Dent Mater I I .•117-125, March.

1995

Adhesion testing of dentin bonding agents: A revjew

David H. Pashleyl, Hidehiko San02, Bernard Ciucchi3,

Masahiro Yoshiyama4, Ricardo M. Carvalh05

IDepartment ofOral Biology, School ofDentistry, Medical College ofGeorgia, Augusta, Georgia, USA
2Department ofOperative Dentistry, Tokyo Medical and Dental University, Tokyo, JAPAN Department
ofRestorative Dentistry and Endodontics, University ofGeneva, Geneva, SWITZERLAND 'Department
ofConservative Dentistry, Tokushima University, Tokushima, JAPAN
5Department ofOperative Dentistry, Bauru School ofDentistry, University ofSão Paulo, BRAZIL
Tao and Pashley (198). However, as
systems have
Imome
ABSTRACT hydmphilic, the sensitivity of bnd strength to
Adhesion testing of dentin bonding agents was reviewed starting dentin depth has
with the adhesion substrate, dentin, the variables involved in etching, (Prati and Pash)ey, IW2). As
priming and bonding, Storage variables and testing variables.
Several recent reports attempting to standardize many of these
variables were discussed. Recent advances in the development of
new bonding systems have resulted in bond strengths on the order
of 20-30 MPa. At these high bond strengths, most of the bond failure
modes have been cohesive in dentin. As this precludes measurement
of interfacial strength, new testing methods must be developed.
One such new
method, a microtensile methodt was described along
with preliminary
results that have been obtained. are wnveniently ü)llected for
The last decade has produced major advances in dentin bonding.
The next decade should prove to be even more exciting.

HISTORICAL PERSPECTIVE
Adhesion testing in dentin bnding studies has
steadily
the pioneering work ofBuor1(DIE ( 1955). Many
impmvements in
testing have
over the
last 40 years. The (nntñbutions of Bowen (1965),
and Kilian (1976), Watanakp et al. (1987) and Retief(1991)
helrpd to standardize
testing meth(xls. However, there
are an enormous
ofvariables that can
testing. 'Ihae have
listed in 'Ihble 1 tmder the bmad
cat.%ories of substrate variables, etching variabla, priming
variables, bnding variables, storage variables and testing
variables.
With regard to substrat,es, much information has
generated using
t.&th. However, the use of human
t.&th is prvferable (Retief et al., IWO). Decreases in knnd
Dental
strength in deep dentin were reported by Causton (1984),
et al. (1985), Mitchem and Gronas (1986) and by
 et al., IW4) and its tubula are generally
(Eluded by mineral crystals. Thus, the k»nd strengths to such
dentin are thought to be Iower than to unerupted third molars.
Nara et al. (1994) rer»rted lower tnnd strengths to sclerotic
suFrficial and deep dentin are different stmcturally, it dentin compared to normal dentin. Clearly, such studies need
to
would seem desirable to screen dentin agents with expanded
denfin is one of
kN)th tYFS the most common
(Tagami et al., 19W). sukxtrates. More informafon is

BONDING SUBSTRATES needa on how to prepare and etch such dentin.

Occlusal dentin tends to give lower SPECIMEN HANDLING
proximal or strengths than The surface preparation of dentin varies widely but few
denün (Causton, 1987; Tilo and Olsson, wmparisons have
190. 'Ihere is greater regional variability ofdentin wetness
(Prati and Pashley, 1992) in cmlusal dentin than in pmñnal or made. Srne Ibratories
buccal denín. As bnding agents impmve, this r%ional
sensitivity ofbnd sú•ength may disaplEar. aluminum oxide abrasive while others use silicon
The use of human unerupted third molars requires comment. While these (nñide (Table 1). Grits van' ñm 320 tn 12(N). While the use
of abrasive is u)nvenient in the lal»ratory,
tnnd testing, it should dentin is never prepared with abrasive
emphasized that they a1E much morv
permeable and wetter than erupted teeth (Pashley, Even when
unpublisha observations). Clinialy, using
dentin knnding is
done to prwiously handpieces, differences have
teeth, carious teeth or abraded found
lesions, mcst of which contain sclerotic dentin. Sclemtic dentin
is less etchable (Duke and Lindemuth, 1991; Gwinnett, 190;Van

1995 117
 A. Substrate B. Etchiro
1. Hurnan or tmine &ntin? 1. Etch or no etch?
2. Suprfaal, mddle or dendn? 2. What type of etchnt?
3. Ocdusal, proximal, btmal? 3. How much etchant? Renewed?
4. Third molars or irw»rs? 4. How
5. Sanded surfaces? Grit? Alzo, Sic, 320, u, or grit. 5. Passive or active?
6. Dental burs? Diam«td, carbide? 6. Rinse? How Icng?
Low•sped vs. high-sped; air-water? 7. Dry ? How long?
7. Reuse of t*th? 8. Rewet? How much?
8. Mount in plastic, Stone, etc.?

c. Priming D. Bording
1. How much adhesive for bow long?
1. Cover entire or within matrix
2. How much primer? 2. Spread with air? How thin, how dry?
3. Passive or adive? How long? 3. What diameter
4. Wash or waprate? How bng? 4. Pack with pressure or area?
5. Light-cure or not? no presure?
5. Pulpal fluid/pressure
6. Wet vs. dry? How wet, nop
dry? 6. LightarirQ. How much light? How bong?

E. Storay F. Testing
1. Water, isotonic saline, etc.? 1. Shear vs. tensile
2.
2. rate
or 370C? 3.
3. 100% RH or water? Immediate vs. 24 hr. vs rrmths.
4. Presentatives? tymol, chbramirw? 4. Express dentin in MPa or as % of
5. enamel
pressure or not magitu&? Compsitbn of aun? strer$?
6. Tiflh 24 hr.? rrmhs? years? 5. Microleakage vs. strength
7. Thermal stress? Tempratures, 6. Gap size vs.
time, strergth
7. Regional bond strengths vs. Hter
number of cycles? I

8. Gingival
8. Tooth fiexure (bad) tests. Magnitude, Class V vs. m'sal noor of Class
number cycls? 9. Configuration factors. Flat surfaces vs. 3-0 cavities.

the etchability of smear layers created with diamond

burs vs carbide burs (Pashley, unpublished systems as a
It frnction ofdentin rouÀmess. Mclnneset al.
would also fotmd
desirable tn little effect from
denún in the Ibrat.ory with mughne.ss on Shear bnd stxength
dental burs ovrata in using
(Vlhgami et al., 2/P-30(3M
1991). A related question involves the USA). Praucts, St. Paul, rvff(,
of With to reusing teeth, there are several pints to
rouÀmess on strength since low-grit abrasives give Ifone is
mugher finisha than high-numkmed grits. Mowery et al. the
( 1987) reg)rted that ofa system to
grit SiC denñn depth, then determinaüon ofbnd stiEngths to
lower rnean Shear cial, middle and
bnd dentin is
of to dentin than did 60 grit SiC kmause it
finished sufaces. Finger (1988) found little in the 1.29
tensile sb•engt.h of a nu.rntH' of measures analysis of variance (Winer, 1971).
However, there is always the danger that the previous

debonding tEt may have prauced cracks in the sulÑrate, or mounted in plastic or Stone, the dentin should
the previous emk»dding ma erial. avoids smeañng the emkEdding
may have positioned so that it Thisalways the surface of the

resin the den6n. However, the dentin

into the
tubules, thetEby alteñg the afinity ofresins for the material over the den6n Still
Careful SEM analysis should provide answerg to those preparaüon of

ques60ns. Ifthe prvvious test failure of du.ring

dentin, then the srzimen is no longer usable. When t.&th are contami-
nated by substances leaching fmm the
during water storage material
k»nding preparation and
prvpare the fierefore, many investigators PIVfer to
irnmediately
h)nding.
PULPA' FLUID
Many embedded specimens have relatively dry pulp
(Table 1). 'Ihus, even though the
a1E
stored in water, there may
a gradient of water cnntent
throuÀ10ut the dentin, which may lead to higher or lower
denfin
the k»nding system. Moisture
have
demonstrata (Mitchem, et al.,
190; Tao and Pashley, 1989; Pratiet al., 1991) although many
ofthe mcst
Innding systems are much less
sensifve to the afwetnas of &nfin than were earlier
bnding agents (Prati and Pashley, IW2; et al.,

attempts1993;PratietaL,tosimulateIW5). Smeoftheproblemsasswiatedinvivownüioninvitm(Paghley,with
Mason et al., IW4) or by
1991) have in vivo but aging in
One way to eliminated by bndingin vivo (Stewartet
al, vitm (Stewart et al.,simulate in vivo
is to fill the

118 Pash3 Wirv

pulp chamk:pr Vit,h water, a physiological salt solufon (Tao BONDING METHODS AND VARIABLES
and Pashley,
Tilo's ( 1,97) review ofdeknnding tests divided them into quali-
or a 1:3 dilution ofplasma with
tative tests and quantitafve tests. fris
cal salt solution (Nikaido et al.,
was based 1.1B)n the
This Oution can also
ofthe "Do we want a
be placed at zero hydrostatic pressure or some positive
of
pressure (Tao and Pashley, 1989) during either bnding or
quality
during storage or under
of tEt tn study H)nd or no
(Table l). Early
and the
studies using simulated pulpal
failure, or do we want to quantitate the k»nd in order to
in vitm utiliza
predict something abut the load capacity and lifetime ofthe
32 cm H20.
bond" (Tilo, 1987). The quality test should be well-
pressures in intact pulps are indicates that nonnal pulpal
and easy to l*lform. It can tensile, shear,
12
torsion, cleavage, pull or extrusion (Haller, 1993) or 4-pint
HP in the cat
t»nding (fio, 1987). The easiest to perforrn
(Vongsavan and Matthews, 1992) and 14
shear tests.
in humans
'fre load can
(Andrews et al., 1972;
distributed (as in lap-shear or blunt-end Shear
et al., 1995).
bar) or interfacial (wire
These
in shear). There is a strong
increase in inflamed pulps (Van Hassel, 1971; Stenvik et al.,
tendency to develop a
1972; 'Ibnder and Kvinnsland, 1983).
moment in most Shear tests.
When Icral anesthetic solutions containing
Tensile tests, in tl-mry, should develop molE uniform strvss
agents are injected in patients, pulpal blood flow is
distributions if there is correct alignment between the
temrnrarily IEduced but 60'70 (Pit-Ford et al., 1993; Odor
slHimen and the adha•ent. However,
et al., IW4). Since pulpal pressure is derived fiX)m perfusion
distribuüons in
pressure, reductions in pulpal blood flow should lead to
such tests have
reductions in pulpa] tissue prasure. This is the driving fcnre
shown to
that
nonuniforrn (Van Noort
pulpal/dentinal fluid to the surface where it can
et al., 1989; 1991). Presumably, this is due to complex
dilute pHmers and
combinations of elastic and plastic deformations of the
with resin monomezs for
resin
or Other
demineraliza dentin
of dentina
and
investigators have
conducted knnding studies where a pulpal pressure of 34 cm
H20 was applied during
but not during storage
(Mitchem et al., 1988). Others have knnded at zero pressure
but st01Ed under 32
H2() (Tho and Pashley, 1988; 1989).
Stil others have Innded and stored under 36 cm H20 (h•ati et
al., 1991; Prati and Pashley, 1992). In View ofwhat is known
taay, k»nding and storage ofdentin
should
done
at simulated pulpal
of 15-33 cm H20 (Table 1). 'Ihe
higher value simulates probable pulpal plessu.res that develop
severa] hours after cavity pru)aration due to pulpal initation
(Pashley et al., 1981).
Thus far, the discussion has
limited to denún as a
knnding substrate. Much
has IEn made over the
last ten years in this area. Investigators should follow the
standarxls published by
( IWI ) and by S&rholm
( 1991) during
studies. 'Ihe next pmblem involves
Innding methods and variables.
mineralized dentin subsurfaces (murring strssing.
simultaneously. Simply sulñtuü.ng a high nmtlu.s resin
FRACTURE MODE/FRACTOLOGY
for a lower In early studies of denún
modulus material has IEn shown to
alm(Ft all bond failures
significantly increase
werv
the apparent Shear sb•engths (Erickson et al., 1989) ofl»nds.
in nature
True interfacial t.&ting, whether in Shear or tension probably
kmomes a cleavage test the Ennds
as as the first Clack kEgins to made to smear
propagate from a defect, void or other source of stress- layer-covered dentin. Careful SEM examination ofbth sides
offailed
Quantitative bond testing involves determination of made to smear layers revealed that the failure
fractur was not adhesive but that the smear layer failed cohesively.
e or the enerv of fracture (O'Brien and That is, k»th sides of the failed knnd '•,vele ü)vera by smear
Rasmussen, 1984; Tam and Pilliar, 1993). It has applied layer particles (Tao and Pashley, 1988). Thus, there is a
bth to the toughnes.s ofbulk materials and to the interfacial danger in classifring the
knnds adhesive of failure visually, whether
lesins and tmt.h structure (Hara.shi.nma usingthenaked eyeora
et al., 1988; Tam and Pilliar, IW3, 1994; Lin and Neithermeth(ll
Douglas,
has the IEsolution required to identifr the m(Re of failure
1994).
which is often micros.ü)pic in detail. However, such visual
FINITE ELEMENT ANALYSIS classification is helpfill in pmviding overall descriptions of
Finite element analysis (FEA) has obvious
to prHiict stress ofbnd failmz, esrmially cohesive fractures in
distributions within teeth and at the of adhesives adhesives,
and dentin (Van N(nrt et al., 1989; 1991). This modeling
or in dentin.
requires knowledge of the strength of materials vs. the It is of interest to note that different Ennding materials
strength of mineralized dental tissues and the
differencps in produ(E diffezent
elasfc of fractu.1E. Burrow et al. (1993)
n•mlli of materials vs. dental tissues. 'fren t.hr&- rq»rted that most of the Innd failures that they observed
dimensional stress distribution within these structures were adhesive in nature for Superbond C&B but were
can primarily cohesive in dentin for Clearfil Liner Bond 2.
aculated during Apparent.ly there are large differen(Es in the stiBxs distribu-
various Gons at the dentin
ofloading. Unfortunately, that lead to vew different
little information is available on the large st1Ess
gradients of fracture
that develop at bonded interfaces because of a lack of these two materials, even though their
knowledge of the modulus of elasticity of apparent tensile bond strengths were not statistically
demineralized different (13.8 ± 3.8
dentin dlagen, resin-infiltrated demineralized dentin for Superbnd D
matrix, vs. 13.4 ±
resin tags, length of resin tags, etc. As this information 4.0 MPa for Clearfil Liner Bond 2) after 3 mon of water
l»corna available, FEA may pmvide imprtant new storage (Burmw et al., 1993).
into the dynamics oftmded interfaces during
application of
cyclic loading ortherma] gradients and during Other of
Dental Materials/March 1995 119
 For systems that bnd to denún by aution of a hybrid
layer, it is of interest to know whether the bond fails
affnesively at the top of the hybrid layer, whether the hybrid
layer fails cohesively or whether the failure occurs at the
bottom of the hybrid layer where one would expect the
st&1Bt gradient in moduli of elasticity
the hybrid
layer and the underlying mineralized denün (Burmw et al.,
As
microscopic struúlres, SEM examination
is requilEd. However, the size of
bnd-dentin
interfaces (ca. 3 mm diameter) is a veo: large area to examine
by SEM at the
to resolve hybrid layer
(i.e.,
Fig. 1. trxture pttxns at interface of boo&d with Charfll
They are so large that one often
Lin« (from Burrow et al., 193); wtth
sees many types of failure patterns in the same sample
(Fig. 1). Similar detailed micmwopic examination is
in analyzing interfacial failures in
(Tam and Pilliar,
1993, 1994; Lin and Douglas, 1994).
STABILIW OF DENTIN BONDS
While the development ofearly (i.e., 15 min)
a vay imprtant variable in evaluafng a strength is
the long-term (i.e., 1 y) Innd strength. frat is, we would like
system, N) is

to have early h)nd strengths in ex(Bs of 20 MPa which do

not fall over the long term. Kiyomura (1987)

that
4-METMMA-TBB denfn bonds fell from 15
to 6 MPa
in I y and to 3 N'fPa in 5 y when sarnples were immersed in
water at 370C. Few long-term studies are done, and hence, it
is unclear how stable the dentin bonds are of recently
systems.
Burrow et al. (1993) recently
published a longitudinal study ofthe effects ofstorage time on
the tensile
stlengths of a numtpr of dentin bonding
systems. frey
that
was little Change in the
tensile
strength of Sul»rbnd D Liner or Clearfil Liner
Bond 2 over a 1 y period, but that the Clearfil Liner Bond
System and Clearfil Photobnd exhibited slow, progressive
decreases in
sti8ngt.h over a 1 y pericxl.
hvsumably, those systems that
infiltrate the
demineralized dentin surfacp to its complete depth should give
more stable bonds than those systems which have only
infiltrated the top halfofthe dernineralized dentin. However,
Fb, 2 fracture of hr. p" of entin *bimd during
the resins must also wet the
A. Frxturd entin (FD) s" of tal% Et-
and r»lyrnerize
(from B. Ff*ülred «'tln
well to provide pmtff'tion against hydrolysis of any collagen
pbe on ruin et al., 1%); with pmiubn.
fibers that are enveloped by resin. High resolution
whether by SEM or TEM, must
way that it done in such a
not artifactually prcxlu(E images ofa)mpletely
 prv:lude measurements ofinteffacial k»nd stiEngths
infiltrated hybrid layers, when they, in fact, contain in
fris can tensile and shear l»nd tesüng methods. Cohesive
done thmugh fractures of the dentin substrate
ofinfiltrated to
vs. uninfiltrated samples, polished vs. fractured at abut
(Erickson and Glasspoole, 1994) and through the use of 12-15 NfPa and increase in frequency until as much as 80% of
fracers. the bnds fail
As the strength of in dentin at 25 MPa (Fig. 2). Bowen
denún
and Rodriguez (1962) remrted the ultimate tensile strength
agents improved, there
ofhuman dentin was 52
has tEen an incrEase in the
10 MPa (Table 2). Inhman (1%7)
of
an ultimate tenále strength (1.118) of 37 ± 11 MPa.
failures of
Smith and Cooper (1971) reported a shear strength of
dentin during bnd strength testing. Cohesive failures ofthe

120 Pashley testirv

 Mineralized Ref.

Enamel 10.3± 2.6 Bowen & Rodriguez (1962) - tensile

84.1 Cratg (1993) - tensife
Dentin (human) 10.3 (9) Bowen & Rodriguez (1962)
Lehman (1967) - tensile
Dentin (human) 36.6 10.9 (12)
Watanabe et al. (In Press) • Shear
Dentin (human) 78.4 13.3 (12)
Sano et al. (1994b) tensile
Dentin (human)
Sano et al. (1994)
Dentin (bovine) 18.9 (8) - tensile

Enamel (human) Smith & Cooper (1971) - Shear

at DEJ Smith & Cooper (1971 ) - Shear
Dentin. Superficial Smith & Cooper (1971) - Shear
Smith & Cooper (1971) - Shear
Dentin, Middle 90.3
Smith & Cooper (1971) • Shear
Dentin. Inner 78.5
Smith & Cooper (1971) - Shear
Dentin, Deep
Smith &
Dentin. Near Pulp 45. I (1971) - Shear

II. Demineralized

Dentin (bovine) 28.0± 3.9 (5) Akimoto (1991 ) - tensile

Dentin (bovine) Sano et al. (1994b) - tensile
Dentin (human) 29.6t 5.9 (10) Sano et al. (1994b) - tensile
Dentin (human) 105.6 ± 16.3 (10) Sano et al. (1994b) - tensile

Resin•infittrated demineralized dentin (RIDD)

RIDD
(AB2) Sano et al. (1995) - tensile
121.6 20.3 (6) Sano et al. (1995) - tensile
(SC.MP)
117.6 ± 12.2 (6) Sano et al. (1995) . tensile
102.6± 3.7 (6) Sano et al. (1995) - tensile
57.6

16.4 (6) Sano et al. (1995) - tensile

suFrficial dentin (done with a micmpunch test) at 132 ± 28 with the failure of dentin that have
N'fPa (Table 2). fie chemical and physical pmF1ties of den- obtained during testing. ms discrvpancy that
tin have rmñewed by Marshall (1993a, 1993b) the develop abnon•nal stress distñbutions
and Kinney et al. (1995). Watanabe et al. (In press) during testing, leading to failures of the dentin sukxtrate at
the Shear stiEngth ofhuman dentin stresses far
78 ± 13 N'IPa and confirmed by Van its ultimate strength. This notion was
91.8 ± 12.7 MPa dqwlding upn et al. (1989; 1991) using finite
and tubule orienta-
tion. Using a microtensile method, Sano et al. (1994b) element analysis to demonstrate the nonuniform stress
obtained a UIS ofhuman dentin of distributions within conventionally bnded
16 rvfPa (Thble 2).
ürn et al. (1995) IEP1ted that resin-infiltrated demineral- TESTING METHODS
ized denün Testing meth(Rs have never
yield well standardized although
a numkpr ofimprtant
different from that that were not statisfcally the substrate have kEn made for
of mineralized dentin, although the 1991) and
modulus ofelasticity was much lower (Table 2). Ald.moto ( IWI ) (Tilo, 1987;
measured the tensile stlvngth ofdemineralized Invine denfin IWI). 'Ihe latter
matrix at 28.0 MPa (Table 2). Sano et al. (1994b) confrmed while very
the h.iàl tenSle strength ofhuman demineraliza denún. frey not
the ultimate tensile strength of the demineralized a standard area
dentin matrix was 29.6 ± 5.9 MPa and that the but rather provides for surface areas of 0.071, 0.196 or
of 0.785 cm2 (diameters of3, 5 or 10 mm). As fracture strengt.h is
elasticity was 250 MPa (Table 2). In a more recent palE (Sano givencanIt per tuit a1Ea, the surfacp arva is extremely
et al., 1995), the authors
t.kut the true st7M1gth ofthe contlX)lled vith appropriate molds or jigs but one
demineralized dentin matrix is closer to 90 MPa when obtains different stress distributions if one coats dentin
calculated on the basis of the cross-sectional area of the
rather than the total mx:ss-sectional area of an adhesive layer Iñre or
uxitioning a matrix (Van
demina•al.iza denún which is Ncnrt et al., 1991). Wang et al. (1972) obtained constant
70% water- 3Wc strengths
organic matrix. Thus, the strength of the demineralized two adherents when the
dentin matrix may was varied. However, fflis was not done
higher than the reprted with a bnding The only reprt that this
value of29.6 NfPa. All writer is aware ofrega.lding variations in dentin
valua for the ultimate strength strength
of dentin are much greater than the 25-30 MPa values with area was anAADR akxtract published by Erickson

Dental Materials/Mar(N1 121

 PMMA I TBS
Com%jsite
(MPa)
Dentin

TBS 58.758-2.792 log SA

80 (P=o.oom.
=0.703)

60 e

40 e
Composite 8
Dentin

o
20

5 10 15
SA (mm2)
a furwtion of
Fig. 4. Tensih bmd strength (TBS) of Clutl Liner Bond 2

surface ara using a m±mterdle buid struvth testing nwth«. clrchs

indicate spcimens exhibiting cohesive tailure in dentin while closd circlg
indicate
failures.

*rength
a ari *inwn pr*tatlon for mbff0tendb saw (Buehler Ltd., Lake Bluff, L, USA). The resu16ng
tat. A, B. P.ratbn of fu C. to entin. a.re ofan upFr halfofrvsin
nwn
D. Pr»aratlm ot for Etioning. E. SMial wcthning of and a lower
halfofdentin (Fig. 3F). Using an ultra-fine diamond bur, the

F. Individual slab shown in profile and full.view. G. Slab trimmed at bonded area at the knnded
interface. H. Trlmm# s» In grips. was
to
form an hour-glass shape to ensure maximum stress
development at that region (Fig. 3G). 'Ihe bnded
et al. ( 1989). Using dentin and 2 adhesive, area
they found significantly that was
was calculated from the
Shear t»nd strengths using a
wire loop compared to knife-edge or blunt shear bars. and yidth which was measura with a digital micrometer.
Fufther, the stiffer P-30 gave higher Shear 'Ihe ends of the slEimens were attached to
did Silux. When they examined the effect ofsurface au, the of a
highest t»nd strengths were obtained with strengthsthesmallestthan Multi-T
that they testa (Danville Engineering, Danville, CA,
cm2), but they were not USA) with cyanoacwlate
stafstialy significnntly different 'Ihe
obtained with was then placed
surfacp aleas of0.123 or 0.1% cm2 in a universal testing machine (Insb•on, Mcnel #1011, Insfron
There is a tendency for large bonded surface areas to Corp., Canton, MA, USA) and stressed at 1 mm/min in
tension. After testing, the
pauce failures in dentin at ofeach slEimen
low l»nd were detennined by examination in a
st1Engths. Using (B&L
teeth and a bnding area ofO.238 NY, USA) at 10x.
(5.5 mm diarneter hole), Perinka et al. (IW2) These
an were
82% using Clearfil Liner Bond 2
System at 9.2failure ofdentin k»nded with Clearfil Liner Bond (KurarayCompanyLtd, Kyoto,Japan). Whenthetensiletnnd
st1Ength was plotted as a fr.ncfon of bnd arva, an
 4.4 MPa When Erickson et al. (1989) used
exponential increase in bond strength was noted with

2/P-30 to bnd to Envine dentin using a decreasing surface area (Fig. 4). At the largest areas
area of0.123 cm2 (3.5 mm diarneter hole), they obtained 800/(, (ca. 0,07-0.12 a•n2), there were some a)háve

ü)hesive fractures in dentin at a 16.9 ± 3.1 NfPa.

Sam et al. (IW4a; 1994c) have report.ed that tensile bond at knnd sbengths ofdenfin
strengths are inversely relata (Fig. 4) to 150
area However, at bnda
using veo,' small areas (OM5-0.12 cm2). In that study, they areas IElow 0.02 cm2, all ofthe failures were adhesive

found that as the cmss-sectional area of bnded spcirnens in nature by visual examination even t ough the bond
was strengths increased to 50-60 MPa. The highest adhesive

the failure
of failura of dentin fell to 'frese was 71 MPa.
Below2 mm2,allfailures were adhesive pmvide additional
in nature. sfrength ofdenfin is much higher than the 25-30 MPa values
In an effort to develop fails mhesively. In that the ilú•insic
tests ofsmall areas, Sano et al
( 1994a; that a.1E this new testing
called the "microtenSle tends to
metha". In measura in bnd tesüng when dentin
this
k»nding adhesive higher k:nnd stREngths than
resins to the entire flat What the results are apparently du»ndent upn

surfa(E it primarily adhaive au, and

which is at
with a kAow
"a•own". After curing and 0.02 cm2. Qualitatively Smilar have
storage in water, the srmimen is vertically sectional into
multiple with Other adhesive systems. obtaina
sKtions (Fig. 3E) using a 'Ihe raN)n forthis in bnd strength wit,h deaEases
diamond in bonded surface arva is probably due to the presen(2 of

122 "hesion testitv

 irregular surfaces can be evaluated after bonding under
clinia (ffhble 3).
Dr. Bemard Ciud1i (University of Geneva) is using this
method to measure differences in the rvãonal k»nd strength
ofClass II
Dr. Hidehiko Sano and his colleagues
1. More adhEsive failures, fewer failures (Tokyo Medical and Dental University) are using the
2. Higtw interfacial micmtensile method to measure the
strengths can be measured strength of resin
3. Permits measurements of regbnal bond strengths adhesives to excavata
4. Means and variances dentin. fris is
be calculated for single teeth the
5. Permits testing of
rr" can measure the
to irregular surfaces strengths ofsmall,
6. Permits testing of very small areas irregularly
7. Facilitates SEM examinatm of areas.
failed bonds since tre sudace The disadvant.ag& of the meth(xi (Table 3) are that it is
area is approximately 1 mm2. technically dificult and lak»r intensive. When the interfacial
region is selected, the cross-sectional surface area is adjusted
with a diamond bur under copious air-water spray. If one
tm much lateral
1. Labor intensive, technically demanding on the bur, the
Will fail. If
2. Difrult to measure bond strengtt•s < 5 MPa. the bur is not concentric, it can
suficient vibrafons to
3. Requires spcial equipment damage the bonded
4. Samples are so snull they dehydrate rap"ly Materials or regions that
low bond strengths
5 MPa) often fail during
defects or stras raisers at the interface or within the trimming. fre samples
substrate, According to the Griffth defEt (Griffth, so small that they must
1920), the tensile strength ofa brittle material danuses with kept
increasing cross-sectional area. Larger slEimens 9em to moist to avoid doping effects. Care must
cont¿ün molE defects than smaller slEimens. The same may taken during
sectioning to avoid heat
true A
dentin saw blade
areas. Adhesive lubricated with water is required. equipment is Special
is IEquired to ensure prolE aligmrnent of the specimens and
not uniform micr(Nopically. The application of uniform tensile stress vôthout any torsion
can cnntain air effects. 'Ihe actual tensile
bubbles, phase separations, surface roughnesses and non that develop are generally
uniform film thicknesses that can lead to nonuniform sü•ess less than 34 kg. Thus, a 5 kg strain gauge is generally used.
distributions. Van Noort et al. (1989; 1991) used finite Adhesion tests, while not perfbct, have enabled the
element stress analyses to demonstrate that tensile and Shear development of impmved tnnding systems and techniques.
k»nd stmngth measuxements welE highly dq»ndent upn the There was a real need for standards with regard to the
geometry of the tested interface, the nature of the load substrate, the various steps in bonding and in testing.
application, the presen(E or Unforamately, now that standards have kEn promulgated,
of adhesive flash, etc. they may have to
m(ñfied k:pcause the newest p:xxiucts
According to their analyses, the probability that
develop such high strength
may there
dominate the propagation (f fractu1E is very high tm many ü)hesive
of m crotensile
failures in the substrate.
To avoid this problem, a new
nonuniformity ofthe interfacial stres distribution, esrmially has
at the ed.ge ofthe under clinically relevant conditions. that has a
This may iniüate fractures at the number of advantages (Table 3). This method permits
defects, IEsulting in lower tensile k»nd strengths than might of 70Presumably,NfPahave new products Will in
 measured in smaller samples. While no st.1Ess analyses
have yet measured in the adhesive failure mcRe.
done on the sFcimens used in the microtensile mineraliza tmth structures. frey should which are
meth(R, it is probable that their small size has led to improved intrinsically stmnger and which develop stronger

stress distributions and hence to tn

ofmaterials that are relatively insensitive to moisture. fris shouldsimplepermittomoreuse,
cl(ser to their true ultimate strengths. This may also k»nd equally well to enamel, surHficial or deep dentin, and be
why to adhesive dentistry.
the
lesearchers obtained higher tensile strengths for uniform, consistent, dentin bonding which Will be of
prtredu18 and prxxiucts have developed over the past ten
dentin (Ihble 2) than were previously
Smith and In conclusion, significant improvements in bonding
(h)Fr ( 1971) also obtaina Shear strengths ofdentin made to acid-etched enamel. These higher dentin bond
in small samples IElative to larger samples.
years.
'IherE are a numkm of advantages and disadvantages to duñng in vitro testing, causing cohesive failures in the
the use of the microtensile tEting method (Table 3). 'Ihe k»nd strengths are often higher than IESin bnds
gzeatest advantage of the technique is that one can obtain a)nventiona] k»nd testing
exclusively adhesive Innd failures of materials ifthe bnded strengths develop nonuniform stress distribufons in dentin
surface area is al:nut 1 mm2. Using can no longer

substrate rather than in the bonded interface. Thus,

tH:hniques, we azE rapidly appmaching the point wherv we

failures that (mur in testing are within dentin rather than

vill not used to
can detect further improvements in product development or
able to distinguish product impmvements if the bonding procedures. New testing methods need to be
obtained
a single tmth. Ifthe cross- tmlsdevelopdneeedandto standardizedmakefrrtheradvancestoprovidein reseaÑhersinadhesionwitoh the
interfacial. Using the microtensile method, multiple

a mean and standard deviation of the k»nd dentin. More emphasis should
area ofeach slEi.rnen is the same, one can aculate sclerotic
of a placed on t»nding to
that the k»nded surfacE dentin and cañes-affected dentin to
material to a single tmth. Another significant advantage is the materials and techniques required to EM)nd to these

not have to be flat. Small, clinically relevant sut:stratE

Dental MateñaB/March 123

 ACKNOWLEDGMENTS Craig RG (1993). Ratorative
Louis: M(Xby, u.
This work was in part by grant from the Duke ES, Lindemuth JS ( 1991). Variability ofclinical dentin
Nafonal Institute of Reseamh and by the Medical
sulxtrates. Am J Ikn.t 4:241-246.
College of (k)rgia Ikntal Reseamh Center. The authors are
Eick JD, Robinson SJ, Chappll RP, Cobb CM,
grateful to Shirley Johnston for secretaria] supprt. P ( 1993).
'Ihe dentin surface - Its on denãn adhesion, Part
Presentcd at the IW4 ADM Annual Bermuda, Novemkm 1994
II.
Address
Int 24:571-582.
and reprint requests to:
Erickson RL, Glassme EA (IW4). to W)th sfruc-
David H. Pashley tu.1E: A (nmparison of giass-ionomer and

systems. J Esth
Medical College ofGeorgia
Augusta, 6227-244.
USA 30912-1129
Erickson RL, Glassme FaA, (1989). of
test parameters on dentin bnd sfrength measurements. J
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