Journal of Alloys and Compounds 602 (2014) 7277

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Journal of Alloys and Compounds

journal homepage: www.elsevier.com/locate/jalcom

Letter

Thermodynamic predictions for the manufacture of Ti2AlC MAX-phase

ceramic by combustion synthesis
T. Thomas , C.R. Bowen
Materials Research Centre, Department of Mechanical Engineering, University of Bath, Bath BA2 7AY, UK

a r t i c l e

i n f o

Article history:
Received 3 December 2012
Received in revised form 2 February 2014
Accepted 25 February 2014
Available online 6 March 2014
Keywords:
Ceramics
Combustion synthesis
Modelling
SHS

a b s t r a c t
This paper presents an analysis of the SHS reaction for the manufacture of Ti2AlC MAX phase materials
using self-propagating high-temperature synthesis (SHS). Enthalpy-temperature calculations are
presented for the reaction 2Ti + (1 + y)Al + C ? Ti2AlC + yAl. The analysis and data presented allows the
determination of the adiabatic combustion temperature as a function of a variety of conditions including
(i) reactant pre-heating to increase the combustion temperature or (ii) the addition of excess aluminium
as a diluent to reduce the combustion temperature. As excess Al is added as a diluent, there is a decrease
in Tad but it offers the potential to control the exothermicity of the SHS process and to form metal
ceramic composites. The range of criteria used for the determination of the appropriate combustion
K
K
=C 298
 2000 K, are shown to be applicable for
condition for SHS, such as Tad P 1800 K and DH298
r
p
Ti2AlC MAX phase ceramics. The data presented is of use to those considering the manufacture of novel
MAX phase ceramics by SHS.
2014 Elsevier B.V. All rights reserved.

1. Introduction
MAX-phases are a class of ceramics with the general molecular
formula Mn + 1AXn (n = 1, 2, or 3), where M is an early transition
element, A is an element from group 13 or 14 of the periodic table
such as Al, Ga, In, Ge, Sn, Pb and Si and X is either a nitride or carbide [1]. Depending on the value of n, M2AX, M3AX2 and M4AX3
phases are referred to 211, 312 and 413 phases respectively and recently MAX-phases with higher values of n such as 514 [2] and 615
[3] phases have been reported. These materials are inherently
nano-laminated ternary carbides or nitrides and there are currently approximately sixty known MAX phases [4]. Although Nowotny undertook their initial discovery and crystallographic analysis
in 1960s, they have only recently found major recognition. The
materials are of interest since they offer both metallic and ceramic
properties. For example their metallic characteristics are excellent
electrical and thermal conductivity; thermal shock resistance, good
machinability and they exhibit plasticity at elevated temperatures.
Their ceramic-like properties include oxidation resistance, a
refractory nature and their ability to maintain their strength at
high temperatures [5]. This intriguing combination of properties
has resulted in researchers exploring the technological importance
Corresponding author.
E-mail addresses: T.Thomas@bath.ac.uk (T. Thomas), c.r.bowen@bath.ac.uk (C.R.
Bowen).
http://dx.doi.org/10.1016/j.jallcom.2014.02.149
0925-8388/ 2014 Elsevier B.V. All rights reserved.

of these materials as a structural ceramic for high temperature

applications, in particular the ternary compounds such as Ti2AlC.
Wang and Zhouy [6] reported that for the TiAlC MAX-phase system the compounds Ti2AlC and Ti3AlC2 are considered to be the
most light-weight and oxidation resistant. These two materials
hold promising applications [1], especially at high temperatures.
Although these materials appear promising in their respective
applications the major disadvantage is the cost and energy associated with their manufacture, in particular the need for high temperature processing (sintering) and post-processing of the
sintered material to achieve the appropriate shape and dimension
[1]. One of the successful routes for preparing these materials is via
a combustion synthesis process, also known as self-propagating
high temperature synthesis (SHS) [7,8]. SHS is a processing technique, which uses a highly exothermic reaction to produce ceramic
materials. The technique begins by initiating an exothermic reaction in an area of a reactant mixture, e.g. with a resistively heated
tungsten wire. Once initiated, sufcient heat is released by the
reaction to become self-sustaining. This leads to the formation of
a combustion wave, which travels along the reactants, converting
them to the required products. Since the heating of the products
is achieved from the exothermic reaction, the process is thought
to be less time and energy consuming compared to the conventional sintering process [6].
In order to exploit the SHS process, it is important to
understand the thermodynamics involved in the reaction and the

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T. Thomas, C.R. Bowen / Journal of Alloys and Compounds 602 (2014) 7277

reaction mechanism that is favourable for the transformation of

the reactants into the desired products. The objective of this paper
is to provide a thermodynamic analysis of the SHS reaction to produce 211 MAX-phase Ti2AlC based ceramics, particularly in terms
of the adiabatic combustion temperature (Tad) and its dependency
on pre-heating and addition of diluents to control the reaction
temperature. The adiabatic combustion temperature is a measure
of the maximum temperature attained when the sample is processed using the SHS process, assuming no energy losses to the surroundings; although in reality some heat will always be lost. For
example, for the ZrB2 system the calculated Tad was 2235 K while
that experimentally measured was 1850 K [9]. Nevertheless, the
precise value of Tad is a measure of the exothermicity of the SHS
reactions and an indicator of whether SHS is possible. For example
it has been reported that a Tad P 1800 K is necessary for SHS reaction to be self-sustaining [10]. In addition to determining whether
SHS is feasible a detailed thermodynamic analysis allows the effect
of (i) pre-heating of the reactants or (ii) the addition of diluents
such as excess Al on the combustion temperature to be examined.
The reactions of the TiAlC system have been studied experimentally in detail by Hendaoui et al. [1115] where excess reactants
such as Al were used to reduce the combustion temperature and
pre-heating used to increase the combustion temperature.
However, while there has been experimental work to examine
the manufacture of Ti2AlC there has been no detailed thermodynamic analysis of the SHS reactions to date.
The thermodynamic study presented here is based on the exothermic reaction (Eq. (1)), using available data on Ti2AlC. Eq. (1) is
the basic reaction for the analysis to form the 211 MAX-phase
Ti2AlC by SHS,

2Ti 1 yAl C ! Ti2 AlC yAl

where y is the excess Al to act as a diluent to tailor the combustion

temperature.

2Ti Al C ! Ti2 AlC

The value of Tad is calculated by considering that the exothermic

enthalpy of the reaction is used to heat up the products with the
assumption of no loss of heat to the surrounding environment. It
is this self-heating makes the reaction self-sustaining, generating
a combustion wave which propagates through the entire reactants
converting it into desired products. This enthalpy, which is used in
the formation of products, can be related to the adiabatic combustion temperature (Tad) by the denition of the heat capacity of the
product Ti2AlC,

DH298

T ad

C p Ti2 AICdT

298

where DH298
is the enthalpy of the reaction and 298 K is the initial
r
temperature of the reactants in this case.
If there is any pre-heating of the reactants to Tstart prior to SHS
we must consider the additional energy supplied by initial heating
of the reactants, such that [19]:

Enthalpy of the reaction Energy supplied by pre-heating reactants

Energy to heat products

DH298

T start

C p 2Ti Al CdT

298

T ad

C p Ti2 AICdT

Often the heating of the reactants or products during SHS leads

to a variety of phase transitions, such as melting of the reactant or
products. These effects must also be considered; for example if the
sample is preheated to 660 C (933 K) and all the aluminium reactant melts the enthalpy of fusion of aluminium (DHm) is considered as in Eq. (6),

DH298

933

C p 2Ti Al CdT DHm Al

298

T ad

C p Ti2 AICdT

298

2. Adiabatic combustion temperature (Tad)

2.1. The conditions necessary for SHS

For a reaction to be self-propagating, Merzhanov [16] has
shown an empirical relation which states that the combustion
wave can be self-sustaining if Tad P 1800 K which also corresponds
K
K
to the condition DH298
=C 298
 2000 K [8]. Other relationships
r
p
can take into account the details of density and thermal conductivity [17] where it is claimed that their effect should be considered
when very high density or very high conductivity reactants are
used [18]. Bowen and Derby [17] derived a relationship based on
a nite-different modelling which has a sounder theoretical foundation compared to the purely empirical observations and stated
that SHS will occur if:

^ p reactants
T ad  T ig
C

T ig  T start C^ p products

298

where Tad is the adiabatic combustion temperature, Tig is the ignition temperature of the SHS reaction, Tstart in the initial temperature
p(reactants) is the
of the reactants (usually room temperature), C
p(products) is
average specic heat between Tstart and Tig, and C
the average specic heat between Tad and Tig [17]. It is of interest
to examine if these criteria are applicable to MAX phase reactions.
2.2. Methodology for calculating Tad
We initially consider a SHS between solid reactants of titanium,
aluminium and carbon to form Ti2AlC with no excess Al (i.e. the
condition y = 0 in Eq. (1)):

For Eq. (1) there may also be excess aluminium that does not
take part in the SHS reaction but decreases the combustion temperature due to an increase in the thermal mass of the system. Excess aluminium can be used in an attempt to create metalceramic
composites. This is also taken into account in a similar manner
such as in Eq. (7) where Tstart = 298 K,

DH298

T ad

C p Ti2 AIC yAldT

298

2.3. Material properties of Ti2AlC for calculating Tad

The thermodynamic analysis for the SHS reaction previously described is typically represented in the form of an enthalpy vs temperature curve [7]. Since MAX-phase materials are relatively new
there is limited data in terms of the enthalpy of formation and specic heat capacities as a function of temperature, which is one of
the reasons that thermodynamic analysis of these materials has
been limited to date. The available thermodynamic data in terms
of specic heat capacities of the reactants (Ti, Al and C) and products (Ti2AlC) and the enthalpy of fusion of the reactants are shown
in Tables 1-3. While data exist for the specic heat capacities of
Ti2AlC [2024] from both experimental measurements [20,23]
and rst principles calculations [21,22,24] with good agreement
between the values, there is limited data for the enthalpy of
formation. Duong et al. [21] have tabulated accurate thermochemical data of Ti2AX phases based on ab initio calculations and have
reported 64.59 kJ/mol-atom (258.36 kJ/mol) for the enthalpy
of formation of Ti2AlC at 298 K. This enthalpy of formation and
the data in Tables 1-3 were then used for the thermodynamic

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T. Thomas, C.R. Bowen / Journal of Alloys and Compounds 602 (2014) 7277

Table 1
Reactant specic heat capacities (Cp) with temperature, T (K), Cp = a + bT + cT2 + dT2 (J K1 mol1).
Element
Tia
Tib
Al(s)
Al(l)
C(s)

c
3

22.11
28.93
20.68
29.31
0.108

10.5  10

12.39  103

38.97  103

148.184  105

Accuracy (%)

Temperature range (K)

Reference

17.413  106

1.5
1
1
3
3

298t.p.
t.p.1350
298933
9331273
2982300

[29]
[29]
[29]
[29]
[10]

Table 2
Product specic heat capacities (Cp) with temperature, T (K), Cp = a + bT + cT2 + dT3 (J K1 mol1).
Compound
Ti2AlC

a
58.10

b
0.10

d
5

7  10

analysis. Ti2AlC has the potential for high temperature heating elements up to 1400 C in air (and higher in vacuum) [5] and it has
been reported to be able to withstand very high temperatures for
short times as long as the temperature does not exceed 3250 C
[25]. Pietzka et al. [26] reported that Ti2AlC melts incongruently
at 1625 C and Hashimoto et al. reported differential thermal analysis data of Ti2AlC formed via SHS which exhibited a melting point
at 1570 C [27]. Since no data on the enthalpies associated with the
observed phase changes have been presented, high temperature
differential thermal analysis (DTA) was undertaken using a Setsys
TG-DTA on Ti2AlC powder (Maxthal 211) using a palladium standard calibration. The results are similar to Hashimoto el al. [27]
in that melting was observed with a DTA peak maximum at
1552 C with an associated enthalpy of 29.6 kJ/mol; this was used
in the enthalpy-temperature curves.
3. Enthalpy-temperature curves for the TiAlC system
Fig. 1 shows the enthalpy-temperature curves, which plot the
enthalpy associated with heating the reactants and products. In
Fig. 1 the vertical line (A ? B) is the offset associated with the enthalpy of the reaction and represents the left hand side of the Eq.
(4). By creating a horizontal line (B ? C) to the enthalpy of the
products the Tad value can be found from the vertical line to x-axis
(C ? D), which represents the right hand side of the Eq. (4).
According to this data, from Fig. 1a in Eq. (1) the adiabatic combustion temperature is 2368 K. Combustion temperatures of
2Ti:1Al:1C molar mixtures have been determined experimentally
using thermocouples have been reported up to 20832110 K
[14,27]. The combustion temperature of 2083 K by Hashimoto
et al. [27] was for a packing density of the reactants of 50% and
XRD was used to conrm the major products as Ti2AlC with some
TiC. The difference between experimental and theoretical results
can be accounted for by heat losses, which are assumed negligible
in the adiabatic calculation and also any incomplete or side reactions producing other products [13]. Fig. 1b is the thermodynamic
predictions when excess Al is used i.e. y > 0 is added to Eq. (1)
where the predicted adiabatic combustion temperature decreases
to 2190 K when y = 0.3 and to 1868 K when y = 1. Clearly as excess
Al is added as a diluent, there is a decrease in the Tad but it offers
the potential to control the exothermicity of the SHS process and
to form metalceramic composites. Hendaoui et al. [12] conducted
a study on the effect of excess Al on Eq. (1) and indicated that excess Al brought in three important effects: (i) a shift of the conditions of the reaction between TiC and TiAl3 yielding more Ti2AlC
compound; (ii) enhancement in the component diffusion due to
the presence of more liquid phase resulting in easy ignition of
the reaction; (iii) dilution of the system and hence reducing the
overall exothermicity and more control over the reaction.

8

1.80  10

Temperature range (K)

Reference

3001600

[20]

If the reactants are preheated prior to SHS, this additional energy is present to increase the combustion temperature. For example if the reactants of reaction 1 are pre-heated to 940 K, the line
A0 B0 C0 D0 can be used to calculate the new adiabatic combustion
temperature as shown in Fig 1a; in this case the line A0 B0 corresponds the left hand side of Eq. (5) while the line C0 D0 corresponds
to the right hand side of Eq. (5). Fig. 2 summarises the change in
adiabatic combustion temperature with start temperature for Eq.
(3) with no excess Al.

4. Ti2AlC satisfying condition for SHS

As explained earlier it has been shown that it is possible to predict whether a reaction will be self-sustaining using the three conditions below,
(i) Tad P 1800 K [16].
K
K
(ii) DH298
=C 298
 2000 K [28].
r
p

(iii)

T ad T ig
T ig T start

^ p reactants
C
^ p products
C

[17].

The manufacture of Ti2AlC by SHS has been examined by

Hendaoui et al. [11,12] and the reaction is self-sustaining, therefore
it is possible to assess whether these three relationships hold true
for this particular MAX phase system.
From the thermodynamic analysis, the Tad is 2368 K (when
y = 0) and therefore satises condition (i). For condition (ii), since
1

DH298
258:36 kJ mol
r

1

and C 298
82:16 J mol
p

K1 (Table 2)

K
K
the ratio DH298
=C 298
3144 K and also exceeds 2000 K. Fig. 3
p
r
shows the relatively linear relationship between DHr(298)/
RCp(298) and Tad for a range of selected compounds in the SHS literature [7]. It is interesting to note that the MAX phase reactions
considered in this work also follow this relationship.
p(reacFor condition (iii), Tstart = 298 K, Tad = 2368 K (Fig. 1a), C
p(products) = 82.16 J mol1
tants) = 83.1 J mol1 K1 (Table 1) and C
K1 (Table 2). An ignition temperature (Tig) of 943 K, which is just
above the melting point of aluminium, was experimentally determined by heating well mixed and pressed powders with a molar ratio
of 2Ti:1Al:1C and measuring the ignition temperature using a type-K
thermocouple. Based on these conditions (TadTig)/(TigTstart) = 2.21
p(products)/C
p(reactants) = 1.01 and criterion (iii) therefore
and C
correctly predicts that the reaction should be self-sustaining. For
completeness, Fig 1a shows the predicted Tad based on an this ignition
temperature of 943 K (line A0 B0 C0 D0 ). These three relatively simple criteria for predicting SHS therefore work for this particular MAX phase
system and may also be applicable to the many other MAX phase
family.

T. Thomas, C.R. Bowen / Journal of Alloys and Compounds 602 (2014) 7277

75

Fig. 1. Enthalpy-temperature SHS analysis of (a) 2Ti + Al + C ? Ti2AlC and (b) 2Ti + (1 + y)Al + C ? Ti2AlC + yAl.

Fig. 2. Effect on Tad

2Ti + Al + C ? Ti2AlC.

with

different

starting

temperatures

for

reaction

Fig. 3. Relationship between DHr(298)/RCp(298) and Tad for selected compounds.

Compounds (s) are reported in [7]. Compounds (d) are the MAX phase reactions
examined in this work.

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T. Thomas, C.R. Bowen / Journal of Alloys and Compounds 602 (2014) 7277
5. Experimental procedure
To validate the potential to form Ti2AlC materials and Ti2AlCAl composites a
custom built SHS rig was used that consisted of silica tube lled with argon. In this
study we used commercial Ti powder (Goodfellow, 99%, 45 lm particle size), Al
powder (Goodfellow, 99%, 25 lm particle size) and carbon (mean diameter
3.55 lm and length 104.142 lm). The powders where mixed according to molar ratios 2Ti:1Al:1C (y = 0 in Eq. (1), Tad = 2368 K) and 2Ti:1.3Al:1C (y = 0.3 in Eq. (1),
Tad = 2190 K). The mixed powders were pressed into compact cylindrical pellets
of 13 mm diameter and 0.3 mm thick in a uniaxial press under a force of 6 tonnes
in an evacuable steel die of 13 mm diameter. The pressed powder compact was inserted into the combustion rig and ignited using a resistively heated V shaped
tungsten wire of 0.5 mm diameter by passing 30A electric current in argon atmosphere at atmospheric pressure. The phases formed where analysed using XRD
(Cu target, Ka) and the microstructure was observed under SEM (JEOL 6480LV)
equipped with Oxford instrumentation IMLA X-act, X-ray detector. Porosity was
determined by the Archimedes method.
Fig. 4. XRD phase formation of reaction Eq. (1) with y = 0 (2Ti:1Al:1C).

5.1. Experimental results

Fig. 5. XRD phase formation of reaction Eq. (1) with y = 0.3 (2Ti:1.3Al:1C).

Both reactions (y = 0 and y = 0.3) underwent self-sustaining SHS reactions, as

K
K
expected from Tad P 1800 K and DH298
=C 298
 2000 K (see Fig 3). The XRD
r
p
analysis for 2Ti:1Al:1C (y = 0) is shown in Fig. 4 where the majority of the peaks
comprise of Ti2AlC with minor peaks of TiC as the secondary phase; the formation
of some TiCx (0 6 x 6 1) in the reaction products has been observed previously [27].
Fig. 5 shows the XRD analysis for the ratio 2Ti:1.3Al:1C (y = 0.3) where the majority
of the peaks comprise of Ti2AlC with again minor peaks of TiC and excess Al as the
secondary phases; this indicates the production of metalceramic composites are
possible by using excess Al metal. The formation of Ti2AlC based ceramic with excess Al has also been studied by Hendaoui et al. [15] for the reaction 6TiO2 +
11Al + 3C ? 3Ti2AlC + 4Al2O3; excess Al could be used as a diluent and at higher
aluminium contents leads to the formation of Ti3AlC reaction products.
Fig. 6a shows the microstructure of the 2Ti: 1Al: 1C (y = 0) sample where the
sample has a porosity of 62%. Fig. 6(b) shows the microstructure of the 2Ti:1.3Al:1C
(y = 0.3) sample and EDX in Fig. 6(c). While the mixture with excess aluminium
(y = 0.3) has a similar morphology to the 2Ti:1Al:1C (y = 0) sample the grains are
more closely packed and more elongated with a higher porosity of 68%, possibly
due to more rapid diffusion as a result of the presence of excess liquid Al.

Fig. 6. (a) SEM of 2Ti:1Al:1C (y = 0) ceramic, (b) SEM of 2Ti:1.3Al:1C (y = 0.3) metalceramic and (c) EDX of 2Ti:1.3Al:1C (y = 0.3) over the selected area (inset, Spectrum1).

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T. Thomas, C.R. Bowen / Journal of Alloys and Compounds 602 (2014) 7277
Table 3
Enthalpy of formation (DHf), transformation (DHt) and fusion (DHm).
Element

DHf,298 (kJ/mol)

Ti

T(K), DHt (kJ/mol)

Melting point (K)

DHm (kJ/mol)

Reference

1155 K

1933

18.8 2

[29]

932

10.5 1

[29]

a?b
Al

3.47

6. Conclusions
In summary, this paper has provided the rst thermodynamic
predictions of the adiabatic combustion temperature of SHS reactions for the formation of Ti2AlC MAX phase materials. The analysis
and data presented allows the determination of the adiabatic combustion temperature as a function of a variety of conditions for
researchers manufacturing these materials by SHS including preheating of the reactants to increase the combustion temperature
and the addition of excess aluminium as diluent to reduce the
combustion temperature. As excess Al is added as a diluent, there
is a decrease in the Tad but it offers the potential to control the exothermicity of the SHS process and to form metalceramic composites; XRD conrms the presence of aluminium in samples with
excess Al (y = 0.3). The predicted adiabatic combustion temperature for the 2Ti:1Al:1C mixture of 2368 K is similar to reported
experimental measurements. The range of criteria used for the
determination of the appropriate combustion condition for SHS,
K
K
such as Tad P 1800 K and DH298
=C 298
 2000 K, are shown to
r
p
be applicable for Ti2AlC MAX phase ceramics and may therefore
be suitable for ease of assessment of other MAX phase systems.
The data presented is of use to those considering the manufacture
of novel Ti2AlC MAX phase ceramics or composites by selfpropagating high-temperature synthesis.

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