Colloidal processing of Al2O3 and BST materials
Colloidal processing of Al2O3 and BST materials
Emilia Pietrzak 0
Paulina Wiecinska 0
Emilia Pawlikowska 0
Mikolaj Szafran 0
0 Faculty of Chemistry, Warsaw University of Technology , Noakowskiego 3 Str., 00-664 Warsaw , Poland
The paper presents the analysis of thermal stability and decomposition of Al2O3 and (Ba,Sr)TiO3 green bodies as well as commercially available organic additives which are used in shaping of ceramics by colloidal processing. The first analyzed ceramic material was Al2O3 green body obtained by gelcasting. The second examined material was elastic ceramic-polymer composite based on ferroelectric powder Ba0.8Sr0.2TiO3 with NiO obtained by tape casting method. This flexible and durable material is characterized by high value of dielectric constant and finds the application in devices operating at very high frequencies up to sub-THz. Most organic additives are indispensable just in forming step but must be then eliminated in order to obtain pure ceramic phase, additionally some of them have to be stable in a wide temperature range. The analyzed organic substances were as follows: 2-carboxyethyl acrylate, SYNTRAN 8250, DURAMAX D-3005, DURAMAX B-1000. The DTA/TG measurements coupled with mass spectrometry allowed to gain new knowledge concerning degradation of selected organic additives, thermal stability of ceramic-polymer composite and type of gases released from samples during thermal treatment.
Ceramic-polymer composites; Thermal decomposition; Mass spectrometry
& Emilia Pietrzak
Nowadays, the innovative ceramics represent a diverse
group of materials which are increasingly used in
electronics, space industry, medicine, and as protection devices
[1–5]. One of the main stages in the preparation of ceramic
elements is forming process including an appropriate
selection of organic additives. Literature data concerning
shaping methods show that ceramic materials are recently
willingly fabricated by colloidal processes [6, 7]:
gelcasting , slip casting , tape casting [10, 11] mechanical
foaming , direct coagulation casting , dip coating
One of the attractive colloidal shaping methods is
gelcasting which combines traditional casting from slips with
polymer chemistry. Gelcasting consists in the organic
monomer polymerization reaction inside ceramic slurry. In
the process the macromolecular gel network, which results
from the in situ polymerization of organic monomers added
to the slurry, is created and holds ceramic particles in the
desired shape. Gelcasting has more advantages than ‘‘dry
methods.’’ This is due to the ability to control and influence
the processes which take place in ceramic slurry, mainly
the interactions between components in ceramic
suspensions. In colloidal processing, it is easier to eliminate some
unfavorable phenomena, like agglomeration of the particles
during milling, what significantly reduces the number of
structural defects and increases the homogeneity and
density of samples. The main advantage of gelcasting, in
comparison with other shaping methods, is high
mechanical strength of green bodies. It is caused by the creation of
strong polymeric network which holds ceramic particles
together [15, 16].
The next and the key stage during preparation of
ceramic materials is sintering process. The organic additives
used during the preparation of green bodies are
subsequently burned out during thermal treatment. The
conditions of sintering should be selected individually for each
type of the material what is possible thanks to DTA/TG
measurements. The important information from thermal
analysis is the temperature at which decomposition of
organics ends. Additionally, the coupling of DTA
apparatus with mass spectrometry allows to observe type of gases
released to the atmosphere during decomposition of any
The second shaping technique based on colloidal
processing is tape casting which is widely used in the
production of thin, flexible tapes. The homogenized slurry
passes beneath the knife’s edge (commonly referred to as a
doctor blade) which controls the thickness of the tapes. A
combination of an elastic polymer with a ceramic powder
having ferroelectric properties allows one to use this type
of composite in devices operating at very high frequencies
up to sub-terahertz . Barium strontium titanate (BST) is
a typical example of a ferroelectric material which is
applied in microwave technologies [26–28]. The described
in the paper ceramic–polymer composites are characterized
by suitable durability, flexibility, homogeneous surface,
and resistance to vibration, additionally they are
environmentally friendly. For this reason, these materials are
competitive in designing many different tunable devices
such as antennas, phase shifters and filters which can
operate at wide temperature range. Therefore, from the
application point of view another important parameter is
thermal stability of the composite which can be
investigated by DTA/TG measurements.
The aim of the research was the preparation of ceramic–
polymer composites based on BST and Al2O3 green bodies
by colloidal shaping of ceramics (gelcasting and tape
casting) and then to examine their behavior during thermal
treatment. Additionally, the thermal characteristics of
organic additives used in the shaping process was
performed, that is commercially available dispersing agents
SYNTRAN 8250 and DURAMAX D-3005, organic
monomer 2-carboxyethyl acrylate and polymeric binder
DURAMAX B-1000. The carried out research allowed to
gain new knowledge about thermal stability of these
materials and type of gaseous products released from the
Materials and experimental procedure
The first ceramic powder used in the research was a-Al2O3
A16SG (Almatis) of the average particle size
D50 = 0.5 lm, specific surface area of 7.5 m2 g-1 and
density of 3.90 g cm-3. As the organic monomer
commercially available 2-carboxyethyl acrylate (CEA,
Aldrich) was used, the role of the dispersing agent was
played by SYNTRAN 8250 (Interpolymer Company).
According to the information given by the supplier
SYNTRAN is a medium molecular weight aqueous solution
based on polyacrylic acid homopolymer and was used in
the form of 40% aqueous solution. Alumina green bodies
have been obtained by gelcasting method, according to the
procedure described elsewhere . The concentration of
Al2O3 powder was 50 vol%, while the concentrations of
SYNTRAN 8250 and CEA equaled 1.4 and 4.0 mass%,
respectively, regarding ceramic powder content.
The second used ceramic powder was Ba0.8Sr0.2TiO3
doped by NiO of the average particle size from 0.5 to
0.9 lm. Barium strontium titanate was prepared using
solid-state synthesis process at 1350 C for 2 h. The
materials used in the synthesis were: BaCO3, SrCO3, and
TiO2. The addition of NiO was 3 mol%. In the literature,
there is information about thermal characterization of BST
powder during sol–gel synthesis process . The results
show that in case of sol–gel-derived barium titanate there
exist several intermediate phases prior to the
transformation of the amorphous phase into the perovskite phase. On
the basis of thermal analysis, the temperature of calcination
was estimated at 850 C. Thermal analysis is therefore a
useful tool in the synthesis of ceramic powders. In this
work, authors have concentrated on the shaping process
using BST as the main component. The elastic ceramic–
polymer composite has been obtained by tape casting
method in which as a dispersing agent DURAMAX
D-3005 (DOW) and as a binder DURAMAX B-1000
(DOW) were used. DURAMAX D-3005 is the ammonium
salt of acrylic homopolymer and was supplied as a 35%
aqueous solution. DURAMAX B-1000 is an aqueous
emulsion (55%) used for enhancing green strength and
improving flexibility of ceramic parts. The concentration of
BST powder was 50 vol%, while the concentrations of
DURAMAX D-3005 and DURAMAX B-1000 equaled 1.5
and 15 mass%, respectively, regarding ceramic powder
content. The thin sample was prepared using
MSK-AFAIII-Automatic Thick Film Coater (MTI Corporation). The
thickness of the composite tape was 180 lm. The aim of
the DTA/TG measurements was to estimate thermal
stability of obtained BST tape.
DTA/TG measurements were carried out by using
Netzsch Jupiter STA 449C coupled with the mass spectrometer
Netzsch QMS 403C Aeolos. The quantities of polymeric
samples taken to measurements equaled from 0.01 to
0.15 g (depending on the sample density and molecular
weight). They have been covered by calcinated
(non-reactive) Al2O3 powder in the quantity of 0.3 g in order to
prevent the polymer creeping from the crucible. The mass
of Al2O3 sample was 0.3308 g, while the mass of BST
sample was 0.1929 g. The heating rate was 5 C min-1
and the final temperature was 1000 C. The measurements
were performed in the constant flow of two gases: argon—
10 mL min-1 (protective gas) and synthetic air (75:25
N2:O2)—60 mL min-1. Mass spectrometer was set to
detect m/z values in mass range 10–300.
Results and discussion
Two types of materials have been obtained. The first one
was BST ceramic–polymer composite (Fig. 1a). It is a
highly elastic sample due to the application of DURAMAX
B-1000 as a binder. The second material was Al2O3 green
body (Fig. 1b) made by gelcasting technique. Al2O3 green
samples exhibit high mechanical strength (ca. 3.77 MPa)
as has been wider described in previous work .
DTA/TG/DTG curves of thermal degradation of
polymer based on 2-carboxyethyl acrylate (shown in Fig. 2a),
indicate that the total mass loss was 93%, what means that
almost all of organic phase has decomposed. Polymer
decomposition goes in two main stages according to TG
curve. It begins at ca. 173 C and ends at ca. 585 C. The
endothermic peak on DTA curve with the minimum at
220 C and the exothermic peak with the maxima at 396,
487, and 550 C are visible. The main m/z values detected
by mass spectrometer were 17 and 18 which can be
ascribed to OH- and H2O molecules (Fig. 2b). This is
therefore the main gaseous product released from the
polymeric sample. The presence of CO2 is confirmed by m/
z values 12 and 44. There is the increase in the intensities
of MS 44 and 12 signals with the maxima at 240 and
550 C what indicates on the decomposition of polymeric
binder and oxidation of decomposition products (light
hydrocarbons) to CO2. The stepped mass loss and the
presence of a few maxima on MS curves indicate that
Fig. 1 Ceramic–polymer composite based on Ba0.8Sr0.2TiO3 with
NiO obtained by tape casting (a) and Al2O3 green body obtained by
thermal decomposition of the polymeric chain proceeds
gradually. The MS signals 22, 24, 42, 45, 46, 55, 72 are
observed with the maxima at 223 and 556 C which can be
ascribed to the first stage of thermal decomposition of the
polymer (Fig. 2c). It must be underlined that the intensities
of these signals are very low in comparison with signals 18
and 44. The major decomposition products come from
main-chain scission, giving shorter polymeric chains (C1–
C5 carbohydrates) like oligomers, trimers, dimers, and
monomers [29, 30]. MS 45 peak of high intensity may
indicate the carboxylic acid, ethoxy group, ethers, and
alcohol groups, which correspond to the polymer structure
[31, 32]. The presence of the m/z value 44 is observed till
ca. 600 C which means that mentioned above organic
groups undergo further oxidation toward CO2.
Thermal degradation of SYNTRAN 8250, used as
dispersing agent for alumina powder, is presented in Fig. 3a.
The total mass loss was 98% what means that all of organic
phase was decomposed. Mass loss starts at 133 C and is
observed until ca. 595 C. The exothermic peak on DTA
curve with maximum at 569 C is visible. This peak
overlaps with the peaks from mass spectrometer of m/
z values 44, 22, 45, and 46 of the maximum at about
542 C. The presence of masses 12 and 44 indicates the
decomposition of the compound toward CO2. The highest
intensities of MS signals 17 and 18 are observed in
temperature range 200–590 C which can be ascribed to H2O
as one of the main products of SYNTRAN degradation
(Fig. 3b). Mass spectrometer has detected also the
following masses 24, 48, 60, and 64 with a maximum at
297 C, 42 with a maximum at 432 C and 22, 45, and 46
with a maximum at 546 C. It can be therefore conducted
that thermal decomposition of the polyacrylic acid
homopolymer proceeds toward light hydrocarbons and
followed by an oxidation of these products to CO2
(Fig. 3c). The decomposition products which come from
main-chain scission, giving shorter hydrocarbons (C1–C5),
are released in much smaller quantities in comparison with
CO2 and H2O.
Comparing the thermal characteristics of polymer based
on 2-carboxyethyl acrylate (Fig. 2) and SYNTRAN 8250
(Fig. 3), it can be concluded that the main stage of CEA
polymer decomposition appears at lower temperatures (ca.
251 C) than of SYNTRAN (ca. 504 C). As a result, gases
are released from the SYNTRAN sample at higher
The DTA/TG/DTG curves of thermal degradation of
Al2O3 green body obtained by gelcasting with the use of
the processing additives CEA and SYNTRAN 8250 are
shown in Fig. 4a. The total mass loss was 5.55% which
corresponds to the organic additives content in the
analyzed sample. It means that all of the organic phase was
burned out, as expected. Mass loss is observed until ca.
514 C. Decomposition of organics goes in two stages
according to TG curve. The endothermic peak on DTA
curve with the minimum at 211 C and the exothermic
peak with the maximum at 385 C are visible (Fig. 4b).
The endothermic peak overlaps with the peaks from the
mass spectrometer of m/z values 17 and 18 which can be
ascribed to H2O, what indicates on dehydration process.
The presence of CO2 is confirmed by m/z values 12 and 44.
There is the increase in the intensities of MS 44 and 12
signals with the maximum at 375 C, what indicates on the
decomposition of the dispersing agent SYNTRAN and
polymeric binder based on CEA toward light
hydrocarbons, oligomers, trimers, dimmers followed by oxidation to
CO2. The MS signals (22, 24, 42, 45, 46, 55, 72) detected
during thermal treatment of Al2O3 green body (Fig. 4c)
correspond to MS signals for analyzed polymer based on
CEA and dispersant SYNTRAN. However, the MS peaks
are much wider than in case of individual additives what
means that in case of ceramic sample gases are released
from the sample in a wide temperature range
The information gained from the above measurements is
essential for suitable selection of sintering conditions of
Al2O3 like sintering temperature and heating rate. It is very
important because decomposition is connected with the
release of high quantities of gases which may cause defects
in the sample, and therefore it is preferable to conduct the
sintering process with low heating rate, for example,
1 C min-1 till the end of the organics decomposition.
Sintering is the key step in the dense ceramic preparation
process which should provide to obtain a high-quality
In the second part of the research, the ceramic–polymer
tape based on BST and organic components were analyzed.
The DTA/TG/DTG curves of thermal degradation of an
ammonium salt of acrylic homopolymer in water
(DURAMAX D-3005) which was used as dispersing agent for
BST powder, are shown in Fig. 5a. The total mass loss was
98% what indicates that the whole DURAMAX D-3005
has decomposed. Mass loss starts at 362 C and is observed
until ca. 544 C what means that DURAMAX D-3005 is
much more thermally stable substance than SYNTRAN
8250 or polymer based on CEA. In case of BST ceramic–
polymer composites it is very useful advantage. Two main
stages of dispersant degradation are observed; nevertheless,
88% of mass loss is visible in the first stage till 397 C.
This first stage is connected with DTA exothermic peak
with the maxima at 325 and 437 C. The highest intensities
of MS signals (of m/z values 12, 17, 18 and 44) are
observed at temperature 386 C (Fig. 5b). This can
indicate partial decomposition of the compound toward H2O
and CO2. The MS signals 22, 25, 42, 45, 55, 56 are
observed at 373 C which can be ascribed to thermal
decomposition of the acrylic homopolymer toward CO2
(Fig. 5c). The main difference between DURAMAX
D-3005 and the rest of the analyzed additives is that the
decomposition of DURAMAX D-3005 proceeds rapidly, in
the temperature range 363–397 C, 88% of the substance is
DTA/TG/DTG curves of thermal degradation of an
aqueous emulsion DURAMAX B-1000 used as a binder in
the preparation of BST samples by tape casting, are shown
in Fig. 6a. The total mass loss was 68% what could
indicate that not whole DURAMAX B-1000 has decomposed;
nevertheless, the mass loss is observed since the very
beginning of the measurement, what can be ascribed to the
sample volatility. The decomposition of DURAMAX
B-1000 ends at ca. 498 C which is 46 C lower than in
case of DURAMAX D-3005. Three stages of dispersant
degradation are observed. The first stage till 102 C is
connected with the DTA endothermic peak at temperature
87 C. The second and the third stages are connected with
DTA exothermic peaks with the maxima at 430 and
670 C. The first peak on MS curve of m/z values 17 and 18
is observed at temperature 53 C (Fig. 6b). This can
indicate dehydration process, but on the other hand confirms
the hypothesis concerning high volatility of the sample.
Mass spectrometer has detected also m/z values 12 and 44
having the highest intensities at 415 C. The other MS
signals 22, 42, 45, 55, and 56 are observed at 357 C. Thus
the situation is similar as in case of previous organic
compounds, that is decomposition proceeds toward light
carbohydrates which are then oxidized to CO2. The second
main oxidation product is H2O. It is worth to underline that
in case of DURAMAX B-1000 mass spectrometer has
detected the smallest number of masses which means that
thermal degradation proceeds with the release of smaller
types of gaseous product (Fig. 6c).
DTA/TG/DTG curves of thermal degradation of the
ceramic–polymer tape based on BST are shown in Fig. 7a.
The total mass loss was 10% what corresponds to the
content of the organic phase in the composite.
Nevertheless, the concentration of dispersant and binder in a slurry
was a little higher than the value of the total mass loss. It
results from the fact that the mass of the sample taken to
the analysis was ca. 0.3 g according to the capacity of the
crucibles . Mass loss starts at ca. 241 C and is
observed until ca. 448 C. Tape decomposition goes in few
stages according to TG curve. Three peaks are visible on
DTA curve with maxima at 250, 383 and 410 C.
According to the information from mass spectrometer
(Fig. 7b), course of curves of m/z values 17 and 18 is
similar what indicates that they correspond to H2O. The
presence of CO2 is confirmed by m/z values 12 and 44.
There is the increase in the intensities of MS 44 and 12
signals with the maximum at 383 C, which overlap with
exothermic peak on DTA at 383 C and indicates on the
decomposition of organic phase toward CO2. The MS
signals 22, 42, 45, 55, and 56 are observed at 342 C
(Fig. 7c) which can be ascribed to thermal decomposition
of organic phase toward CO2. The most important
information gained from this measurement is that the BST tape
with the addition of the polymeric phase is thermally
stable till 241 C what is very beneficial from the
application point of view. The BST tapes do not undergo the
sintering process, because they are used as elastic ceramic–
polymer materials exhibiting ferroelectric properties.
Based on the literature review one can find thermal analysis
of raw BST powder, but there was as yet no information
about thermal stability of BST composites .
The microstructure of green body based on Al2O3 and
ceramic–polymer composite based on BST is shown in Fig. 8.
In SEM image of Al2O3 green body one can observe the
polymer in the form of bridges which connect alumina particles
(Fig. 8a). These polymeric bridges are responsible for high
mechanical strength of Al2O3 sample before sintering. The
particles in green body are highly densified. In BST composite
a polymeric binder surrounds particles like a glue (Fig. 8b),
what is responsible for elasticity of this composite tape. On the
basis on SEM image, it can be estimated that the particles size
was in the range of 0.3–1.2 lm. The polymeric phase visible in
SEM images corresponds to the total mass loss estimated on the
basis of TG curves of Al2O3 and BST samples.
Thermogravimetry coupled with mass spectrometry is a
very useful tool to characterize the decomposition process
of organic compounds as well as ceramic green bodies
containing polymeric phase. Decomposition of the
analyzed organics such as polymer based on 2-carboxyethyl
acrylate or commercially available additives: SYNTRAN
8250, DURAMAX D-3005, and DURAMAX B-1000
proceeds toward light hydrocarbons with further oxidation
to CO2. Rapid and fast degradation was observed for
DURAMAX D-3005 which exhibited the highest thermal
stability. In case of Al2O3 green body obtained by
gelcasting, decomposition of organic additives ends at 514 C,
which is the important information in determination of the
sintering program. BST tape is thermally stable till 241 C
which is very beneficial from the application point of view,
because Ba0.8Sr0.2TiO3 together with the applied polymer
exhibits ferroelectric properties and is used in a form of
ceramic–polymer composite material.
Acknowledgements The project has been financially supported by
National Science Centre, Poland (Agreement No. UMO-2014/15/D/
ST5/02574). Authors would like to thank Interpolymer Company for
free sample of SYNTRAN 8250, DOW for free samples of
DURAMAX D-3005 and DURAMAX B-1000 and Almatis GmbH for free
sample of Al2O3 A16SG which were used in the research.
Open Access This article is distributed under the terms of the Creative
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credit to the original author(s) and the source, provide a link to the
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1. Li J , Hastings GW . Oxide bioceramics: inert ceramic materials in medicine and dentistry . In: Murphy W, Black J , Hastings G, editors. Handbook of biomaterial properties . New York : Springer; 2016 . p 339 - 352 .
2. Ying S , Fuping W , Yu Z . Progresses of research on microwave dielectric ceramics . 1998 ; 02 .
3. Hvizdos P , Puchy V , Duszova A , Dusza J , Balazsi C. Tribological and electrical properties of ceramic matrix composites with carbon nanotubes . Ceram Int . 2012 ; 38 : 5669 - 76 .
4. Kovalcikova A , Balazsi C , Dusza J , Tapaszto O. Mechanical properties and electrical conductivity in a carbon nanotube reinforced silicon nitride composite . Ceram Int . 2012 ; 38 : 527 - 33 .
5. Antosik A , Gluszek M , Zurowski R , Szafran M. Effect of SiO2 particle size and length of poly(propylene glycol) chain on rheological properties of shear thickening fluids . Arch Metall Mater . 2016 ; 61 : 1165 - 8 .
6. Tallon C , Franks GV . Recent trends in shape forming from colloidal processing: a review . J Ceram Soc Jpn . 2011 ; 119 : 147 - 60 .
7. Nieto MI , Suarez I , Moreno R. Shaping of dense advanced ceramics and coatings by gelation of polysaccharides . Adv Eng Mater . 2014 ; 16 : 637 - 54 .
8. Pietrzak E , Wiecinska P , Szafran M. 2-carboxyethyl acrylate as a new monomer preventing negative effect of oxygen inhibition in gelcasting of alumina . Ceram Int . 2016 ; 42 : 13682 - 8 .
9. Burgos-Montes O , Moreno R , Baud´ın C. Effect of mullite additions on the fracture mode of alumina . J Eur Ceram Soc . 2010 ; 30 : 857 - 63 .
10. Wiecinska P , Graule T , Bachonko M. Organic additives in geltape casting of ceramic powders-a novel approach to the problem of elasticity and cracking of thin tapes . J Eur Ceram Soc . 2015 ; 35 : 3949 - 57 .
11. Fan K , Ruiz-Hervias J , Gurauskis J , Sanchez-Herencia AJ , Baud´ın C. Neutron diffraction residual stress analysis of Al2O3/ Y-TZP ceramic composites . Bolet´ın de la Sociedad Espan˜ola de Cera´mica y Vidrio . 2016 ; 55 : 13 - 23 .
12. Takahashi M , Menchavez RL , Fuji M , Takegami H. Opportunities of porous ceramics fabricated by gelcasting in mitigating environmental issues . J Eur Ceram Soc . 2009 ; 29 : 823 - 8 .
13. Si W , Graule T , Baader F. Direct coagulation casting of silicon carbide components . J Am Ceram Soc . 1999 ; 82 : 1129 .
14. Schabikowski M , Zalewska M , Kata D , Graule T. The effect of CuO coatings on the electrokinetic properties of stone wool fibres determined by streaming potential measurements . Ceram Int . 2016 ; 42 : 13944 - 51 .
15. Bednarek P , Szafran M , Sakka Y , Mizerski T. Gelcasting of alumina with a new monomer synthesized from glucose . J Eur Ceram Soc . 2010 ; 30 : 1795 - 801 .
16. Szudarska A , Sakka Y , Suzuki TS , Mizerski T , Szafran M. Magnetic field alignment in highly concentrated suspensions for gelcasting process . Ceram Int . 2016 ; 42 : 294 .
17. Wiecinska P. Thermal degradation of organic additives used in colloidal shaping of ceramics investigated by the coupled DTA/TG/MS analysis . J Therm Anal Calorim . 2016 ; 123 : 1419 - 30 .
18. Bednarek P , Szafran M. Thermal decomposition of monosaccharides derivatives applied in ceramic gelcasting process investigated by the coupled DTA/TG/MS analysis . J Therm Anal Calorim . 2012 ; 109 : 773 - 82 .
19. Leszczynska A , Pielichowski K. Application of thermal analysis methods for characterization of polymer/montmorillonite nanocomposites . J Therm Anal Calorim . 2008 ; 93 : 677 - 87 .
20. Sczygiel I , Winiarska K. Synthesis and characterization of manganese-zinc ferrite obtained by thermal decomposition from organic precursors . J Therm Anal Calorim . 2014 ; 115 : 471 - 7 .
21. Golofit T , Zysk K. Thermal decomposition properties and compatibility of CL-20 with binders HTPB, PBAN, GAP and polyNIMMO . J Therm Anal Calorim . 2015 ; 119 : 1931 - 9 .
22. Thom AJ , Summers E , Akinc M. Oxidation behavior of extruded Mo5Si3Bx-MoSi2-MoB intermetallics from 600 to 1600 C. Intermetallics. 2002 ; 10 : 555 - 70 .
23. Etienne S , Becker C , Ruch D , Germain A , Calberg C. Synergetic effect of poly(vinyl butyral) and calcium carbonate on thermal stability of poly(vinyl chloride) nanocomposites investigated by TG-FTIR-MS . J Therm Anal Calorim . 2010 ; 100 : 667 - 77 .
24. Alcolea A , Ibarra I , Caparros A , Rodriguez R. Study of the MS response by TG-MS in an acid mine drainage efflorescence . J Therm Anal Calorim . 2010 ; 101 : 1161 - 5 .
25. Pietrzak E , Pawlikowska E , Godziszewski K , Yashchyshyn Y , Szafran M. Tunable ceramic-polymer composites for electronic applications . Compos Theory Pract . 2015 ; 1 : 54 - 7 .
26. Balachandran R , Ong BH , Wong HY , Tan KB , Muhamad Rasat M. Dielectric characteristics of barium strontium titanate based metal insulator metal capacitor for dynamic random access memory cell . Int J Electrochem Sci . 2012 ; 7 : 11895 - 903 .
27. Osinska K , Czekaj D. Thermal behavior of BST//PVDF ceramicpolymer composites . J Therm Anal Calorim . 2013 ; 113 : 69 - 76 .
28. Hu T , Juuti J , Jantunen H , Vilkman T. Dielectric properties of BST/polymer composite . J Eur Ceram Soc . 2007 ; 27 : 3997 - 4001 .
29. Bertini F , Audisio G , Zuev V. Investigation on thermal degradation of poly-n-alkyl acrylates and poly-n-alkyl methacrylates (C1-C12) . Polym Degrad Stab . 2005 ; 89 : 233 - 9 .
30. Zuev VV , Bertini F , Audisio G. Investigation on the thermal degradation of acrylic polymers with fluorinated side-chains . Polym Degrad Stab . 2006 ; 91 : 512 - 6 .
31. Database of Mass Spectroscopy of Royal Society of Chemistry . www.rsc.org.
32. Database of Mass Spectroscopy of Kaye&Laby, National Physical Laboratory. www.kayelaby.npl.co.uk.