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Figure Captions
Fig. 1 SEM image of the PEEK surface by using a scanning electron microscope operating at
1.7 kV and at a distance of 5.0–6.0 mm after each surface treatment. A: no surface pretreatment
(no treatment), smooth and homogeneous surface B: air abrasion with 50 μm alumina oxide
particles at 0.1 MPa at a 10 mm distance for 10 seconds (sandblasting treatment), many convex
precipitates compared with the untreated PEEK surface C: acid etched with sulfuric acid (98%)
for 1 min and then rinsed with deionized water for 1 min (sulfuric acid etching), large pits and
pores surface D: Nd:YVO4 laser irradiation at an interval of 200 μm in the side and vertically
and at a depth of 150 μm (laser groove treatment), regular grooves in a grid pattern and
undercutting surface
Fig. 2 Mean and standard deviation for surface roughness values (n=20)
Note: Asterisks represent significant difference (p<0.05)
Fig. 3 Mean and standard deviation for water contact angle values (n=20)
Note: Asterisks represent significant difference (p<0.05)
30
Fig. 4 Wide-scan spectra of (A) no treatment, (B) sandblasting treatment, (C) sulfuric acid
treatment, and (D) Nd:YVO4 laser groove treatment PEEK surfaces by XPS.
Fig. 5 C1s spectra of (A) no treatment, (B) sandblasting treatment, (C) sulfuric acid treatment,
and (D) Nd:YVO4 laser groove treatment PEEK surfaces by XPS.
Abbreviated word: CC: C-C bonds, CO: C-O bonds, COO: O-C=O bonds
Fig. 6 Mean and standard deviation for shear bond strength (MPa) of specimens with different
surface treatment of 24h after specimen preparation and after thermal cycling (10,000 cycles)
for no treatment, sandblasting treatment, sulfuric-acid etching, and laser groove treatment
Note: Within the same column, the same superscripted letters indicate no significant differences
(p>0.05)
Interaction of surface treatment and thermal cycle for RelyX Ultimate Resin Cement: p=0.0402,
for Super-Bond C&B: p=0.0641
31
Fig. 7 SEM image of the fractured surfaces of PEEK following shear bond test after the thermal
cycle (A group: no treatment, B group: sandblasting treatment, C group: sulfuric acid
etching).
A-1 (low magnification), A-2 (medium magnification), A-3 (high magnification),
B-1 (low magnification), B-2 (medium magnification), B-3 (high magnification),
C-1 (low magnification), C-2 (medium magnification), C-3 (high magnification)
A and B group: No resin cement was observed on both the surface of the no treatment and the
sandblasting treated specimens.
C group: A resin cement was observed on the surface of the sulfuric-acid-etched specimens.
Abbreviated word: a: PEEK, b: Adhesive resin cement
Fig. 8 SEM image of the fractured surfaces of PEEK following shear bond test after the thermal
cycle
D-1, D-2, D-3: laser groove treatment/Rely X Ultimate Resin Cement
D-4, D-5, D-6: laser groove treatment/Super-Bond C&B
D-1 (low magnification), D-2 (medium magnification), D-3 (high magnification),
D-4 (low magnification), D-5 (medium magnification), D-6 (high magnification),
32
On the surfaces of laser-groove-treated specimens, large amounts of resin cement and broken
PEEK material were observed remaining in the groove.
Abbreviated word: a: PEEK, b: Adhesive resin cement
33
Fig. 1 SEM image of the PEEK surface by using a scanning electron microscope operating at 1.7 kV
and at a distance of 5.0–6.0 mm after each surface treatment. A: no surface pretreatment (no treatment),
smooth and homogeneous surface B: air abrasion with 50 μm alumina oxide particles at 0.1 MPa at
a 10 mm distance for 10 seconds (sandblasting treatment), many convex precipitates compared with
the untreated PEEK surface C: acid etched with sulfuric acid (98%) for 1 min and then rinsed with
deionized water for 1 min (sulfuric acid etching), large pits and pores surface D: Nd:YVO4 laser
irradiation at an interval of 200 μm in the side and vertically and at a depth of 150 μm (laser groove
treatment), regular grooves in a grid pattern and undercutting surface
34
Fig. 2 Mean and standard deviation for surface roughness values (n=20)
Note: Asterisks represent significant difference (p<0.05)
35
Fig. 3 Mean and standard deviation for water contact angle values (n=20)
Note: Asterisks represent significant difference (p<0.05)
36
Fig. 4 Wide-scan spectra of (A) no treatment, (B) sandblasting treatment, (C) sulfuric acid treatment,
and (D) Nd:YVO4 laser groove treatment PEEK surfaces by XPS.
37
Fig. 5 C1s spectra of (A) no treatment, (B) sandblasting treatment, (C) sulfuric acid treatment, and (D)
Nd:YVO4 laser groove treatment PEEK surfaces by XPS.
Abbreviated word: CC: C-C bonds, CO: C-O bonds, COO: O-C=O bonds
38
Fig. 6 Mean and standard deviation for shear bond strength (MPa) of specimens with different surface
treatment of 24h after specimen preparation and after thermal cycling (10,000 cycles) for no treatment,
sandblasting treatment, sulfuric-acid etching, and laser groove treatment
Note: Within the same column, the same superscripted letters indicate no significant differences (p>0.05)
39
Fig. 7 SEM image of the fractured surfaces of PEEK following shear bond test after the thermal cycle
(A group: no treatment, B group: sandblasting treatment, C group: sulfuric acid etching).
A-1 (low magnification), A-2 (medium magnification), A-3 (high magnification),
B-1 (low magnification), B-2 (medium magnification), B-3 (high magnification),
C-1 (low magnification), C-2 (medium magnification), C-3 (high magnification)
A and B group: No resin cement was observed on both the surface of the no treatment and the
sandblasting treated specimens.
C group: A resin cement was observed on the surface of the sulfuric-acid-etched specimens.
Abbreviated word: a: PEEK, b: Adhesive resin cement
40
Fig. 8 SEM image of the fractured surfaces of PEEK following shear bond test after the thermal cycle
D-1, D-2, D-3: laser groove treatment/Rely X Ultimate Resin Cement
D-4, D-5, D-6: laser groove treatment/Super-Bond C&B
D-1 (low magnification), D-2 (medium magnification), D-3 (high magnification),
D-4 (low magnification), D-5 (medium magnification), D-6 (high magnification),
On the surfaces of laser-groove-treated specimens, large amounts of resin cement and broken PEEK
material were observed remaining in the groove.
Abbreviated word: a: PEEK, b: Adhesive resin cement
41
Table 1. List of materials used in the present study
Materials
Product name
Main composition
PEEK
Vestakeep
DC4450
Polyetheretherketone, 20%
Titanium dioxide pigments
Adhesive
system
Visio.link
MMA, pentaerythritol
triacrylate, photo initiators
Adhesive
resin cements
RelyX Ultimate
Resin Cement
Adhesive
resin cements
Super-Bond
C&B
Lot. number
Manufacturer
Daical-Evonik
171018
Bredent GmbH
& Co KG
Methacrylate monomer,
silica, polymerization
initiator
653276
3M ESPE
MMA, 4-META, TBB,
PMMA
SS1
Sun Medical
Co. Ltd.
MMA: methyl methacrylate, 4-META: 4-methacryloxyethyl trimellitate anhydride, TBB: tributylborane,
PMMA: polymethyl methacrylate
42
Table 2. Atomic compositions of C, O, N, Al, and Ti elements (Upper Table) and of CC, CO, and COO
functional groups (Lower Table) in No treatment, Sandblasting treatment, Sulfuric acid treatment, and
Laser groove treatment from XPS analysis
Group
%C
%O
%N
%Al
%Ti
No treatment
81.9
16.0
2.1
Sandblasting treatment
62.9
31.7
5.3
0.1
Sulfuric acid etching
73.5
26.2
0.3
Laser groove treatment
72.1
23.5
1.4
2.9
Group
%CC
%CO
%COO
No treatment
65.5
29.5
5.1
Sandblasting treatment
63.9
20.7
15.4
Sulfuric acid etching
64.6
25.8
9.6
Laser groove treatment
57.1
29.1
13.9
43
Table 3. Failure modes
Group
Failure mode
No treatment
Sandblasting treatment
Sulfuric acid etching
Laser groove
treatment
Shear bond strength tested 24h
after specimens preparation
Shear bond strength tested after
thermal cycling (10,000 cycles)
RelyX Ultimate
Resin Cement
Super-Bond
C&B
RelyX Ultimate
Resin Cement
Super-Bond
C&B
a/b/c/d
a/b/c/d
a/b/c/d
a/b/c/d
10 / 0 / 0 / 0
9/0/0/1
10 / 0 / 0 / 0
10 / 0 / 0 / 0
9/0/0/1
10 / 0 / 0 / 0
10 / 0 / 0 / 0
9/0/0/1
4/0/0/6
6/0/0/4
5/0/0/5
5/0/0/5
0 / 0 / 10 / 0
0 / 0 / 10 / 0
0 / 0 / 10 / 0
0 / 0 / 10 / 0
Failure modes:
a) adhesive failure between materials and luting agents
b) cohesive failure within adhesive luting agents
c) cohesive failure within materials
d) mixed failure with both cohesive and adhesive failures
44
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