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Relationship between sandblasting and composite resin-alloy bond strength by a silica coating

Masami Mukai, DDS, PhD, a Hisao Fukui, DDS, PhD, b and Jiro Hasegawa, DDS, PhD c

Aichi-Gakuin University, School of Dentistry, Nagoya, Japan


Modification of alloys for resin-bonded fixed partial dentures has b e e n suspect since the introduction of the conservative procedure. This study investigated the effect of sandblasting on composite resin-alloy bond strengths with the Silicoating technique. Ag-Pd and Ni-Cr alloys w e r e prepared for casting. The specimens then were sandblasted w i t h 37 p m or 250 p m A1203 particles u n d e r the following conditions: 3 kg/cm 2 for 30 seconds; 5 kg/cm 2 for 10 seconds, 30 seconds, and 45 seconds; and 7 kg/cm 2 for 30 seconds. After each sandblasting treatment, the surfaces of the alloys w e r e e x a m i n e d w i t h the s c a n n i n g electron microscope and the wettability of the alloy surfaces w a s measured. After sandblasting, the alloy surface was silica-coated, and light-cured composite resin t h e n was b o n d e d to the alloy. S p e c i m e n s w e r e divided, stored in dry air for I week, and thermocycled from 4 ~ to 60 ~ C for 104 cycles. B o n d strength was m e a s u r e d by applying compressive shear stress. It was found that sandblasting m a d e the alloy-water contact angle smaller and wettability greater. The adhesive strength of composite resins w i t h alloys was influenced by sandblasting. (J PROSTHETDENT 1995;74:151-5.)

C o m p o s i t e resin-veneered artificial crowns and resin-bonded metal restorations have generated interest as an alternative to a porcelain-fused-to-metal restorations. Composite resin-metal bonding systems have been developed to enhance the bonding capacity of composite resin veneers to metal surfaces.I, 2 One problem with composite resin-metal restorations is the relatively low bond strength between metal and composite resin cements. Surface treatment of the metal by sandblasting with A 1 2 O 3 particles (37-250 pm) has improved the effectiveness of the surface area of the metal and increased the composite resin-metal bond strengths. 3 Electrolytic etching of base metal, Ag-Pd, and other types of alloy has improved mechanical bonding of composite resin-metal retainers. Concern has been expressed regarding the long-term effectiveness of resin-bonded restorations, however, because of interfacial separation. Chemical bonding is more desirable than mechanical bonding when the former is available. Silane bonding agents have been used successfully to chemically bond ceramic glass filler particles to the resinous matrix of traditional composite resin materials. Silane bonding agents are ineffective in bonding composite resin to metal, however, because of the lack of suitable bonding sites on the metal, such as Si-OH or A1-OH groups. 4

An approach that involves chemical bonding between composite resin and alloy has been presented. In this method, after the alloy substrate is sandblasted, a bond layer, proported as SiOx-C, is flame-sprayed on the substrata. The next step is silanization of the surface to create a bond between the alloy substrata and a layer of a light-curing dimethacrylate-based composite resin veneer. The complete process is frequently called the Silicoating system (Kulzer and Co. GmbH, Friedrichsdorf, Germany). A special technique is used to apply the SiOx-C:layer, in which Si-organic molecules are decomposed in the oxidizing part of a propane-air flame to create a thin intermediate bonding layer. This study investigated the relationship between sandblasting conditions and the composite resin-alloy bond strengths with Silicoating. MATERIAL AND METHODS
Alloy specimen preparation

aAssociate Professor, Department of Operative Dentistry. bAssociate Professor, Department of Dental Materials. cProfessor and Chairman, Department of Dental Materials. Copyright 9 1995 by The Editorial Council of THE JOURNALOF PROSTHETICDENTISTRY. 0022-3913/95/$3.00 +0. 101116412~

Two alloys were selected for this investigation. The first alloy was an Ag-Pd alloy (Pd 25 wt%, Ag 55 wt%, Cu 18 wt%, and other 2 wt%) (MIROCAST MC, G-C Co., Tokyo, Japan) and the second a Ni-Cr alloy (Ni 71 wt%, Cr 19 wt%, and Cu 5 wt%) (AD-CAST II, Nihon Shiken Co., Tokyo, Japan). The alloys were cast with a centrifugal casting machine in 20 x 10 x 1.5 mm plates with gypsum-bonded and phosphate-bonded investment for Ag-Pd and Ni-Cr alloy, respectively. The alloy specimen was made by grinding the alloy surface with #400 grit sandpaper to create a flat, even surface. Specimens were then sandblasted; their conditions are listed in Table I.

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Shearing load

Metal

Light-cured opaque resin

Light-cured composite resin

Fig. 1. Schematic illustration of shear compressive apparatus for measurement of bond strength.

Table I. Conditions of sandblasting


Particle size Sandblasting pressure (kg]cm2) Sandblasting
time

sandblasted alloy surface to indicate the bond site. Thereafter, a thin layer of the methylmethacrylate-containing composite resin, Dentacolor opaquer (Kulzer and Co.) was applied to the sandblasted alloy surface to a thickness of approximately 200 ~m and cured with a photo-curing apparatus (Dentacolar XS, Kulzer and Co.) for 90 seconds. A plastic ring 2 mm thick with a circular hole 6 mm in diameter was positioned over the tape. The ring was filled with a light-cured veneering resin (Dentacolar D-120, Kulzer and Co.), which then was cured for 90 seconds. Ten alloy specimens were used for each sandblasted condition for a total of 200 specimens. Ten specimens from each treatment were divided into two groups of five pieces and were subjected to the following: (1) dry storage for 7 days, and (2) 10,000 thermal cycles between 4 ~ and 60 ~ C. The alloycomposite resin bond strength then was measured by shear stress (Fig. 1) mounted on an Instron testing machine (Model 1125, Instron Co., Canton, Mass.) at the crosshead speed of 1 mm/min and recorded. The means of each sandblasted group were analyzed by ANOVA. RESULTS

(sec)

Observation of alloy surfaces


Scanning electron microscopy was used to compare the surface of Ag-Pd and Ni-Cr alloys after sandblasting with 37 pm A1203 (#400) particles, but revealed no significant differences. When 250 pm A1203 (#60) particles were selected as the sandblasting medium, however, the scale of surface deformation was different on the surface of Ag-Pd alloy (Fig. 2).

#400 A1203 (371~m) #60


A1203

(2501~m)

3 5 7 3 5 7

3o 10. 30. 45. 30 30 10. 30. 45. 30

Scanning electron microscopic observation


The sandblasted alloy surfaces were observed using scanning electron microscopy (JCMA model 733, JEOL).

Wettability of alloy surface a f t e r sandblasting


The contact angle of water to a polished surface was 58.5 ~ and 50.5 ~ for Ag-Pd and Ni-Cr alloys, respectively, but this angle decreased for both alloys after sandblasting (Fig. 3). ANOVA demonstrated statistically significant differences between particle size (p < 0.001, contribution rate 32.8%), alloys (p < 0.001, contribution rate 19.7%), and pressure and time (p < 0.001, contribution rate 13.7%) (Table II).

Measurement of contact angle (wettability)


The wettability of the surface of the alloy after sandblasting was determined by the following: 4 pl of water from a micro-pipette was positioned on the alloy surface in the thermostatic chamber, and a photograph was made at the moment of contact. The contact angle was measured from the shape of the drop of water in this photograph. The contact angle was determined from five measurements of each condition and the data were analyzed using a threefactor analysis of variance (ANOVA). 5

Resin-alloy bond strengths


The resin-alloy bond strengths improved remarkably after sandblasting regardless of whether the specimens were stored dry or thermocycled. After 1 week of dry storage after sandblasting with 37 l~m A1203 (#400) particles, the maximal bond strength improved from 9.8 (polished surface) to 19.5 MPa and 9.9 (polished surface) to 19.5 MPa for Ag-Pd alloy and Ni-Cr alloy, respectively. Conversely, when 250 > ~na h l 2 0 3 (#60) particles were used, the maximal bond strength reached 20.9 (Ag-Pd alloy) and 19.5 MPa (Ni-Cr alloy). When using 37 ~m A1203 (#400) particles followed by thermocycling, the bond strengths increased from 3.9 (polished surface) to 12.7 MPa for Ag-Pd alloy and 4.4 (polished surface) to 15.7 MPa for Ni-Cr alloy, respectively. By using 250 ~m A1203 ( # 6 0 ) particles to sandblast, the bond strengths reached a maximal of 7.9
VOLUME 74 NUMBER2

Shear bond strength testing


After the sandblasted alloy specimens were cleaned with Siliclean (ethyl acetate, Kulzer and Co.), theywere mounted in the Silicoating apparatus (Silicoater, Kulzer and Co.), and coated with specimens sustained in the oxidizing region of a propane-tetraethoxysilane-oxygen flame according to the manufacturer. After being cooled, the surface was painted with Silicoup adhesion primer solution (Kulzer and Co.). The silane coupling agent of Silicoup is 3-methacryloxypropyl-trimethoxy-silane. A piece of tape with a circular hole 6 mm in diameter was secured to the
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and 12.7 M P a for Ag-Pd a n d Ni-Cr, respectively (Fig. 4). Tables III a n d IV show ANOVA d a t a from the Ag-Pd and Ni-Cr alloys. The contribution coefficient of storage after s a n d b l a s t i n g was the g r e a t e s t percentage for both alloys.

DISCUSSION
Various adhesive bonding methods have been used in laboratory procedures. 4, 6-13 Ishijima et al. 9 reported t h a t adhesive strengths of composite resins and alloys with Silicoating was superior to t h a t of other adhesive methods. U s i n g this technique, the surface t r e a t m e n t of sandblasting t h a t was performed as p r e t r e a t m e n t for the Silicoating process exerted a n inordinate influence. S a n d b l a s t i n g increased surface a r e a of the alloy surfaces, expanded the energy of alloy surfaces, a n d also heightened activity of the surfaces. The w e t t a b i l i t y of s a n d b l a s t e d metallic surfaces was confirmed by m e a s u r i n g t h e contact angle by use of a liquid drop method. It was discovered t h a t the type of alloy and size of the particle used for s a n d b l a s t i n g influenced wettability. It was hypothesized t h a t the activated alloy surfaces a n d s t r e n g t h e n e d coating of the SiOx-C layer, and by bettering wetting with adhesives, chemical adhesion between composite resins a n d metals was improved. A s u b s t a n t i a l difference was clearly observed for the adhesive s t r e n g t h of composite resins with alloys between the group preserved in a t m o s p h e r e for 1 week and the thermocycled group for both Ag-Pd and Ni-Cr alloys. For all conditions of sandblasting, m e a s u r e d values were less in the thermocycled group. The decrease for Ag-Pd alloy was a p p r o x i m a t e l y 45% in the thermocycled group compared with the group preserved in a t m o s p h e r e for 1 week, and a p p r o x i m a t e l y 67% for Ni-Cr alloy. Peutzfeldt and Asmussen, 2 Tiller et al., 14 J a k o b e a n d Marx, 15 Re et al., 16 and Hill et a l ) 7 reported t h a t the adhesive strengths of composite resins with alloys by Silicoating despite higher h u m i d i t y were not reduced, b u t in this research, the adhesive strengths were lowered. The adhesive s t r e n g t h in the Ag-Pd alloy was s h a r p l y reduced. The reduction was a t t r i b u t e d to g r e a t e r shearing stresses at the interface of Ag-Pd alloys and composite resins t h a n those found in Ni-Cr alloys. The differences in properties of the alloys, such as t h e r m a l coefficient of expansion, hardness, roughness, a n d surface properties were responsible for this result. The effect of t e m p e r a t u r e change a n d w a t e r absorption of composite resins were also responsible for this result. Moreover, because the Ag-Pd alloy is soft compared with the Ni-Cr alloy (Fig. 2 ), the surfaces of Ag-Pd alloy samples t r e a t e d by sandblasing were a b r a d e d a n d rounded. This indicated t h a t reductions in surface a r e a s and rounding of the edges were also considered to be causes of diminished adhesive strength. The adhesive s t r e n g t h of composite resins with alloys was significantly improved by sandblasting. CLINICAL IMPLICATION

F i g . 2. Scanning electron micrographs of Ag-Pd alloy and Ni-Cr alloy surface sandblasted (7 kg/cm 2 30 sec). A, Ag-Pd alloy surface s a n d b l a s t e d with 37 p m A1203 particles; B, Ag-Pd alloy surface s a n d b l a s t e d with 250 ]am A1203 particles; C, Ni-Cr alloy surface s a n d b l a s t e d with 37 ]am A1203 particles; D, Ni-Cr alloy surface sandblasted with 250 tim A120 3 particles. ing increased surface a r e a a n d improved alloy surfaces.

CONCLUSION
1. Statistically significant differences were observed for adhesive s t r e n g t h s of composite resins with alloys between the group preserved in a t m o s p h e r e for 1 week a n d the group thermocycled for both Ag-Pd and Ni-Cr alloys. Adhesive strengths were less in t h e thermocycled group for both alloys. 2. A significant difference was observed for the Ag-Pd alloy in particle size, time, a n d p r e s s u r e during sandblasting t r e a t m e n t , b u t the contribution rate was 2.8 and 0.9%. A significant difference in time a n d pressure was observed for the Ni-Cr alloy during s a n d b l a s t i n g t r e a t m e n t , but the contribution r a t e was 1.4%. REFERENCES 1. Greene LL, Greene NA. Technicfor repair of acrylicresin veneers and incisal fractures. Dent Survey 1973;49:50-3. 2. Peutzlfeldt A, Asmussen E. Silicoatingevaluation of a new method of bonding compositeresin to metal. Scand J Dent Res 1988;96:171-6. 3. Fuang SM. In vivoand in vitro evaluation of goldand palladium alloys for etched metal resin bondedretainer [MastersThesis].Birmingham, Alabama: University of Alabama at Birmingham, 1985. 4. MusilR, Tiller DH. Molecularcouplingofresin veneers to alloysurfaces (Die molekulare Kopplung der Kunststof- Verblendung an die Legierungsoberfltiche).Dent Labor 1984;32:1156-61. 5. SokalRR, RohlfFJ. Biometry.2nd ed. San Francisco:Freeman, 1981: 222-9. 6. Hansson O. The silicoatertechnique for resin-bondedprostheses:clinical and laboratory procedures. Quintessence Int 1989;20:85-99.
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The adhesive s t r e n g t h between composite resins and alloys were clearly improved by sandblasting. SandblastAUGUST 1995

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60.
"~ 50.

Ag-Pd alloy
[] 37 ~m AI203(#400)Particles [ ] 250 i~m AI203( #60 )Particles Mean + S.E.

~ e-4 0 . E 30
20. 10,

o 0

Polished Surface

3kg/cm2 30sec

5kq/cm 2 10sec

5kg/cm2 30sec

5kg/cm2 7kg/cm2 45sec 30sec Sandblast condition

60 50 40

Ni-Cr Alloy
T
[ ] 37 ~m AIzO3(#400)Particles [ ] 250 ~m AI203( #60 )Particles Mean + S.E.

(D <D r

-~ 30 o
o

20 10

Polished Surface

3kg/cr'n2 30sec

5kg/cm2 10sec

5kg/cm2 30sec

5kg/cmz 7kg/crnz 45sec 30sec Sandblast Cnodition

F i g . 3. Relationship between contact angle and sandblasted condition of alloy.


T a b l e II. Analysis of variance for the data of contact angle*
Source S u m of square Degrees of freedom Mean s q u a r e F-value p-value Contribution (%)

(A) (B) (C) (AB) (AC) (BC) Error Total

710.22 1179.92 520.53 280.56 92.62 109.17 681.17 3574.19

1 1 4 1 4 4 84 99

710.22 1179.92 130.13 280.56 23.15 27.29 20.69 2371.96

90.20 149.86 16.53 35.63 2.94 3.47 1.63

0.000 0.000 0.000 0.000 0.025 0.012 0.175

19.65 32.79 13.68 7.63 1.71 2.17 22.37 100.00

A, Alloy; B, particle size; C, sandblasting pressure and time. *Five specimens were used for each sandblast treatment.

7. Barzilay I, Myers ML, Cooper LB, Graser GN. Mechanical and chemical retention of laboratory cured composite to metal surfaces. J PRosWHETDENT 1988;59:131-7. 8. Naegeli DG, Duke DE, Schwartz R, Norling BK. Adhesive bonding of composites to a casting alloy. J PROSTHETDENT 1988;60:279-83. 9. Ishijima T, Caputo AA, Mito R. Adhesion of resin to casting alloys. J PROSTHETD~NT 1992;67:445-9. 10. Guggenberger R. Rocatec system: adhesion by tribochemical coating. (Das Rocatec-System - HafLung durch tribochemische Beschichtung). Dtsch Zahnfirztl Z 1989;44:874-6. 154

11. Pr6bster L, Kourtis S. Surface morphology of alloys treated with the Rocatec system (Zur Oberflfichennmorphotogie von mit dem RocatecSystem behemdelten Legierungen). Dtsch Zahn~rztl Z 1991;46:135-9. 12. Hansson O, Moberg L-E. Evaluation of three silicoating methods for resin-bonded prostheses. Scand J Dent Res 1993;101:243-51. 13. Chang JC, Powers JM, Hart D. Bond strength of composite to alloy treated with bonding systems. Int J Prosthdont 1993;2:110-4. 14. Tiller HJ, Musi] R, Magnus B, Garschke A, GSble R, Lockowandt P. Sand blasting procedures and its effect on the surface properties of dental alloys: II (Der SmldstrahlprozeB und seine Ein Wirkung aufden VOLUME 74 NUMBER2

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Ag-Pd alloy
3O
Q.

37~mAI203(#400)Particles
(3_
J~

Ni-Cr alloy
3O

Mean +_S.E.

371~mA1203(#400) Particles 9 in dry air for 7 days [] thermal cycles between 4~Cand 60"C 250t~mAI203(#60)Particles m in dry air for 7 days thermal cyctes between 4~Cand 60=C

2O

2 20

==
o m

10

10

Polished Surface

3kg/cm 2 30sac

5kg/cm2 lOsec

5kg/cm2 30sec

5kg/cm2 45sac

7kg/om2 30sac

Polished Surface

3kg/cm 2 30sec

5kg/cm 2 10sec

5kg/cn12 30sec

5kg/cm2 45sac

7kg/om2 30seo

F i g , 4, B o n d s t r e n g t h s of r e s i n - a l l o y a s a f u n c t i o n of s t o r a g e .

Table HI. A n a l y s i s of v a r i a n c e for d a t a of A g - P d alloy*


Source Sum of square Degrees of freedom Mean square

F-value

p-value

Contribution (%)

(A) (B) (C) (AB) (AC) (BC) Error Total

2456.59 116.25 93.88 65.61 152.34 100~08 657.68 3642.44

1 1 4 1 4 4 84 99

2456.59 116.25 23.47 65.61 38.09 25.02 15.53 2740.56

313.50 14.84 3.00 8.37 4.86 3.19 0.98

0.000 0.000 0.023 0.005 0.001 0.017 0.422

67.02 2.77 0.87 1.37 2.48 1.04 24.45 100.00

A, Storage; B, particles size; C, sandblasting pressure and time. *Five specimens were used for each sandblast treatment.

Table IV. A n a l y s i s of v a r i a n c e for d a t a of N i - C r alloy*


Source S u m of square D e g r e e s of freedom Mean square F-value p-value
Contribution (%)

(A) (B) (C) (AB) (AC) (BC) Error Total

654.11 0.89 100.72 26.08 68.85 47.35 590.74 1479.74

1 1 4 1 4 4 84 99

654.11 0.89 25.18 26.08 17.21 11.84 20.11 746.41

96.07 0.13 3.75 3.88 2.56 1.76 1.99

0.000 0.717 0.008 0.052 0.045 0.145 0.103

42.24 -1.37 0.40 --55.99 100.00

*Five specimens were used for each sandblast treatment. Key as in Table III.

Oberfl~ichenzustandvon Dentallegierungen: II). Die Quintessenz 1985; 11:2151-8. 15. Jakobe E, Marx R. Silicoater method for bonded bridgework (Silicoaterverfahren fiir die K]ebebrticke). Dtsch Zahnarztl Z 1988;43:461-4. 16. Re GJ' Kaiser DA' Mal~ WF' Garcia'G~176F" Sheer b~ strengths and scanning electron microscope evaluation of three different retentive methods for resin-bonded retainers. J PROSTHETDENT 1988;59:568-73. 17. Hill GL, Zidan 0, Gomez-Marin O. Bond strengths of etched base metals: effects of errors in surface area estimation. J PROSTHET DENT 1986;56:41-5.

DEPARTMENT OF OPERATIVEDENTISTRY SCHOOL OF DENTISTRY A I C H I G A K U I NU N I V E R S I T Y 2-11 S U E M O R I D o R IC H I K U S A K U N A G O Y A464 JAPAN

CONTRIBUTING AUTHOR I{aruo Nakagaki, DDS, PhD, P r o f e s s o r a n d C h a i r m a n ,


D e p a r t m e n t of P r e v e n t i v e D e n t i s t r y a n d D e n t a l P u b l i c H e a l t h , School of D e n t i s t r y , A i c h i - G a k u i n U n i v e r s i t y , Nagoya, Japan. 155

Reprint requests to." DR. MASAMIMUKAI


AUGUST 1995