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CHARACTERIZATION OF POROUS NITRIDED Ti6Al4V BIOMEDICAL

ALLOYS PRODUCED BY SOLID STATE SINTERING


Faras Velzquez, Ivn Gerardo, Jimnez Alemn Omar, Olmos Navarrete Luis, Alvarado Hernndez Francisco, Vergara Hernndez
Hctor Javier, Cabezas Villa Jos Luis.
Contact: Departamento de ingeniera de proyectos
Jos Guadalupe Zuno #48, los Belenes, Zapopan,
Jalisco, Mxico C.P. 45100.
Email: ivanger@gmaiil.com

Relative high elastic Modulus in materials such as 316L, CoCrMo and Ti6Al4V in long term implant devices (<10 years), can lead to stress shielding effect, inducing a boneimplant mismatch. A
reduction in elastic modulus was possible using the space holder method, achieving a maximum total porosity of 48% and a total reduction of Young modulus 47.8 times in comparison with
wrought Ti6Al4V. However, induced porosity implied a substantial increase of specific area, accelerating the corrosion rate. Hence, nitrogen was flowing during 0.5 h and 2h in the sintering
processes at 1250 C. The corrosion resistance of nitrided sintering was a minimum two times higher in comparison with sintering compacts.
Keywords: Powder metallurgy, biomaterials, corrosion , Ti6Al4V

Pore volume fraction on samples


ranges from 27 to 50%. Larger
induced pores increased around
20% of the volume fraction.

Two pairs of samples are shown: Sample Without


Induced Porosity (SWIP) and Induced Porosity
Sample (IPS). Sintered at 1100C and 1300 C
respectively.

MATERIALS AND METHODS

Element mapping by EDS of in situ nitrided samples

Shape, distribution and particle size.

The sintering compacts were fabricate using prealloyed powders of Ti6Al4V,


according to ASTM B348 standard grade 23.
The space method was carried out according to follow diagram.

Plastic deformation of the


sample during compression is
controlled by the large pores.
First pores close to the punch
were deformed until they are
close, with small changes in
the lower part of the sample.
this behavior prevents the
fissure propagation on the
direction of charge.

b)

a)

Fissures go in perpendicular
direction to the charge. Larger
pores
appeared
after
compaction and the volume
fraction of small pores is
significantly reduced.

Porous Ti6Al4 fabrication by means space holder method.

Elastic Modulus
7

E(GPa)
6

Sample

It
was
two
finals
products, where one was
sintered under argon
atmosphere, the other
one was sintered first
under argon during 1
hour and after nitride
during 0.5 and 2 hours
respectively at 1250 C.
In each case, the cooling
was
under
argon
atmosphere.
All
the
sintering
cycles
are
summarizing.

IPS1300
IPS1100
SWPI1300

E(GPa)
6.657
4.484
3.894

(MPa)
551.3
418.6

Yield strength
(MPa, off set =0.2%)
237.5
108

335.4

79.3

SWPI1100

2.608

138.1

58.7

0
IPS1300

IPS1100

SWPI1300

SWPI1100

Mechanic behavior in of different sintering samples.

Corrosion Rate
6.00E-05

5.00E-05

Icorr (A/cm)
4.00E-05

3.00E-05

2.00E-05

1.00E-05

Sintering cycles.
0.00E+00

Elastic modulus was determined from the graph stress vs deformation with
universal testing machine, in compression mode. Using cylindrical specimen
with dimensions of 0.8 in diameter by 1 cm in height.
RESULTS

Ti6Al4V

Ti6Al4V, Nitrided Ti6Al4V, Nitrided Sintered 1100C Sintered 1300C Sintered, Nitrided Sintered, Nitrided
0.5h
2h
0.5h
2h

Potentiodinamic polarization curves

CONCLUSIONS
In the present work samples with different values of porosity from 27 to 50% were
studied in terms of their mechanic and corrosion properties. In order to enhance the
corrosion properties a film of TiN was developed during the sintering process by passing
N2 gas at high temperature. The following conclusions can be drawn:
1. Compression tests showed that increasing sintering temperature increased the elastic
modulus. This is mainly because the size and number of necks increased during the
process. It was also identified that porosity diminished the mechanical properties.

Porous samples sintered: a) 1100 C and b) 1300C


Compacts sintered and nitrided in situ.

The SEM
micrographs shown the
difference between shrinkage of particles
and the macropores yielded by the space
holder.

2. The corrosion rate in sintering Ti6Al4V were until 254 times higher in the worst cases
compared with wrought Ti6Al4V. However, it was found a enhancement reducing that
path at 45 times by means the used of nitrogen atmosphere during the sintering
process.
3. Compression tests were evaluated by Computed microtomography showing that large
pores drives the deformation mechanism.

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