The aim of this study was to evaluate the changes in the mechanical behavior and bonding capability of Zn-doped resin-infiltrated caries-affected dentin interfaces. Dentin surfaces were treated with 37% phosphoric acid (PA) followed by application of a dentin adhesive, single bond (SB) (PA+SB) or by 0.5 M ethylenediaminetetraacetic acid (EDTA) followed by SB (EDTA+SB). ZnO microparticles of 10 wt. % or 2 wt. % ZnCl2 was added into SB, resulting in the following groups: PA+SB, PA+SB-ZnO, PA+SB-ZnCl2, EDTA+SB, EDTA+SB-ZnO, EDTA+SB-ZnCl2. Bonded interfaces were stored for 24 h, and tested or submitted to mechanical loading. Microtensile bond strength was assessed. Debonded surfaces were evaluated by scanning electron microscopy and elemental analysis. The hybrid layer, bottom of the hybrid layer, and peritubular and intertubular dentin were evaluated using a nanoindenter. The load/displacement responses were used for the nanodynamic mechanical analysis III to estimate complex modulus, tan delta, loss modulus, and storage modulus. The modulus mapping was obtained by imposing a quasistatic force setpoint to which a sinusoidal force was superimposed. Atomic force microscopy imaging was performed. Load cycling decreased the tan delta at the PA+SB-ZnCl2 and EDTA+SB-ZnO interfaces. Tan delta was also diminished at peritubular dentin when PA+SB-ZnO was used, hindering the dissipation of energy throughout these structures. Tan delta increased at the interface after using EDTA+SB-ZnCl2, lowering the energy for recoil or failure. After load cycling, loss moduli at the interface decreased when using ZnCl2 as doping agent, increasing the risk of fracture; but when using ZnO, loss moduli was dissimilarly affected if dentin was EDTA-treated. The border between intertubular and peritubular dentin attained the highest discrepancy in values of viscoelastic properties, meaning a risk for cracking and breakdown of the resin–dentin interface. PA used on dentin provoked differences in complex and storage modulus values at the intertubular and peritubular structures, and these differences were higher than when EDTA was employed. In these cases, the long-term performance of the restorative interface will be impaired.

1.
J. H.
Kinney
,
S. J.
Marshall
, and
G. W.
Marshall
,
Crit. Rev. Oral Biol. Med.
14
,
13
(
2003
).
2.
L. E.
Bertassoni
,
S.
Habelitz
,
J. H.
Kinney
,
S. J.
Marshall
, and
G. W.
Marshall
,
Caries Res.
43
,
70
(
2009
).
3.
J.
De Munck
,
K.
Van Landuyt
,
M.
Peumans
,
A.
Poitevin
,
P.
Lambrechts
,
M.
Braem
, and
B.
Van Meerbeek
,
J. Dent. Res.
84
,
118
(
2005
).
4.
Y.
Wang
,
P.
Spencer
, and
M. P.
Walker
,
J. Biomed. Mater. Res., A
81
,
279
(
2007
).
5.
H. A.
Wege
,
J. A.
Aguilar
,
M. A.
Rodríguez-Valverde
,
M.
Toledano
,
R.
Osorio
, and
M. A.
Cabrerizo-Vílchez
,
J. Colloid Interface Sci.
263
,
162
(
2003
).
6.
R.
Osorio
,
M.
Yamauti
,
E.
Osorio
,
M. E.
Ruiz-Requena
,
D.
Pashley
,
F.
Tay
, and
M.
Toledano
,
Eur J. Oral Sci.
119
,
79
(
2011
).
7.
M.
Toledano
,
E.
Osorio
,
F. S.
Aguilera
,
S.
Sauro
,
I.
Cabello
, and
R.
Osorio
,
J. Mech. Behav. Biomed. Mater.
30
,
61
(
2014
).
8.
P.
Spencer
and
Y.
Wang
,
J. Dent. Res.
80
,
1400
(
2001
).
9.
Y.
Liu
,
S.
Mai
,
N.
Li
,
C. K.
Yiu
,
J.
Mao
,
D. H.
Pashley
, and
F. R.
Tay
,
Acta Biomater.
7
,
1742
(
2011
).
10.
T.
Takatsuka
,
K.
Tanaka
, and
Y.
Iijima
,
Dent. Mater.
21
,
1170
(
2005
).
11.
M.
Toledano
,
S.
Sauro
,
I.
Cabello
,
T.
Watson
, and
R.
Osorio
,
Dent. Mater.
29
,
e142
(
2013
).
12.
Z.
Yang
and
C.
Xie
,
Colloids Surf., B
47
,
140
(
2006
).
13.
J.
Pasquet
,
Y.
Chevalier
,
J.
Pelletier
,
E.
Couval
,
D.
Bouvier
, and
M.
Bolzinger
,
Colloids Surf., A
457
,
263
(
2014
).
14.
R.
Osorio
,
M.
Yamauti
,
E.
Osorio
,
J. S.
Román
, and
M.
Toledano
,
Eur. J. Oral Sci.
119
,
401
(
2011
).
15.
M.
Toledano
,
F. S.
Aguilera
,
E.
Osorio
,
M. T.
López-López
,
I.
Cabello
,
M.
Toledano-Osorio
, and
R.
Osorio
,
Biointerphases
10
,
041004
(
2015
).
16.
C. M.
Hayot
,
E.
Forouzesh
,
A.
Goel
,
Z.
Avramova
, and
J. A.
Turner
,
J. Exp. Bot.
63
,
2525
(
2012
).
17.
M. A.
Meyers
and
K. K.
Chawla
,
Mechanical Behavior of Materials
(
Prentice-Hall
,
New Jersey
,
1999
), pp.
98
, 103.
18.
T. M.
Wilkinson
,
S.
Zargari
,
M.
Prasad
, and
C. E.
Packard
,
J. Mater. Sci.
50
,
1041
(
2015
).
19.
G. W.
Marshall
,
S.
Habelitz
,
R.
Gallagher
,
M.
Balooch
,
G.
Balooch
, and
S. J.
Marshall
,
J. Dent. Res.
80
,
1768
(
2001
).
20.
A.
Misra
,
P.
Spencer
,
O.
Marangos
,
Y.
Wang
, and
J. L.
Katz
,
J. Biomed. Mater. Res., B
70
,
56
(
2004
).
21.
M. C.
Erhardt
,
M.
Toledano
,
R.
Osorio
, and
L. A.
Pimenta
,
Dent. Mater.
24
,
786
(
2008
).
22.
H.
Koibuchi
,
N.
Yasuda
, and
N.
Nakabayashi
,
Dent. Mater.
17
,
122
(
2001
).
23.
M.
Toledano
,
F. S.
Aguilera
,
I.
Cabello
, and
R.
Osorio
,
Biomech. Model. Mechanobiol.
13
,
1289
(
2014
).
24.
M.
Toledano
,
R.
Osorio
,
A.
Albaladejo
,
F. S.
Aguilera
,
F. R.
Tay
, and
M.
Ferrari
,
Operative Dent.
31
,
25
(
2006
).
25.
L.
Han
,
A. J.
Grodzinsky
, and
C.
Ortiz
,
Annu. Rev. Mater. Res.
41
,
133
(
2011
).
26.
H.
Hertz
,
J. Reine Angew. Math.
92
,
156
(
1881
).
27.
W. C.
Oliver
and
G. M.
Pharr
,
J. Mater. Res.
7
,
1564
(
1992
).
28.
T.
Nikaido
,
K. H.
Kunzelmann
,
H.
Chen
,
M.
Ogata
,
N.
Harada
,
S.
Yamaguchi
,
C. F.
Cox
,
R.
Hickel
, and
J.
Tagami
,
Dent. Mater.
18
,
269
(
2002
).
29.
C.
Prati
,
S.
Chersoni
, and
D. H.
Pashley
,
Dent. Mater.
15
,
323
(
1999
).
30.
M.
Toledano
,
E.
Osorio
,
I.
Cabello
,
F. S.
Aguilera
,
M. T.
López-López
,
M.
Toledano-Osorio
, and
R.
Osorio
,
J. Mech. Behav. Biomed. Mater.
54
,
33
(
2016
).
31.
M.
Toledano
,
I.
Cabello
,
M.
Yamauti
, and
R.
Osorio
,
Microsc. Microanal.
18
,
497
(
2012
).
32.
V.
Gopalakrishnan
and
C. F.
Zukoski
,
J. Rheol.
51
,
623
(
2007
).
33.
R.
Agrawal
,
A.
Nieto
,
H.
Chen
,
M.
Mora
, and
A.
Agarwal
,
ACS Appl. Mater. Interfaces
5
,
12052
(
2013
).
34.
D. M.
Espino
,
D. E. T.
Shepherd
, and
D. W. L.
Hukins
,
BMC Musculoskeletal Disord.
15
,
205
(
2014
).
35.
M. L.
Lee
,
Y.
Li
,
Y. P.
Feng
, and
C. W.
Carter
,
Intermetallics
10
,
1061
(
2002
).
36.
G.
Balooch
,
G. W.
Marshall
,
S. J.
Marshall
,
O. L.
Warren
,
S. A.
Asif
, and
M.
Balooch
,
J. Biomech.
37
,
1223
(
2004
).
37.
I. D.
Brown
,
The Chemical Bond in Inorganic Chemistry: The Bond Valence Model
(
Oxford University
,
Oxford
,
2006
).
38.
K. L.
Van Landuyt
,
Y.
Yoshida
,
I.
Hirata
,
J.
Snauwaert
,
J.
De Munck
,
M.
Okazaki
,
K.
Suzuki
,
P.
Lambrechts
, and
B.
Van Meerbeek
,
J. Dent. Res.
87
,
757
(
2008
).
39.
S.
Sauro
,
M.
Toledano
,
F. S.
Aguilera
,
F.
Mannocci
,
D. H.
Pashley
,
F. R.
Tay
,
T. F.
Watson
, and
R.
Osorio
,
Dent. Mater.
27
,
563
(
2011
).
40.
L.
Angker
and
M. V.
Swain
,
J. Mater. Res.
21
,
1893
(
2006
).
41.
J. H.
Kinney
,
M.
Balooch
,
G. W.
Marshall
, and
S. J.
Marshall
,
Arch. Oral Biol.
44
,
813
(
1999
).
42.
J. L.
Katz
,
S.
Bumrerraj
,
J.
Dreyfuss
,
Y.
Wang
, and
P.
Spencer
,
J. Biomed. Mater. Res. Appl. Biomater.
58
,
366
(
2001
).
43.
H.
Ryou
,
E.
Romberg
,
D. H.
Pashley
,
F. R.
Tay
, and
D.
Arola
,
J. Mech. Behav. Biomed. Mater.
42
,
229
(
2015
).
44.
M.
Balooch
,
S.
Habelitz
,
J. H.
Kinney
,
S. J.
Marshall
, and
G. W.
Marshall
,
J. Struct. Biol.
162
,
404
(
2008
).
45.
M.
Toledano
,
F. S.
Aguilera
,
E.
Osorio
,
I.
Cabello
,
M.
Toledano-Osorio
, and
R.
Osorio
,
Microsc. Microanal.
21
,
214
(
2015
).
46.
M.
Toledano
,
F. S.
Aguilera
,
E.
Osorio
,
I.
Cabello
,
M.
Toledano-Osorio
, and
R.
Osorio
,
Biointerphases
10
,
031002
(
2015
).
47.
See supplementary material at http://dx.doi.org/10.1116/1.4979633 for representation of scanning mode nano-DMA analysis, mean and standard deviation values of tan delta and complex modulus attained in other experimental groups. A table of materials composition is provided.

Supplementary Material

You do not currently have access to this content.