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Characterization of borided AISI 316L stainless steel implant

Article  in  Vacuum · May 2002

DOI: 10.1016/S0042-207X(01)00466-3

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 Vacuum 65 (2002) 521–525

Characterization of borided AISI 316L stainless steel implant

.
I. Ozbek a
, B.A. Kondukb, C. Bindala,*, A.H. Ucisikb
a
Engineering Faculty, Department of Metallurgical and Materials Engineering, Materials Engineering, Sakarya University,
54187 Esentepe Campus-Sakarya, Turkey
b
Department of Prostheses, Materials and Artificial Organs, Institute of Biomedical Engineering, Bogazic-i University,
80815 Bebek-Istanbul, Turkey

Abstract

The present study reports on characterization of borided AISI 316L stainless steel implant. Boronizing heat
treatment was performed on a cylindrical bar of AISI 316L austenitic surgical stainless steel with a diameter of 2 mm
and a length of 10 mm using slurry salt bath consisting of borax, boric acid and ferro-silicon. The susbstrate AISI 316L
was essentially containing 0.022 wt% C, 0.79 wt% Si, 1.6 wt% Mn, 0.25 wt% P, 0.002 wt% S, 15.30 wt% Cr 14.09 wt%
Ni, 2.63 wt% Mo and 0.05 wt% Cu, respectively. Boronizing treatments were conducted at 8501C, 9001C, 9501C, and
10001C, for 2, 4 and 6 h, respectively. Depending on process time and temperature, the thickness of boride layer formed
on substrate ranged from 12 to 40 mm. The hardness of borides formed on the surface of substrate was over 1500 VHN.
The presence of borides (e.g. Fe2B, CrB, Ni3B) formed on the surface of borided AISI 316L stainless steel was
confirmed by classical metallographic technique combined with X-ray diffraction analysis. The distribution of alloying
elements was determined by means of energy dispersive X-ray spectroscopy spectrum from surface and line-scan
analysis from surface to interior. r 2002 Published by Elsevier Science Ltd.

Keywords: Boronizing; Stainless steel; Borides; Slurry salt; Hardness

1. Introduction although they can be appreciably strengthened by

In orthopaedic surgery and, particularly in total
hip replacement, metals are the most favored
materials because of their good mechanical stabi-
lity. On the other hand, metals corrode in contact
with aggressive body fluids or tissue [1]. Therefore,
the designer must be careful when selecting
materials of this type. Austenitic stainless steels,
as their name implies, have an austenitic micro-
structure (FCC) at room temperature and cannot
be hardened to any great extent by heat treatment,
*Corresponding author. Fax: +90-264-346-0351.
E-mail address: hucisik@hotmail.com (C. Bindal).
0042-207X/02/$ - see front matter r 2002 Published by Elsevier Science Ltd.
PII: S 0 0 4 2 - 2 0 7 X ( 0 1 ) 0 0 4 6 6 - 3
cold-work. They are, however, usually quenched,
not to produce martensite but to minimize the
formation chromium carbide as this causes a
reduction in the corrosion resistance of the alloy.
These steels are austenitic and low carbon,
chromium–nickel–molybdenum stainless steels.
The presence of higher molybdenum enhances
the corrosion resistance. AISI 316L stainless steel
has low carbon and high nickel and chromium.
Low carbon content does not cause intercrystalline
corrosion. But this type of steels may corrode
inside the body under certain conditions such as
that in a highly stressed and oxygen-depleted
region. Mainly, these steels are used as implant
522 .
I. Ozbek et al. / Vacuum 65 (2002) 521–525
materials in biomedical applications, for example,
in temporary devices such as fracture plates,
screws, and hip nails [2–5].
Boronizing is a thermochemical diffusion sur-
face treatment in which boron atoms are diffused
into the surface of work piece to form hard borides
with the base material [6–10]. The aim of the
present study is an attempt to characterize borided
AISI 316L austenitic stainless steel implants in
conventional slurry salt bath, e.g. hardness,
distribution of alloying elements, etc. Specifically,
we used a Vickers indenter, an optical microscope,
scanning electron microscope (SEM) to determine
mechanical and microstructural properties of
boronized 316L stainless steels. To determine
distribution of alloying elements from surface to
interior energy dispersive X-ray spectroscopy
(EDS) was used.
2. Experimental details
2.1. Substrate materials
The substrate material used for this study was
AISI 316L austenitic surgical stainless steel. AISI
316L austenitic surgical stainless steel test piece
had a cylindrical shape and was 10 mm in length
and 2 mm in diameter. The susbstrate AISI 316L
was essentially containing 0.022 wt% C, 0.79 wt%
Si, 1.6 wt% Mn, 0.25 wt% P, 0.002 wt% S,
15.30 wt% Cr, 14.09 wt% Ni, 2.63 wt% Mo and
0.05 wt% Cu, respectively.
2.2. Boronizing
Boronizing was carried out using a slurry salt
bath consisting of borax, boric acid and ferro-
silicon. Boronizing treatments were performed at
8501C, 9001C, 9501C, and 10001C, for 2, 4 and 6 h,
respectively. Test materials to be boronized were
immersed in a slurry salt bath using a sealed
container then they were sealed including test
materials and they were placed in an electrical
resistant furnace. Test materials were heated to
desirable temperature under atmospheric pressure
and held for a predetermined amount of time. This
is followed by quenching in air.
2.3. Film characterization, coating layer and
hardness
The nature and type of borides formed in
coating layer are closely related to chemical
composition of substrates concerned. The presence
of borides formed in coating layer was confirmed
by means of X-ray diffraction (XRD), SEM and
optical microscope. The distribution of alloying
elements was confirmed via EDS from surface to
interior. The microhardness of borides formed on
the surface of AISI 316L austenitic surgical
stainless steel was measured using a Vickers
microhardness tester and a load of 0.5 N. Vickers
hardness values of borides formed on the surface
of AISI 316L stainless steel and matrix were 22
and 6 GPa, respectively. The thicknesses of borides
were measured by means of a digitial thickness
measuring instrument attached to optical micro-
scope.
3. Results
3.1. Microstructure
Both optical and SEM cross-sectional examina-
tions of the borided AISI 316L austenitic stainless
steel implants revealed a compact and smooth
morpholgy to a depth ranging from 12 to 40 mm.
Coating layer formed on the stainless steel
substrate essentially have three distinct regions
which are; (i) layers having borides (i.e. Fe2B, CrB,
Ni3B), (ii) the region below boride layers, where
boron makes solid solution, which has hardness
less than that of borides and higher than that of
original alloy, and (iii) steel matrix, which is not
affected by boron.
Fig. 1 shows an optical cross-sectional view of
AISI 316L stainless steel borided in slurry salt bath
medium. As can be seen in Fig. 1, borides formed
on the stainless steel substrate had a compact and
smooth morphology compared to borides formed
on the surface of plain carbon steels. The
distribution of alloying elements was determined
by means of EDS spectrum from surface and line-
scan analysis from surface to interior (Figs. 2
and 3).
 .
I. Ozbek et al. / Vacuum 65 (2002) 521–525 523

3.2. Hardness, film characterization and boride

layer

The hardness of borides formed on the surface

Fig. 1. The optical cross-sectional view of borided AISI 316L
stainless steel sowing morphology of borides, 850  .
of borided AISI 316L austenitic surgical stainless
steel is much higher than that of substrate. It is
possible to claim that these are a consequence of
presence of hard Fe2B, CrB, and Ni3B (see Fig. 4).
Fig. 4 shows X-ray diffraction patterns of AISI
316L austenitic surgical stainless steel borided in
slurry salt bath medium. Vickers hardness values
of borides formed on the surface of AISI 316L
stainless steels and matrix were 22 and 6 GPa,
respectively. The depth values of borides are given
in Table 1 as a function of process time and
temperature.

Fig. 4. X-ray diffraction pattern of borided AISI 316L

austenitic surgical stainless steels for slurry salt bath medium.

Fig. 2. The distribution of alloying elements from surface to

interior confirmed by EDS from surface to interior. Table 1
The variation of depth of boride layer thickness as a function of
process temperature and time

Steel Temperature Time Thickness of boride

(1C) (h) layer (mm)

AISI 316L 850 2 5

4 8
6 10
900 2 7
4 9
6 12
950 2 14
4 25
6 32
1000 2 15
4 30
6 40
Fig. 3. EDS spectrum of borided AISI 316L stainless steel.
524 .
I. Ozbek et al. / Vacuum 65 (2002) 521–525
4. Discussion
The above results demonstrated that it is
possible to characterize some properties of stain-
less steel by using conventional slurry salt bath
boriding technique. Optical and SEM examina-
tions of borides formed on the surface of
AISI 316L austenitic surgical stainless steel sub-
strates revealed a smooth and compact morphol-
ogy and good bonding of the film to the steel
substrates.
As is well-known, alloying elements by changing
the diffusivity of boron atoms modify coating-
substrate interface. The higher the alloy, the
smooth the compact interface. The diffusivity of
boron at 9501C is 1.82  10 8 cm2 s 1 for boride
layer and 1.53.10 7 cm2 s 1 for diffusion zone. As
a consequence, the boron containing diffusion
zone is extended several fold the depth of non-
oxide ceramic boride layer into the steel substrates.
Depending on boronizing time and chemical
compositions of steel substrates, the depth of
borides ranged from 10 to 40 mm (Fig. 5). It was
observed that increase in temperature results in
thick coating layer. There is nearly a parabolic
relationship between depth of borides and diffu-
sion time. Previous studies done by Pelleg [11] and
Ucisik et al. [12] showed that boronizing of carbon
steels usually leads to formation of two borides,
FeB and Fe2B, FeB near the surface and Fe2B in
the vicinity of steel matrix.
Fig. 5. The variation depth of coating layer as a function of
process time and temperature.
In the present study, the presence of borides was
identified via XRD analysis (see Fig. 4). EDS
revealed that nickel concentrates in the base metal
beneath the coating, chromium and manganese
preferentially enter the coatings by substituting for
iron in the Fe2B and FeB. Silicon, which is
insoluble in iron borides, concentrates strongly at
the interface with the coatings. The boriding
coatings grown on the ternary alloys generally
constituted an inner Fe2B single-phase and an
outer FeB-base polyphase region containing FeBx
with x > 1 and, external surface, an iron in boron
solid solution. With increasing contents of the
third alloying element in the alloys, both the depth
of FeB-base region and FeB/FeBx ratio increases.
Hardness measurements showed that the hardness
of borides are much higher than that of base steel.
We believe that this is a consequence of the
presence of hard Fe2B, CrB, and Ni3B in the
coating layer. In thermo-chemical boronizing
treatments, high hardness is attained directly
through formation of borides during boronizing
and does not require quenching. Vickers hardness
values of borides and AISI 316L stainless steels
substrate were 22 and 6 GPa, respectively.
5. Conclusion
The results obtained from present study can be
summarized as follows:
(a) Optical and SEM examinations of boride
types ceramics formed on the surface of AISI
316L surgical stainless steel has a compact
and smooth morphology.
(b) Depending on holding time and process
temperature the layer thickness of boride
types of ceramics ranged from 5 to 40 mm It
was found that increase in temperature results
in thick coating layer.
(c) EDS revealed that nickel concentrates in the
base metal beneath the coating, while chro-
mium and manganese preferentially enter the
coatings by substituting for iron in the Fe2B
and FeB. Silicon, which is insoluble in iron
borides, concentrates strongly at the interface
with the coatings.
 .
I. Ozbek et al. / Vacuum 65 (2002) 521–525 525

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