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ORIGINAL ARTICLE

Analysis of surface roughness and surface free


energy characteristics of various orthodontic
materials
Hyo-Beom Ahn,a Sug-Joon Ahn,b Shin-Jae Lee,c Tae-Woo Kim,d and Dong-Seok Nahme
Seoul, Korea

Introduction: The purpose of this study was to analyze the differences in surface characteristics of various
orthodontic materials; this might provide valuable information on bacterial adhesion to orthodontic materials.
Methods: Surface roughness (SR) and surface free energy (SFE) characteristics of 5 orthodontic adhesives
(2 composites resins, 2 resin-modified glass ionomer cements, and 1 compomer), 5 bracket materials (2 stain-
less steel, 1 monocrystalline sapphire, 1 polycrystalline alumina, and 1 plastic) and bovine incisors were inves-
tigated by using confocal laser scanning microscopy and the sessile drop method. Results: There were
significant differences in SR and SFE characteristics among orthodontic materials. Bovine incisors showed
the roughest surface, and monocrystalline sapphire showed the smoothest surface. However, there were
only small variations in SR (less than 0.3 mm) among the materials, except for bovine incisors. In contrast to
SR, there were big differences in SFE characteristics among materials. Generally, bracket materials showed
lower SFE—specifically, dispersive and polar components on their surfaces—than orthodontic adhesives.
Resin-modified glass ionomer cements had the highest SFE, dispersive component, and polarity; these
conditions are more favorable for bacterial adhesion. Conclusions: This study suggests that SFE character-
istics can influence bacterial adhesion to orthodontic materials more than SR, and bracket materials might
have less favorable SFE characteristics for bacterial adhesion than orthodontic adhesives. (Am J Orthod
Dentofacial Orthop 2009;136:668-74)

M
any orthodontic materials provide proper streptococci to orthodontic materials is considered to
conditions for the colonization of oral micro- play a key role in the pathogenesis of enamel deminer-
organisms in the oral cavity, because they alization. Previous studies reported that the placement
impede access to the tooth surfaces for cleaning and of a fixed orthodontic appliance induces increased
provide additional adhesion sites for oral bacteria, lead- volumes and numbers of mutans streptococci in dental
ing to pathogenic plaque formation.1-4 The resultant plaque, but the elevated levels return to normal levels
increase in plaque retention places patients at higher after removal of the appliance.5,6
risk for enamel demineralization adjacent to the ortho- Surface characteristics of biomaterials influence
dontic materials. In particular, adhesion of mutans bacterial adhesion in vitro.7-9 Surface roughness (SR)
and surface free energy (SFE) have significant impacts
a
Clinical instructor, Department of Orthodontics, School of Dentistry, Seoul on bacterial adhesion.8,9 A rough surface allows bacte-
National University, Seoul, Korea. rial colonization by increasing the adhesion areas and
b
Assistant professor, Dental Research Institute and Department of Orthodon-
tics, School of Dentistry, Seoul National University, Seoul, Korea. preventing dislodgement of bacterial colonies. A mate-
c
Associate professor, Dental Research Institute and Department of Orthodon- rial with high SFE attracts more bacteria to its surface
tics, School of Dentistry, Seoul National University, Seoul, Korea. than one with low SFE; this is governed by thermody-
d
Professor, Dental Research Institute and Department of Orthodontics, School
of Dentistry, Seoul National University, Seoul, Korea. namic rules.7-9 In addition, nonspecific physicoche-
e
Professor emeritus, Dental Research Institute and Department of Orthodontics, mical interactions, consisting of van der Waals,
School of Dentistry, Seoul National University, Seoul, Korea. electrostatic, and acid-base interactions, play important
Supported by a grant of the Korea Healthcare Technology R&D Project,
Ministry for Health, Welfare and Family Affairs, Republic of Korea (A091074). roles in initial bacterial adhesion, which can be defined
The authors report no commercial, proprietary, or financial interest in the by the SFE components.7,10
products or companies described in this article. Brackets and adhesives are the representative ma-
Reprint requests to: Sug-Joon Ahn, Dental Research Institute and Department of
Orthodontics, School of Dentistry, Seoul National University, 28-22 Yunkeun- terials available in clinical orthodontics. Among them,
Dong, Chongro-Ku, Seoul 110-768, Korea (ROK); e-mail, titoo@snu.ac.kr. composites and glass ionomers are the 2 main classes
Submitted, August 2007; revised and accepted, November 2007. of orthodontic bonding adhesives, and metal, ceramic,
0889-5406/$36.00
Copyright Ó 2009 by the American Association of Orthodontists. and plastic are widely used bracket materials.
doi:10.1016/j.ajodo.2007.11.032 Although their physical and mechanical properties
668
American Journal of Orthodontics and Dentofacial Orthopedics Ahn et al 669
Volume 136, Number 5

Fig 1. Box plots for surface roughness (mm) of various orthodontic materials: 2 composite adhesives
(Enlight [EN] and Lightbond [LB]), 2 RMGIs (Fuji Ortho LC [FO] and Multi-cure [MC]), 1 compomer
(Transbond Plus [TP]), 2 stainless steel bracket materials (MB1 and MB2), 1 monocrystalline sapphire
bracket material (MCS), 1 polycrystalline alumina bracket material (PCA), and 1 plastic bracket ma-
terial (PB), and bovine incisor (BI).

Fig 2. Box plots for surface free energy (mJ/m2) of various orthodontic materials: 2 composite adhe-
sives (Enlight [EN] and Lightbond [LB]), 2 RMGIs (Fuji Ortho LC [FO] and Multi-cure [MC]), 1
compomer (Transbond Plus [TP]), 2 stainless steel bracket materials (MB1 and MB2), 1 monocrystal-
line sapphire bracket material (MCS), 1 polycrystalline alumina bracket material (PCA), and 1 plastic
bracket material (PB), and bovine incisor (BI).

have been extensively studied, their surface character- bacterial-adhesion and plaque-retaining capacities
istics associated with bacterial adhesion have not been associated with enamel demineralization during or-
as well investigated. Differences in bacterial adhesion thodontic treatment. We compared SR and SFE
to the various orthodontic materials can be expected characteristics of 10 representative orthodontic mate-
because of their different surface characteristics. rials with those of bovine enamel to determine which
Knowledge of surface characteristics of orthodontic material has a higher retaining capacity for oral
materials can provide valuable information on the bacteria.
670 Ahn et al American Journal of Orthodontics and Dentofacial Orthopedics
November 2009

Table I. One-way ANOVA results for surface roughness (mm) in various orthodontic materials
Orthodontic adhesive (mean 6 SD)

EN LB TP FO MC

0.39 6 0.01C 0.44 6 0.01E 0.41 6 0.01D 0.41 6 0.02C,D 0.44 6 0.01E

The same superscripts indicate no statistically significant difference between the groups (P .0.05).
Increasing group mean values were expressed with ascending alphabetical order.
EN, Enlight; LB, Lightbond; FO, Fuji Ortho LC; TP, Transbond Plus; MC, Multi-cure; MB1, stainless steel bracket material (Tomy); MB2, stainless
steel bracket material (Biomaterials); PCA, polycrystalline alumina bracket material; MCS, monocrystalline sapphire bracket material; PB, plastic
bracket material; BI, bovine incisor block.

Table II.One-way ANOVA results for SFE and its components (mJ/m2) (dispersive, polar, acid, and base components)
in various orthodontic raw materials
Orthodontic adhesive (mean 6 SD)

EN LB TP FO MC

SFE 38.38 6 1.40E 38.84 6 1.54E 45.24 6 1.11F 46.98 6 0.99G 47.11 6 1.08G
Dispersive 39.92 6 1.12F 39.85 6 0.95F 42.02 6 0.73H 41.14 6 0.65G 42.76 6 0.63I
Polar –1.53 6 1.95BC –1.04 6 1.75C 3.23 6 1.03E 5.91 6 1.04F 4.29 6 1.27E
Acid 0.09 6 0.10AB 0.05 6 0.07A 0.27 6 0.17B 1.19 6 0.47C 0.23 6 0.15B
Base 10.51 6 2.35C 13.81 6 3.41D 10.99 6 2.08C 7.91 6 1.43AB 17.19 6 3.31E

The same superscripts indicate no statistically significant difference between the groups (P .0.05).
Increasing group mean values were expressed with ascending alphabetical order.
EN, Enlight; LB, Lightbond; FO, Fuji Ortho LC; TP, Transbond Plus; MC, Multi-cure; MB1, stainless steel bracket material (Tomy); MB2, stainless
steel bracket material (Biomaterials); PCA, polycrystalline alumina bracket material; MCS, monocrystalline sapphire bracket material; PB, plastic
bracket material; BI, bovine incisor block.

MATERIAL AND METHODS Each material was fabricated and polished the same as
Five light-cured orthodontic bonding adhesives real brackets and provided in a uniform size (12.0 3
were used in this study: a nonfluoride-releasing com- 10.0 3 2.0 mm) by the manufacturers.
posite (Enlight [EN], Ormco/A Company, Glendora, Three freshly extracted, healthy bovine incisors
Calif), a fluoride-releasing composite (Lightbond (BIs) were cleaned with a rotary brush and pumice,
[LB], Reliance Orthodontics, Itasca, Ill), 2 resin-modi- and stored in 1% aqueous solution of chloramine-T
fied glass ionomer (RMGI) cements (Fuji-Ortho LC (Junsei Chemical, Tokyo, Japan) at 4 C. Each incisor
[FO], GC Corporation, Tokyo, Japan; Multi-cure was embedded in an acrylic mold with the labial surface
[MC], 3M Unitek, Monrovia, Calif), and a compomer parallel to the mold base.
(Transbond Plus [TP], 3M Unitek). Specimens were Every specimen was carefully cleaned with the
prepared by using Teflon (DuPont, Seoul, Korea) following procedures immediately before measuring sur-
templates (diameter,12.0 mm; depth, 2.0 mm) accord- face characteristics to maintain the same surface condition
ing to the manufacturer’s instructions. Template plates and prevent any changes in surface characteristics during
were positioned on the top of glass slides. Each bonding the experiments. All specimens were soaked for 10
material was placed into the holes until the material was minutes in 1% sodium dodecyl sulfate. Then they were
flush with the top of the template. A second slide was washed 3 times with phosphate-buffered saline solution
placed on top, pushed down to ensure a flat dorsal sur- (pH 7.4) and cleaned rigorously by using an ultrasonic
face and then gently removed. All materials were han- cleaner in a solution of methanol and distilled deionized
dled according to the manufacturers’ instructions and water for 1 minute. Additional cleaning was done by using
light cured for 40 seconds (20 seconds from the top the ultrasonic cleaner in distilled water for 10 minutes.
and 20 seconds from the bottom). All specimens were air dried after cleaning.
Five kinds of bracket materials were used in this SR was analyzed by using confocal laser scanning
study: 2 stainless steel ([MB1], Tomy, Tokyo, Japan; microscopy (Axiovert 200 M, Carl Zeiss, Thornwood,
[MB2] Biomaterials, Seoul, Korea), a polycrystalline NY). The multi-argon laser emits light with a wavelength
alumina (PCA, Tomy), a monocrystalline sapphire of 633 nm. This allows the calculation of the arithmetic
(MCS, HT, Seoul, Korea), and a plastic (PB, Tomy). mean of SR from a mean plane in the sampling area (245
American Journal of Orthodontics and Dentofacial Orthopedics Ahn et al 671
Volume 136, Number 5

Table I. Continued
Bracket material (mean 6 SD)
BI
MB1 MB2 PCA MCS PB (mean 6 SD)

0.54 6 0.02F 0.58 6 0.02G 0.45 6 0.02E 0.28 6 0.03A 0.33 6 0.02B 0.98 6 0.03H

Table II. Continued

Bracket material (mean 6 SD)


BI
MB1 MB2 PCA MCS PB (mean 6 SD)

31.80 6 1.03A 36.66 6 1.36D 34.33 6 1.52B 33.47 6 2.16B 35.48 6 1.51C 39.03 6 1.94E
31.64 6 1.01A 39.68 6 1.06F 33.72 6 0.93B 35.29 6 1.35C 37.83 6 0.89D 38.88 6 1.08E
0.21 6 1.08D –2.99 6 1.49A 0.60 6 1.99D –1.83 6 1.79A,B,C –2.36 6 1.64AB 0.17 6 1.48D
0.04 6 0.05A 0.45 6 0.38B 0.05 6 0.04A 0.17 6 0.19AB 0.05 6 0.05AB 0.06 6 0.06A
6.45 6 1.87A 9.98 6 1.94BC 20.74 6 3.34F 6.49 6 3.50A 9.91 6 2.28BC 7.95 6 2.94AB

3 245 3 60 mm). SFE consists of dispersive (gLW) and RESULTS


polar acid-base components (gAB). The polar acid-base SR ranged from 0.28 to 0.98 mm, and there were
components were further divided into acid (g1) and significant differences among the orthodontic materials
base (g–) components. SFE and its component parts (Table I, Fig 1). MCS had the smoothest surfaces,
were measured by the sessile drop method. Three probe whereas BIs showed the roughest surfaces.
liquids of different polarities were used: 1-bromonaph- There were also significant differences in SFE and
thalene (ACROS Organics, Fairlawn, NJ), formamide its components among the materials, but the pattern
(Mallinckrodt Baker, Phillipsburg, NJ), and distilled de- was different from SR (Table II, Fig 2). The range of
ionized water. A video camera equipped with an image SFE was 31.8 to 47.11 millijoules (mJ) per square me-
analyzer (Phoenix 300, Surface Electro Optics, Seoul, ter. The RMGIs (FO and MC) had the highest SFE,
Korea) visualized the shape of the drop and determined whereas MB1 had the lowest SFE. The dispersive com-
the contact angle. Right and left contact angles of each ponent of SFE, gLW, was 31.64 to 42.76 mJ per square
drop were averaged to give 1 contact angle per drop. meter. MB1 had the lowest value, and MC had the
The SFE and its components—gLW, gAB, g1, and g–— highest value. The polar component of SFE, gAB, had
were calculated by combining contact angle measure- values from –2.99 to 5.91 mJ per square meter. MB2
ments from the interfaced computer according to the had negative and lower values than the other materials,
approach proposed by van Oss et al.11 and FO had positive and significantly higher values than
Three specimens of each material were used. Each the others. All surfaces of the orthodontic materials
experiment was performed 5 times for each specimen. were strongly basic and weakly acidic except FO, which
The surface characteristics of the 5 orthodontic adhe- showed the lowest g– and the highest g1 (Table II).
sives, the 5 bracket materials, and the BI block were an- Generally, orthodontic adhesives had higher SFE
alyzed by using 1-way analysis of variance (ANOVA) to and dispersive components than did bracket materials.
investigate which material showed the greatest SFE. Mul- The RMGIs had the highest value in SFE, particularly,
tiple comparisons were done with the Duncan multiple the dispersive and polar components among the ortho-
range tests at a level of P \0.05. Pearson correlation dontic materials. BIs showed intermediate SFE, and
analysis was used to compare the relationships between its components were between the bracket materials
SR and SFE characteristics of the various materials. and the orthodontic adhesives.
672 Ahn et al American Journal of Orthodontics and Dentofacial Orthopedics
November 2009

Table III. Results of Pearson correlation coefficient test the materials (Table II). The differences in SFE and its
between surface roughness and surface free energy of components might be due to different physicochemical
various orthodontic materials (no significant correla- properties and compositions. In particular, the RMGIs
tions) (FO and MC) had the highest SFE, gLW and gAB, which
Dispersive Polar Acid Base
means that RMGI surfaces have higher SFE—particu-
SFE component component component component larly, stronger dispersive and polar properties than the
other materials. The highest SFE, gLW and gAB, might
SR –0.017 –0.002 –0.024 –0.180 –0.136
be mainly due to different chemical compositions.
RMGIs contain highly reactive fluoro-aluminosilicate
glass fillers from which fluoride ions are continuously
As a result of the Pearson correlation coefficient diffused and released as the result of ion exchange in
test, there was an unclear relationship between the SR the aqueous environment.14-16 These differences can
and the SFE components of orthodontic materials be partly explained by the differences in setting mecha-
(Table III). nisms and reaction activities in the surfaces. The initial
setting of the RMGIs is performed by light-activated po-
lymerization, followed by an acid-base reaction from
DISCUSSION the absorption of water.14,16 The dynamic reaction pro-
It is well known that rough surfaces favor the accu- cesses from the surface of RMGIs might be associated
mulation of plaque and increase the available surface with high SFE, particularly dispersive property and
areas for bacterial colonization.8 A previous study acid-base polarity on the surfaces. In contrast to the
showed that SR varied among different dental mate- RMGIs, the main filler in composite adhesives is inert
rials.12 We also found significant differences in SR glass dispersed in methacrylate monomers, which might
among orthodontic materials. Although there were sta- contribute to relative lower SFE characteristics than
tistically significant differences in SR, there were only RMGIs. Intermediate SFE values of the compomer
small variations in SR except BIs (Table I). can be explained by its intermediate composition be-
BI enamel was used to analyze the surface charac- tween that of the RMGIs and the composite (Table II).
teristics of enamel instead of human enamel, because The differences in SFE characteristics between or-
it is difficult to achieve sufficient surface areas to mea- thodontic adhesives and bracket materials can be ex-
sure SFE characteristics from natural untreated human plained by their differences in surface reactivities.
teeth, and a previous study reported that bovine teeth Bracket materials might have fewer reactive surfaces
are a reliable substitute.13 This study showed that BIs than orthodontic adhesives, because bracket materials
had the roughest surfaces, which might be due to ridges, are made from stable metal alloys or ceramics, and
grooves, and curved surfaces of enamel. A previous have stable crystal structures and orientations. In case
study reported that the SR of human enamel was up to of RMGIs and compomers, however, polymerization
4.50 mm.12 Because BIs are larger than human incisors, and polyacid neutralization including fluoride release
the SR of BIs (about 1.0 mm) in this study would be continue in the aqueous phase for long periods.17 In ad-
smoother than those of human enamel. Although the dition, relatively impermeable composites are reported
enamel surfaces of BIs are rougher than the other ortho- to react to exogenous components, such as fluoride, af-
dontic materials, we did not flatten the enamel surface ter exposure.16 The differences in surface reactivity can
of the BIs because surface grinding and polishing can influence SFE characteristics of orthodontic materials.
significantly influence SFE components; this could pro- In the study of Eliades et al,18 bracket metal
vide undesirable information about bacterial adhesion showed the highest critical surface tension among the
to enamel surface. bracket materials, suggesting a higher potential for in-
Except for the BI surfaces, stainless steel had creased plaque-retaining capacity. A significant corre-
rougher surfaces than the other orthodontic materials; lation between SFE and its plaque-retaining capacity
the smoothest surface was found in MCS. Of the ortho- has been established, with the higher energies showing
dontic adhesives, SR was intermediate among those of a favorable effect on bacterial adherence.19 A recent
bracket materials. However, the ranges in SR of ortho- study showed that Streptococcus (S) mutans adhered
dontic adhesives were relatively uniform (\0.05 mm to metal brackets more than to ceramic and plastic
of mean SR) despite statistical significance. brackets.20 However, Fournier et al21 showed that bind-
In contrast to SR, completely different results were ing affinity of S mutans to metal brackets was lower
observed in the SFE and its components. There were than to plastic and porcelain brackets. The opposite re-
significant variations in SFE and its components among sults might be due to the differences in SFE
American Journal of Orthodontics and Dentofacial Orthopedics Ahn et al 673
Volume 136, Number 5

characteristics between the materials used in the previ- characteristics between bracket materials and composite
ous studies. In our study, the 2 metals showed signifi- adhesives. This study suggests that oral bacteria can ad-
cantly different SFE characteristics; MB1 had the here to human enamel more than to composite adhesives
lowest SFE, the lowest dispersive component, and in- and bracket materials, because BIs had significantly
termediate polar property, whereas MB2 had interme- rougher surfaces than composites and bracket materials.
diate SFE and dispersive component and the lowest Clinical observation has indicated that the most
polar property. These differences might be mainly common sites for enamel demineralization are at the
due to the type of metals, which can influence bacterial junction between the bonding adhesive and the enamel,
binding. Differences in fabrication procedures can just peripheral and commonly gingival to the bracket
partly influence the differences in SFE components, base.28 This study suggests that orthodontic adhesives
since physical and chemical changes in materials can have more favorable surface characteristics for bacterial
affect relevant surface properties.22 adhesion than bracket materials, because bracket mate-
Changes in SR of a solid surface influence the con- rials have lower SFE, specifically in the polarity and dis-
tact angle, which can cause changes in SFE characteris- persive components than adhesives. Also, orthodontic
tics.9 However, we found no evident relationships adhesives are peripheral to brackets and closer to the
between SR and SFE characteristics (Table III) in this enamel surfaces. Furthermore, the clinical methods to
study. This might be due to small variations in SR prepare orthodontic adhesives would provide much
among the different materials and among the same ma- rougher surfaces than those used to prepare the adhesive
terials. Previous studies reported that minor variations surfaces (between the glass slab and Teflon) in this
in SR (\0.2 mm) had no significant effects on the con- study. The remaining adhesive around bracket bases
tact angles for SFE measurement and bacterial adhe- could provide suitable sites for the rapid attachment
sion.9,23 In addition, different chemical compositions and growth of oral microorganisms.29 These findings in-
of the materials can influence insignificant relationships dicate that the adhesive around brackets should be re-
between SR and SFE characteristics. As a result, SFE moved carefully during the bonding procedure.
and its components could influence the bacterial adhe- Although bacterial adhesion to bracket materials
sion to orthodontic materials more than SR. might be lower than that to bonding adhesives, careful
Because a material with higher SFE attracts more oral hygiene should be required to prevent enamel de-
cariogenic bacteria, greater bacterial adhesion would mineralization around brackets because the complex
be expected in a material with higher SFE.7-9 In partic- configuration of the brackets can impede access to the
ular, the van der Waals interaction defined by the disper- tooth surfaces for cleaning, and the rougher surface of
sive component and the acid-base polar interaction the enamel retains more oral bacteria.
defined by the polar component tend to create strong ini-
tial adhesion between oral bacteria and a material sur- CONCLUSIONS
face.24,25 In contrast to SFE and its dispersive and
This study was undertaken to analyze the difference in
polar components, the effect of acid and base compo-
SR and SFE components of various orthodontic materials.
nents on bacterial adhesion has not been clearly ex-
There were significant differences in SR and SFE charac-
plained. In addition, all surfaces of the orthodontic
teristics among orthodontic materials. There were small
materials were strongly basic and weakly acidic except
variations in SR among orthodontic materials despite sta-
FO (Table II). Considering SFE and its dispersive and
tistically significant differences in SR. Stainless steel
polar properties, one would expect higher bacterial ad-
showed the roughest surface, and monocrystalline sap-
hesions in the order of RMGIs, compomer, composites,
phire had the smoothest surface. In general, orthodontic
and bracket materials. Some bracket materials (PCA
bonding adhesives showed higher SFE and higher disper-
and MB1) showed higher polarities than composites,
sive components on their surfaces than bracket materials.
but the differences in polarity might be too small to
RMGIs showed the highest SFE. However, no significant
have a significant effect on bacterial adhesion (Table
relationship was found between SR and SFE of orthodon-
II). This is partly supported by previous studies that
tic materials. This study suggests that orthodontic adhe-
showed that oral bacteria adhered to RMGI more than
sives have more favorable surface characteristics for
to composite adhesives, and adhesion of cariogenic
bacterial adhesion than bracket materials.
streptococci to orthodontic adhesives is significantly
higher than that to bracket materials.26,27 We thank Tomy, Reliance Orthodontic Products,
BIs showed a similar SFE to composite adhesives but Rocky Mountain Orthodontics, 3M Unitek, Ormco/A
a slightly higher SFE than bracket materials. In case of dis- Company, and GC Corporation for kindly supplying the
persive and polar components, BIs showed intermediate materials.
674 Ahn et al American Journal of Orthodontics and Dentofacial Orthopedics
November 2009

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