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Advances in Applied Ceramics

Structural, Functional and Bioceramics

ISSN: 1743-6753 (Print) 1743-6761 (Online) Journal homepage: http://www.tandfonline.com/loi/yaac20

Exploring inexpensive processing routes to


prepare dense TiB2 components

C. Tallon & G. V. Franks

To cite this article: C. Tallon & G. V. Franks (2016): Exploring inexpensive processing
routes to prepare dense TiB2 components, Advances in Applied Ceramics, DOI:
10.1080/17436753.2016.1172166

To link to this article: http://dx.doi.org/10.1080/17436753.2016.1172166

Published online: 13 Apr 2016.

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Download by: [University of Sussex Library] Date: 05 May 2016, At: 23:00
Exploring inexpensive processing routes to
prepare dense TiB2 components
C. Tallon∗ 1,2,3 and G. V. Franks1,2
Titanium diboride (TiB2) is considered one of the most suitable candidate materials for applications
as wettable cathodes in redesigned aluminium smelting cells. In this work, titanium diboride
compacts have been produced from powders using a wet colloidal processing approach
combined with pressureless sintering for densification. The approach has good potential to
reduce the manufacturing cost compared to hot-pressing. Owing to the elevated cost of the raw
materials, the possibility of mixing powders with different particle sizes (more expensive fine and
less expensive coarse powder) has been explored. The outcome of this study is very promising,
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since using two different particle sizes improved the particle packing of the green material
resulting in sintered densities around 80% of the theoretical density at 2000°C.
Keywords: Titanium diboride, Colloidal processing, Pressureless sintering, Particle packing

Introduction strength, low cost and ease of fabrication into particular


shapes.3–5
The smelting of alumina into aluminium in the Hall- This is why titanium diboride (TiB2) was identified as
Heroult process consumes enormous amounts of energy one of the most promising candidates for this application
and produces significant CO2 emissions1,2 but today it is in the late 1950s.3 Its wettability, low solubility in alumina
a much more productive and efficient method than 50 (melt pool primary component), high melting point and
years ago. This is mainly due to continuous research, its high electrical conductivity make this material the
development and advancement in engineering solutions only feasible material option versus other refractory cer-
to extend the cell life.3–5 One of the approaches to do so amics and other metals and composites. Unfortunately,
is to find inert electrodes (and their corresponding design this material is quite expensive to produce (expensive
configuration) which could replace the current carbon raw material and high cost for processing the material
electrodes (which are consumed or worn) and last longer due to high temperature and pressure for hot-pressing),
in operation. This will reduce the maintenance costs and and this could limit their applicability. In order to avoid
the leakage of power out of the cell, improving the effi- such high cost of a monolithic cathode of TiB2, several
ciency of the overall process. It is difficult to find materials different configurations for the cathode, such as a coating
which could be cost-effective in electrode applications, of the carbon cathode or as part of a composite have been
and in the case of cathodes it is particularly much more considered.3,8,9–12
challenging. The environment in which inert cathodes Apart from TiB2, other materials have been con-
need to operate in is quite severe1,2,6,7 and the number sidered, mainly from the group called ultra-high-temp-
of candidate materials to withstand these conditions is erature ceramics or refractory ceramics. For example,
quite restricted. ZrB2 has a superb wettability with molten aluminium,
Before considering the materials properties or the oper- or Ta and Nb borides, but they have not been considered
ating conditions of the cathodes, it is important to note further because they are even more expensive than TiB2.
that the most important constraint to find a replacement The rest of compounds (carbides and nitrides) in this
is related to the gap between the anode and cathode in the group are not good conductors or react with the liquid
cell.4 Therefore, it is crucial that the material of choice aluminium.13 Mroz4 suggested the use of compounds
first of all is wetted by the melt pool. Additionally, the from the MAX phases families, due to their high
material must exhibit a superb electrical conductivity strength, refractoriness, high electrical and thermal con-
and withstand an extremely corrosive high-temperature ductivity, and high machinability, but he found that the
environment, among other criteria such as mechanical Ti3SiC2 was corroded by the cryolite solution, although
to a lower extent than TiB2. Also, some of the materials
1
Department of Chemical and Biomolecular Engineering, The University of
used for the side wall of the cell, such as SiC or nickel
Melbourne, Victoria 3010, Australia ferrite14 could be further explored in the future. How-
2
Defence Materials Technology Centre, DMTC, Victoria 3122, Australia ever, despite of the limitations mentioned before, there
3
Department of Materials Science and Engineering, Polytechnic Institute
and State University, Blacksburg, VA 24061, USA is no known material which could compete with TiB2

as a true replacement for carbon cathodes.
Corresponding author, email tallon@vt.edu

© 2016 Institute of Materials, Minerals and Mining


Published by Taylor & Francis on behalf of the Institute
Received 1 November 2015; accepted 25 March 2016
DOI 10.1080/17436753.2016.1172166 Advances in Applied Ceramics 2016 1
Tallon and Franks Exploring inexpensive processing routes to prepare dense TiB 2 components

Since the materials properties of TiB2 and the operating (ii) The use of colloidal processing techniques. Titanium
conditions of the cell could not be easily changed, the aim diboride,16–18 as other borides and carbides,19 require
of this work focuses on exploring other options to very high temperature and pressures for processing due
decrease the cost of the components. The double strategy to their strong covalent bond and low diffusion rates.
we will discuss in this work is: Owing to this, the manufacturing and state-of-the-art pro-
(i) The use of cheaper raw materials. The available TiB2 cessing require the use of hot-pressing and hot-isostatic
powders vary widely in particle size (from 1 to 100 μm), pressing to prepare dense component, which are very
purity and cost. High purity and fine powders (with par- expensive and time consuming. Traditionally, the use of
ticle sizes below 3 μm approximately) are the easiest to other processing routes has not been pursued due to the
process to produce dense ceramic material, due to the lar- need for pressure and temperature for sintering and for
ger surface area to drive the densification. For example, the possibility of oxidation and secondary phase for-
the synthesis of high purity nanopowders with large sur- mation when mixing powders with solvents, binders or
face area has also been considered15 but the yield and other organic additives. However, our group has been suc-
the cost of these type of synthesis process is still an issue cessfully working on the colloidal processing approach for
to face in the preparation of such large components. How- other borides and carbides for ultra-high-temperature
ever, the finer the powder, the more expensive it is, which applications for the past 5 years, and we have shown
makes the whole process very costly. Therefore, the first that using the same powder, the samples prepared via col-
approach we used in this project was to combine a ‘fine’ loidal processing exhibit higher sintered densities when
TiB2 powder and a ‘coarser’ less expensive TiB2 that compared with samples produced via hot-pressing.20
would act as a filler. We aimed to mix various ratios of The use of colloidal processing allows one to control the
fine powders and coarse filler TiB2 and see what is the interaction forces between particles in suspension. This
minimum amount of fine (expensive) powder we need to exhaustive control leads to a much better homogeneity of
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obtain high density TiB2 ceramics. the particles in suspension, and particle packing in the
green body.21–24 A very close and efficient particle packing
in the green body prepared via colloidal processing routes
has been shown to improve the sintering behaviour of cer-
amic materials, reducing the temperature needed for sinter-
ing, and in cases, removing the need for pressure for the
sintering stage.20,24 The pressureless sintering option is
very attractive, not only from an economical and oper-
ational point of view, but also, from a shaping capability
point of view. Hot-pressing and hot-isostatic-pressing typi-
cally produced very simple shapes (tiles, cylinders, discs)
that need to be machined to the required shape using
expensive diamond tools. Therefore, the titanium diboride
materials for this study will be produced following this
approach: colloidal processing and pressureless sintering.
The aim of this project is to produce and evaluate
different TiB2 materials prepared from a range of powders
using colloidal (wet) processing of ceramic powders and
pressureless sintering (densification without applying
pressure) in a vacuum furnace at up to 2100°C. Under-
standing how the different parameters affect the densifica-
tion and microstructure is crucial for the development of
the right material for wettable cathodes. The colloidal
processing technique is known to produce green bodies
with higher and more uniform particle packing.24 The
higher and uniform green density promotes sintering
and pore elimination leading to high density reliable
final ceramics.24–26 This reduces the sintering temperature
and pressure, leading to a significant reduction of the pro-
duction cost.

Experimental
Materials
Two powders were selected for the present study (Fig. 1):
(i) Fine powder: TiB2 grade F from H.C. Starck, with
fine particle size (dv50 = 1.5 μm) to enhance the densifi-
cation process.
(ii) Coarse powder: ESK, type S −70 μm, TiB2 powder
provided by Rio Tinto (Australia), which would act
1 SEM images of the raw powders used in this study: a fine as a less expensive filler.
powder and b coarse powder

2 Advances in Applied Ceramics 2016


Tallon and Franks Exploring inexpensive processing routes to prepare dense TiB 2 components

The particle size of each powder was measured using Suspensions of 40 vol.-% total solids loadings were pre-
laser diffraction (Mastersizer 2000, Malvern), and the pared in cyclohexane with 3 wt-% of dispersant with
results are plotted in Fig. 2. The powder was first respect to the total powder. The suspension was then soni-
measured as received (blue lines), and then sonicated to cated for 2 min (Ultrasonic Horn, Misonix 400, Farming-
break down possible aggregates in the as-received powder dale, NY) to break down any aggregates. Suspensions
(orange lines). The fine powder has a narrow size distri- with 0% fine powder (100% coarse powders) were not
bution, and it is weakly aggregated, since after applying used in this study, since due to their larger size a signifi-
sonication the particle size decreased from 3.8 to 2.9 cant sedimentation of the powder was observed at the bot-
μm. However, the coarse powder (or filler) showed a tom of the container.
much wider size distribution with average particle size The suspensions were then slip cast using cylindrical
around 10 μm after sonication. rings (22 mm diameter, 20 mm height) placed on plaster
Cyclohexane (Sigma Aldrich) was used as the solvent of Paris and covered with parafilm. Once the consolida-
to prepare the TiB2 suspensions and Hypermer A70 tion process is completed (overnight), the samples were
(Croda, Australia) was selected as the dispersant. The unmoulded and dried at room temperature for 2 days
use of an organic solvent to prepare the suspensions, and then 80°C for 2 h before further characterisation.
not only decrease the probability of further oxidising the The green samples were then cut in halves and sintered
powder particle surfaces, but also, allows for a better dis- in a graphite vacuum furnace (Red Devil, RD Webb,
persion of the particles in suspension. The Hamaker con- Massachusetts, USA) at temperatures of 1900, 2000°C
stant of borides and carbides in organic solvents is lower and 2100°C for 1 or 2 h. The heating rate was 5°C
than in water, therefore, the van de Waals attraction min−1, with an isothermal hold at 400°C to burn out
between particles is lower.27 This minimises the aggrega- any dispersant and the rest of the solvent. The chamber
tion of particles in the suspension and guarantees an hom- was backfilled with argon above 1800°C. The cooling
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ogenous and close packing of the particles in the green rate was 5°C min−1.
body, which is key for densifying under pressureless When TiC was added as a sintering aid, suspensions
conditions.20,24 with 40 vol.-% solids using the previous formulation
TiC (H.C. Starck, grade HV 120) was used as a sinter- were prepared. The powder mixture contained 50% fine
ing aid for the last part of this work. This powder was and 50% coarse powder as optimised before. Sintering
sourced, with fine particle size (dv50 = 1.5 μm) to enhance aids were added in 1, 3 and 5 wt-% with respect to the
the densification process. The oxygen content reported by total powder. The suspension was slip cast and sintered
the manufacturer is a maximum of 1%. using the same procedure explained before.
In order to compare the suitability of the colloidal pro-
cessing approach to the conventional dry pressing of pow-
Sample preparation procedure ders, some pellets were produced by dry pressing the
Different percentages of filler and fine powder were mixed powder mixtures with 75, 90 and 100% of fine powder,
together, 25, 50, 75, 90 and 100% of fine powder. and sintered at 2000°C. The uniaxial dry pressing was per-
formed by loading the dry powder mixture into a tool
steel die, using a layer of oleic acid as lubricant. Pellets
of 15 mm diameter and 12 mm height were produced by
applying a pressure of 416 MPa for 30 s.

Characterisation
The green and sintered densities of the samples were
measured using Archimedes’ method and the reported
value is an average of 3–5 samples. In the case of the
green samples, in order to protect the pieces when immer-
sing them in the liquid for the measurement, they were
coated with a layer of wax of known density.
The sintered samples were cut (Accutom-50, Struers,
Australia) and polished (TegraPol-21 with TegraForce-5
and TegraDoser-1, Struers, Australia) for studying the
microstructure by Scanning Electron Microscopy
(ESEM, Quanta XL-30, Phillips). The slices observed in

Table 1 Density of the green bodies produced using


different percentage of fine and coarse powders

Percentage of fine powder Relative green density/% (respect


in the mixture/% to theoretical density of TiB2)

0 n/a
25 69.7
50 71.8
2 Particle size distribution of the TiB2 powder used in this 75 66.3
study. a Fine powder, b coarse powder. The average par- 90 65.9
100 61.4
ticle size before and after sonication is shown

Advances in Applied Ceramics 2016 3


Tallon and Franks Exploring inexpensive processing routes to prepare dense TiB 2 components

temperatures. The sintered densities are plotted in Fig.


3. There was not any change in the density after sintering
at 1900°C compared to the green density. Only a slight
increase in density was found when sintering at 2000°C,
except for the 50/50 mixture which densified somewhat.
The best result obtained for green and sintered samples
correspond to materials prepared with 50% fine and
50% coarse powders. This is due to the high initial particle
packing of the green body. Increasing the sintering temp-
erature and time produced an increase in the densification
of the 50/50 samples. Those samples were sintered at
2100°C for 1 h, reaching values of 80% of the theoretical
density (TD).
3 Sintered densities of samples with different per cent of The images of the polished surfaces of the samples (Fig.
fine and coarse powder, sintered at different temperatures 4) reveal that despite no change of the density with respect
and times to that in the green state, there was necking between the
fine and coarse particles at 1900°C just to strengthen
the samples. Increasing the temperature to 2000 and
the microscope were taken from the centre of the sample
2100°C, lead to an increase of the necking between the
in a transversal cut. Energy dispersive analysis (EDS) was
particles, although significant porosity is still observed.
used to confirm the presence of phases in the sintered
There seems to be a coarsening in grain size with increas-
materials.
ing sintering temperature. Despite using particles with
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two very different sizes, the distribution of both fine and


Results and discussion coarse particles in the top and bottom of the sample
was studied, as shown in the images below (Fig. 5).
Green density and particle packing There is no significant segregation of particles along the
The relative densities of the green bodies as a function of height of the sample, confirming the good quality of par-
the fraction of coarse and fine powders are summarised in ticle packing and homogeneity reached in the green
Table 1. For most of the cases, the green densities are bodies as a consequence of using the colloidal processing
above 64%; that value represents the theoretical random approach.
spheres particle packing. The fine particles are packed fill- Pressureless sintering of pure TiB2 is not a trivial task
ing the voids between larger particles, resulting in a denser to perform, as it has been reported in the
green body. In particular, the green density of 50% fine literature9,16,17,30–32. Even hot-pressing of pure TiB2 is
powder samples reached a maximum value of 71.8%. very challenging commonly reaching only 90% of the
The maximum packing of compacts produced from fine TD at 2000°C, requiring temperatures up to 2477°C to
and coarse powder depends on the ratio fine/coarse in reach above 98% TD. Some of the highest sintered den-
the suspension, but also on the overall solid fraction in sities under pressureless sintering conditions reported in
the suspension.28,29 Lange and co-workers extensively the literature (90–99%) were achieved by using very fine
investigated this phenomenon using alumina powders of (below 140 nm) and high purity powders produced in an
0.23 and 0.59 μm, and reported a maximum packing den- arc-plasma reactor which were uniaxially pressed and
sity of 68% for dispersed particles28 and 57% for floccu- then cold isostatically pressed18,33; these authors indicated
lated particles29 when working with 40% fines total solid that if the powder was not milled to break down aggre-
fraction in slurries around 40 vol.-%. These values are in gates it did not sinter above 80%TD. In this work, we
good agreement with the ones obtained in this work, use commercially available powders more than one
despite the different shape of the particles. order of magnitude larger, with more impurities and with-
out expensive grinding or compaction stages, we reach
Sintered density 80%TD after sintering at 2100°C. This already could rep-
The slip cast compact produced with different percentages resent a significant decrease of the production cost of TiB2
of fine and coarse powders were sintered at different components. This approach could also be adopted to

4 Microstructures of samples produced with 50% fine powder and 50% coarse powder sintered at 1900, 2000 and 2100°C

4 Advances in Applied Ceramics 2016


Tallon and Franks Exploring inexpensive processing routes to prepare dense TiB 2 components

Table 2 Green densities of samples prepared with 50% fine


and 50% coarse powders and different amounts of
TiC as sintering aid

wt-% TiC added to the Relative green density/% (respect to


powder mixture theoretical density of TiB2)

0% 71.8
1% TiC 70.1
3% TiC 70.0
5% TiC 70.1

6 Densities of samples sintered at 2000°C for 1 h produced


produce composites and coatings of TiB2. In order to con- from different percentage of fine and coarse powders
firm the better suitability of the colloidal processing using colloidal processing and dry pressing
approach than the conventional dry pressing of powders,
some pellets were produced by dry pressing of the powder
using 75, 90 and 100% of fine powder in the powder These authors recommended keeping the oxygen concen-
mixture, and sintered at 2000°C (Fig. 6). For all the tration below 0.5 wt-%. The amount of oxygen in our
percentages, the colloidal processing samples produced powder is reportedly to be a maximum of 2.5 wt-% (man-
better results than dry pressing, confirming that colloidal ufacturer data), which could explain some the coarsening
processing is the right approach for producing TiB2. The we saw in the microstructures.
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colloidal approach produces higher green densities than However, it is necessary to reach temperatures above
the dry pressed pellets.20 Since only necking is occurring 2000°C to attempt pressureless densification of this
without significant densification, the density of the sin- material,16 and above that temperature, some preferential
tered bodies does not increase much more than the growth was observed and potentially could affect the
green body. mechanical performance of the component.16,30,31,34
Temperatures up to 2100°C have been explored in this This is why the bulk of work about TiB2 has focused in
work. It has been seen that the increase from 2000 to the use of hot-pressing, hot-isostatic pressing and the
2100°C produced a significant improvement on the densi- use of large concentration of sintering aids to promote
fication behaviour, mainly in terms of necking and grain densification below 2000°C.
growth, although the sintered density value is only 80%. The next stage of this work contemplated the addition
It is expected that a further increase of sintering tempera- of titanium carbide (TiC) as sintering aids to try to
ture up to 2200°C may trigger a significant densification improve the value of 80% relative density using the ratio
(we observed a similar situation for other borides and car- 50/50 which produced the better packing and better sin-
bides above certain value of temperature, materials have tering results so far.
gone from 75 to 80% density to above 90%).20 However,
due to the limitations of our furnace (maximum operative TiC as sintering aid
temperature) this option will not be directly explored. The sintering aid explored in this work was titanium car-
Despite the potential improvement in terms of proces- bide (TiC), based on previous work reported in the litera-
sability, the sintered densities achieved so far in this ture.16,35 The idea behind this choice was that this powder
work remain around 80%. One of the main reasons for could form C solid solutions in the TiB2 crystal structure,
this problem is that at temperatures above 1800°C, the thus increasing the vacancies and potentially increasing
presence of oxygen contamination in the powder pro- the solid state diffusion rate within the material. The
motes pore and grain coarsening by increasing the surface solid solution limit for TiC in TiB2 has been reported to
diffusivity, as Baik and Becher reported,33 and this coar- be around 2.7–3.2 mol-%36,37 (equivalent to 2.3–2.8 wt-
sening determines the maximum density achievable. %). However, some researchers have reported the use of

5 SEM images of the microstructure of sample produced from 50% fine powder and 50% coarse powder sintered at 2000°C cor-
responding at different height of the cross-sectioned sample. (left image: top of the sample; right image: bottom of the
sample)

Advances in Applied Ceramics 2016 5


Tallon and Franks Exploring inexpensive processing routes to prepare dense TiB 2 components

The use of transition metal11,38 (Cr and Fe), disili-


cides39 (TiSi2 and MoSi2), nitrides17,30,34 (TiN, AlN and
Si3N4) and carbides34,39,40 (B4C and SiC) have been
reported to improve the densification of TiB2. For
example, Popov et al. 41 prepared dense TiB2 components
(TiB2–Al2O3) via reactive hot-pressing using additions of
B4C and Al. However, the addition of these compounds
occurs in quite large percentages of the overall material
(up to 25 wt-%), which could have a significant influence
on the overall properties of the final material. There is not
much information available about how these compounds
may affect the conductivity or wettability of TiB2 or its
chemical resistance to molten salts and therefore its suit-
ability for cathode applications. We consider that TiC
7 Sintered densities of samples prepared with 50% fine and has very similar properties to TiB2 in terms of mechanical
50% coarse powders and different amounts of TiC as sin- strength and toughness and melting point, so it will not
tering aid sintered at different temperatures and times compromise the service conditions of this material.
The green densities of the samples prepared with 50%
fine and 50% coarse powder as a function of the amount
up to 15% TiC, which led to 99% density using hot-press- of sintering aid are shown in Table 2. The addition of up
ing.16 Although this reported 15% is above the solubility to 5 wt-% of TiC to the powder mixture did not affect the
value of TiC in TiB2, this value is still well below the stability of the suspension and the green densities
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molar fraction corresponding to the eutectic composition remained close to 70% in all cases, indicating very close
of TiB2–TiC phase diagrams, which is around 40 mol-% packing of all the different particles in the green body.
TiC36,37 (equivalent to 35 wt-% approx.). The range of The sintered results are summarised in Fig. 7. In gen-
concentrations used in this work ranged from1 to 5 wt- eral, the sintered density increased with the sintering
%, which are much closer to the solubility limit of TiC temperature/time as expected. The highest sintered den-
in TiB2, to keep the TiB2 as pure as possible to not affect sity reached was 80.8% for 1% of TiC sintered at 2100°
its conductivity. C/1 h. However, there was not a big change with respect

8 Microstructure of samples prepared with 50% fine and 50% coarse powder and different per cent of TiC sintered at 2100°C for
1h

6 Advances in Applied Ceramics 2016


Tallon and Franks Exploring inexpensive processing routes to prepare dense TiB 2 components

9 Microstructure of samples prepared with 50% fine and 50% coarse powder and 1% of TiC sintered at 2000°C for 1 and 2 h
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10 Microstructures of samples prepared with 50% fine and 50% coarse powder and 1% of TiC sintered at 2000°C for 1 h at differ-
ent height of the cross-sectioned sample (left image: top of the sample; right image: bottom of the sample)

to the pure TiB2. Increasing the percentage of sintering Conclusions


aids in the amounts chosen for this study does not seem
to help with the densification process, and in any case, Titanium diboride materials have been produced using a
the sintered densities were lower. The samples with 3 wet colloidal processing approach combined with pres-
and 5% TiC did not change their density value with respect sureless sintering. The approach has good potential to
to the green density measurement, even after sintering at reduce the manufacturing cost compared to hot-pressing.
2100°C. The microstructures of the samples sintered at Owing to the elevated cost of the fine powders, the possi-
2100°C (Fig. 8) are in good agreement with the sintered bility of mixing powders with different particle sizes (fine
density values registered. The sample with 1% TiC shows and coarse powder) has been explored. The outcome of
more densification and grain growth than the other this study is very promising, since using two different par-
samples, as expected from the 80.8% sintered value. The ticle sizes improved the particle packing of the green
sample with 3% TiC which produced the lowest density material resulting in final sintered densities around 80%.
at this temperature only present necking between the par- This result was achieved using 50% of fine powder and
ticle and more porosity when compared with other 50% coarse powder, significantly reducing the amount
samples. We have no explanation for this unexpected result. of ‘expensive’ powder required. However, the sintered
The effect of sintering time was seen in the microstruc- materials only showed densities around 80% at 2100°C,
ture, as depicted in Fig. 9. Increasing the sintering time even with the addition of TiC as sintering aid, and these
for the samples with 1% TiC produced an overall results are still well below the density required for closed
improvement of the necking of the particle and slight porosity (≈92%). The approach described in this paper
grain growth at 2000°C. Despite the difference in par- has the potential to open new avenues for the processing
ticle size and the addition of a third type of powder of these materials, since it has been demonstrated that
(TiC), no segregation of particles was observed when the high green density particle packing achieved with a
the top and bottom sections of the samples were exam- simple colloidal approach is an excellent (and inexpen-
ined, as demonstrated in Fig. 10. The samples were ana- sive) starting point for the pressureless sintering of these
lysed by EDS. No significant increase in the oxygen materials in comparison with uniaxial hot-pressing. The
content was observed with respect to the initial powder. addition of sintered aids and/or carbon to react with the
No indication of additional phases apart from TiB2 and oxygen impurities together with the use of sintering
TiC were observed. temperatures around 2300°C could lead to closed

Advances in Applied Ceramics 2016 7


Tallon and Franks Exploring inexpensive processing routes to prepare dense TiB 2 components

porosity-high density monoliths of TiB2 for use in cathode 18. H. R. Baumgartner and R. A. Steiger: ‘Sintering and properties of
applications. This approach could also be adopted to pro- titanium diboride made from powder synthesized in a plasma-arc
heater’, J. Am. Ceram. Soc., 1984, 67, (3), 207–212.
duce composites and coatings of TiB2. 19. W. G. Fahrenholtz, G. E. Hilmas, I. G. Talmy and J. A. Zaykoski:
‘Refractory diborides of zirconium and hafnium’, J. Am. Ceram.
Soc., 2007, 90, (5), 1347–1364.
Acknowledgements 20. C. Tallon, D. Chavara, A. Gillen, D. Riley, L. Edwards, S. Moricca
and G. V. Franks: ‘Colloidal processing of zirconium diboride ultra-
The authors of this report acknowledge the work of the stu- high temperature ceramics’, J. Am. Ceram. Soc., 2013, 96, (8), 2374–
dents Sarah Castelino, Allan Phu, Nicholas Chamberlain 2381.
21. F. F. Lange: ‘Colloidal processing of powder for reliable ceramics’,
and Dennis Kurniawan during their Research Project sub- Curr. Opin. Solid State Mater. Sci., 1998, 3, (5), 496–500.
ject. We thank Interdisciplinary Seed 2013 Funding from 22. W. M. Sigmund, N. S. Bell and L. Bergstrom: ‘Novel powder-proces-
the University of Melbourne for the funding provided to sing methods for advanced ceramics’, J. Am. Ceram. Soc., 2000, 83,
work on this project. We specially thank Lynne Davies of (7), 1557–1574.
23. J. A. Lewis: ‘Colloidal processing of ceramics’, J. Am. Ceram. Soc.,
Rio Tinto for providing the coarse TiB2 powder for this
2000, 83, (10), 2341–2359.
study. We thank Mr Samuel Pinches and Mr Roger Curtain 24. F. F. Lange: ‘Powder processing science and technology for
for their help with the SEM images of the raw powder. increased reliability’, J. Am. Ceram. Soc., 1989, 72, (1), 3–15.
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loidal processing of difficult-to-densify ceramics: suspension rheol-


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