorride ions
burns th
penetra
ate through all layers of the epid
dermis, dermis and ev
ven the deeeper subcu
utaneous
tissues causing se
evere destrruction, neccrosis and injuries to the underl aying bone
e due to
decalciffication.
The hig
gh toxic po
otential is th
he reason why in som
me countrie
es the appplication of ceramic
etching gel is forbidden. A saffer but also
o efficient allternative would
w
be a ggreat beneffit for the
user.

Scientific Documen
ntation Mon
nobond Etch
h & Prime

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e 4 of 22

1.4 Mo
onobond Etch
E
& Prim
me

bond Etch & Prime is a single bottle cera


ramic prime
er which
Monob
allows
s etching an
nd silanizattion of the glass cera mic surface
e in one
step. It
I contains a trimethox
xypropyl me
ethacrylate for silaniza
ation and
a new
w polyfluoriide for the
e etching step.
s
The etching crreates a
roughn
ness patterrn which is less pronou
unced than with HF ge
el but as
efficient for bond
ding. The fo
ollowing sila
anization reeaction is siimilar as
M
S or Mono
obond Plus. The efficieency of Mo
onobond
with Monobond
Etch & Prime is proved by a number of intra- annd extramural bond
streng
gth tests (se
ee chapter 3).
3

SEM photo of the etch pattern of IPS e.max Press after applicationn of Monobo
ond Etch
Fig. 4: S
& Prime
e. R&D Ivocclar Vivaden
nt AG, Scha
aan, FL

Scientific Documen
ntation Mon
nobond Etch
h & Prime

Page
e 5 of 22

With Mo
onobond Ettch & Prime
e the pretre
eatment of glass ceramic surfacees for the adhesive
a
luting iss faster du
ue to less application steps and
d less harm
mful due too the avoid
dance of
hydroflu
uoric acid. Although
A
Monobond
M
E
Etch & Prim
me is corros
sive its cytootoxicity sho
own in a
XTT asssay is with a XTT50 valuue of 1970.1 g/ml less
s toxic than many of w
well-accepte
ed dental
productts. The heallth risk for th
he user is in
n an acceptted level.
r
there is no rrisk of dama
age to sanitary ceram
mic. A neutrralization
Due to its milder reactivity
efore dispo
osal is not necessarry. Monobo
ond Etch & Prime iis stable at
a room
step be
tempera
ature.

1.5 The
e mechan
nism
plication of Monobond Etch & Prim
me is linked to its reaction mechannism:
The app
Monobo
ond Etch& Prime
P
is ap
pplied onto the luting surface
s
with
h a microbrrush and is rubbed
for 20 s.

Monobond Etch & Prim


me removess saliva and
d silicon con
ntaminationss.

Monobo
ond Etch & Prime rema
ains on the surface for further 40 s for sufficieent reaction.

A
Ammonium
m polyfluorid
de reacts w
with the cle
ean ceramic
c surface tto achieve a rough
e
etching patttern
Due to the
e increased
d surface a
area a kind of activation of the ceramic su
urface is
g
generated

Monobo
ond Etch & Prime is thoroughly
t
washed offf with wate
er and thenn dried with
h air for
anotherr 10 s.

T
The polyfluo
oride and th
he reaction products with
w the cera
amic are rem
moved
T
The reactio
on between the silane a
and the active glass ce
eramic startss
A chemically bond thin
n layer of sillane remain
ns.

The com
mposition off Monobond
d Etch & Pr ime reflects
s its purpose
e (table 1).
Purpose
e

Ingre
edient

Etching

Amm
monium poly
yfluoride

Silaniza
ation

Silan
ne system based onn trimethox
xypropyl
meth
hacrylate
Solv
vents: alcohols and watter

Handlin
ng

Visibilityy
Food
d Colorant: Fast Greenn
Table 1: Compositiion of Mono
obond Etch & Prime

Scientific Documen
ntation Mon
nobond Etch
h & Prime

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e 6 of 22

Fig. 5: Structure of Ammonium polyfluoride


Ammonium polyfluoride reacts with the silicon in the glass ceramic without release of HF due
to the high chemical affinity between silicon and fluoride. By 19F-NMR spectroscopy (see fig.
6) the absence of HF can be confirmed.

156.6
ppm

Ammoniu
m
polyfluorid

165.8
ppm

-120

-140

-160

HF

-180

-200

[ppm]

Fig. 6: 19F-NMR spectrum of ammonium polyfluoride and HF (D20/EtOD). R&D Ivoclar


Vivadent AG, Schaan, FL
After the extraoral application the remaining liquid is thoroughly rinsed off. After drying a thin
silane layer in molecular scale remains at the luting surface (see fig. 3), which reacts via the
methacrylate group with the luting composite during curing.

Scientific Documentation Monobond Etch & Prime

Page 7 of 22

2. Technical Data for Monobond Etch & Prime


Product category

Product

Monobond Etch & Prime

Primer for silica glass ceramics

Function

Substance/Component

Etchant

Ammonium polyfluoride

Weight

15 - 25
Silane

Silane methacrylate

Solvent

Alcohol and water

Pigment

Colourant

Characteristics1
Bond strength2

1
2
3

75 - 85

<1

Unit
MPa

Specification
20

Example value
49

Physical properties,
Tensile bond strength (24h), light-cured, with dual-curing resin-based dental luting material
IPS e.max CAD, Multilink Automix

Scientific Documentation Monobond Etch & Prime

Page 8 of 22

3. Ma
aterials science
s
and
a phys
sical inve
estigatio
ons
3.1 Adhesion to restorativ
ve materia
als
Monobo
ond Etch & Prime is a bonding ag
gent and as such must promote a strong and durable
bond be
etween the restorative material (cceramic) and
d luting com
mposite. Too confirm that this is
the case, the bond
ding perform
mance of M
Monobond Etch
E
& Prime has beenn extensivelly tested
us material combinatio
ons and testt conditions.
in variou
Bonding
g strength is determin
ned using vvarious test setups; often
o
the shhear bond strength
(SBS) and tensiile bond strength ((TBS) are measured
d. In sheaar bond strength
measurrements, the
e load is applied para
allel to the bonded
b
surrface. In tennsile bond strength
measurrements, the
e load is applied perpe
endicular to the bonded
d surface.
Tensile strength measuremen
nts should d
demonstrate
e less scatte
ering than sshear bond strength
ndent on th
he surface structure
s
off the materrial. The
measurrements, ass they are less depen
bonding
g material is applied onto a p
prepared, flat, retentio
on-free subbstrate block (e.g.
restorattive material) accordiing to the
e instruction
ns. Subseq
quently, annother bloc
ck of a
previoussly defined size is adh
hesively bo
onded to the
e substrate block. Thee tensile strrength is
then determined ussing a suitable universa
al testing machine.
m
he results are
a highly dependent
d
on the tes
st setup and
d the test pprocedure (e.g.
(
the
Since th
diamete
er of the sp
pecimens), the results of differen
nt test serie
es can onlyy be compa
ared with
each other to a limited extent [9, 10].
ustration be
elow shows
s a typical test setup
p for meas
suring the tensile stre
ength of
The illu
restorattive materia
als.

Fig. 7: T
Test specim
men for tens
sile strength
h testing

3.1.1

T
Tensile strrength on various
v
sub
bstrates
R
R&D Ivoclar Vivadent AG,
A Schaan
n, FL

The bon
nd strength of Monobo
ond Etch & Prime on va
arious ceramic substraates was ev
valuated.
Test sp
pecimens ettched with hydrofluoric
h
c acid and silanized
s
with Monoboond Plus we
ere used
as referrence.
To cond
duct the measurements, ceramicc specimens were fabricated usinng lithium disilicate
d
Empress CAD,
(IPS e.max CAD, IVAG), leu
ucite (IPS E
C
IVAG)), lithium m
metasilicate (Celtra,
Scientific Documen
ntation Mon
nobond Etch
h & Prime

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e 9 of 22

Dentsply) and feldspar (Mark II, Vita) and conditioned either with 5% hydrofluoric acid gel
(IPS Ceramic Etching Gel) and Monobond Plus according to the manufacturer's instructions
or with Monobond Etch & Prime. Subsequently, the specimens were bonded to Multicore
Flow cylinders using Variolink Esthetic (see Fig. 7: Test specimen for tensile strength testing.
Whilst the reaction time required for hydrofluoric acid etching varied from material to material,
Monobond Etch & Prime allowed all the ceramic samples to be conditioned using the same
contact time (scrubbing for 20s; leaving to react for 40s).
To determine the aging resistance of the adhesive bond, a number of specimens were
artificially aged by subjecting them to thermocycling (10,000 cycles between 5 and 55C).
After thermocycling, the tensile bond strength was determined using a universal testing
machine (Z010, Zwick-Roell).

Zughaftung mit Variolink Esthetic


70

Zughaftung [MPa]

60
50

HF/MBP 24h

40

HF/MBP 10kTC

30
MB E&P 24h

20

MB E&P 10kTC

10
0
e.max CAD

Empress CAD

Celtra

Mark II

Fig. 8: Tensile bond strength on different ceramic materials: Monobond Etch & Prime (MB
E&P) versus Monobond Plus (MBP) with hydrofluoric acid etching (HF), both in combination
with Variolink Esthetic as the luting composite. The test specimens were examined after 24-h
immersion in water or after 10,000 episodes of thermocycling between 5 and 55C (10k TC).

Monobond Etch & Prime was also tested in combination with Multilink Automix on IPS e.max
CAD and IPS Empress CAD samples. In this combination, Monobond Etch & Prime also
showed tensile bond strength values comparable to the conventional combination of
hydrofluoric acid etching plus Monobond Plus.

Scientific Documentation Monobond Etch & Prime

Page 10 of 22

Tensile Bond Strength with Multilink Automix

Tensile Bond Strength [MPa]

70
60
50

HF/MBP 24h

40

HF/MBP 10kTC

30

MBEP 24h
MBEP 10kTC

20
10
0
e.max CAD

Empress CAD

Fig. 9: Tensile bond strength on different ceramic materials: Monobond Etch & Prime
(MBEP) compared with Monobond Plus (MBP) and hydrofluoric acid etching (HF), both in
combination with Multilink Automix as the luting composite. The test specimens were
examined after 24-h immersion in water or after 10,000 thermocycles between 5 and 55C
(10k TC).
Conclusion: Monobond Etch & Prime produces a similarly high aging-resistant adhesive
bond on various ceramic materials as Monobond Plus after hydrofluoric acid etching.

3.1.2

Tensile strength of various adhesives and primers on IPS e.max CAD


R&D Ivoclar Vivadent AG, Schaan, FL

Some manufacturers claim that their universal adhesives can generate a sufficiently strong
bond to both the tooth structure and restorative material and are therefore suitable for being
used as a bonding agent on ceramic materials after hydrofluoric acid etching. The bonding
strength of various product combinations consisting of adhesive / primer and luting
composite was examined in relation to the following products:
Manufacturer
3M ESPE
Kerr
BISCO
Ivoclar Vivadent

HF
HF
HF
HF
no HF

Primer / Adhesive
Scotchbond Universal
Optibond XTR
Allbond Universal
Monobond Plus
Monobond Etch & Prime

Luting composite
RelyX Ultimate
Nexus NX-3
Duolink
Variolink Esthetic DC

Table 2
The following tensile bond strength results were measured on sandblasted titanium or
sandblasted & anodized titanium samples after 24 hours and after 10k TC:

Scientific Documentation Monobond Etch & Prime

Page 11 of 22

TensileBondStrengthone.maxCAD
60
initial

10kThermocycles

50

TensileBondStrength[MPa]

40
30
20
10
0
VariolinkEstethic
MonobondPlus

RelyxUltimate
ScotchbondUniversal

NexusNX3
OtpibondXTR

Duolink
AllbondUniversal

VariolinkEstethic
MonobondEtch&Prime

Fig. 10: Tensile bond strength of various adhesives and primers on IPS e.max CAD
* RU/SBU, DL/ABU: 1 debonding episode each (included as a value of 0 MPa in the mean value calculation)
** NX3/OBX: 2 debonding episodes each (with each episode being given 0 MPa in the mean value calculation)

Conclusion: The investigation has shown that Monobond Etch & Prime produces an
adhesive bond that is similarly strong and reliable as the bond established with Monobond
Plus after hydrofluoric acid etching. By contrast, the universal adhesives resulted in a clearly
weaker adhesive bond with spontaneous bond rupturing occurring in some samples in the
course of thermocycling.

3.1.3

Shear bond strength of various adhesives and primers on IPS e.max CAD
R&D Ivoclar Vivadent AG, Schaan, FL

Similar to the tensile bond strength investigation described in Section 3.1.2, the shear bond
strength was also evaluated in a comparison with other systems. The following adhesives /
primers and luting composites were tested:
Manufacturer
3M ESPE
Kerr
BISCO
Ivoclar Vivadent

HF
HF
HF
HF
no HF

Primer / Adhesive
Scotchbond Universal
Optibond XTR
Allbond Universal
Monobond Plus
Monobond Etch & Prime

Luting composite
RelyX Ultimate
Nexus NX-3
Duolink
Multilink Automix

Table 3

Scientific Documentation Monobond Etch & Prime

Page 12 of 22

Shea
ar Bon
nd Strength on
o IPS e.max
e
C
CAD
SBS (24h) [MPa]

60
0

SBS
S (24h, 37C
C)

SBS
S (10kTC)

50
0
40
0
30
0
20
0
10
0
0

Mono
obond
Etch&
&Prime
Multilinkk Automix

Monobond
M
Pluss

Optibon
nd XTR

Multilink
M
Automixx

NX-3

AllBond Universall Scotchbond Universal


U
RelyX Ulttimate
Duolink

Fig. 11: Shear bond strength on


o IPS e.ma
ax CAD: co
omparison of
o Monobondd Etch & Prrime,
Monobo
ond Plus (HF) and vario
ous universsal adhesive
es
Conclusion: The shear bond
d strength i nvestigation
n showed a similar piccture as the
e tensile
strength
h investigattion: the hiighest and most relia
able bond strengths
s
w
were achiev
ved with
Monobo
ond Plus and
a
Monobo
ond Etch & Prime. The
T
adhesiv
ve bonds oof all the universal
u
adhesivves - exce
ept for Scotchbond Universal failed to withsttand stress
sing by
thermoccycling.
3.1.4

S
Shear bond
d strength on IPS e.m
max CAD
M
M. Irie, Oka
ayama University, Japa
an

The she
ear bond strength of Monobond
M
E
Etch & Prime on IPS e.max CAD w
was also ex
xamined
by Prof. Irie at Oka
ayama Univ
versity. The
e bond strength values
s were deteermined on 3.6-mm
ecimens acccording to ISO TR 1 1405: 2003
3 [11, 12]. Hence, thee results ca
annot be
test spe
directly compared with the sh
hear bond sstrength values obtained in otherr investigations that
erent metho
ods.
use diffe

ShearBondStrength[MPa]

ShearrBondSStrength
h
50
0
40
0
30
0

MBEP

20
0

MBP

10
0
0
30min

1d

Fig. 12: Shear bond strength value


v
of Mo
onobond Etc
ch & Prime (MBEP) annd Monobon
nd Plus
(MBP) o
on IPS e.ma
ax CAD.
Scientific Documen
ntation Mon
nobond Etch
h & Prime

Page 13 of 22

Also in this study Monobond


M
Etch
E
& Prim
me and Mon
nobond Plus
s achieved comparativ
vely high
bond sttrength valu
ues on IPS e.max CA
AD both at the
t
initial measuremen
m
nt after 30 minutes
and afte
er 24 hours..
3.1.5

C
Conclusion
n

Tensile and shearr bond stre


ength invesstigations clearly
c
show
w that deddicated prim
mers are
oviding an aging-resistant adhe
esive bondd to glass--ceramic
clearly better suitted for pro
materials than univversal adhesives.

3.2 Etc
ching effect of Mono
obond Etc
ch & Prime versus hydrofluor
h
ric acid
Monobo
ond Etch & Prime repla
aces the co
onventional two-step ceramic con ditioning prrocedure
of etchin
ng with diluted hydroflu
uoric acid (1
1) and priming with Mo
onobond Pluus (2) with a singlestep pro
ocedure. In the process of ceramiic etching, the
t microretentive surfface increas
ses. The
reaction
n time of hyydrofluoric acid
a
has to be adapted
d to each ce
eramic to aachieve a propitious
surface structure. By
B contrastt, the appliccation of Mo
onobond Etch & Primee requires th
he same
n time for all ceramic materials:
m
sccrub for 20s and leave to react for 40s.
reaction
3.2.1

S
Scanning electron
e
microscope investigatiion
R
R&D Ivoclar Vivadent AG,
A Schaan
n, FL

The etcching effectt of Monob


bond Etch & Prime and hydroflu
uoric acid w
was examin
ned and
comparred by mea
ans of a scanning
s
e
electron mic
croscope investigationn. To cond
duct the
investig
gation, surfa
ace-ground flat ceram
mic samples
s made of lithium dissilicate (IPS
S e.max
VAG), leuccite (IPS Empress
E
CA
AD, IVAG),, lithium metasilicate (Celtra, De
entsply),
CAD, IV
feldsparr (Mark II, Vita)
V
were conditioned
c
with IPS Ceramic
C
Etc
ching Gel orr Monobond
d Etch &
Prime a
according to
t the instrructions forr use and then rinsed
d with wateer. In addittion, the
sampless were rinssed with alc
cohol and ccleaned in an ultrason
nic cleaner. Subseque
ently, the
surfacess were analysed in a scanning
s
ele
ectron micro
oscope (SEM).
Table 4 lists the ce
eramic mate
erials and ap
pplication processes
p
used:
Ce
eramic
IPS e..max CAD
IPS Em
mpress CAD
C
Celtra
M
Mark II

IPS Ceramic
C
Etch
hing Gel

Mono
obond Etch & Prime

20
2 s
rinse with
w water
60s
6
rinse with
w water
30s
rinse with
w water
60s
6
rinse with
w water

scrrub for 20s


lea
ave to react fo
or 40s
rins
se with water
blo
ow dry

Table 4

Scientific Documen
ntation Mon
nobond Etch
h & Prime

Page 14 of 22

Without conditioning

Monobond Etch & Prime


(60s)

IPS Ceramic Etching Gel


((reaction time b/w 20 60s, depending on
material; acc. to IfU)

IPS
e.max
CAD

IPS
Empres
s CAD

Celtra

Mark II

Fig. 13: SEM images of glass-ceramic samples after conditioning with hydrofluoric acid or
Monobond Etch & Prime
Monobond Etch & Prime produced a clear etching pattern on all the ceramic materials
investigated; the etching effect, however, was less pronounced than the etching effect of
hydrofluoric acid. Although the etching effect of Monobond Etch & Prime is weaker than that
of hydrofluoric acid, it is still strong enough to produce sufficient microretention for a reliable
adhesive bond, as confirmed by the bond strength measurements (see Section 3.1)

Scientific Documentation Monobond Etch & Prime

Page 15 of 22

MBE
EP (6
60s)

MB
BEP (1
120s))

HF
F (20s
s)

HF
F (12
20s)

Fig. 14:: SEM imag


ges of IPS e.max
e
CAD
D surfaces after
a
varying
g lengths oof contact time with
5% hydrofluoric accid (HF) and
d Monobond
d Etch & Priime (MBEP)
The sca
anning elecctron micros
scope invesstigation cle
early shows
s that ceram
mic surfaces do not
Etch & Prim
become
e over-etche
ed even aftter having b
been in con
ntact with Monobond
M
me for a
prolonged length of
o time (120
0s). After a contact time of 120s, 5% hydrofluuoric acid results
r
in
a substtantially stro
onger etching effect o
on the ceram
mic than it does afterr the recom
mmended
reaction
n time (20s)).
3.2.2

M
Mechanica
al propertie
es (flexural strength)
R
R&D Ivoclar Vivadent AG,
A Schaan
n, FL

Etching may weake


en the flexu
ural strength
h of ceramic
c materials.. For this reeason, the effects
e
of
ond Etch & Prime and hydrofluoriic acid etch
hing on the flexural streength of IPS e.max
Monobo
CAD sa
amples were
e examined.
The cerramic samp
ples were either
e
etche
ed with Cerramic Etching Gel for 20s or con
nditioned
with Mo
onobond Etcch & Prime for 60s. Un
ntreated ceramic was used as refeerence.

Scientific Documen
ntation Mon
nobond Etch
h & Prime

Page 16 of 22

800

Flexu
uralStre
ength

700

[MPa]

600
500
400
300
200
100
0
non-etc
ched

Mono
obond
Etch & Prime

Hydroffluoric Acid

Fig. 15: Flexural sttrength of un


ntreated IPS
S e.max CA
AD and afte
er conditioniing with Monobond
Etch & P
Prime, hydrrofluoric acid or hydroflluoric acid and
a Monobo
ond Etch & Prime
The flexxural streng
gth of the IPS e.max CAD samples was only
o
minimaally affected
d by the
applicattion of Mon
nobond Etch
h & Prime and does not
n differ significantly from the re
eference
sampless. The pracctical effect of weaken
ning the cerramic streng
gth by etchhing is mino
or; it has
been re
eported thatt flexural sttrength redu
uced by etc
ching was reconstituteed when co
omposite
was app
plied [13].

3.3 Tolerance to
o contamin
nation
R&D Ivo
oclar Vivade
ent AG, Sch
haan, FL
Ceramicc restoratio
ons often become
b
co ntaminated with saliva during inntraoral try--ins and
these ccontaminations are not always completely
y removed afterwardss. In addittion, the
ceramicc surfaces may become contam
minated with
h silicone material duuring the fit-check.
f
Remain
ning silicone
e residue is
s difficult to
o remove and
a
may im
mpair the addhesive bo
ond. It is
thereforre importantt that Mono
obond Etch & Prime establishes a reliable adhhesive bond
d even if
contamination with
h saliva or with
w a silicon
ne-containin
ng material is present.
olerance to
o saliva con
ntamination
n, IPS e.ma
ax CAD tesst specimens were
To examine the to
man saliva and rinsed with waterr before Mo
onobond
contaminated with freshly collected hum
Prime as ap
pplied.
Etch & P
To exam
mine the tollerance to silicone
s
resiidue, the ce
eramic samples were bbrought into
o contact
with Virrtual Extra Light Body impression
n material for
f 7.5 minutes and thhen the impression
material was remo
oved. No other
o
meassures were taken to clean
c
the ssamples be
efore the
applicattion of Mono
obond Etch & Prime.
Subsequently, the samples were
w
conditio
oned with Monobond
M
Etch
E
& Prim
me and bond
ded with
D
Variolink Esthetic DC.

Scientific Documen
ntation Mon
nobond Etch
h & Prime

Page 17 of 22

TTBSafterContaaminatio
on
60
0

TBS[MPa]

50
0
40
0
24h

30
0

10kTC

20
0
10
0
0
Saliva

Virtual

Fig. 16: Tensile bo


ond strength
h of Monob
bond Etch & Prime / Va
ariolink Estthetic on IPS e.max
CAD sa
amples afterr contamina
ation with sa
aliva and Virtual Extra Light Body respectively
The ressults show that Monobo
ond Etch & Prime prod
duces an ad
dhesive bonnd that is to
olerant of
the conttamination that
t
is likely
y to occur d uring clinica
al procedures in the deental practic
ce.

3.4 User toleran


nce
R&D Ivo
oclar Vivade
ent AG, Sch
haan, FL
To ena
able a strreamlined working p
procedure during the
e placemennt of multtiple-unit
restorattions, excee
eding the reaction
r
tim
me of Mono
obond Etch & Prime sshould not have an
adverse
e effect on the
t adhesiv
ve bond. Likkewise, it sh
hould be possible to coondition resttorations
some time in adva
ance before they are in
nserted. Forr this reason, the tensiile bond strrength of
ceramicc samples conditioned with Mo
onobond Ettch & Prim
me was deetermined after
a
an
extende
ed applicatio
on time (2 minutes)
m
an d after 2 we
eeks of storrage.
Subs
strate

Protocol

Te
ensile bond
d
streng
gth value [M
MPa]

2-minu
ute applicat ion time

43.0 5.9

2
2-week
stora
age of cond
ditioned spe
ecs

46.0 6.3

e.m
max
Table 5: Tensile bo
ond strength
h values ass an indicato
or of the use
er tolerancee of Monobo
ond
Etch & P
Prime, appllied in conju
unction with
h Variolink Esthetic
E
DC
As can be seen in Table 5, reliable te nsile bond strength values exceeeding the required
accepta
Prime is therefore
ance criteria of 20 MPa
M
were achieved. Monobond
d Etch & P
conside
ered to be sufficiently
s
tolerant
t
of ssurfaces co
onditioned in advance and stored
d for two
weeks a
and contactt times doub
bled in leng th.

Scientific Documen
ntation Mon
nobond Etch
h & Prime

Page 18 of 22

4. Bio
ocompattibility
4.1 Introduction
n
Medicall devices are
a subjectt to very sstrict requirrements, which are d esigned to
o protect
patientss and opera
ators from any potentia l biological risks. ISO 10993
1
Bioloogical evalu
uation of
medicall devices defines
d
how
w the biolog
gical safety
y of a medical device is to be ev
valuated.
Furtherm
more, denttal medical devices a
are subject to ISO 74
405 Precli nical evalu
uation of
biocomp
patibility of medical devices used in dentistry
y. The biocompatibilityy of Monobo
ond Etch
& Prime
e has been examined according
a
to
o these stan
ndards.

4.2 Cytotoxicity
Cytotoxxicity refers to the destructive actio
on of a sub
bstance or mixture
m
of s ubstances on cells.
The XTT assay is used to exa
amine whetther or not a substanc
ce causes ccell death or inhibits
ure. The XT
TT50 value refers to the
e concentraation of a su
ubstance
cell proliferation in a cell cultu
e cell number by half. The lower the XTT50 concentratiion of a substance,
which re
educes the
the morre cytotoxic it is.
The cytotoxicity of Monobond Etch & Prim
me was tes
sted in vitro according tto ISO 1099
93-5 (1).
Monobo
ond Etch & Prime is wa
ater soluble
e and only showed
s
a cy
ytotoxic effeect on the L929
L
cell
line exa
amined whe
en applied in very hig
gh concentrrations. The
e calculatedd XTT50 va
alue was
1979.1 g/ml Givven that Monobond Etcch & Prime is applied only
o
in smalll amounts at
a a time
and the application
n procedure
e is performe
ed extraora
ally, the cyto
otoxic risk oof Monobond
d Etch &
Prime iss very low fo
or the patient and userr.

4.3 Ge
enotoxicity
y
Genotoxxicity referss to the cap
pability of a substance
e or a mixture of subsstances to damage
genetic material.
ond Etch & Prime has been exam
mined regard
ding its pote
ential gene damaging effect in
Monobo
a numb
ber of muta
agenicity tes
sts. Neitherr the Ames
s assay norr the mousee lymphom
ma assay
(MLA) sshowed anyy gene dam
maging effecct for Monob
bond Etch & Prime (2, 3): On the basis of
these re
esults, it can be assum
med that Mo
onobond Etc
ch & Prime does not hhave any mutagenic
potentia
al.

4.4 Skin irritatio


on and skin damage
e
The irrittation potential of Monobond Etcch & Prime
e was measured usingg an EpiDe
erm skin
model ((4). To cond
duct the test, undiluted
d Monobond
d Etch & Prime was dirrectly applie
ed to the
EpiDerm
m model forr 60 minute
es before the
e irritation effect
e
was assessed.
a
T
The test sho
owed an
irritation
n potential for
f Monobon
nd Etch & P
Prime.
The corrrosive effe
ect of Mono
obond Etch & Prime was
w examin
ned in anotther epiderm
mal skin
model ((5). After a 3-minute application tiime, the corrosive effe
ect of Monoobond Etch & Prime
was low
w; after 60 minutes
m
the corrosive e
effect had in
ncreased.
Monobo
ond Etch & Prime is designed to have an ettching effec
ct on ceram
mic surfaces
s. It may
thereforre be expe
ected that itt has also an irritating
g and corrosive effecct on the skin. The
results sshowed tha
at a short co
ontact time d
does not da
amage the skin.
s

Scientific Documen
ntation Mon
nobond Etch
h & Prime

Page 19 of 22

Once th
he etching procedure
p
has
h been co
ompleted, Monobond
M
Etch
E
& Primee is rinsed from the
restorattion. Thereffore, patientts are not a
at risk of be
eing affecte
ed by the ettching effec
ct. Users
are mad
de aware of
o the materrial's etching
g effect in the
t Instructions for Usse and notes on the
packagiing. Furtherrmore, the etching
e
effe
ect of Monob
bond Etch & Prime is ffar less sev
vere than
the etch
hing effect of hydrofluo
oric acid, w
which is wid
dely used in
n ceramic eetching proc
cedures.
Given th
he widespre
ead dental use of hydrrofluoric acid, it is assu
umed that uusers have practice
in handling corrosivve substanc
ces.

4.5 Sensitization
n
Monobo
ond Etch & Prime con
ntains meth
hacrylate derivatives. Such mateerials may have an
irritating
g effect and
d cause sen
nsitization, w
which can le
ead to allerrgic contactt dermatitis.. Allergic
reaction
ns are extre
emely rare in patients but are inc
creasingly observed
o
inn dental pe
ersonnel,
who handle uncure
ed composite material on a daily basis. Thes
se reactionss can be minimized
n working conditions
c
and avoiding
g contact off the unpolymerized maaterial with the skin.
by clean
Commo
only employyed gloves, made of latex or vinyl, do no
ot provide eeffective prrotection
against sensitizatio
on to such compounds
c
.

4.6 Co
onclusions
s:
-

Monobond Etch & Prim


me is slightlyy cytotoxic.
It is in the nature of Monobond
M
E
Etch & Prim
me to have an
a etching effect beca
ause it is
d
designed to
o etch glass
s-ceramic m
materials. Th
he etching compounds
c
s are rinsed off after
ccompletion of the exttraoral appllication pro
ocedure and
d thereforee do not co
ome into
ccontact with
h the patien
nt.
Monobond Etch & Prrime contaiins methac
crylates, wh
hich may ccause sensitization;
a
allergic reacctions, how
wever, are exxtremely rare in patients.
O
On the bassis of the information known to date, Mon
nobond Etcch & Prime can be
cconsidered non-genoto
oxic.

The ressults have shown


s
that Monobond Etch & Prim
me is safe for use in hhumans if itt is used
accordin
ng to the In
nstructions for Use. It can be con
ncluded tha
at the beneffits provided by the
productt exceed any potential risk.

4.7 Tox
xicologica
al data
(1)
(2)
(3)
(4)
(5)

Heppenheimer A. Cytottoxicity assa


ay in vitro (XTT-Test). Harlan Reeport No. 1626302.
16
6 June 2014
4.
So
okolowski A.
A Salmone
ella typhimu
urium and Escherichia
a coli reverrse mutatio
on assay
Harlan Report No. 1626301. 10 Jul y 2014.
W
Wollny H-E. Cell muta
ation assayy at the thy
ymidine kin
nase locus (TK+/-) in
n mouse
lymphoma L5
5178Y cells
s Harlan Re port No. 16
642302. 02 September
S
2014.
Heppenheimer A. In vitrro skin irrita
ation test: human
h
skin model testt Harlan Re
eport No.
16
642303. 26 August 201
14.
Heppenheimer A. In vitro skin corro
osion test: human
h
skin model test . Harlan Re
eport No.
16
642304. 28 August 201
14.

Scientific Documen
ntation Mon
nobond Etch
h & Prime

Page 20 of 22

5. References
[1] R. Frankenberger, M. Taschner, F. Garcia-Godoy, A. Petschelt, N. Krmer: Leucitreinforced glass ceramic inlays and onlays after 12 years; J. Adhes. Dent. 10, 393 (2008)
[2] A. A. Galiatsatos, D. Bergou: Six-year clinical evaluation of ceramic inlays and onlays;
Quintessence Int. 39, 407 (2008)
[3] P. C. G, C. F. Selz, A. Voulgarakis, S. Stampf, C. F. Stappert: Prospective clinical
study of press-ceramic overlap and full veneer restorations: 7-year results; Int. J.
Prosthodont. 27,355 (2014)
[4] R. Stenberg, L. Matsson: Clinical evaluation of glass ceramic inlays (Dicor); Acta Odontol.
Scand. 51, 91 (1993)
[5] A. Della Bona, J. R. Kelly: The clinical success of all-ceramic restorations; J. Am. Dent.
Assoc. 139, 8S (2008)
[6] A. Attia, M. Kern: Long-term resin bonding to zirconia ceramic with a new universal
primer; J. Prosthet. Dent. 105, 319 (2011)
[7] X. F. Meng, K. Yoshida, N. Gu: Chemical adhesion rather than mechanical retention
enhances resin bond durability of a dental glass-ceramic with leucite crystallites;
Biomed. Mater. 5, 044101 (2010)
[8] M. zkan, A. Allahbeickaraghi, M. Dndr: Possible hazardous effects of hydrofluoric acid
and recommandations for treatment approach: a review; Clin. Oral. Invest. 16, 15 (2012)
[9] S.D. Heintze, V. Rousson (2011). Pooling of dentin microtensile bond strength data
improves clinical correlation. J Adhes Dent 13:107-10.
[10] S.S .Scherrer, P.F. Cesar, M.V. Swain (2010). Direct comparison of the bond strength
results of the different test methods: a critical literature review. Dent Mater 26:e78-93.
[11] M. Irie, Y. Maruo, G. Nishigawa, K. Suzuki, D.C. Watts (2010). Physical properties of
dual-cured luting-agents correlated to early no interfacial-gap incidence with composite inlay
restorations. Dent Mater 26:608-15.
[12] E.C Munksgaard, M. Irie, E. Asmussen (1985). Dentin-polymer bond promoted by
Gluma and various resins. J Dent Res 64:1409-11.
[13] L. Xiaoping, R. Dongfeng, N. Silikas; Dent. Mater. 30, e330 (2014)

Scientific Documentation Monobond Etch & Prime

Page 21 of 22

We take no responsibility for the accuracy, validity or reliability of information provided by


third parties. We accept no liability regarding the use of the information, even if we have
been advised to the contrary. Use of the information is entirely at your own risk. It is provided
as-is or as received without any explicit or implicit warranty, including (without limitation)
merchantability or fitness for a particular purpose, or regarding (without limitation) usability or
suitability for a particular purpose.
The information is provided free of charge. Neither we, nor any party associated with us are
liable for any incidental, direct, indirect, specific, special or punitive damages (including but
not limited to lost data, loss of use, or any costs of procuring substitute information) arising
from your or anothers use/non-use of the information, even if we or our representatives are
informed of the possibility thereof.

Ivoclar Vivadent AG
Research & Development
Scientific Services
Bendererstrasse 2
FL - 9494 Schaan
Liechtenstein

Contents:
Edition:

Dr. Thomas Vlkel and Dr. Erik Braziulis


March 2015

Scientific Documentation Monobond Etch & Prime

Page 22 of 22