Int.

Journal of Refractory Metals & Hard Materials 27 (2009) 900–906

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Int. Journal of Refractory Metals & Hard Materials

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Hot isostatic pressing (HIP) of a-Al2O3 submicron ceramics pressureless sintered

at different temperatures: Improvement in mechanical properties
for use in total hip arthroplasty (THA)
M.H. Bocanegra-Bernal a,*, C. Domínguez-Rios a, A. Garcia-Reyes b, A. Aguilar-Elguezabal a,
J. Echeberria c, A. Nevarez-Rascon d
a
Centro de Investigación en Materiales Avanzados, CIMAV S.C., Miguel de Cervantes #120, Complejo Industrial Chihuahua 31109, Mexico
b
Interceramic, Depto. de Investigacion y Desarrollo, Av. Carlos Pacheco 7200, Chihuahua 31060, Mexico
c
CEIT and TECNUN, University of Navarra, 20018 San Sebastian, Spain
d
Escuela de Odontologia, Universidad Autonoma de Chihuahua, Ciudad Universitaria, Campus 1, CP 31000, Mexico

a r t i c l e i n f o a b s t r a c t

Article history: The effect of hot isostatic pressing (HIPing) on as-sintered a-Al2O3 ceramics for total hip arthroplasty
Received 10 February 2009 (THA) was investigated. The sinterability of these powders and the minimum temperature required to
Accepted 7 May 2009 obtain closed porosity have been determined by pressureless sintering in air at temperatures between
1280 and 1460 °C for 2 h. Temperatures of 1300 and 1325 °C and applied pressures of 150 MPa for
30 min were utilised in the HIP cycles. Densities >98% of the theoretical density (TD) have been obtained
Keywords: after HIPing, and the grain sizes previously obtained during pressureless sintering increased slightly dur-
Hip arthroplasty
ing the HIP treatment. The microstructures before and after HIP treatments were observed by means of
Alumina ceramics
Hot isostatic pressing
scanning electron microscopy (SEM). The fracture toughness was obtained by the indentation fracture
Ultra-high-molecular-weight polyethylene technique using a Vickers hardness tester at a load of 10 N with a dwell time of 15 s for all cases. The
ceramics obtained at the lowest HIP temperature (1300 °C) presented a grain size of 0.62 ± 0.04 lm, hard-
ness of 20.5 ± 0.6 GPa, and fracture toughness of 4.8 ± 0.3 MPa m1/2. The reported values were higher than
those obtained by other authors and were in concordance with international standards that could make
these ceramics available as a replacement for metal-on-polyethylene in orthopaedic surgery.
Ó 2009 Elsevier Ltd. All rights reserved.

1. Introduction
The excellent benefits of fine-grained alumina microstructures
with submicrometre grain sizes are well-known. Alumina compo-
nents with submicrometre grain sizes have improved hardness,
wear resistance, and strength, as well as good biocompatibility
and excellent corrosion resistance [1–6]. However, it is very impor-
tant to stress that at very small grain sizes (approximately <100 nm)
certain mechanical properties can deteriorate as a consequence of
the increasing contribution from grain boundaries to the deforma-
tion [7,8]. On the other hand, ceramic materials, mainly aluminium
oxide, have been used as an alternative in total hip arthroplasty
(THA) and total knee arthroplasty (TKA) Today, the prostheses for
both of these applications consist of a cobalt–chromium (CoCr) al-
loy articulating against ultra-high-molecular-weight polyethylene
(UHMWPE) [9]; their estimated lifetime is 10–15 years [10]. On
the other hand, 25% of total hip and knee joint replacements have
presented premature failure by aseptic loosening [11].
* Corresponding author. Tel.: +52 614 439 11 11; fax: +52 614 439 11 12.
E-mail address: miguel.bocanegra@cimav.edu.mx (M.H. Bocanegra-Bernal).
As was outlined above, ceramics have been used in both THA
[12–14] and TKA [15–17] for many years. Aluminium oxide
(Al2O3) was introduced as a material for orthopaedic bearings in
the 1970s and has been the most widely used ceramic material
in THA due to its low cost and high hardness [18]. Similarly, the
biocompatibility of Al2O3 ceramics is related to its high chemical
stability, which confers corrosion resistance and reliable in vivo
behaviour over time [9,19]. Currently, improved mechanical and
physical properties have been obtained with Al2O3 ceramic bear-
ings as compared to earlier bearings of the same material. For
example, Willmann [20] reported Vickers hardness values of
1800, 1900, and 2000; grain sizes (lm) of 4.5, 3.2, and 1.8; bending
strengths (MPa) of 400, 500, and 580 for alumina in the 1970s,
1980s, and 1990s, respectively. However, during this time period,
its low fracture toughness (<4 MPa m1/2) has been a persistent lim-
itation. Al2O3 bearings are currently manufactured with additions
of 250 ppm MgO as a grain growth inhibitor and by hot isostatic
pressing at temperatures of 1250–1400 °C in order to obtain an al-
most fully dense material with a grain size smaller than 2 lm, as
has been reported by De Aza et al. [21], Hench and Wilson [22],
Piconi and Maccauro [23], and Ratner et al. [24].

0263-4368/$ - see front matter Ó 2009 Elsevier Ltd. All rights reserved.
doi:10.1016/j.ijrmhm.2009.05.004
 M.H. Bocanegra-Bernal et al. / Int. Journal of Refractory Metals & Hard Materials 27 (2009) 900–906 901

The first generation of alumina ceramic bearings was produced
by conventional sintering, where severe flaws already present in
the green body were enhanced. Taking into account the generally
low fracture toughness of ceramics, Al2O3 material improvements
are related to their long-term reliability: minimizing the presence
of strength-limiting flaws in the fabricated material and improving
the fracture toughness. Therefore, by controlling the main param-
eters of the starting materials, it is possible to obtain alumina with
a dense microstructure and submicrometre grain size for the pur-
poses of improving their mechanical properties and reliability for
use in orthopaedic surgery [1,9,25,26]. Defect-free processing will
be the key to enabling the industrial manufacturing of new submi-
crometre Al2O3 ceramics. For this purpose a number of different
approaches such as cold isostatic pressing (CIP) [2,4,27–29] and
various wet shaping methods [4] have been found to be applicable
for the powder and lead to high-density green bodies with good
homogeneity of compaction; consequently, full density at rela-
tively low temperatures can be attained. Hot isostatic pressing
(HIPing) of as-sintered alumina samples is a method used to im-
prove the mechanical properties. This method guarantees an al-
most fully dense material with a fine grain size and eliminates
porous regions produced by agglomerates or the burn-out of or-
ganic inclusions, as has been reported by Kellet and Lange [30]
and Tressler et al. [31]. In the HIPing technique pressures are typ-
ically higher, by up to an order of magnitude, than those used in
uniaxial hot pressing [32].
Although HIPing of Al2O3 ceramics has a long history of develop-
ment and therefore is the most familiar for use in the processing of
the many existing ceramics materials [33], this technique is still
being improved to meet optimal HIPing schedules such that the de-
sired mechanical properties and reduced processing costs required
for both THA and TKA applications are obtained. According to re-
search reported by Manabe et al. [34] on Al2O3 powders of greater
than 99.99% purity and with a 0.6 lm mean particle size, certain
physical properties of some oxide ceramics degrade when HIPed in
an inert atmosphere such as argon. Kim et al. [35] also reported on
the HIPing of alumina with an average particle size of 0.4 lm and
specific surface area of 8.0 m2 g1 where they obtained a final grain
size between 0.25 and 1.43 lm after different HIPing conditions.
Similar investigations were undertaken by Echeberria et al. [25] on
three ultrafine high-purity commercial a-alumina powders with
particle sizes ranging 0.1–0.4 lm. They produced ceramics with
fracture toughness values between 2.5 and 3.5 MPa m1/2 for HIPing
temperatures of 1250–1400 °C in an argon atmosphere. Based on
this and other reported studies, the current research was under-
taken with the goal to analyse the potential of HIPing of as-sintered
alumina ceramics at different temperatures as an alternative tech-
nique to obtain full densification. In addition, the mechanical prop-
erties, such as hardness and fracture toughness, that can be
currently achieved with the best alumina powders available will
be reviewed. To substitute alumina for ultra-high-molecular-weight
polyethylene (UHMWPE) in the socket, the optimal selection of HIP
schedules will also be reviewed. We were able to obtain Al2O3
pressed at 100 MPa into discs of 16 mm in diameter and 5 mm in
height using a rigid steel die. The compaction was carried out using
an Elvec Hydraulic Press at a constant strain rate. After ejection
from the die, green samples were measured and weighed to calcu-
late the green density. Green compacts were placed into an
alumina crucible with an Al2O3 powder bed and sintered at tem-
peratures of 1280, 1325, 1375, 1425, and 1460 °C for 2 h in air at
a heating rate of 30 K min1 in order to determine the minimum
temperature for obtaining closed porosity. The sintered samples
were introduced into a boron nitride crucible with an alumina
powder bed to minimize possible reactions with the graphite heat-
ing element and subsequently hot isostatic pressed in an ASEA-HIP
(QIH-6) at 1300 and 1325 °C at a heating rate of 20 K min1 under
an argon atmosphere and isostatic pressure of 150 MPa for 30 min.
Fig. 1 shows the selected HIP heating and pressure cycle. As shown
in this figure, a pressure of 0.5 MPa was maintained up to 800 °C
and subsequently increased, and finally, the temperature and pres-
sure were maintained at a constant for the same time period. This
HIP treatment was applied to the powder in order to produce a
fine-grained material with a final density >98%. The density was
measured geometrically and by a Quanta Chrome Multi-Pycnome-
ter using helium as the displacement gas for the as-sintered and
HIPed samples. To characterize the microstructure, the specimens
were ground and polished through 0.5 lm diamond paste. After
preparing the surfaces by grinding and polishing, the microstruc-
ture was revealed by thermal etching in air for 45–60 min at
temperatures 150 °C below the sintering temperature and charac-
terized by scanning electron microscopy (SEM: JEOL JSM 5800 LV,
Japan) and Field-emission SEM (FEG SEM: JEOL JMS 7000F, Tokyo,
Japan) using an accelerating voltage of 2–10 kV. Samples were car-
bon coated to avoid charging during exposure to the electron
beam. The average grain size was measured using the linear inter-
cept technique for samples of 500 grains each. Similarly, trans-
mission electron microscopy (TEM) and SEM were employed to
observe the morphology of the starting powders.
Vickers hardness measurements were carried out on sintered
samples by using a microhardness tester FM-7. Indentations were
made on polished surfaces with a load of 1 kg held for 15 s.
Approximately 10–15 indents were made for each composition,
and the average hardness was determined. The corresponding
indentation sizes and crack lengths were determined using an opti-
cal microscope, the Olympus PMG3. The indentation fracture
toughness (KIC) was derived from the average crack length and ap-
plied to the following formula [36]:
K IC ¼ 0:0752P=C 3=2 ð1Þ
where KIC is the fracture toughness, P is the load, and C is the crack
length.
1700 200
1600 HIP temperature (ºC)
1500 175
1400 HIP pressure (MPa)
1300 150
HIP Temperature (ºC)

ceramics with improved grain size, hardness, and fracture toughness 1200
Pressure (MPa)

1100
as compared to those properties obtained by other authors for alu- 125
1000
mina during the 1970s–1990s; these results suggest that Al2O3 900 o
800 C 100
ceramics are available for orthopaedic surgery. 800
700
600 75
500
2. Experimental procedure 400 50
300
200 25
High-purity Baikalox SM8 (>99.99%) Al2O3 powders (mean par- 100
ticle size 0.3 lm, surface area 11.1 m2 g1, and crystal structure 0 0
0 10 20 30 40 50 60 70 80 90 100 110
100% a manufactured by BAIKOWSKI, USA) were selected as the Time (min)
starting material. For all cases, the alumina powder was used with-
out the addition of MgO. The Al2O3 powders were uniaxially Fig. 1. Typical temperatures and pressures for the experimental HIP cycle.
902 M.H. Bocanegra-Bernal et al. / Int. Journal of Refractory Metals & Hard Materials 27 (2009) 900–906

3. Results and discussion 50

Both SEM and TEM micrographs of the starting Al2O3 powder 45

Relative Density (%)

revealed a homogeneous particle size where large agglomerates
40
were absent, as shown in Fig. 2. With both of these characteristics
and the high purity, it was possible to produce a homogeneous 35
microstructure in the final sintered body with a submicron grain
size. Fig. 3 shows the density-compaction pressure response of 30
the Al2O3 powders whose results were plotted by adjusting the 25
elastic deformation effect of the die-punch system [37]. As can
be seen in this figure, at an applied pressure of 100 MPa, the 20 Pure Al 2O3
achieved relative density was approximately 47% TD. At lower Pressing rate: 0.5 cm.min-1
15
compaction pressures (up to approximately 15 MPa) the density 0 10 20 30 40 50 60 70 80 90 100 110
of the compact increased quickly as a consequence of a rearrange- Applied Pressure (MPa)
ment process, suggesting that the sliding had favoured the densifi-
cation in this stage due to the difference in size and shape of the Fig. 3. Relative density versus applied pressure for uniaxially pressed pure Al2O3
powder.
particles. With a further increase in applied pressure, the densifica-
tion was restricted.
As was previously mentioned, it was necessary to determine the 100
minimum temperature to obtain closed porosity. Fig. 4 shows the
Pure Al2O3
relative densities obtained by means of pressureless sintering in
95
air (heating rate = 30 K min1) as a function of the temperature.

Relative Density (%)

In this figure the dotted line represents the minimum density re-
quired for closed porosity, prior to HIPing (92%, corresponding 90
Minimum density for HIP
to 1360 °C), which are in agreement with results reported by Ech-
eberria et al. [25] for aluminas with particle sizes ranging 0.1– 85
0.4 lm. It is also observed that the final relative density reached
Pressureless conditions
at 1460 °C was 97%. The variation in the relative density with the
80
HIP temperature for the pressureless sintered samples is shown Heating rate: 30 ºC.min-1
Atmosphere: Air
in Fig. 5. In all cases nearly full density ( 98%) at temperatures be- Time: 120 min
tween 1375 and 1460 °C was obtained when samples were HIPed 75
1275 1300 1325 1350 1375 1400 1425 1450 1475
at temperatures of 1300 and 1325 °C, suggesting that the materials Sintering Temperature (ºC)
achieved higher densities when treated with HIPing rather than
when treated with pressureless sintering. The maximum density Fig. 4. Bulk density by pressureless sintering at different temperatures. Minimum
obtained after sintering was approximately 99% TD. Thus, in all density for closed porosity (92%) is represented by the dotted line.
cases, after a HIP treatment a small amount of open porosity re-
mained, impeding the attainment of full density. Total pore closure
might be achieved by an increase of temperature or pressure, Fig. 6 shows SEM micrographs of alumina samples before and
according to an investigation performed by Seidel et al. [38] with after a HIP treatment at 1300 and 1325 °C under Ar gas at
different alumina powders. On the other hand, Evans and Hsueh 150 MPa. An almost fully dense surface morphology can be seen,
[39] observed that for the purposes of large pore removal by hot as well as regions of smaller equiaxed grains (Figs. 6b, d, and e).
isostatic pressing in ceramics, the predicted trend indicated that However, elongated grains are also revealed, for example, in Figs.
pressure was most beneficial when pores were large; meanwhile, 6c, f, g, and l. According to this figure, all materials exhibited sim-
as the pores shrank, their subsequent shrinkage rate decreased ilar microstructures with grains that averaged in size from 0.6–
such that their ultimate removal might have required long times. 1.2 lm (see Fig. 7) and a few trapped pores (Fig. 6e and j). After
The presence of small-sized pores in the uniaxially pressed sam- analysing Fig. 7, it is observed that a larger grain size was obtained
ples could reduce the effect of the pressurized gas in preventing by the HIP treatment with appreciable grain growth in some cases.
shrinkage during the HIP treatment [40,41]. This larger grain size can be seen in micrographs corresponding to

Fig. 2. (a) SEM and (b) TEM micrographs of the high-purity Al2O3 starting powder.
 M.H. Bocanegra-Bernal et al. / Int. Journal of Refractory Metals & Hard Materials 27 (2009) 900–906 903

100 At relative densities >0.9, the isolated pores were less effective
Pressureless sintering
o
in pinning the grain boundaries; hence, grain growth dominated
HIP at 1300 C
(see Figs. 6e and j) [44]. Although grain growth readily occurred
95 o
HIP at 1325 C
during the high temperature consolidation of nanocrystalline
Relative Density (%)

materials [45], abnormal grain growth had been reported in ceram-

90 ics during the high pressure consolidation processes [46,47]. Bes-
son and Abouaf [46] observed abnormal grain growth in samples
85 prepared under pressure, although it was not observed during
pressureless sintering even after prolonged sintering times
(100 h) at a temperature of 1400 °C. Likewise, they reported grain
80
growth enhancement during HIPing due to deformation rather
than external pressure. In HIPed samples abnormal growth of a
75 certain small number of grains, whose surface areas exceeded
1275 1300 1325 1350 1375 1400 1425 1450 1475 manifold the surface areas of the adjacent grains, was observed,
Sintering Temperature (ºC) as is shown in Fig. 6i. In spite of the grain growth observed in this
investigation, the grain size obtained after HIPing at 1300 and
Fig. 5. Evolution of the sintered density with the HIP temperature for pressureless
samples at different temperatures. 1325 °C (0.6–1.2 lm) in samples pressureless sintered between
1375 and 1460 °C is smaller than the 2–3 lm reported by Furuka-
wa [48] and Graule et al. [49], who started with 0.4–0.5 lm pow-
Fig. 6 for HIP temperatures of 1300 and 1325 °C for the different der particles, and the 0.8–1 lm grain size, obtained from
pressureless sintered cases. Grain growth in alumina ceramics particles that were originally 0.2–0.3 lm, reported by Hayashi
has been studied for more than 30 years [42] because the grain size et al. [50] and Goh et al. [51]. On the other hand, our reported grain
of ceramics is of vital importance. Many of their physical, in partic- sizes were in agreement with the values obtained with BioloxÒforte
ular mechanical, properties show a marked dependency on the (mean grain size <1.8 lm), the trade name for medical grade
post-processed grain size and distribution, and the grain shape ceramics from CeramTec AG [52]. In fact, the grain size values ob-
evolution and distribution. The larger grains in HIPed samples tained in this work fulfil the required specifications for high-purity,
can be related to pore removal, as was observed by Bannister dense aluminium oxide for load-bearing surgical implant applica-
[43]. This behaviour is supported in Fig. 5 where an increase in rel- tions, according to ASTM F603-00 [53].
ative density after the HIP treatment denotes additional shrinkage When Al2O3 ceramics are carefully manufactured and the opti-
as a consequence of the removal of closed porosity. mization of powder processing is possible, Vickers hardness values

Fig. 6. SEM micrographs of HIPed specimens. (a), (d), (g), and (j) are pressureless sintered samples; (b), (e), (h), and (k) are pressureless and 1300 °C HIPed samples; (c), (f), (i),
and (l) are pressureless and 1325 °C HIPed samples. For all cases bar = 1 lm.
904 M.H. Bocanegra-Bernal et al. / Int. Journal of Refractory Metals & Hard Materials 27 (2009) 900–906

1.3 5.0
Pressureless sintering Pressureless sintering
1.2 o

Fracture Toughness (MPa.m1/2)

HIP at 1300 C
o HIP at 1300 C
4.5 o
HIP at 1325 C
o HIP at 1325 C
1.1
Grain Size (µm)

1.0 4.0

0.9
3.5
0.8

0.7 3.0

0.6
2.5
1370 1380 1390 1400 1410 1420 1430 1440 1450 1460 1470 1480 1370 1380 1390 1400 1410 1420 1430 1440 1450 1460 1470
o
Sintering Temperature ( C) Sintering Temperature (oC)

Fig. 7. Grain size evolution as a function of HIP temperature for pressureless Fig. 9. Indentation fracture toughness as a function of HIP temperature for
sintered samples at different temperatures. pressureless sintered samples at different temperatures.

ical grade ceramic; Daguano et al. [55] (3.4 ± 0.5 MPa m1/2); Rack
HV > 18 GPa are obtained, which are among the highest data values
and Pfaff [56] (4.3 MPa m1/2) in HIPed alumina ceramic materials
observed in alumina without additions of MgO as a grain growth
for medical applications; and Celli et al. [57] (4.2 ± 0.4 MPa m1/2).
inhibitor [1] and can be used as a biomaterial in THA. By plotting
Considering the hardness and fracture toughness values re-
material microhardness versus the pressureless sintered tempera-
ported in this work for the two HIP tested temperatures, the slight
ture, Fig. 8 illustrates the effects of HIPing at 1300 and 1325 °C on
reduction of these properties with increasing pressureless sinter-
the microhardness. In this figure it is clearly observed that for both
ing temperature could be attributed, as mentioned above, to the
HIP temperatures, the microhardness increased when the sintering
increase in grain size (Fig. 7). This increase in grain size therefore
temperature decreased. The improved hardness may be attributed
reduced the number of grains per area and produced a smaller de-
to the smaller grain size that occurs at low pressureless sintering
gree of crack deflection due to the decrease in grain boundary area.
temperatures, as can be seen in Fig. 7, and is in concordance with
On the other hand, this observed decrease might be due to the
that reported by Krell and Blank [2] for alumina. They observed
segregation of pores along the grain boundaries (see Figs. 6f, h).
hardness values of 20–22 GPa for samples having a grain size of
Conversely, a change of fracture mode from transgranular to inter-
0.5–0.6 lm and also reported values of 20–21 GPa for a grain size
granular mode [58], as well as a reduction of the critical flaw size,
of 0.5 lm after consolidation by HIPing [1]. Moreover, their reported
led to an increase in fracture toughness [58,59]. The fracture
hardness values were slightly higher than those obtained in the
toughness determined by the Vickers indentation fracture method,
present study (20.6 GPa for HIPing at 1300 °C for alumina ceram-
although widely used due to its ease of use, has not been widely
ics pressureless sintered at 1375 °C) under different processing con-
accepted due to the complex stress state involved in the Vickers
ditions. The fracture toughness as a function of HIP temperature in
indentation. Therefore, it is believed that the fracture toughness
samples pressureless sintered at temperatures between 1375 and
values obtained from applying this technique may not represent
1460 °C is illustrated in Fig. 9. It is observed that when samples
the true KIC [60]. An economical and effective technique to charac-
sintered at 1425 °C were HIP treated at 1300 °C, the resulting high
terize the fracture toughness in ceramics is currently not readily
fracture toughness value (4.8 ± 0.5 MPa m1/2) is higher than
available [61].
those reported by Echeberria et al. [25] (2.5 ± 0.1 and 3.4 ± 0.3
As was outlined above, the great majority of total hip joints are
MPa m1/2) at sinter-HIP temperatures of 1350 and 1250 °C, respec-
composed of UHMWPE [9] due to good biocompatibility, high
tively; Chakravarty et al. [54] (3.2 ± 0.3 and 3.4 ± 0.6 MPa m1/2) for
resistance to wear, and durability. However, wear debris may accu-
spark plasma sintered pure and MgO-doped Al2O3, respectively;
mulate and cause a biological response, such as osteolytic and/or
CeramTec AG [52] (4 MPa m1/2) with their Bioloxforte alumina med-
allergic reactions [62,63]. With the aim to reduce the effect of wear
debris, Al2O3 has been used in hip prostheses as a substitute for
UHMWPE [14,62], despite its inferior crack resistance [21]. Also,
22
when considering THA, the problems originated by polyethylene
Pressureless sintering
20 o wear particles are more severe when compared with problems
HIP at 1300 C
o from hip surgery that are due to the different curvatures of the
Microhardness (GPa)

18 HIP at 1325 C
femoral condyles and the top of the tibia plateau [6]. It has been
16 demonstrated that femoral heads composed of Al2O3 or yttria-sta-
bilized, tetragonal zirconia polycrystals (Y-TZP) articulating
14 against UHMWPE reduce the wear by at least a factor of two when
compared with the standard CoCr femoral head. Al2O3–Al2O3 bear-
12
ing couples provide the lowest wear rate with a value that is often
10 at least 50 times lower than that of the standard CoCr-UHWMPE
couple, according to the reported by Rahaman et al. [9]. Due to this
8 reason, it is important to develop an alumina ceramic based on a
combination of good strength, optimal fracture toughness, high
1275 1300 1325 1350 1375 1400 1425 1450 1475
wear resistance, and good biocompatibility, as well as excellent
Sintering Temperature (oC)
corrosion resistance properties that are better than those achieved
Fig. 8. Microhardness evolution as a function of HIP temperature for pressureless by employing the hot isostatic pressing of alumina powders. This
sintered samples at different temperatures. improvement may be accomplished by following international
 M.H. Bocanegra-Bernal et al. / Int. Journal of Refractory Metals & Hard Materials 27 (2009) 900–906
standards that give specifications for implants subjected to high
loads: high purity in the chemical composition and a homogeneous
size distribution, both of which are characteristic of the powder
used in our experimental work.
4. Conclusions
From the investigated HIPed as-sintered a-Al2O3 ceramics, we
can conclude the following:
(1) By employing HIPing at 1300 and 1325 °C with high-purity
and submicrometre alumina powder, it is possible to achieve
a near theoretical density value without exaggerated grain
growth.
(2) The grain size was maintained at the submicron scale when
HIPed at temperatures of 1300 and 1325 °C in samples pre-
viously pressureless sintered at temperatures below
1425 °C. For a constant HIP temperature treatment, the grain
size increased slightly with the pressureless sintering
temperature.
(3) An increase of fracture toughness was observed and could be
attributed to the smaller grain size, as well as the crack
deflection, and there was a probable contribution from the
change in fracture mode from transgranular to intergranular.
A slight decrease in Vickers hardness was also observed with
the pressureless sintered temperature for both HIP treat-
ments tested. The results reported in this work showed that
Al2O3 manufactured by a conventional sintering process and
subsequently HIPed at 1300 and 1325 °C presented high
density, hardness values greater than 18 GPa, and a fracture
toughness >4.1 MPa m1/2. These results, in turn, are in agree-
ment with the international standards for the application of
metal-on-polyethylene in orthopaedic surgery for joint pros-
theses. Indeed, the hardness and fracture toughness values
reported here were the highest among the much-reported
values in the literature for pure Al2O3 processed under sim-
ilar conditions.
(4) An enhancement of the mechanical properties, such as hard-
ness and fracture toughness, could be expected when using a
small amount of MgO (0.25 wt%) in combination with the
HIPing forming technique. The MgO served as a sintering
aid in controlling the grain size and promoting the achieve-
ment of full density. The resulting ceramic material could
improve both the lifetime and reliability of ceramic prosthe-
ses, thus contributing to a significant improvement in the
quality of life for a great number of patients as well as avoid-
ing the high cost of surgical operations. The authors are cur-
rently working on this theme.
Acknowledgements
The authors wish to express their appreciation to Roal Torres for
his assistance in the hardness and fracture toughness measure-
ments, and Wilber Antunez for the SEM characterization. The
authors thank Centro de Estudios e Investigaciones Tecnicas de
Guipuzcoa, CEIT, Spain, for providing the necessary test facilities
for the HIP cycles.
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