Differential Scanning Calorimetry Traces Research Articles

Nanometer Ammonium Perchlorate and Ammonium Nitrate Prepared with 2D Network Structure via Rapid Freezing Technology.

Nanometer (nano) ammonium perchlorate (AP) and ammonium nitrate (AN) were prepared with 2D network structures by the ultra-low temperature spray method. Scanning electron microscopy (SEM), X-ray diffractometry (XRD), differential scanning calorimetry (DSC) and thermogravimetric analysis/infrared spectrometry (TG-IR) were employed to probe the micron structure, crystal phase, and thermal decomposition of nano AP and nano AN. SEM images revealed that the sizes of nano AP and AN were in the nanometer scale (<100 nm) in one dimension. XRD patterns showed that the crystal phases of nano AP and AN were in accordance with those of raw AP and raw AN, respectively. DSC traces indicated that the thermal decomposition process of AP depended on its particle size, while the thermolysis of AN was independent of the particle size of AN. TG-IR analyses illustrated that the decomposition products of nano AP were NO2, N2O, HCl and H2O, with a small amount of NOCl, and the main decomposition products of nano AN were N2O and H2O, with a small amount of NH3. The results of mechanical sensitivity tests indicated that nano AP was more sensitive than raw AP and both nano AN and raw AN were very insensitive to impact and friction stimuli.

Phase transitions in higher-melting imidazolium-based ionic liquids: Experiments and advanced data analysis

As thermal energy storage becomes an increasingly important topic, good knowledge of properties of phase-change materials (PCM) is essential. Among other properties, a good PCM should show a large enthalpy of melting, reproducible melting/solidification cycles, and long-term thermal stability. Temperatures and enthalpies of fusion should be determined at a possibly large range of conditions to allow for a critical evaluation of the experimental data and assessment of the material application potential.In this work, imidazolium-based ionic liquids (ILs) with long alkyl chain substituents 1-hexadecyl-3-methylimidazolium chloride and 1-hexadecyl-3-methyl-imidazolium saccharinate were studied in view of their possible use as phase-change materials. Differential scanning calorimetry (DSC) and the heat-leak modulus (HLM) methods were used to determine the temperatures and the enthalpies of phase transitions in the studied ILs, enabling us to study the influence of the heating and cooling rates on the measured properties. Enthalpies of fusion near to or larger than 100 J·g−1 were found in the studied ionic liquids, making them promising candidates for thermal energy storage. Peaks corresponding to possible liquid crystalline phases in the DSC traces of 1-hexadecyl-3-methylimidazolium saccharinate were observed, pointing to more complex phase behaviour of the studied ionic liquids.Finally, to critically evaluate the experimental data measured in this work, methods based on mathematical gnostics were used. Repeatability of measurements and the degree of mutual agreement between the methods used in this work could thus be determined.

Phase Behavior of cis–trans Mixtures of Double-Decker Shaped Silsesquioxanes for Processability Enhancement

Closed double-decker shaped silsesquioxanes (DDSQ-(Ph)8-2((Me)(R))) with R as phenyl, para-phenylamine, and para-phenylethynyl phenyl were synthesized. Isolation of nearly pure trans and cis isomers was obtained by fractional recrystallization. Crystallographic and thermal characteristics of these isolated isomers were obtained by X-ray diffraction of a single crystal and differential scanning calorimetry (DSC). It was observed that melting temperature increases as the size of the R group decreases from para-phenylethynyl phenyl to phenyl and the magnitude of the entropy difference at melting increases as the size of the R group increases. Isolated isomers were then mixed to different cis-to-trans ratios, and their thermal characteristics investigated by DSC. The upper portion of the phase diagram was constructed for these DDSQ compounds using results from DSC traces. Interestingly, cis and trans isomers of these DDSQ compounds form a binary eutectic. Experimentally observed eutectic composition and tempe...

Effect of Sn contents on thermodynamic, microstructure and mechanical properties in the Zn90–Bi10 and Bi88–Zn12 based ternary alloys

The thermal conductivity variations with temperature for Zn90 − x–Snx–Bi10 (x = 5,10, 40 and 85 wt%) and Bi88 − x–Snx–Zn12 (x = 1.39, 43.26 and 79.3 wt%) alloys were measured by using the linear heat flow method. From thermal conductivity–temperature plots, the coefficients of thermal conductivity for the Zn–Sn–Bi alloys were calculated. The microstructures of Zn–Sn–Bi alloys were observed using scanning electron microscopy (SEM). The existing phases into microstructure were identified energy dispersive X-ray (EDX) analysis. The melting temperatures, the enthalpy of fusion and specific heat change between the liquid and solid phases in the Zn–Sn–Bi alloys were determined from Differential Scanning Calorimetry (DSC) trace. The tensile strength and microhardness of the alloys were measured using a Shimadzu Universal Testing Instrument (Type AG-10 KNG) and Future-Tech FM-700 model microhardness device.

Photo-induced non-linear optical studies on gallium alkali borate glasses doped with TiO2

30 Li2O − (5 − x) Ga2O3 − 65 B2O3 glasses containing small concentrations of TiO2 varying from 0 to 1.0 mol% are prepared by the melt quench technique. The X-ray diffraction results showed the amorphous nature of the sample. Various physical parameters like density, molar volume, Ti4+ ion concentration, molar refraction, polarizability, polaron radius, etc., are evaluated. The differential scanning calorimetry traces of all the samples are recorded and displayed inflection points due to glass transition Tg in the temperature region 446–460 °C. Fourier transform infrared spectra, optical absorption spectra and photoluminescence spectra of all the samples are recorded at room temperature and analyzed. Optical absorption spectra of all these glasses exhibited two clearly resolved absorption due to the excitation of Ti3+ ions. At room temperature, the recorded electron paramagnetic resonance (EPR) spectrum of present glasses exhibited a resonance signal at g ~ 1.911 referred to tetragonaly compressed octahedral sites of Ti3+ ions. Laser-induced second-harmonic generation (SHG) studies are carried out for all the glasses. These results have signified that the glass doped with 0.8 mol% of TiO2 exhibited the highest intensity of SHG signal. These results are further analyzed using the other spectroscopic studies and reasons for the highest SHG efficiency of the glass GT8 are identified and reported.

Phase Transitions in Higher-Melting Ionic Liquids: Thermal Storage Materials or Liquid Crystals?

To assess the application potential of a material in thermal energy storage, the knowledge of their thermophysical properties is of key importance. Specifically, an efficient material has to show, among others, large enthalpies of phase change and a sufficiently large thermal conductivity.In this work, imidazolium-based ionic liquids (ILs) with long alkyl chain substituents 1-hexadecyl-3-methylimidazolium chloride and 1-hexadecyl-3-methylimidazolium saccharinate were studied in view of their possible use as phase-change materials. Differential scanning calorimetry (DSC) and the heat-leak modulus methods were used to determine the temperatures and the enthalpies of phase transitions in the studied ILs, enabling us to study the influence of the heating rates on the measured properties. Enthalpies of fusion near to or larger than 100 J·g–1 were found in the studied ionic liquids, making them promising candidates for thermal energy storage. Furthermore, peaks corresponding to possible liquid crystalline phases in the DSC traces of 1-hexadecyl-3-methylimidazolium saccharinate were observed.The measured properties are not only essential characteristics of a thermal storage material, temperatures and enthalpies of melting are necessary in thermodynamic description and modelling of solid-liquid phase behavior and thus in the possible utilization of the material in separation and crystallization processes.

Kinetics study on non-isothermal crystallization of Ni1.5MnSn0.5Co alloy thin films

ABSTRACTThe crystallization kinetics of the Ni1.5MnSn0.5Co free-standing alloy thin films is investigated by continuous heating differential scanning calorimetry (DSC). The results show that all the DSC traces have a single exothermic peak, with a long high temperature tail. The DSC curves have been analyzed in terms of activation energy and kinetic model. We find that the activation energy of film obtained by both the Kissinger and Ozawa equation methods can give consistent results, the activation energy for crystallization is determined as 221.2 and 220.9 KJ/ mol, respectively. Moreover, the volume fraction crystallized has significantly influence on the local activation energy, and the regular of the nucleation and growth of films has been changed at crystallization process. Our work would enrich the mechanism of the crystallization kinetics for annealing applications of Ni-Mn-Sn-Co thin films in microelectro mechanical systems (MEMS).

Crystallization kinetics of PCL and PCL–glass composites for additive manufacturing

The non-isothermal crystallization kinetics of polycaprolactone (PCL) and PCL–glass composites, used in fused filament fabrication (FFF), was investigated. Films of PCL and PCL reinforced with powders of a bioactive glass, from the CaO·P2O5·MgO·SiO2 system, were prepared by solvent casting process. Crystal structure of the samples was examined by X-ray diffraction (XRD), and thermal properties were assessed by differential scanning calorimetry (DSC), at different cooling rates (5, 10, 15 and 20 °C min−1). The DSC curves of non-isothermal crystallization showed a significant dependence of crystallinity (Xc) on the cooling rate. The relevant crystallization kinetic parameters were determined from DSC traces applying a combination of Avrami and Ozawa methods (Mo’s method), Jeziorny method and Friedman method. It was observed that the presence of inorganic particles within the polymeric matrix clearly influenced the composite crystallization. The addition of glass particles allowed a decrease in Xc and accelerated the PCL crystallization rate. The slower cooling rates tested proved to be suitable for the biofabrication of PCL–glass composites by FFF techniques.

Cr additive effects on the nanostructure, magnetic properties, and ordering kinetics of FePtCu thin films

In this study, the (FePt)94–xCu6Crx (x = 0, 6.54, 8.33, 11.11) alloy films were prepared by sputtering and then the effects of Cr content and heat treatment on the nanostructures and magnetic properties of polycrystalline FePtCu films are examined. After adding Cr atoms to FePtCu films, the surrounding Cr layer of the grain limited grain growth of (FePt)94−xCu6Crx (x = 0, 6.54, 8.33, 11.11) alloy films, even when those films had been annealed at temperatures as high as 600 °C. The differential scanning calorimetry traces revealed that the addition of Cr atoms enhanced the activation energy of ordering from 87 kJ mol−1 for the (FePt)94–xCu6 film to 264 kJ mol−1 for the (FePt)94–xCu6Crx film (x = 6.54). The (FePt)94–xCu6Crx (x = 6.54) film displayed a coercive force of 12.8 kOe and a magnetization of 658 emu cc−1.

Separation and kinetic analysis of the thermo-oxidative reactions of polyacrylonitrile upon heat treatment

A polyacrylonitrile (PAN) homopolymer and a copolymer with methyl acrylate were analyzed by differential scanning calorimetry (DSC) in order to establish a method for the kinetic analysis of the stabilization reaction steps during heat treatment. The application of a program rarely used for the study of the chemical transformation of PAN and its copolymers resulted in five separate steps, which can be assigned with large probability to various cyclization and oxidation reactions. A more exact identification of the reactions needs further measurements and considerations. Overlapping peaks appearing in the DSC traces were deconvoluted and then quantitatively analyzed to obtain kinetic parameters. The kinetics of the processes were described by the Kissinger model. The model could be fitted well to four of the five processes that may indicate that these belong to individual reactions of the first order. The parameters obtained agree well with the few values of similar investigations published in the literature up to now. The results have large practical relevance, since the kinetic parameters obtained can be used in the preparation of intermediates and for the optimization of the stabilization process.

Mesogenic complementary absorbing dyads based on porphyrin and perylene units

Five novel dyads, consisting of a tetraphenylporphyrine unit connected to a perylene monoimide diester unit via a flexible bridge -CONH-(CH[Formula: see text]- (n [Formula: see text] 4, 6, 8, 10 and 12), have been synthesized. Their structures were characterized by [Formula: see text]C and [Formula: see text]H nuclear magnetic resonance spectroscopy, infrared spectroscopy, mass spectrometry and elemental analysis. The UV-vis absorption spectra revealed these dyads have broad optical absorption in the ultraviolet and visible regions due to the complementary absorption of the two units. The differential scanning calorimetry traces and polarized optical microscopy textures showed all these dyads have columnar liquid crystal phases. Cyclic voltammetry revealed the highest occupied molecular orbitals of the dyads located on the porphyrin units, and the lowest unoccupied molecular orbitals located on the perylene units. In addition, these results were in agreement with that of the theoretical modeling. When excited at 423 or 473 nm, the photoluminescent emission spectra showed that the degree of fluorescence quenching of porphyrin units increased as the spacers became shorter. This quenching was ascribed to intramolecular photoinduced electron transfer, which also induced the dyad molecules to form the charge-separated states. The charge-separated molecules were further confirmed by the photocurrent response curves. These behaviors of broad absorption of the ultraviolet-visible light, yielding the charge-separated states of the molecules when excited and the formation of columnar liquid crystal phase made these dyads candidates for single-component photovoltaic active materials.

Non-isothermal crystallization kinetics and soft magnetic properties of the Fe67Nb5B28 metallic glasses

Differential scanning calorimetry (DSC) was used to investigate the thermal behavior and non-isothermal crystallization kinetics of the Fe67Nb5B28 metallic glasses prepared by melt-spinning method. DSC traces exhibit that the crystallization takes place through a single exothermic reaction, and it processes a good thermal stability in thermodynamics. The activation energies for nucleation and grain growth processes were calculated to be 536 ± 22 and 559 ± 20 kJ mol−1 by Kissinger equation, respectively, and 551 ± 24 and 574 ± 20 kJ mol−1 by Ozawa equation, respectively. It means that the grain growth process is more difficult than the nucleation process. The variation of local Avrami exponent n(x) with crystallized fraction x demonstrates that the crystallization mechanism varies at different stages. The n(x) is larger than 2.5 at the initial stage of 0 < x < 0.3, implying a mechanism of diffusion-controlled three-dimensional growth with increasing nucleation rate. The n(x) decreases from 2.5 to 1.5 in the range of 0.3 < x < 0.65, suggesting that the crystallization belongs to three-dimensional nucleation and grain growth with decreasing nucleation rate. And n(x) lies between 1.0 and 1.5 in the range of 0.65 < x < 0.95, indicating that the crystallization corresponds to the growth of particles with an appreciable initial volume. Low-temperature annealing corresponds to the precipitation of α-Fe, Fe2B, and Fe23B6 phases, and further annealing leads to the formation of α-Fe, Fe2B, and FeNbB phases. The magnetic properties in relation to microstructure change of the Fe67Nb5B28 metallic glasses are discussed.

Alcohol Stabilization of Low Water Content Pyrolysis Oil during High Temperature Treatment

The addition of alcohols is a promising method to pretreat and stabilize pyrolysis oil by converting carboxylic acids and reactive carbonyl compounds into esters, ethers, and acetals. In this study a series of alcohols—methanol, ethanol, 1-propanol, 2-propanol, or 1-octanol—was added to crude pyrolysis oil, and these mixtures were stored at 200 °C for different periods from 6 to 50 h to investigate the impact of heat treatment on the oils’ physicochemical properties. All oil/alcohol mixtures were characterized by Karl Fisher titration, viscometer/rheometer, differential scanning calorimetry (DSC), gel permeation chromatography (GPC), Fourier transform infrared (FTIR) spectroscopy, and gas chromatography–mass (GC-MS) spectrometry. Phase separation is observed for all aged oil/alcohol mixtures. The time-dependent rheologies of heat treated oil/1-propanol, oil/2-propanol, and oil/1-octanol mixtures are found to be well fitted by the Herschel–Bulkley model. Isothermal DSC traces directly confirm that low mole...

The effect of Ag addition on the non-isothermal crystallization kinetics and fragility of Zr56Co28Al16 bulk metallic glass

The non-isothermal crystallization kinetics and fragility of Zr56Co28Al16 and Zr56Co24Ag4Al16bulk metallic glasses (BMGs) were studied by differential scanning calorimetry (DSC). The X-ray diffraction (XRD), transmission electron microscopy (TEM) and microhardness test were used to investigate the glassy alloys structure. DSC traces exhibited two crystallization processes for both alloys. The activation energies of characteristic temperatures were obtained by Kissinger and Ozawa methods. Also, the heating rate sensitivity of characteristic temperatures was determined. The Ag-bearing Zr-based BMG presented higher activation energies and lower heating rate sensitivity in regard to characteristic temperatures, indicating a higher stabilization of the supercooled liquid, which can be correlated with the existence of strong icosahedral short range order (ISRO) clusters in the structure. In addition, the local Avrami exponents at various heating rates were calculated by the Johnson–Mehl–Avrami equation. The n value variations for each crystallization process pursued almost similar trends for both alloys with n>2.5, revealing that the transformation kinetics is dominated by a diffusion-controlled three-dimensional growth, as well as an increase in the nucleation rate. Moreover, both BMGs were classified into “strong glasses”, depending on the fragility index calculated values.

Characterization and Thermal Decomposition of Nanometer 2,2′, 4,4′, 6,6′-Hexanitro-Stilbene and 1,3,5-Triamino-2,4,6-Trinitrobenzene Fabricated by a Mechanical Milling Method

ABSTRACTNanometer 2,2ʹ, 4,4ʹ, 6,6ʹ-hexanitro-stilbene (HNS) and 1,3,5-triamino-2,4,6-trinitrobenzene (TATB) were fabricated on a high-energy ball mill. The particle sizes of nano-HNS and nano-TATB were 98.4 and 57.8 nm, respectively. An SEM analysis was employed to image the micron morphology of nano-explosives. The particle size distribution was calculated by measuring the size of 300 particles in SEM images. XRD, IR, and XPS analyses were used to confirm whether the crystal phase, molecule structure, and surface elements were changed by the milling process. Thermal decomposition of nano-HNS and nano-TATB was investigated by differential scanning calorimetry (DSC) and thermal-infrared spectrometry online (DSC-IR) analyses. Using DSC traces collected from different heating rates, the kinetic and thermodynamic parameters of thermolysis of raw and nano-explosives were calculated (activation energy (EK), pre-exponential factor (lnAK), rate constant (k), activation heat (ΔH≠), activation free energy (ΔG≠), activation entropy (ΔS≠), critical temperature of thermal explosion (Tb), and critical heating rate of thermal explosion (dT/dt)Tb). The results indicated that nano-explosives were of different kinetic and thermodynamic properties from starting explosives. In addition, the gas products for thermal decomposition of nano-HNS and nano-TATB were detected. Although HNS and TATB are both nitro explosives, the decomposition products of the two were different. A mechanism to explain the difference is proposed.

Investigating aging effects for porous silicon energetic materials

When infused with an oxidizer, on-chip porous silicon (PS) shows tremendous potential as an energetic material. However, applications such as fuzing and propulsion require long-term material stability. The present work utilizes accelerated lifetime testing for PS samples with sodium perchlorate (NaClO4) oxidizer. Devices were exposed to elevated temperatures for various time intervals, then subjected to an electrical pulse through an integrated bridgewire to test for ignition. The pass/fail data from ignition testing was then analyzed to determine the mean and median failure point at each temperature using an Arrhenius aging model and a lognormal probability density function (PDF). Samples were heated over a temperature range of 185–300 °C for up to 46 h with median failure times ranging from 0.4–20 h. Differential scanning calorimetry (DSC) and Fourier transform infrared (FTIR) spectroscopy were used to evaluate chemical changes of PS/NaClO4 during aging. Comparison of DSC traces for aged samples showed differences for heating above and below 250 °C, suggesting two different aging mechanisms. FTIR results suggest that for low temperature aging (below ∼250 °C) the hydrogen termination layer of the porous silicon was still intact, but backbond oxidation did occur. Above ∼250 °C the hydrogen termination layer was no longer evident in FTIR and considerable oxidation occurred, suggesting reaction or dissociation of the hydrogen layer. This corresponds with an exothermic peak shown during DSC at 300 °C. Thermogravimetric analysis/mass spectroscopy (TGA/MS) was also performed, and confirmed hydrogen gas release beginning at ∼280 °C. A DSC peak at ∼400 °C is evident for fresh samples, but is greatly reduced or not evident for all aged samples. We attribute this peak to backbond oxidation, which is shown to occur in FTIR for all aged samples. Variable heating rate DSC experiments were also performed to determine activation energy of fresh and aged samples. Activation energy was calculated using the Kissinger Method for the first two exothermic peaks in DSC experiments. For the first peak, corresponding to hydrogen desorption (∼300 °C), activation energy for fresh and aged samples was 132.1 kJ/mol and 132.7 kJ/mol, respectively. The activation energy of the second exothermic peak, corresponding to backbond oxidation, for fresh and aged samples was 183.8 kJ/mol and 159.6 kJ/mol, respectively. Device failure during accelerated aging tests was also used to predict the mean lifetime of porous silicon/sodium perchlorate at room temperature (25 oC) as 100 years with a 90% confidence interval of 31 to 328 years.

Multiple endothermic transitions of acid hydrolyzed and heat-moisture treated corn starch

The multiple thermal transitions of acid-hydrolyzed and heat-moisture treated corn starch samples in excess water were measured using differential scanning calorimetry (DSC) and interpreted using a polymer swelling and dissolution theory. The dual treatment of acid hydrolysis (AH) and heat-moisture treatment (HMT) with different extent of reaction generates starches with various degrees of residual crystalline structure. Multiple endothermic transitions (G and M1) were firstly observed in DSC traces even in excess water. In this study, the G and M1 endotherms were proposed to be related with the energy consumption associated with granule swelling and crystallites dissolution respectively. In contrast, only a single M1 endotherm transition from a broad to a sharp and narrow endotherm upon HMT was consistently observed for starch samples acid hydrolyzed for 48 and 72 h, which testified the dominance of rearrangement over the destruction upon HMT. This novel theory describing the multiple phase transition was also evidenced by the variation of swelling power and relative crystallinity.

Effects of Rapid Solidification on Phase Formation and Microstructure Evolution of AgSbTe₂-Based Thermoelectric Compounds.

We report on rapid solidification of an Ag(16.7)Sb(30.0)Te(53.3) compound using planar flow casting to stabilize the δ-AgSbTe₂ single phase and avoid precipitation of the interconnected Sb₂Te₃ phase, which leads to deterioration of thermoelectric properties. Rapidly solidified samples are in form of flakes with different thickness (60–400 μm). Precipitation of Sb2Te₃ phase is fully inhibited in thin flakes (thickness below 100 μm), which consist of an homogeneous δ-AgSbTe₂ matrix, whereas isolated Sb₂Te₃ precipitates, dispersed throughout the δ-AgSbTe₂ matrix, were found in thick flakes (thickness above 100 μm). The lattice parameter of the δ-AgSbTe₂ phase progressively increases with the cooling rate, indicating progressive supersaturation of the matrix for high degree of supercooling. Bulk specimens were prepared by hot pressing of the rapidly solidified flakes to evaluate thermoelectric properties. After sintering of the rapidly solidified flakes, the differential scanning calorimetry (DSC) traces indicates partial decomposition of the non equilibrium δ-AgSbTe₂ into the stable phases. Measurements of the thermoelectric transport properties indicate the positive effects of rapid solidification on thermal conductivity and Seebeck coefficient and its negative effect on electrical conductivity, suggesting an operative way to improve thermoelectric performance.

The Effect of Anodic Oxide Films on the Nickel-Aluminum Reaction in Aluminum Braze Sheet

The influence of an anodic oxide surface film on the nickel-aluminum reaction at the surface of aluminum brazing sheet has been investigated. Samples were anodized in a barrier-type solution and subsequently sputtered with nickel. Differential scanning calorimetry (DSC) and metallography were used as the main investigative techniques. The thickness of the anodic film was found to control the reaction between the aluminum substrate and nickel coating. Solid-state formation of nickel-aluminum intermetallic phases occurred readily when a relatively thin oxide film (13 to 25 nm) was present, whereas intermetallic formation was suppressed in the presence of thicker oxides (~60 nm). At an intermediate oxide film thickness of ~35 nm, the Al3Ni phase formed shortly after the initiation of melting in the aluminum substrate. Analysis of DSC traces showed that formation of nickel-aluminum intermetallic phases changed the melting characteristics of the aluminum substrate, and that the extent of this change can be used as an indirect measure of the amount of nickel incorporated into the intermetallic phases.

Determination of degradation kinetics of polyvinyl alcohol/X-zeolite nanocomposite

Poly(vinyl alcohol) (PVA) containing Ag-modified X-zeolite (PVA/X-zeolite) nanocomposite was successfully fabricated using solution casting technique. Morphology, structural and thermal properties of the pure PVA and its nanocomposite were characterized by FE-scanning electron microscopy (FE-SEM), energy-dispersive X-ray (EDX), X-ray diffraction, and differential scanning calorimetry (DSC), respectively. Results from DSC traces showed that the X-zeolite acts as efficient nucleating agent toward PVA crystallization. Photographs of FE-SEM demonstrate the nanosize and homogenous dispersion of the X-zeolite in PVA matrix. Moreover, EDX analysis confirmed the presence of constituent elements of the X-zeolite in the nanocomposite as well. Thermal degradation of PVA and PVA/X-zeolite nanocomposite was addressed in details by thermogravimetry analysis under non-isothermal conditions. Similar to pure PVA, the PVA/X-zeolite nanocomposite thermally degraded in two steps ranged from 400 to 690 K and 700 to 780 K, respectively. Values of the apparent activation energies were estimated using Friedman’s isoconversional method. A strong dependence of the Ea on conversion (α) was observed. To confirm the anticipated reaction models, differential master plot analysis was applied to the experimental data. Results showed that the degradation of PVA and its nanocomposite could be described by the reaction-order (A type) kinetic model.