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Properties of Super Stainless Steels for Orthodontic Applications

Article  in  Journal of Biomedical Materials Research Part B Applied Biomaterials · May 2004

DOI: 10.1002/jbm.b.30002 · Source: PubMed

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Properties of Super Stainless Steels for Orthodontic Applications
Keun-Taek Oh,1 Young-Sik Kim,2 Yong-Soo Park,3 Kyoung-Nam Kim1
1
Research Institute of Dental Biomaterials and Bioengineering, College of Dentistry, Yonsei University,
134 Shinchon-Dong, Seodaemun-Gu, Seoul, 120-752, South Korea

2
School of Metals and Materials Engineering, Andong National University, 388 Songchun, Andong,
Kyungbuk, 760-749, South Korea

3
Department of Metallurgical Engineering, Yonsei University, 134 Shinchon-Dong, Seodaemun-Gu,
Seoul, 120-749, South Korea

Received 10 March 2003; revised 28 July 2003; accepted 3 October 2003

Published online 28 January 2004 in Wiley InterScience (www.interscience.wiley.com). DOI: 10.1002/jbm.b.30002

Abstract: Orthodontic stainless-steel appliances are considered to be corrosion resistant, but

localized corrosion can occur in the oral cavity. This study was undertaken to evaluate the
properties of super stainless steels in orthodontic applications. Accordingly, the metallurgical
properties, mechanical properties, corrosion resistance, amount of the released nickel, cyto-
toxicity, and characteristics of the passive film were investigated. Corrosion resistances of the
specimens were high and in the following order: super austenitic stainless steel (SR-50A) >
super ferritic stainless steel (SFSS) ⴝ super duplex stainless steel (SR-6DX) > 316L SS >
super martensitic stainless steel (SR-3Mo) in artificial saliva, 37 °C. At 500 mV (SCE), current
densities of SR-50A, SFSS, SR-6DX, 316L SS, and SR-3Mo were 5.96 ␮A/cm2, 20.3 ␮A/cm2,
31.9 ␮A/cm2, 805 ␮A/cm2, and 5.36 mA/cm2, respectively. Open circuit potentials of SR-50A,
316L SS, SR-6DX, SR-3Mo, and SFSS were ⴚ 0.2, ⴚ 0.22, ⴚ 0.24, ⴚ 0.43, and ⴚ 0.46 V (SCE),
respectively. SR-50A, SFSS, and SR-6DX released below 3 ng/ml nickel for 8 weeks, and
increased a little with immersion time, and 316L SS released about 3.5 ng/ml nickel, but
SR-3Mo released a large amount of nickel, which increased with immersion time. The study
demonstrated that SR-50A, SR-6DX, and SFSS have high corrosion resistance and mild or no
cytotoxicity, due to the passive film enhanced by synergistic effect of Mo ⴙ N or by high
addition effect of Cr ⴙ W. All super stainless steels showed very low cytotoxicity regardless
of their nickel contents, although SR-3Mo was found to be relatively cytotoxic. From these
studies, these steels are considered suitable for orthodontic applications. © 2004 Wiley Periodi-
cals, Inc. J Biomed Mater Res Part B: Appl Biomater 69B: 183–194, 2004

Keywords: super stainless steels; corrosion resistance; passive film; biocompatibility; metal
ion release; cytotoxicity; orthodontic appliance

INTRODUCTION chrome alloys, which have high corrosion resistance due to

Many kinds of orthodontic appliances have been developed to
move the teeth ideally during orthodontic treatment. Metallic
orthodontic appliances consist of bands, arch wires, ligature
wires, hooks, tubes, brackets, and springs. Conventionally
used orthodontic appliances are mainly made of stainless
steels, nickel–titanium alloy, titanium or its alloys, or cobalt-
Correspondence to: Kyoung-Nam Kim, Research Institute of Dental Biomaterials
and Bioengineering, College of Dentistry, Yonsei University, 134 Shinchon-Dong,
Seodaemun-Gu, Seoul, 120-752, South Korea (e-mail: kimkn@yumc.yonsei.ac.kr)
Contract grant sponsor: Brain Korea 21 Project for Medical Science, Yonsei
University
Contract grant sponsor: Medical Science and Engineering Research Program of the
Korea Science & Engineering Foundation; contract grant number: R13-2003-13
Contract grant sponsor: National Research Laboratory Project
© 2004 Wiley Periodicals, Inc.
their passive films.1
During the earliest years in orthodontic practice, appliances
were mainly constructed of precious metals, but around 1929
austenitic (18/8) stainless steel was introduced in the form of
hard-drawn arch wire. During the early 1930s, stainless steel
was also produced in an annealed strip form for the fabrication
of bands. Over the years, stainless steel has proven to be a better
material than noble metal alloys for orthodontic appliances. This
superiority is primarily due to its low cost, greater strength,
higher modulus of elasticity, good formability, and high corro-
sion resistance in the mouth. These advantages have been rec-
ognized by orthodontists, and as a result stainless steel is used
extensively for bands, brackets, and arch wires.2 However, re-
cently it has become apparent that there are needs for even
higher corrosion resistance, high strength, improved formability,
and lower cytotoxicity.
183
184 OH ET AL.
Much effort has gone into satisfying these needs and into
improving the properties of stainless steels. Super stainless
steels that have higher corrosion resistances and greater me-
chanical strengths than the conventionally used stainless
steels have been developed,3–5 and these could overcome
disadvantages such as high cost, low shear strength, low wear
resistance, low formability, and low weldability of titanium
alloys.6 – 8 Super austenitic stainless steel (SR-50A) was re-
ported to have localized corrosion resistance which is similar
to those of titanium alloys, because the passive film is en-
hanced by the synergistic effects of high nitrogen and mo-
lybdenum content.5–11 It was believed that this passive film
minimized the amount of metal dissolved in the mouth. The
super stainless steels used in this study are super austenitic
stainless steel (SR-50A),6 – 8,11 super martensitic stainless
steel (SR-3Mo),12 super duplex stainless steel (SR-6DX),13
and super ferritic stainless steel (SFSS).14 These steels were
developed for the enhancement of passive film by synergistic
effects of Mo-N or high addition effect of Cr-W.6 –14
Recently, many orthodontists have voiced concern about
the use of miniscrews as orthodontic anchorages, in terms of
their claimed advantages, which include immediate force
application after implant placement, no requirement for eden-
tulous ridges, minimal anatomic limitation, ease of placement
and removal, cost effectiveness, simple treatment mechanics,
and reduction of treatment time.15 Moreover, miniscrews
made of titanium, which offer high corrosion resistance, good
biocompatibility, and good physical properties are used ex-
tensively. However, titanium has low shear strength, low
torsional strength, and low wear resistance, it also has low
formability, machinability, and castability, and it suffers from
hydrogen embrittlement.16 –18 During orthodontic treatments,
miniscrews are used as orthodontic anchorages not only in
small diameter and optimum length, but also in high strength
because of its frequent fracture and wear during its placement
and removal. In view of the relatively short implantation
period into alveolar ridge bone and no need of osseointegra-
tion with bone,19 it is thought that super stainless steels can be
used as substitutes for titanium miniscrews.
To date, relatively few studies have been made on the
mechanical properties and corrosion resistance of super aus-
tenitic stainless steel and on their applicability to the or-
thodontic field.20 Oh and co-workers7,8,20 reported upon the
biocompatibility of super austenitic stainless steel and upon
hydroxyapatite and porous-metal-coated super stainless
steels. Comparison of the results of corrosion testing for the
HA and porous steel coating on the super stainless steels and
316L SS in Hank’s solution and 3.5% NaCl solution shows
that the super stainless steel had higher crevice and pitting
corrosion resistance than the 316L SS.7,8 The properties of
super stainless steel wire in orthodontic application have also
been studied.20 However, no study has been made on the
properties of super stainless steels, according to their phases
or nickel content for biomedical or dental applications. Prac-
tically, the corrosion resistance of stainless steels should be as
high as possible in the human body, and nickel content should
be reduced to a minimum, because nickel is a known toxin
TABLE I. Classification of Stainless Steels Used in this Study
Nickel Contents
Code Phase (wt%)
SR-50A Super austenitic stainless steel 20–22
316L SS Austenitic stainless steel 10–14
SR-6DX Super duplex stainless steel 7–10
SFSS Super ferritic stainless steel 2–3
SR-3Mo Super martensitic stainless steel 0–3
and allergen.21 However, because nickel has an essential role
in the stabilization of the austenitic phase and in the corrosion
resistance of stainless steels, it is difficult to remove nickel
totally. Therefore, the purpose of this study was to investigate
properties such as corrosion resistance, nickel-ion release
rate, cytotoxicity, and the mechanical properties of super
stainless steels with respect to nickel content; to find out the
effect of passive film characteristics on corrosion resistance,
ion release rate, and cytotoxicity; and to evaluate the potential
of these super stainless steels for orthodontic applications,
and eventually to test these steels in the medical and dental
fields.
MATERIALS AND METHODS
Super stainless steels examined in this study were SR-50A,
SR-3Mo, SR-6DX, and SFSS, and these were compared
against 316L SS, which is commonly used in the medical and
dental fields. Table I itemizes the classifications and nickel
contents of the stainless steels used in this study.
Specimens of the super stainless steels were manufactured
as rods by investment casting in a ceramic mold after air
induction melting. The steels were then given homogeniza-
tion and solution heat treatment. 316L stainless steel was
purchased from Changwon Specialty Steel Ltd. (Changwon,
South Korea) and solution heat-treated for 1 h at 1090 °C,
then water quenched. All specimens were machined into
buttons 15 mm in diameter and 5 mm in thickness, and
polished step by step with silicon carbide papers from 100 to
2000 grit. They were then ultrasonically cleaned in acetone
and ethyl alcohol solution each for 5 min, and finally rinsed
in distilled water and dried.
The chemical compositions of the specimens were ana-
lyzed by energy dispersive spectroscopy (EDS, Kevex Su-
perdry, Kevex Instruments) for the elements: Fe, Cr, Ni, Mo,
Si, and W. Carbon and nitrogen elements were detected with
a CS and NO analyzer (CS-200 and TC-300, LECO, St.
Joseph, MI). Phase identification by X-ray diffraction (XRD,
D-Max Rint 2400, Rigaku, Japan) was performed with the
use of the K␣ rays of a Cu target in the scan range of 30 –95°,
at a scan rate of 4°/min. Phase fractions of the specimens
were determined by Feritscope (MP30, Helmut Fisher
GmbH, Germany). A micro-Vickers hardness tester (MXT-␣
7E, Matsuzawa Seiki Co., Japan) was used to determine the
hardness values of the specimens, and the hardness measure-
 PROPERTIES OF SUPER STAINLESS STEELS 185

TABLE II. Composition of Artificial Saliva positive and negative controls, respectively. Four replicate
Concentration samples were prepared in a circular shape (1 cm2 contact
Constituent (g/l) area). The samples were then carefully placed on the solidi-
fied agar layer in each dish, and the dishes were placed in an
NaCl 0.40
incubator at 37 ⫾ 1 °C in a 5% carbon-dioxide atmosphere,
KCl 0.40
CaCl2 䡠 2H2O 0.795
as appropriate for the buffer system. The zone index was
NaH2PO4 䡠 2H2O 0.780 obtained from the decolorization index and the cell lysis
Na2S 䡠 9H2O 0.005 index was determined from the lysed cell fraction in discol-
CO(NH2)2(Urea) 1.0 ored parts with the use of a phase contrast microscope (CK2,
Distilled water 1000 ml Olympus, Japan). The response index was calculated by
averaging the zone index and lysis index obtained from four
replicate samples.
The average and standard deviation of the cumulative
ment was done at a loading of 1000 g, 10 times per specimen. amount of nickel ion released from the specimen having been
To investigate the corrosion properties of the stainless steels, immersed for 8 weeks in artificial saliva were calculated. To
potentiodynamic testing was performed in artificial saliva, as prove statistical significance, the amounts of nickel ion re-
described in Table II, at 37⫾1 °C, with the use of a poten- leased from each stainless steel according to the immersion
tiostat (263A, EG&G Instruments). The area exposed to the time were compared with the use of the paired t-test, and the
solution was 1 cm2, the potential scanning rate used was 1 amount of nickel ion released from stainless steels at each
mV/s, and the scanning range was ⫺ 600 to 1600 mV vs. a immersion time was compared with the use of Tukey’s stu-
saturated calomel electrode (SCE). Potentiostatic testing was dentized range test.
performed at 500 mV (SCE) for 2 h after the samples were
held for 2 h at the open circuit potential. The tested samples
were removed from the corrosion cell under the applied
potential, carefully rinsed with distilled water, dried in a RESULTS
stream of nitrogen, and held under nitrogen flux until the
sample was transferred to the fast entry lock. The chemical composition of super stainless steels and 316L
X-ray photoelectron spectroscopy (XPS, PHI 5700 ESCA, SS are presented in Table IV. SR-50A showed the highest
Perkin-Elmer) was used to investigate the surface species and nickel content, and the order of nickel content was 316L SS
chemical state of the passive film formed at 500 mV (SCE) in (12.6 wt%), SR-6DX (9.3 wt%), SFSS (2.9 wt%), and SR-
artificial saliva. All the XPS analyses were carried out with 3Mo (2.2 wt%). Table I presents the nickel contents of the
the use of an Al-K␣ excitation (1486.6 eV) and an analyzer super stainless steels examined in this study. These stainless
pass energy of 23.5 eV for high-resolution scans. Take-off steels also contained relatively high quantities of molybde-
angles of 10, 45, and 75° were used to investigate what kinds num in order to improve localized corrosion resistance, es-
of and how many species were present according to the depth
of the passive film. All spectra were compensated by charge
shifting the carbon spectrum to adventitious carbon at 284.6 TABLE III. The Binding Energies of Some Chemical Species
eV. The spectra were resolved into their components after for XPS Analyses
iterative background subtraction according to the Shirley
Chemical Binding Chemical Binding
fitting and the curve fitting with the Gaussian–Lorentzian Species Energy (eV) Species Energy (eV)
formula. The binding energies of some chemical species for
XPS analyses are presented in Table III. Fe 2p Mo 3d
In vitro metal ion release testing was performed upon each Fe 706.8 Mo 5/2d 227.7
of three specimens, which were inserted into a Teflon spec- Fe2⫹ 709.2 Mo 3/2d 230.9
Fe3⫹ 710.8 MoO(OH)2 5/2d 230.2
imen holder. The area exposed to the solution was 1 cm2.
Each specimen was immersed in a separate screw-topped Cr 2p
glass bottle containing 100 ml of artificial saliva, and the Cr 574.1 MoO(OH)2 3/2d 233.4
bottles were stored in an incubator at 37 °C in ambient air Cr2O3 576.3 MoO2⫺
4 5/2d 231.9
containing 5% CO2. After being immersed for 1 (1D), and 3 Cr(OH)3 577.0 MoO2⫺
4 3/2d 235.1
days (3D), and 1 (1W), 2 (2W), 4 (4W), and 8 weeks (8W), CrO3 578.1 MoO2 5/2d 229.1
CrO24 579.3 MoO2 3/2d 232.3
5 ml of the solution was removed from each bottle and
analyzed for nickel by graphite furnace atomic absorption O 1s N 1s
spectroscopy (6601, Shimadzu Co. Ltd., Japan); 5 ml of fresh O2⫺ 530.2 Mo 3p 393.8
artificial saliva was re-added to each bottle. OH⫺ 531.4 Mo4⫹ 3p 395.7
The agar overlay method, described in ISO 7405:1997(E), H2O 532.9 N 396.9
Mo6⫹ 3p 397.8
was used to evaluate the cytotoxicity of these materials. Cu
NH3 399.9
alloy (NPG, Albadent Co.) and polyethylene were used as
186
TABLE IV. Chemical Compositions of Various Stainless Steels (wt%)
Stainless Steels Cr Ni Mo
SR-50A 23.2 21.0 6.6
316L SS 17.9 12.6 2.7
SR-6DX 23.5 9.3 5.3
SFSS 28.0 2.9 0.1
SR-3Mo 15.0 2.2 3.1
pecially in the cases of SR-6DX and SFSS, which also
contain tungsten.
X-ray diffraction patterns of the stainless steels are pre-
sented in Figure 1. SR-50A and 316L SS exhibited an aus-
tenitic phase with (111), (200), (311), and (220) planes, and
SFSS a ferritic phase with (110), (200), and (211) planes.
SR-6DX was found to have a mixed austenitic and ferritic
structure, and SR-3Mo a martensitic phase with (110), (200),
and (211) planes. From the results of phase fractions mea-
sured by Feritscope, SR-50A and 316L SS exhibited full
austenitic phase, and SFSS and SR-6DX, 83.6 ⫾ 4.39 and
52.2 ⫾ 3.36% ferritic phase fractions, respectively. Ferritic
phase fraction of SR-3Mo could not be determined by Ferit-
scope.
Microhardness values of the stainless steels are shown in
Figure 2. All super stainless steels showed hardness values
higher than 316L SS (227 Hv) and SR-3Mo had the highest
hardness value (646 Hv). SR-50A, SR-6DX, and SFSS ex-
hibited similar hardness values of about 265 Hv.
Anodic polarization curves of the stainless steels in arti-
ficial saliva are presented in Figure 3. SR-50A exhibited the
lowest passive current density of 1 ␮A/cm2, 316L SS had a
passive current density in the range of 3– 4 ␮A/cm2, SFSS
and SR-6DX had similar passive current densities of 20
␮A/cm2, and SR-3Mo had a passive current density of 3000
␮A/cm2. In terms of breakdown potential, SR-50A, SFSS,
and SR-6DX did not exhibit film breakdown to 1 V (SCE)
and showed stable passive regions. However, 316L SS
Figure 1. X-ray diffraction patterns of various stainless steels.
OH ET AL.
Si W N C Fe
0.8 – 0.28 0.03 Bal.
0.2 – – 0.01 Bal.
0.5 1.0 0.234 0.05 Bal.
0.1 8.6 0.002 0.01 Bal.
0.5 – 0.100 0.21 Bal.
showed film breakdown at 380 mV (SCE) and SR-3Mo at 75
mV (SCE).
Open circuit potentials of the stainless steels are presented
in Figure 4. SR-50A, 316L SS, SR-6DX, SR-3Mo, and SFSS
exhibited open circuit potentials of ⫺ 0.2, ⫺ 0.22, ⫺ 0.24, ⫺
0.43, and ⫺ 0.46 V (SCE), respectively. Current densities of
these steels measured at 500 mV (SCE) are presented in
Figure 5. Current densities of SR-50A, SFSS, SR-6DX, 316L
SS, and SR-3Mo were 5.96 ␮A /cm2, 20.3 ␮A /cm2, 31.9 ␮A
/cm2, 805 ␮A /cm2, and 5.36 mA/cm2, respectively. Current
densities of SR-50A, SFSS, and SR-6DX decreased abruptly
after starting the tests, and were kept as they were. On the
other hand, those of SR-3Mo and 316L SS decreased abruptly
and then increased slightly.
The XPS analysis results of the stainless steels are pre-
sented in Figure 6, Table V, and Figure 7. Figure 6 shows the
distribution of alloying elements according to the depth of the
surface, that is, take-off angle (10, 45, and 75 °C). In SR-50A,
SR-6DX, and 316L SS, the concentration of iron was higher
in the inner layer than in the outer layer; however, in SR-
3Mo, it was higher in the outer layer, and in SFSS, it was the
lowest in the intermediate layer. In the case of chromium,
SR-50A showed the highest concentration in the outer layer
and the concentration of chromium tended to decrease with
the depth of the surface. But the other stainless steels showed
a tendency contrary to SR-50A. The oxygen concentration of
the stainless steels was higher in the outer layer than in the
inner layer; however, in SFSS, it was the highest in the
intermediate layer, and in SR-3Mo, it maintained an even
Figure 2. Hardness value of various stainless steels.
 PROPERTIES OF SUPER STAINLESS STEELS
Figure 3. Potentiodynamic polarization curves of various stainless
steels in artificial saliva.
concentration regardless of the depth. Excluding SFSS, the
molybdenum concentration of the stainless steels showed a
tendency to increase with the depth. It was the highest among
the stainless steels in SR-3Mo, second highest in SR-50A,
and relatively low in the others. The nitrogen concentration
had a tendency to increase toward the inner layer. Almost no
nickel content was observed in all the measured cases.
Atomic concentration ratios of metallic elements to oxy-
gen (the sum of atomic concentrations of Fe, Cr, Ni, and Mo
(W) / atomic concentration of oxygen) are presented in Figure
7. The ratios of SR-50A and SFSS were above 1 and the
others, below 1. SR-50A exhibited the highest concentration
ratio among the stainless steels. The ratios in the outer layer
were lower than those in the inner layer. Distribution and
concentration of chemical species according to the depth of
the surface are presented in Table V. The concentrations of
chemical species are presented with an inequality sign, as
they are difficult to analyze quantitatively. In the case of iron,
Figure 4. Open circuit potentials of super stainless steels measured
at 500 mV (SCE) in artificial saliva, 37°C.
187
Figure 5. Current densities of the stainless steels measured at 500
mV (SCE) in artificial saliva, 37°C.
chemical species of Fe, FeO, and Fe2O3 were observed in the
surface layer of SR-50A, SR-6DX, SFSS, and 316L SS.
However, almost no metallic Fe was observed in the surface
of SR-3Mo. In the case of chromium, Cr2O3, CrO3, CrO2⫺ 4 ,
Cr(OH)3, and metallic Cr were observed. SR-50A, SR-6DX,
and SFSS exhibited a high concentration of Cr2O3 in the
outer layer, 316L SS showed a high concentration of CrO3,
and SR-3Mo showed a very high concentration of CrO2⫺ 4 . In
the case of molybdenum, many kinds of chemical species
were observed, and they are presented in Table V. In the case
of nitrogen, NH3 exhibited high concentrations in the surface
layer.
Cumulative amounts of nickel ion released from the stain-
less steels in artificial saliva at 37 °C versus immersion time
are presented in Figure 8. SR-50A showed a slight increase in
nickel-ion release with immersion time, but this was not
statistically significant. 316L SS showed no nickel-ion in-
crease with immersion time, whereas SFSS and SR-6DX
exhibited a increase in nickel-ion release over 8 weeks of
immersion, and the amount of nickel ion released during 2
and 4 weeks immersion were significantly different (p ⬍
.05). SR-3Mo showed greatest nickel-ion release among the
stainless steels used in this study. With respect to the statis-
tical significance of nickel release versus immersion time,
after 1 and 3 days of immersion, 316L SS and SFSS and 316L
SS and SR-3Mo were significantly different, and after 2
weeks of immersion, SR-3Mo and SR-6DX and SR-3Mo and
SFSS were different. Similarly, after 4 weeks of immersion,
SR-3Mo differed from the other steels (p ⬍ .05).
Cytotoxicities of the stainless steels evaluated with the use
of the agar overlay test are presented in Table VI. All super
stainless steels exhibited no or only mild responses, and
SR-50A and SR-6DX produced the lowest response indices.
SR-3Mo was found to have a relatively high response index
among the stainless steels.
188 OH ET AL.

Figure 6. Atomic concentration distribution of the stainless steels according to the surface depth.

DISCUSSION
Because biomaterials are used directly or indirectly in
contact with human body, biocompatibility is probably
their most important property. The biocompatibility of
metallic materials essentially equates to corrosion resis-
tance;22,23 that is, the alloying element can only enter the
surrounding organic system and develop toxic effects by
being converted to ions. Therefore, studies on the devel-
opment or on the selection of new materials with high
corrosion resistance must be undertaken to inhibit metallic
ion release in vivo.
 PROPERTIES OF SUPER STAINLESS STEELS 189

TABLE V. Distribution of Chemical Species with the Surface Depth Analyzed by Peak Deconvolution of XPS Spectrum

Specimen Outer Layer Inner Layer

Fe
SR-50A Fe ⬎ FeO ⬎ Fe2O3 Fe ⬎ FeO ⬎ Fe2O3
316L SS FeO ⬎ Fe ⬎ Fe2O3 Fe ⬎ FeO ⬎ Fe2O3
SR-6DX FeO ⬎ Fe2O3 ⬎ Fe Fe ⬎ FeO ⬎ Fe2O3
SFSS Fe ⬎ FeO ⬎ Fe2O3 Fe ⬎ FeO ⬎ Fe2O3
SR-3Mo FeO ⬎ Fe2O3 ⬎⬎ Fe FeO ⬎ Fe2O3 ⬎⬎ Fe
Cr
SR-50A Cr2O3 ⬎ CrO2⫺
4 ⬎ CrO3 ⬎⬎ Cr(OH)3 ⬎⬎ MCr Cr2O3 ⬎ CrO2⫺
4 ⬎ CrO3 ⬎ Cr(OH)3 ⬎⬎ MCr
316L SS CrO3 ⬎ Cr2O3 ⬎ Cr(OH)3 ⬎ CrO2⫺
4 ⬎ MCr CrO3 ⬎ Cr2O3 ⬎ CrO2⫺
4 ⬎ Cr(OH)3 ⬎⬎ MCr
SR-6DX Cr2O3 ⱖ CrO3 ⬎ Cr(OH)3 ⬎ MCr ⬎ CrO2⫺
4 Cr2O3 ⬎ CrO3 ⱖ MCr ⬎ CrO2⫺
4 ⫽ Cr(OH)3
SFSS Cr2O3 ⬎ MCr ⬎ CrO3 ⱖ CrO2⫺
4 ⬎⬎ Cr(OH)3 Cr2O3 ⬎ MCr ⬎ CrO3 ⱖ CrO2⫺
4 ⬎⬎ Cr(OH)3
SR-3Mo CrO42⫺ ⬎ CrO3 ⬎ Cr(OH)3 ⬎ CrO2O3 ⬎⬎ MCr CrO42⫺ ⬎ CrO3 ⬎ Cr(OH)3 ⫽ Cr2O3 ⬎⬎ MCr
O
SR-50A O2⫺ ⬎ OH⫺ ⬎ H2O OH⫺ ⬎ O2⫺ ⬎ H2O
316L SS OH⫺ ⬎ O2⫺ ⬎⬎ H2O OH⫺ ⫽ O2⫺ ⬎⬎ H2O
SR-6DX OH⫺ ⬎ O2⫺ ⬎ H2O OH⫺ ⬎ O2⫺ ⬎ H2O
SFSS H2O ⬎ OH⫺ ⬎⬎ O2⫺ OH⫺ ⬎ H2O ⬎⬎ O2⫺
SR-3Mo OH⫺ ⬎ O2⫺ ⫽ H2O OH⫺ ⬎ O2⫺ ⬎ H2O
Mo
SR-50A MoO23/2d ⫽ MoO(OH)23/2d ⬎ MoO2⫺
4 3/2d ⫽ MoO23/2d ⫽ MoO(OH)23/2d ⫽ MoO2⫺
4 5/2d ⬎
Mo3/2d ⫽ MoO25/2d ⬎ MoO(OH)25/2d ⬎ MoO(OH)25/2d ⬎ MoO25/2d ⬎ MoO2⫺
4 3/2d
MoO2⫺
4 5/2d ⫽ Mo5/2d ⬎ Mo3/2d ⫽ Mo5/2d
316L SS Mo5/2d ⬎ MoO25/2d ⫽ MoO23/2d ⬎ Mo3/2d ⬎ MoO25/2d ⫽ MoO23/2d ⫽ MoO2⫺
4 5/2d ⬎
MoO2⫺4 5/2d ⫽ MoO(OH)23/2d ⬎ Mo5/2d ⬎ MoO2⫺
4 3/2d ⫽
MoO(OH)25/2d ⬎ MoO2⫺4 3/2d MoO(OH)23/2d⬎MoO(OH)25/2d ⬎ Mo3/2d
SR-6DX Mo3/2d ⬎ MoO(OH)23/2d ⬎ MoO2⫺
4 5/2d ⬎ MoO25/2d⬎MoO(OH)23/2d⬎
Mo5/2d⬎MoO2⫺4 3/2d⬎ MoO23/2d⬎MoO2⫺
4 5/2d⬎
MoO25/2d⬎MoO(OH)25/2d ⬎⬎ MoO23/2d MoO(OH)25/2d⬎MoO2⫺4 3/2d ⬎⬎ Mo5/2d ⫽
Mo3/2d
SFSS – –
SR-3Mo Mo5/2d ⫽ MoO23/2d⬎ MoO(OH)23/2d ⬎ Mo5/2d ⫽ MoO23/2d ⫽ MoO25/2d⬎
MoO25/2d ⫽ MoO2⫺4 5/2d⬎Mo3/2d ⬎ MoO(OH)23/2d ⫽ MoO2⫺4 5/2d ⫽
MoO(OH)25/2d ⬎ MoO2⫺4 3/2d Mo3/2d⬎MoO(OH)25/2d⬎ MoO2⫺ 4 3/2d
N
SR-50A Mo 3p ⬎ Mo6⫹ 3p ⬎ Mo4⫹ 3p ⬎ NH3 ⬎⬎ N Mo4⫹ 3p ⬎ NH3 ⬎ N ⬎ Mo6⫹ 3p ⬎ Mo 3p
316L SS NH3 ⬎ Mo6⫹ 3p ⬎ Mo4⫹ 3p ⬎ Mo 3p ⬎⬎ N NH3 ⬎ Mo4⫹ 3p ⬎ Mo6⫹ 3p ⬎ Mo 3p ⬎⬎ N
SR-6DX Mo 3p ⬎ Mo6⫹ 3p ⬎ Mo4⫹ 3p ⬎ NH3 ⬎⬎ N Mo4⫹ 3p ⬎ NH3 ⬎ N ⬎ Mo6⫹ 3p ⬎ Mo 3p
SFSS NH3 ⬎⬎ Mo6⫹ 3p ⫽ N ⫽ Mo4⫹ 3p ⫽ Mo 3p Mo6⫹ 3p ⱖ NH3 ⬎⬎ N ⫽ Mo4⫹ 3p ⫽ Mo 3p
SR-3Mo NH3 ⬎ Mo2⫹ 3p ⬎ N ⬎ Mo4⫹ 3p ⬎ Mo 3p NH3 ⬎ Mo6⫹ 3p ⬎ N ⬎ Mo4⫹ 3p ⬎⬎ Mo 3p

316L stainless steel and the corresponding medical grade
ASTM F138 have been widely used for biomedical applica-
tions in particular for osteosynthetic devices, due to their high
generalized corrosion resistance, easy workability, good me-
chanical properties after cold working, and a relatively low
price. However clinical experiences have shown that tradi-
tionally used austenitic stainless steels are susceptible to
crevice corrosion in the human body, causing the release of
metallic ions into the tissues surrounding the implants. This
may cause local irritations or systemic effects, which are
among the principal causes of clinical failure. In particular,
the adverse effect of nickel has been delineated, and is
attributed to the allergic sensitization of many people to this
element. Consequently, the development of new steels with
low nickel content, high mechanical properties, and improved
localized corrosion resistance, compared with the steels tra-
ditionally used for biomedical and dental application, is re-
quired. Super stainless steels have produced considerable
190 OH ET AL.
Figure 7. Concentration ratios of the sum of metallic elements to
oxygen of the stainless steels after holding at 500 mV (SCE) for 2 h in
artificial saliva, 37 °C.
interest for these applications because, as reported in the
literature,24 their higher molybdenum and nitrogen levels
increase localized corrosion resistance and mechanical prop-
erties.
Chemical analysis showed that the nickel content of SR-
50A (21.0%) was the highest of the experimental materials;
those of 316L SS, SR-6DX, and SFSS were 12.6%, 9.3% and
2.9%, respectively; and that of SR-3Mo (2.2%) was the
lowest. Nickel, which is an austenite stabilizing element in
stainless steel, is known to improve the strength, ductility,
and corrosion resistance, including crevice corrosion and
erosion corrosion resistance.12 The amount of nitrogen used
to increase the corrosion resistance of stainless steel was
found to be dependent on the amount of nickel contained in
the stainless steel. Therefore, the nickel content should be
increased to increase the nitrogen content of a stainless steel.
However, because nickel is known to induce allergic and
carcinogenic reactions and contact dermatitis, the nickel con-
tent of stainless steel should be decreased or another element,
which is not toxic to the human body, should be substituted
for the nickel in biomedical and dental applications. There-
Figure 8. Cumulative nickel-ion release amount from stainless steels.
TABLE VI. Cytotoxicity of Various Stainless Steels
Zone Lysis Response
Specimen Index Index Index Cytotoxicity
SR-50A 0–0 0–0 0/0 None (⫺)
316L SS 0–1 1–1 0/1 Mild
SR-6DX 0–0 0–0 0/0 None (⫺)
SFSS 0–1 0–1 0/1 Mild
SR-3Mo 1–1 1–2 1/2 Mild (⫹)
Positive (NPG) 2–4 4–4 2/4 Moderate (⫹⫹)
Negative (Polyethylene) 0–0 0–0 0/0 None (⫺)
fore, it is important in such applications that materials with
high corrosion resistance and low nickel content are used.
It has been reported that the addition of nitrogen and
molybdenum greatly increase corrosion resistance, because
the passive film so formed is more resistant to attack by
aggressive ions due to the synergistic effects of these ele-
ments.3–5 Because molybdenum is an important alloying el-
ement in stainless steels, many studies25–31 have attempted to
determine the effects of molybdenum on the localized corro-
sion resistance of stainless steels in chloride containing me-
dia. However, there are different opinions about the mecha-
nism by which molybdenum improves corrosion resistance:
Newman32 found enriched molybdenum at surface kinks or
step sites in the active state. Newman’s33 electrochemical
data concluded that molybdenum exerted a strong inhibiting
effect on pitting because it reduces the anodic kinetics (5–10
times) in the pit environment. Newman also suggested that pit
initiation and propagation were related to the inhibition of
active dissolution due to the submonolayer surface enrich-
ment of molybdenum. Hashimoto, Asami, and Teramoto34
concluded that molybdenum eliminated the active surface
sites by forming molybdenum oxide or molybdate on these
sites. Kolotyrkin35 concluded that adding a small amount of
molybdenum had a favorable effect against corrosion because
this element, with respect to its strong inclination to passiva-
tion, blocked the most active centers of the surface in the
process of dissolution. According to Wanklyn36, the inhibi-
tive effect from alloyed molybdenum was produced by insol-
uble Mo4⫹ oxide films deposited on the stainless steels.
Regarding the corrosion of alloys, Wanklyn suggested that
molybdenum passed directly from the metal into the protec-
tive film, and that soluble Mo compounds played no part in
this process. On the basis of a bipolar model suggested by
Sakashita and Sato37, Clayton and Lu38 proposed that the
incorporation of MoO2⫺ 4 and CrO2⫺ 2 in the passive film
modified the immediate surrounding lattice and the resulting
bipolar film rectified ionic current so as to resist the ingress of
anions such as Cl⫺ and OH⫺, and enhance the egress of
protons. As an indirect result of bipolarity, an interfacial
glassy oxide of XCr2O3 䡠 YCrO3 was developed, which acted
as a barrier layer. Therefore, from the above-mentioned stud-
ies, the roles of molybdenum in improving the localized
corrosion resistance of stainless steels can be classified into
two categories: an elimination of active site and formation of
 PROPERTIES OF SUPER STAINLESS STEELS
molybdenum oxide or molybdate, and a formation of molyb-
date and modification of bipolarity of the film.
Nitrogen is considered an important additive element to
austenitic stainless steels in terms of corrosion resistance as it
promotes passivity, widens the passive range in which pitting
is less probable, improves the stress corrosion cracking re-
sistance in certain media, and enhances the resistance to
intergranular corrosion.39 – 43 The beneficial effects of nitro-
gen appear to be greater when there is molybdenum in the
stainless steel. For example, in an alloy containing 2.8%
molybdenum, the addition of ⬃0.3% nitrogen raises the pit-
ting potential to transpassive potential,10 which thereby ex-
tends the noble end of the passive range to the maximum in
a chromium-protected alloy. The beneficial effects of nitro-
gen-plus-molybdenum are now applied in several commercial
stainless steels.
According to the results of Irhzo,44 the addition of tung-
sten to stainless steel reduces the anodic dissolution rate and
enhances passivation. Bui et al.45 have reported that pure
tungsten does not develop a protective layer, but in alloy form
it improves the pitting resistance of stainless steels in acid or
neutral chloride solutions. In the results of Ogura and
Ohama,46 however, tungstate has no positive effect on the
pitting resistance, and pitting was accelerated at a higher
concentration, which was rationalized by assuming that the
polytungstate neither adsorbed on passive iron nor precipi-
tated as a salt with iron ions. Gluszek et al.47 reported that the
presence of tungstate in the passive film leads to increased Cr
content in the film that was formed on Cr-Ni stainless steels
and thus enhanced passivity. Other results48 reported that the
tungsten-added amorphous alloys exhibited higher corrosion
resistance than the molybdenum-added amorphous alloys in
6-M HCl solutions, and this means that tungsten is more
effective than molybdenum in assisting the formation of
Cr-enriched passive film.
SR-50A exhibited the highest corrosion resistance among
the super stainless steels in this study. It was reported that
SR-50A showed the same level of localized corrosion resis-
tance as the titanium alloys, because the resistance of the
passive film is enhanced by the synergistic effect5,9 –11 of high
content nitrogen (0.28%) and molybdenum (6.6%). Although
it contained the highest nickel level, it released the lowest
amount of nickel into artificial saliva, among the super stain-
less steels tested. It is believed that the stable passive film
minimizes the amount of metal ions released in the corrosive
conditions present in the body after implantation. SR-6DX
exhibited a high pitting potential and the passive current
density of about 20 ␮A/cm2. Duplex stainless steel exhibited
a similar corrosion resistance to SFSS. SR-6DX has good
corrosion resistance and has improved localized corrosion
resistance, because of the passive film enhanced by the high
nitrogen and molybdenum (above 5%) content.13 It is thought
that because this steel contains relatively little nickel, and has
high corrosion resistance in vivo, that it has the potential to
satisfy the requirement to reduce the nickel ion to a mini-
mum. SFSS has good corrosion resistance against polluted
seawater and ammonia. It also has good antivibration prop-
191
erty because of high elasticity and good resistance to erosion
corrosion. Typical chemical composition of ferritic stainless
steel is Fe-29Cr-4Mo.14 Typical pitting resistance equivalent
[PREW ⫽ %Cr ⫹ 3.3(%Mo ⫹ 0.5%W) ⫹ 30%N] of com-
mercial super ferritic stainless steels is at a range of 39 – 42,
and it has good corrosion resistance thanks to high Cr and Mo
addition.49 316L SS had a relatively low passive current
density, but had a pitting potential at about 380 mV (SCE). It
is considered that these properties of 316L SS reflect its low
corrosion resistance in artificial saliva. SR-3Mo was reported
to exhibit higher corrosion resistance than AISI type 420
stainless steel in high chloride environments, again because
of the enhanced barrier properties of high nitrogen/molybde-
num passive film.12 But in this study, SR-3Mo had the lowest
corrosion resistance of the experimental stainless steels. It is
thought that the additional amounts of alloying elements such
as chromium, molybdenum, nickel, and nitrogen, which can
improve the corrosion resistance of stainless steels, are in-
hibited for the martensitic phase formation in SR-3Mo.
Open circuit potentials of the stainless steels are consid-
ered to be dependent on nickel content or the type of phase,
in other words, open circuit potential of austenitic stainless
steel was high; duplex stainless steel, intermediate, and mar-
tensitic and ferritic stainless steel, low. These results are
related to the metallic ion release, which increased according
to the immersion time. It is thought that, even though the
stainless steels contain a low nickel content such as SFSS and
SR-3Mo, they may release many nickel ions because of their
low open circuit potentials.
The current densities of the stainless steels measured in the
potentiostatic test (at 500 mV (SCE)) were similar to those
measured in the potentiodynamic test. SR-50A, SFSS, and
SR-6DX were passivated immediately when they were im-
mersed and potential loaded, but in case of 316L SS and
SR-3Mo, they exhibited an increase of current density. These
steels exhibited high current densities when the potentials
were loaded at 500 mV (SCE) in the potentiostatic test
because 316L SS and SR-3Mo showed film breakdown at 380
and 75 mV (SCE) in the potentiodynamic curves. The three
others exhibited stable and low current densities because they
did not exhibit film breakdown up until 1 V (SCE) in the
potentiodynamic test. Current densities of these steels mea-
sured at 500 mV (SCE) are presented in Figure 5. Current
densities of SR-50A, SFSS, SR-6DX, 316L SS, and SR-3Mo
were 5.96 ␮A/cm2, 20.3 ␮A /cm2, 31.9 ␮A /cm2, 805 ␮A
/cm2, and 5.36 mA/cm2, respectively. Current densities of
SR-50A, SFSS, and SR-6DX decreased abruptly after starting
the tests, and did not show any changes. On the other hand,
those of SR-3Mo and 316L SS decreased abruptly and then
increased slightly.
From the results of XPS, it is thought that the stable
passive film, Fe-Cr oxide in which the Cr content is higher
than the Fe content, is formed on the SR-50A surface. The
oxide also contains high concentrations of molybdenum and
nitrogen. This result indicates that SR-50A has a stable pas-
sive film and thus a high corrosion resistance. On the surface
of SR-6DX, low content of iron and chromium, and high
192 OH ET AL.
content of oxygen were observed. This means that the passive
film is formed with iron– chromium oxide. However, it is
difficult to evaluate the stability of the passive film because of
the existence of the dual phases with different constituents.
SFSS is thought to have a stable passive film because of the
similar high concentration of iron and chromium. 316L SS
and SR-3Mo are thought to have an unstable oxide film
because of the low content of iron and chromium.
To investigate the state of the surface oxide, concentration
ratios were calculated by dividing the sum of metallic ele-
ment concentration by the concentration of the oxygen. If the
concentration ratio is over 1, the oxide is thought to be dense.
Thus, it is concluded that SR-50A and SFSS, which exhibited
a ratio of over 1, had a dense and stable passive film when
they were loaded at 500 mV (SCE) in artificial saliva. The
low ratios of the outer layers of the stainless steels mean that
the outer layers contain high concentrations of oxygen. It was
noted that the stainless steels with high corrosion resistance
exhibited high atomic concentrations when the atomic con-
centration ratios were compared with the results of potentio-
dynamic and potentiostatic tests. SR-6DX has exceptionally
low atomic concentration ratio. Nevertheless, it has high
corrosion resistance. It is difficult to estimate the corrosion
resistance of the duplex stainless steels with the atomic con-
centration because the ferritic and austenitic phases have
different alloying elements.
Currently, orthodontic metallic appliances are made
mainly of austenitic stainless steel containing 18 –20% chro-
mium and 8 –12% nickel, or alternatively are made of nickel–
titanium alloy.1 If these alloys are used in the human body,
the ions released from them over the long or short term could
cause adverse effects. Their predominant systemic effects in
humans are allergies, dermatitis, and asthma. Nickel is one of
the most common causes of allergic contact dermatitis, espe-
cially in women.21,50,51 Tsalev and Zaprianov52 reported that
nickel is a toxic element, but essential in animal and humans,
and a carcinogen, which induces neoplasms in the respiratory
system and in the nasal sinuses. Some clinical evidence of
carcinogenicity resulting from implanted alloys is available in
the literature.53,54
Maijer and Smith55,56 reported that the factors affecting
metallic ion release from orthodontic appliances were corro-
sion resistance of orthodontic materials, soldering or welding,
galvanic corrosion between the dissimilar metals, interaction
with microbacterial metabolism in dental plaque, surface
area, and cleanness of the appliances. Many studies have
measured the metallic ions released from metallic appliances
in various environments;22,57,58 however, most of these stud-
ies have reported that corrosion or ion release from metallic
orthodontic appliances does not present any problem clini-
cally.59 – 61 On the other hand, arguments that hypersensitivity
to alloys could occur in certain patients with metallic pros-
theses62,63 have generated reports to the effect that stainless-
steel–sourced nickel-ion release into the oral cavity or contact
with soft tissue, can induce hypersensitivity to stainless steel
brackets.64
The SFSS, which contains a small amount of nickel
(2.9%), has very high corrosion resistance, and the amount of
nickel ion released to artificial saliva upon immersion was
low; however, the amount of released nickel increased with
immersion time. The cytotoxicity of SFSS was nevertheless
mild, though it exhibited a slightly higher response than
SR-50A and SR-6DX. It is believed that SFSS may release
nickel ions and induce cytotoxic reaction when used in the
human body over a long time. It is thought that modification
of the chemical composition and increased barrier properties
of the passive film of SFSS are required before it is used as
a biomaterial. SR-50A, SR-6DX, and 316L SS did not exhibit
an increase in the amount of nickel ion released with immer-
sion time, and are thought to be very stable in artificial saliva.
Although SR-50A contained twice as much nickel content as
316L SS, it exhibited lower nickel-ion release than 316L SS.
SR-3Mo, containing 2.2% nickel, exhibited very low nickel-
ion release when first immersed, however, it exhibited very
high rates of nickel-ion release upon increasing the immer-
sion time. Subsequently, it exhibited the highest nickel-ion
release level of the experimental stainless steels used in this
study.
In summary, it is considered that the nickel-ion release
property is not dependent on nickel content as in stainless
steel, but depends on the properties of the passive film. With
the exception of SR-3Mo and SFSS, the stainless steels
examined did not exhibit significantly increased nickel-ion
release with immersion time. It is considered that the super
stainless steels used in this study have high corrosion resis-
tances by virtue of their stable passive films, and that this led
to comparatively low nickel-ion release.
From the point of view of the cytotoxicity, super stainless
steels, except for SR-3Mo, exhibited mild or no response
index because of their high corrosion resistance and low
levels of ion release.
In the orthodontic field, in order for miniscrews to be used
more effectively, it is necessary to develop or select new
materials that can overcome the known deficiencies of tita-
nium miniscrews, such as low strength, wear, and fracture
resistance. SR-50A, SFSS, and SR-6DX show high corrosion
resistance and relatively good biocompatibility, and are be-
lieved to be suitable for orthodontic applications, especially
for miniscrews.
CONCLUSION
Super stainless steels showed higher microhardness values
than 316L stainless steel, and the super martensitic stainless
steel (SR-3Mo) showed the highest microhardness. From
anodic polarization curves, the corrosion resistance of these
steels was high, and in order SR-50A, SFSS ⫽ SR-6DX,
316L S S, to SR-3Mo. There was no increase in the amount
of nickel ion released from SR-50A, SR-6DX, and 316L SS
with immersion time in artificial saliva, whereas some in-
crease was observed from SFSS and SR-3Mo according to
immersion time. All super stainless steels showed very low
 PROPERTIES OF SUPER STAINLESS STEELS
cytotoxicities regardless of their nickel contents, although
SR-3Mo showed relatively higher cytotoxicity. It is consid-
ered that SR-50A, SFSS, and SR-6DX with high corrosion
resistance and good cytocompatibility, due to the passive film
enhanced by synergistic effect of Mo ⫹ N or by high addition
effect of Cr ⫹ W, can be used for orthodontic applications.
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