A review on current trends in thermal analysis and hyphenated techniques in the investigation of physical, mechanical and chemical properties of nanomaterials

A review on current trends in thermal analysis and hyphenated techniques in the investigation of physical, mechanical and chemical properties of nanomaterials

Journal of Analytical and Applied Pyrolysis 149 (2020) 104840 Contents lists available at ScienceDirect Journal of Analytical and Applied Pyrolysis ...

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Journal of Analytical and Applied Pyrolysis 149 (2020) 104840

Contents lists available at ScienceDirect

Journal of Analytical and Applied Pyrolysis journal homepage: www.elsevier.com/locate/jaap

A review on current trends in thermal analysis and hyphenated techniques in the investigation of physical, mechanical and chemical properties of nanomaterials


Hooman Seifia, Tahereh Gholamib, Soodabe Seific, Sayed Mehdi Ghoreishia,*, Masoud Salavati-Niasarib,* a b c

Department of Analytical Chemistry, Faculty of Chemistry, University of Kashan, Kashan, Iran Institute of Nano Science and Nano Technology, University of Kashan, P.O. Box 87317–51167, Kashan, Iran Department of Chemical Industries, Faculty of Girl’s Technical, Kermanshah Branch, Technical and Vocational University (TVU), Kermanshah, Iran



Keywords: Thermal analysis Nanomaterials Thermogravimetric analysis Hyphenated system Differential thermal analysis Differential scanning calorimetry

The applications of nanomaterials have been a multidisciplinary active research area in recent years because of their unique structure, surface chemistry, chemical and physical properties. Moreover, further research on the physical, mechanical and chemical properties of nanomaterials is as vital as synthesis. Thermal analysis (TA) methods are used in a wide range of areas, including quantitative and qualitative analysis, the characterization of mechanical, chemical and physical properties of nanomaterials, and to obtain further insight into their structure. This review illustrates the applications of TA techniques in nanomaterials research in the past decade (2010–2020). The highlighted studies bring valuable insight into the evidence of the ability of TA techniques to investigate the physical and chemical properties of the nanomaterials.

1. Introduction Nanomaterials are the materials that have sizes on the order of a billionth of a meter. Since the mechanical, thermal, electrical, optical, electrochemical, catalytic properties of the nanomaterials are different from the bulk materials, nanomaterials can be used in a wide variety of application fields. Some of these applications are batteries with high energy density, pollutants removal, powerful magnets, sensitive sensors, fuel efficiencies automobiles with greater, more excellent weapons platforms, satellites with longer-lasting, better insulation materials, next-generation computer chips, food additives, agricultural production, food processing, animal feed, biomedical, high-frequency, machinable ceramics, large electrochromic display devices [1–7]. Nanomaterials' thermal futures are depending on several factors that are generally insignificant in bulk materials. Thermal conductivity, specific heat, melting point and glass-transition temperature are just a few examples of thermal features that strictly depend on the feature size

or particle size of materials (the main difference between bulk and nanomaterial). The phase diagrams of nanomaterials are dependent upon the particle size and their shape. A melting point is one of the vital thermodynamic properties of all materials. It is well confirmed both theoretically and experimentally that the Tm of nanoparticles depends on the particle size. The high ratio of surface to volume of nanoparticles leads to the excessive influence of surface atoms on physical and chemical properties. Nanoparticles with diverse sizes have different Tm which states in the phenomenon of Tm reduction of particles in small dimensions. This phenomenon is fascinating in nanoscale particles; for instance, the reduction in Tm of metals with nanometer dimensions can be on the order of tens to hundreds of Kelvin degrees. The Gibbs-Thomson equation (so-called equilibrium melting point) describes the size dependence of the (melting) temperature at a fixed pressure. The Gibbs-Thomson equation state the condition for the unstable equilibrium between the solid particle and the melt, and so denotes the melting transformation pathway. The

Abbreviations: TA, thermal analysis; TGA, thermogravimetric analysis; DSC, differential scanning calorimetry; EGA, evolved gas analysis; TMA, thermomechanical analysis; DMA, dynamic mechanical analysis; DTA, differential thermal analysis; TGA-GC, thermogravimetric analysis joined with gas chromatography; TGA-GC–MS, thermogravimetric analysis coupled with gas chromatography and mass spectroscopy; TGA-FTIR, thermogravimetric analysis -Fourier transform infra-red spectrometry; TGA-FTIR-MS, thermogravimetric analysis joined with Fourier transform infrared spectrometry and mass spectroscopy; Tg, glass transition temperature; Tm, melting point temperature; Tc, crystallization temperatures ⁎ Corresponding authors. E-mail addresses: [email protected] (S.M. Ghoreishi), [email protected] (M. Salavati-Niasari). https://doi.org/10.1016/j.jaap.2020.104840 Received 18 March 2020; Received in revised form 29 April 2020; Accepted 4 May 2020 Available online 07 May 2020 0165-2370/ © 2020 Elsevier B.V. All rights reserved.

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Thermal conductivity is an important property of nanomaterial, which directly influence its application. Nanomaterials possess low thermal conductivity because of their interatomic bonding and intrinsic atomic structure (includes those doped to create point defect scattering and nano-grain sized materials). According to published papers, the relationship between the thermal conductivity of nanomaterials (for example nanofilm) and their particle size is as follows [13,14]:

k p = kb 1

depression of the melting point with respect to the inverse of the particle radius is related to the Gibbs–Thomson effect [8]:

2 sl Tm r H s




Where the d and are the nanosolid diameter and height of the nanofilm, respectively. One can see that thermal conductivity decreases as the diameter reduces, therefore, the thermal conductivity of nanomaterials is less than bulk material. According to published papers, the surface and grain boundary effects influenced the thermal conductivity of the Sn nano-size so that is greatly lower than that of the Sn bulk (Fig. 1b). A similar tendency was detected for the heat conductivity of aligned carbon nanotube forests [15]. Another exciting hybrid system is covalently bonded parallel graphene sheets join to carbon nanotube pillars each other. By changing the geometry of this exclusive system, i.e., the separation and length of the pillars, one can tune for different lateral and vertical thermal conductivities (Fig. 1c) [16]. Today, the appropriate characterization of nanomaterials is a very fascinating field. Researchers and scientist claim that insurable characterization of nanomaterial restrict the validity and reliability of obtained results from scientific investigations that could limit both commercialization and future investigation of nanotechnology [13–15]. Several thermal analysis (TA) techniques can be utilized to inspect the required special properties of the nanomaterials. TA techniques are a subdivision of materials science that investigate the properties of the material which change as a function of temperature [17,18]. Several approaches are generally employed (distinguished by the measured property) such as thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), evolved gas analysis (EGA), differential thermal analysis (DTA), dynamic mechanical analysis (DMA), thermomechanical analysis (TMA). DSC, TGA, TMA, DTA, EGA and DMA are the most common techniques of thermal analysis that can be used to investigate the properties of the nanomaterials as a function of temperature or time in a large range of temperatures. Today, these common techniques have been hyphenated with various techniques that lead to release better characterization of nanomaterial. In Table 1, one can see that several techniques have been commonly used for the evaluation of nanomaterial in the last decade. As mentioned above, thermal analysis methods have many applications in the investigation of the nanomaterials, in which each of them investigated specific properties of nanomaterials. In this comprehensive review, the applicability and capability of each of these methods in various areas are reviewed which is a comprehensive guide for future studies. Consequently, scientists can select suitable and efficient

Fig. 1. Relationship between melting point with the particle diameter (a) grain size dependent thermal conductivity of Sn (spherical nanosolids, nanowires and nanofilms) (b) change of thermal conductivities by varying the geometry (c).

Tm =

2d 3h

Table 1 Common thermal analysis techniques used for the evaluation of nanomaterial.


Where Tm is the melting point depression, Tm is the bulk system melting point, s is the solid phase number density, r is the nanoparticle radius, H is the melting latent heat and, sl is the solid-liquid interfacial energy. Melting of a small (nanoscale) particle with a surface liquid layer is attended by an energy reduction because of the decrease in the interfacial area between the melt and the solid, and an energy increase because of the creation of the thermodynamically less stable phase. The Gibbs-Thomson models revealed that the difference in the behavior of nano-systems compared to macro-systems is because of their high specific surface area [9,10]. As an example, for spherical Au particles, it found that the melting point difference has an inverse relation with the particle diameter (Fig. 1a) [11,12]. 2

Main measured property


Accepted acronym

Common hyphenated technique

Change of mass



Heat flux


Change of temperature Volatiles

Differential scanning calorimetry Differential thermal analysis Evolved gas analysis

Mechanical properties

Thermomechanical analysis



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techniques from thermal analysis methods to meet their goals in nanomaterials investigation. 2. Applications 2.1. TGA TGA is a commonly used technique to provide insight into mass changes through the desired temperature range that allows specific determinations. By monitoring the weight of a sample within a furnace, thermal effects that cause a weight change can be recognized and investigated. This is perfect for the thermal analysis of a decomposition temperature of nanomaterial, adsorption and desorption, thermal stability, combustion, and dehydration. In this method, the material weight loss from volatile components formation under degradation due to temperature rising and heating is monitored [19,20]. 2.1.1. Investigation effects of the additive modification on nanomaterial Nanotechnology is one of the most important fields in almost all modern society, targeting efficient and high-quality market potential. The most attention in the range of nano-scale is nano-additives have improved properties related to its bulk material. The unique advantages of nano-additives are anticipated to change the edges of controlled technology. The main nanotechnology target is to change material to acquire special functionalities. The developments based on nanotechnology deliver evolutionary and incremental changes and are a novel means that are currently added to a wide range of applications [21,22]. Recently, scientists focused on the developments in thermal stabilization of nanostructured to using these materials in a wide verity of applications. According to the polished papers, one can see that attention has currently shifted from utilizing the regular solution approximation to assessing thermal possessions of nanomaterials by considering both grain boundaries and their inner regions of nanograins [23,24]. In one aspect of the application of TGA techniques, the modification effects of additive (such as MWCNT, clay, montmorillonite, vinyl acetate, etc.) on the flammability and thermal properties of polymer (such as polyimide, PET, etc.) nanocomposites were investigated by TGA in air and nitrogen atmosphere. TGA results exhibited that the additive addition lead to a considerable change of the thermal stability, flame retardancy property, and nanocomposites char yields associated with those of the neat polymers [25–38]. As an example, Chen and coworkers [39] investigated the amount influence of MQ silicone resin loading on the thermal stability of the polydimethylsiloxane (PDMS) composites by TGA in N2 atmosphere (Fig. 2). Their results showed that the SMQ-0 sample (composites of PDMS without MQ silicone resin) have the higher temperature of decomposition than those of all the composites of PDMS with MQ silicone resin (from SMQ-I to SMQ-IV) after they missing the equal weight percent of their initial mass; thus, these results indicated that adding MQ silicone resin is unfavorable to enhance the thermal degradation resistance of the PDMS composites.

Fig. 2. Thermal degradation of PDMS composites [39].

Fig. 3. TGA curves of specimens containing different amount of nPOFA [53].

Besides, a mechanism of nPOFA hydration was suggested based on TGA results. The products of hydration involving cement paste are principal Ca(OH)2 and C-S-H; it is problematic to accomplish an exact quantitative analysis for C-S-H since the C-S-H dehydration of is not easy to originate because of its amorphous features, while it is not for Ca(OH)2. Wi and coworkers used this assumed that Ca(OH)2 is consumed by a reaction of pozzolanic and the total SiO2, reacted with Ca(OH)2, increases with more content of nPOFA, consequently via the growth in the C-S-H amount. TGA results confirmed that SiO2 and Ca(OH)2 consumed through reactions of pozzolanic and C-S-H was formed. 2.1.3. TGA-MS and TGA-GC–MS The ability of hyphenated systems allowing the qualitative and quantitative analysis of evolved species, such as TGA-GC, TGA-MS and TGA-GC–MS, that further improved the TGA. GC is a performance technique for separating volatile and semivolatile compounds. The mixture gases are separated according to the differences in constituent distribution between a mobile and stationary phase [54,55]. Since the separation of gas in the column of GC is timeconsuming, it is not suitable to directly couple with a continuous online gas flow of sample as the TGA method. Therefore, several companies developed a direct coupling in a quasi-continuous approach by applying heated automatic valves that permit for software-controlled gas

2.1.2. Investigation of composition and purity of nanomaterial The composition and purity of nanomaterial are two of the most imperative factors to consider previous to arranging nanomaterials in other fields. TGA is a rapid method for characterization purity and composition of nanomaterials through the decomposition of nanomaterials, with minimal sample preparation. An imperative feature of evaluating the composition and purity of nanomaterial is the characterization of the chemical components of a nanomaterial, particularly during synthesis and formation [40–52]. As an example, Wi and coworkers [53] studied the properties of the established nano-sized Palm Oil Fuel Ash (nPOFA) and assessed its kinetics of hydration within cement paste via TGA analysis (Fig. 3). 3

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sampling (flow-through sampling loop) and injection of gas even at short intervals [56–58]. The MS can be committed directly to the port of the outgassing of the TGA device. MS can detect the extremely small amount of substances, distinguish components to 1 ppm or better, and the recognition is carried out in real-time as the TGA scans. Generally, MS is utilized for identification only. Nevertheless, there are conditions where it would be required to quantify the MS data [59–61]. The TGA- MS technique has a disadvantage that products simultaneously released could only be distinguished from one another and recognized with significant difficulty. This problem could be resolved by separating of decomposition products before the determination step, which is possible via applying the TGA-GC–MS technique [62–64]. In TGA-GC–MS, due to this pre-separation of the resultant gases via the GC, and the resolution and sensitivity of the MS, determination of the molecular composition and comprehensive information about the molecular structure is obtained, which permitting most nanomaterial to be accurately identified. In several types of research, scientists used these hyphenated techniques to qualitative and quantitative analysis of nanomaterial [65–68]. For example, Kou and Varma [69] used the TGA-GC–MS to investigate the organics in the as-prepared nanoparticles Ag sample and the dried bee (Fig. 4). The total ion chromatogram and weight loss data detected via TGA-GC–MS. The results show noticeably different between the samples without MW irradiation. The major organic decomposition of the dried beet and Ag sample occurs, with a mass loss of 62.4 % in 200–400 °C, and with a mass loss of 14.7 % in 200–445 °C, respectively. Therefore, the attained peaks of the chromatogram of the dried beet and Ag sample are also dissimilar. The highest peak of the Ag sample is maybe organics with ethyl fragments and the highest peaks in dried beet could be allotted to methoxy phenol and phenol. The TGAGC–MS tests further demonstrate the chemical changes in the beet before and after irradiation of microwave.

FTIR (Fig. 5). The results show that the chief product evolved from asprepared nanocomposite degradation is CO2 (the greatest intensive band of absorbance at 2360 cm−1). In addition, it should be mentioned that the substituted kinds of aromatic constitute can be distinguished by FTIR. The band at 830 cm−1 and 750 cm−1 are the distinctive absorbance band of aromatic compounds. 2.2. DSC DSC can detect every phenomenon which involve energy change; thus, DSC is the basic thermal process utilized in the industrial field. DSC can measure the transition such as the melting, crystallization, and glass transition. Moreover, the chemical reaction such as specific heat capacity, heat history, thermal curing and also purity analysis are measurable. DSC technique distinguishes the differences of temperature between the reference and the sample; nevertheless, DSC can accomplish the quantitative measurement of the heat amount on the top [77–79]. 2.2.1. Determination of the glass transition temperature (Tg) The Tg is one of the most important properties of amorphous and semi-crystalline nanomaterials and describes the temperature region where the mechanical properties of the nanomaterials change from hard and brittle to more soft, deformable or rubbery. In some studies, the influence of composition and modification on the glass transition temperature (Tg) of nanocomposites have been investigated by DSC analysis [80–88]. In the DSC analysis, Tg is demonstrated by a change in the baseline, representing a variation in the heat capacity of the nanomaterial. The baselines after and before the transition are extrapolated to the temperature where the heat capacity change is 50 %. The heat capacity change is identified at the 50 % point. Subsequently, Tg is stated as the temperature at the baseline intersection and the extrapolated linear portion during the transition of phase [89–91]. As an example, Mohapatra and coworkers [92] used DSC to determine the Tg of a polymer-nanocomposite electrolyte (PNCE) via dispersed CeO2 nano-fillers in Poly(ethylene)oxide-LiClO4 matrix (Fig. 6). The endothermic peak detected in the 48 °C–61 °C range is allotted to the polymer matrix crystalline-melting that its peak area can be associated with the fraction of PNCEs crystallinity and it becomes thinner on the dispersion of nano-CeO2 in comparison to polymer-salt complex. The PNCEs glass transition can be detected between −30 °C and −50 °C with a change of slope in the thermograms. The decreasing of PNCE films Tg at lower nano-CeO2 loading shows growing PNCEs segmental motion. In another work, Huang and Lee [93] investigated the Tg of a cycloaliphatic epoxy/anhydride system incorporated with different contents of hydrophobic fumed silica via DSC. The Tg was characterized

2.1.4. TGA-FTIR and TGA-FTIR-MS As mentioned above, TGA is a commonly utilized method for investigation of the weight change of nanomaterial as a function of time or temperature in a controlled atmosphere. FT-IR has been used for the successful identification of gases. The combination of TGA, FT-IR and/ or MS techniques allows a comprehensive characterization of nanomaterials in terms of decomposition mechanisms and thermal stability [70–75]. Feng and coworkers [76] employed TGA-FTIR due to their authoritative ability for in situ investigating the products of pyrolysis from degradation. Results show that this investigation help to more understands the mechanism of flame retardancy of the as-prepared nanocomposite. Evolved gases from TGA were simultaneously studied via

Fig. 4. TGA-GC–MS image of as-prepared Ag nanoparticles and dried beet [69]. 4

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Fig. 5. TGA curves and their corresponding FTIR [76].

Fig. 7. Typical DSC temperature scans for uncured and cured samples [93].

2.2.2. Determination of the melting point temperature (Tm) Generally, melting is frequently determined with a simple melting point device. Nevertheless, the obtained number is often difficult to reproduce and inexact. The employment of DSC for this measurement achieves the Tm from a highly precise and calibrated system. Besides, this technique attains significantly more information about nanomaterial. Tm and energy changes give information about, for example, the amorphous content of nanomaterial. Thus, the melting endotherm can be used for the determination of the purity of the sample. In other researches, the effect of modification and composition on the Tm of nanocomposites has been inspected using the DSC analysis [94–99]. For example, Masoud and coworkers [100] prepared polymer nanocomposite electrolytes (Al2O3)x(PEO)12.5x(LiClO4) and investigated their Tm with DSC (Fig. 8). It can be seen that the Tm of the crystalline polyethylene oxide (PEO) phase declines via growing the Al2O3 amount. This denotes to flexibility increasing of the nanocomposite samples via increasing the Al2O3 amount in the matrix of PEO. In another work, Shahabi-Ghahfarrokhi and coworkers [101] studied the influence of ZnO nanoparticles (ZN) as a UV-protective agent of kefiran biopolymers by DSC (Fig. 9). The Tm of the different films was measured as the temperature where the endotherm peak occurs. The Tg of films were characterized by the resultant thermograms where the temperature of the midpoint of a step-down shift in the baseline, because of the discontinuity of the specimen specific heat. The thermal characteristic of samples, investigated via DSC, exhibited that the content of ZN had a positive effect on Tm and a negative effect on nanocomposites’ Tg.

Fig. 6. DSC thermograms of PNCEs for different wt.% of nano-CeO2 [92].

from the point of inflexion of the endothermic stepwise transition on the temperature scan. Fig. 7 shows typical DSC thermograms of samples with different amounts of silica. These results show that the Tg (noted by arrows) decreasing from 120 °C for cured to 49.4 °C for the uncured sample. The rescanned curves are displayed in Fig. 7. Upon the first scanning up through Tg, the aged nanomaterial showed a specific endothermic peak in the interval of the glass transition. The cured nanomaterial at longer cure times was rapidly cooled from temperatures above the endothermic peak and then instantly rescanned. Results show that the endothermic peak of aging that complicates the Tg assignment can be eliminated in this process. 5

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For example, Klongkan and Pumchusaka [114] investigated the effects of plasticizers and nano Alumina on thermal properties of PEOLiCF3SO3 Solid Polymer Electrolyte via DSC. The degree of crystallinity of the composites containing Al2O3 reduced significantly while the effects of dioxyphthalate (DOP) and polyethylene glycol (PEG) were trivial. The small increase of Tm and Tg of the nanocomposites containing PEG and DOP could be explained via the possibility of the polymer chains crosslinking through the plasticizer action. Though higher Tm and Tg were attained, the crystallinity degree slightly decreased. This proposed that the short-distance sequential arrangements of chains of polymer were also disturbed by the plasticizer’s addition. As another example, Zhang and coworkers [115] fabricated a 3D composite membrane composed of the tri-block copolymer poly(ε-caprolactone)-poly(ethylene glycol)- poly(ε-caprolactone) (PCEC-PEGPCL) and magnetic Fe3O4 nanoparticles. The DSC curves of the PCEC/ Fe3O4 membranes with the different mass of loadings of Fe3O4 was investigated (Fig. 10). The only one endothermic peak in Fig. 10A of all samples exhibited a Tm of about 59 °C (the exception is membrane via 10 % iron oxide content about 59 °C). Fig. 10B displays the cooling process curves that comparable to the curves of heating; all samples displayed a clear peak of crystallization, indicated their crystalline nature. The highest temperature of crystallization (at 31.2 °C) is related to pure 0 % Fe3O4 (PCEC membrane). 2.2.4. Investigation of thermal stability and thermal degradation behavior Thermal stability and thermal degradation behavior are some of the most important physical properties of nanomaterial products in the industry. Nowadays, DSC has become common in nanomaterial research and development for the evaluation of the thermal stability and thermal degradation behavior of nanomaterial. DSC is a comparatively straightforward and fast technique to characterization the thermal stability of nanomaterial, while it is not without limitations. This achievement is typically due to improvements in terms of sensitivity and automation of the instrumentation used to carry out the experiment. In some studies, the thermal degradation behavior and thermal stability of nanomaterials investigated by DSC [116–121]. As an example, Pourmortazavi and coworkers [122] fabricated composite nanofibers with three additives comprising Fe2O3 nanoparticles, aluminum nanoparticles, and diaminofurazan (DAF). Thermal behaviors of the nanofibers and pure nitrocellulose (NC) were investigated by the DSC method (Fig. 11). The results show a sharp exothermic peak for the electrospun nanofibers (at 197 °C). The assessment thermogram of electrospun nanofibers (Fig. 9a) and pure NC (Fig. 9b) approves that this peak is related to the NC decomposition.

Fig. 8. The curves of DSC analysis of pure PEO and (Al2O3)x(PEO)12.5x (LiClO4), (x = 0, 0.25, 0.75, 1 and 1.25 mol) [100].

2.2.3. Investigation of the crystallization behavior The crystallization behavior of crystalline and semi-crystalline nanomaterials is an intriguing and important field of investigation in the area of nanomaterial research. Many factors, including composition, temperature and bonding interactions between the functional groups as well as the conditions of processing, may affect the phase structure of nanomaterial. Without a principally comprehensive understanding of the behavior of crystallization, it is incredible to attain suitable, predictive correlations of structure-property. In some studies, results show that the crystal structure and crystallization behaviors of the nanocomposites are different from those of neat materials [102–113].

Fig. 9. Thermogram and thermal properties of kefiran film and ZnO–kefiran nanocomposites [101]. 6

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Fig. 10. The curves of DSC of the PCEC/Fe3O4 membranes. (A) process of heating, and (B) process of cooling [115].

Fig. 11. DSC curve of (a) Al/Fe2O3/DAF/NC nanofibers and (b) pure NC [122].

Also, a comparison of thermal behaviors of pure NC and Al/Fe2O3/ DAF/NC nanofibers displays that Al/Fe2O3/DAF nanocomposite introducing to the NC results in minor shifting of the NC thermal decomposition to a higher temperature (be more thermal stable). 2.3. DTA

Fig. 12. DTA-TGA photograph of (a) nano-AP and (b) coarse-AP [131].

DTA is a method for quantitatively analyzing and identifying the chemical composition of nanomaterials by investigation of the thermal performance of a substance as it is heated. The method is according to the principle that as a sample is heated, it undergoes phase changes and reactions that include emission or absorption of heat [123,124].

TGA and the curves (Fig. 12 a and b, respectively). The sharp endotherm (244–245 °C) demonstrating a change of phase of AP from orthorhombic form to cubic. Nevertheless, micrometer-sized AP exhibited two at 311.19 and 394.78 °C (exothermic peaks) that representing two-step decomposition, while nano-AP presented a peak at 368.78C (only one exothermic), obviously signifying one-step decomposition. Due to the absence of the peak at 311.19 °C and a large surface area can be concluded that fast decomposition.

2.3.1. Investigation of the thermal stability The main goal of the thermal stability test is collecting reaction rate data and employing that data to evaluate whether a definite amount of nanomaterial can be utilized in a way such that runaway reactions are avoided. This qualifying is more important when considering long-term storage, processing, or material shipping. In various researches, the thermal stability of nanomaterials has investigated by DTA [125–127]. It must be mentioned that almost of published papers used TGADTA techniques for the determination of thermal stability [128–132]. For instance, Kumari and coworkers [131] studied the thermal behavior of nano-ammonium perchlorate (AP) and coarse AP via DTA-

2.3.2. Determination of Tg DTA has been used to the determination of Tg in nanomaterials [133–135]; DTA can distinguish the discontinuous changes definite heat that is related to such transitions. The device applied must have significantly superior sensitivity than that vital for measuring transitions involving latent heats. As an example, Monmaturapo [136] prepared nano-sized 7

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Fig. 13. HA powders via varying concentration (high, medium and low) [136].

hydroxyapatite (HA) powders via the wet-chemical process and analyzed with DTA (Fig. 13). The DTA exhibited a wide dip corresponding to Tg for all samples (at 430 °C–480 °C) and exothermic dips related to crystallization temperatures (Tc) of HA with tricalcium phosphate (at 690 °C–760 °C). In another example, to investigation effect of nanocrystallization on the electrical conduction of silver lithium phosphate glasses containing iron and vanadium, Hassaan and coworkers [137] prepared 5Ag2O·15Li2O·5V2O5·15Fe2O3·60P2O5 glass (ALVFP) and xLi2O·(20x)Ag2O·20Fe2O3·60P2O5 glasses and characterized their Tg and Tc via DTA (Fig. 14). The DTA results of LAVFP show that Tg, Tm and Tc increase via a growing content of lithium. Normally, Tg displays a distinct increase where the number of coordination of the network former rises, whereas construction of NBO (nonbridging oxygen) leads to a decrease of Tg. The continuous Tg improving proposes a continuing reduction in the number of coordination of Fe2+ and Fe3+ ions and the destruction of atoms of NBO. This shows that the structure of glass develops more closed as a result of substitution via a larger ionic radius (Li+ with Ag+). Th values of Tg/Tm measured for all prepared nanomaterial were in 0.78 ∼ 0.80 range, demonstrating high thermal stability since the value of Tg/Tm of preferably stable glass is testified to be 0.67.

Fig. 15. DTA curves of the nanocomposites [141].

is measurement of melting points and decomposition. In many studies, melting and decomposition of nanomaterials have examined the by DTA [138–140]. For instance, Aydemir and coworkers [141] prepared TiO2 filled Polypropylene (PP) nanocomposites. The thermal behavior of the nanocomposites is an imperative property for many applications due to the changes in the viscosity and viscoelastic behavior; therefore, the thermal properties of the nanocomposites were inspected by DTA (Fig. 15). Fig. 12 displays the DTA curves that show the degradation point of the PP nanocomposites and the neat PP. There were two degradation dip, i.e., degradation and melting. The endothermic peaks (at 165 and 460 °C) are related to the Tm and the degradation point, respectively. As another example, Mat Jan and coworkers [142] synthesized series of glasses based on (75-x)TeO2-15MgO-10Na2O-xNd2O3 and determined their Tg, Tc and Tm using DTA (Fig. 16). The results show that all of The Tm, Tc, and Tg have increased via the rising concentration of Nd2O3. The Tg increasing is due to the structural changes in the network. In glasses material, thermal stability is a very important characteristic for glasses perform fabrication and is a quantity of disorder degree of state of glassy. There are two commonly utilized factors (S and kg) for assessing glasses thermal stability which their equations are:

2.3.3. Investigation melting and decomposition DTA is a method that the physical property of nanomaterial is investigated as a function of temperature. One of the applications of DTA

S = Tc Kg =








The value of S is an indication of the tendency of devitrification of

Fig. 14. DTA for LAFVP glass and composition dependence of Tg, Tc and Tm [137].

Fig. 16. The thermal characteristic of the glass as measured by DTA [142]. 8

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glass where above of Tg is heated. It explains the range of temperature for glass drawing. The larger amount of S and the smaller difference between Tm and Tc slow down the process of crystallization and formation of facilitating glass. The results show that dopant concentration leads to increasing in stability.

both samples are include CO2, H2O, SO2, CO and aromatic hydrocarbons. It is outstanding that evolved gases peaks of AO-PPS fiber move backward related to the neat PPS fiber peaks. This shows that the AO-PPS fiber decomposition reaction starts at a higher temperature and also approves the deduction that the oxidation resistance of AO-PPS is greater than neat PPS.

2.4. EGA 2.5. DMA

EGA is an exciting technique used to the investigation the gas evolved from a heated sample that undergoes desorption or decomposition. EGA is the analysis of the chemical processes and effluent of analytical equipment. The composition understanding of the gases released by thermal continuous flow analysis can offer insight into the nanomaterial area [143,144]. The scientific researches now plan progress in EGA methods because the opportunity to on-line distinguish the vapors or released gases nature has become important to verifying a supposed reaction, either under heating conditions [145].

Because of measuring damping coefficient and dynamic modulus properties, the DMA is normally an extra sensitive method for distinguishing transitions than the DTA and DSC techniques. These are meaningful when changes transition of crystalline structures to the amorphous phase have occurred. The principle of operating is that in these transitions, a comparably larger change occurred in the mechanical assets of nanomaterial than in its definite heat. Consequently, DMA is the preferred technique of Tg determination and other minor structure/phase changes of nanomaterial [153–159]. For instance, Jiang and coworkers [160] studied the thermo-mechanical behavior of epoxy resins/nano-Al2O3 composites The DMA of the DGEBA/nano-Al2O3 was investigated by inspection of the tanẟ and storage modulus as a function of temperature (Fig. 18). The Tg was resulting from the DMA analysis via investigative the a-relaxation temperatures. The Tg of the epoxy resins/nano-Al2O3 (2 wt%) and neat epoxy resins was 181.8 8 °C and 170.4 8 °C, respectively; the nanocomposites had a higher Tg than the neat epoxy resins. The modulus of storage in the region of glassy declined with increasing content of nanoAl2O3, while the modulus of storage in the region of rubbery enlarged

2.4.1. EGA-MS and EGA-FTIR The employment of MS and FTIR in the evolved gaseous species determination in EGA researches is well established. In thermal analysis researches, the characterization of the evolved gases composition is very important, particularly when inspecting gas–solid reactions or decomposition processes occurring in systems with multicomponent [146–151]. As an example, Lian and coworkers [152] investigated the model of decomposition kinetics of the neat PPS fiber and nano TieSiO2 modified PPS fiber (AO-PPS). Thermo-oxidative decomposition of PPS and AOPPS produces volatile gases. Hence, EGA is utilized in tandem with the analysis of the decomposition mechanism (Fig. 17). The results of EGAFTIR of neat PPS and AO-PPS show that the chief evolved gases from

Fig. 17. FTIR spectra of thermal decomposition processes of neat PPS and AOPPS [152].

Fig. 18. Tan ẟ and storage modulus of DGEBA/nano-Al2O3 with different amount of nano-Al2O3 content [160]. 9

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the field of nanoparticles are TGA, DSC, DTA, DMA, EGA. The TGA technique, which involves the study of sample mass changes as a function of temperature, is typically used in the study of structure, composition, thermal stability, dissociation temperature, adsorption and desorption of solvents and volatiles components, the effect of modifiers, combustion and purity of nanomaterials. The DSC technique, which involves investigating energy changes in the heating process, has been applied to the study of the glass transition temperature, melting temperature and the determination of thermal behavior, crystallization, purity, thermal curing, heat history, and specific heat capacity of nanomaterials. The DTA technique, which is based on the thermal performance of the material as a function of temperature (includes phase changes and reaction), has been used to investigate the thermal behavior, glass transition temperature, melting and decomposition behavior of nanomaterials. The DMA technique, which is based on the measurement of dynamic modulus properties, has been used to determine transitions, especially glass transition, which is much more sensitive than the DSC and DTA methods. The EGA technique is used to investigate the released gases from the sample during the heating process. This technique has greatly useful to investigate the composition, structure and purity of nanomaterials. The TMA technique, which is based on the deformation of a sample under non-oscillatory stress as a function of time or temperature while the sample is heated programmatically in a specific atmosphere, has been used to investigate the structure and composition of nanomaterials. As mentioned above, there are many efforts in the field of thermal analysis of nanomaterials that led to improved understanding of nanomaterials and increased scope of its applications in recent years. However, there are still many areas for improvement, most notably hyphenated techniques which widely interested by scientists in recent years. In this regard, conventional thermal analysis methods are coupled with separation and identification devices such as GC, FTIR and MS. FTIR and MS have the specific advantage that the components obtained from thermal analysis methods are identified with high accuracy. But these tools have a disadvantage that released simultaneously components could only be distinguished from one another and recognized with significant difficulty. This problem can be solved by separating of decomposition products before the determination step, which is now carried out via applying the TGA-GC–MS technique. However, common separation and identification methods are currently limited to GC, MS, and FTIR, so there is a need for more efficient methods in the field of nanomaterial determination. For future research, which cautiously selects an efficient thermal analysis technique, uses some form of adaptive hyphenated systems such as EGA-GC–MS, DSC-FTIRS-TMA, TA-inductively coupled plasma and DSC-Raman Spectroscopy will be very helpful.

Fig. 19. TMA curves of epoxy/CF, p-MWCNTs/epoxy/CF, and f-MWCNTs/ epoxy/CF composites [166].

with increasing content of nano-Al2O3. Consequently, these arrangements have good heat resistance by the addition of particles of nanoAl2O3. 2.6. TMA TMA rapidly and easily measures the deformation of the nanomaterial under non-oscillating stress (tension, compression, torsion or flexure) as a function of temperature or time, while the programmed temperature is applied. Usually, TMA is applied to the determination of Tg, softening points, and linear expansion of nanomaterials by using a constant force to nanomaterial whereas changing temperature. Analyses of TMA can now offer appreciated understanding into the structure, composition and possibilities of application for numerous nanomaterials [161–183]. Kim and coworker [166] fabricated epoxy/carbon fiber (CF) modified with MWCNTs). The Tg of epoxy/CF, p-MWCNTs/epoxy/CF, and fMWCNTs/epoxy/CF composites are obtained from the transition point on the thermal-expansion curves of TMA (Fig. 19). Because of poor dispersion of p-MWCNTs or lower crosslinking, the Tg of the neat epoxy/CF composite was higher than that of the p-MWCNTs/epoxy/CF composite. Therefore, the difference in Tg may be ascribed to the change in the degree of epoxy crosslinking reactions. Also, the TMA was conducted to inspect the influence of MWCNT-filled epoxy on the coefficient of thermal expansion (CTE) of epoxy/CF in the thickness direction. The values of CTE of epoxy/CF composite is higher than fMWCNTs/epoxy/CF and p- MWCNTs/epoxy/CF (22 and 11 %, respectively). This proposes that even small quantities of MWCNTs, when functionalized, can meaningfully enhance the dimensional stability of the matrix of the polymer. This enhancement in matrix dimensional stability then results in enhanced dimensional stability in the resultant f-MWCNTs/epoxy/CF. The CTE reduction of p-MWCNTs/epoxy/CF was not noteworthy (11 %) possibly because of weak dispersion and poor bonding interface between epoxy and the p-MWCNTs.

Declaration of Competing Interest The authors declare that there are no conflicts of interest regarding the publication of this manuscript. Acknowledgments Authors are grateful to the council of Iran National Science Foundation; INSF (97017837) and University of Kashan for supporting this work by Grant No (211037-2).

3. Conclusion and future discussion


A better understanding of the physical, mechanical and chemical properties of nanomaterial will lead to better synthesis and employment of the nanomaterial in industrial fields. This paper presents a comprehensive review of the literature on the applications of thermal analysis techniques in the identification and investigation of nanomaterials in recent decades. The most common thermal analysis techniques used in

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