Nonisothermal crystallization behaviors and conductive properties of PEO‐based solid polymer electrolytes containing yttrium oxide nanoparticles

Lithium solid polymer electrolytes (SPE) composed of polyethylene oxide (PEO) and yttrium oxide (Y₂O₃) nanoparticles were prepared. The influence of the Y₂O₃ nanoparticles on the non‐isothermal crystallization behaviors, crystal structure, and conductive properties of the SPE were investigated. The peak temperature, crystallinity, and crystallization half‐time (t_1/2) of the SPE were strongly dependent on the concentration of Y₂O₃ and the cooling rate. The non‐isothermal crystallization data were analyzed by the modified Avrami model, which successfully described the nonisothermal crystallization process of the SPE. The Avrami exponents suggested that the Y₂O₃ nanoparticles significantly affected both the nucleation mechanism and crystal growth of the PEO matrix. The nucleating and crystallization activation energies (ψ and E_c) estimated with different theories indicated that the Y₂O₃ nanoparticles were inclined to serve as heterogeneous nucleating agents to benefit the crystallization at lower concentration whereas as physical hindrance to inhibit the crystal growth at relatively higher concentration. The maximum conductivity (σ) of 5.95 × 10^?5 S cm^?1 at room temperature for the SPE was obtained at the Y₂O₃ weight ratio of 0.10. POLYM. ENG. SCI., 2011. © 2011 Society of Plastics Engineers     

Effect of nano‐TiO2 dispersion on PEO polymer electrolyte property

Polymer electrolyte membranes based on poly(ethylene oxide) (PEO) doped with TiO₂ nanoparticles were synthesized by simple solution cast technique. Mesoporous TiO₂ film was prepared by doctor‐blade method. The modified polymer membranes and the mesoporous films were characterized by SEM, TEM, AFM, ionic conductivity, and J‐V measurements. Dye‐sensitized solar cells (DSSC) have been fabricated in which PEO‐polymer electrolyte doped with and without nano‐TiO₂ were sandwiched between porous TiO₂ and counter electrodes. The DSSC with nano‐TiO₂ doped polymer electrolyte shows better performance (1.68%) in comparison with pristine polymer electrolyte (1.07%), which is due to improved ionic conductivity value in polymer electrolyte system by nano‐TiO₂ doping. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Preparation and ionic conductivity of solid polymer electrolyte based on polyacrylonitrile‐polyethylene oxide

The transparent and flexible solid polymer electrolytes (SPEs) were fabricated from polyacrylonitrile‐polyethylene oxide (PAN‐PEO) copolymer which was synthesized by methacrylate‐headed PEO macromonomer and acrylonitrile. The formation of copolymer is confirmed by Fourier‐transform infrared spectroscopy (FTIR) measurements. The ionic conductivity was measured by alternating current (AC) impedance spectroscopy. Ionic conductivity of PAN‐PEO‐LiClO₄ complexes was investigated with various salt concentration, temperatures and molecular weight of PEO (Mn). And the maximum ionic conductivity at room temperature was measured to be 3.54 × 10^?4 S/cm with an [Li⁺]/[EO] mole ratio of about 0.1. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 101: 461–464, 2006     

Nanocomposite solid polymer electrolytes based on polyethylene oxide,modified nanoclay,and tetraethylammonium tetrafluoroborate for application in solid‐state supercapacitor

Nanocomposite solid polymer electrolytes (SPEs) have been prepared from polyethylene oxide (PEO), organically modified nanoclay (MNclay), and tetraethylammonium tetrafluoroborate (TEABF₄) salt. The concentration of the salt has been varied in the respective SPE, wherein PEO/MNclay ratio was kept constant. It has been proposed that three types of complex formation could be operative in the SPEs due to the interactions among PEO, MNclay, and the salt. The complex formation mechanism has been postulated on the basis of X‐ray diffraction (XRD) analysis, transmission electron microscopic (TEM) observation, differential scanning calorimetric (DSC) analysis, and polarized optical microscopic (POM) observation. ‘Complex 1’ and ‘complex 3’ formation could be involved in the crystalline phase as indicated by DSC and XRD analyses, whereas ‘complex 2’ formation might be restricted in the amorphous phase as suggested by TEM observation. The ionic conductivity of the SPEs has been correlated with the results obtained from XRD, DSC, and POM analyses. The formation of complex 1 and complex 2 could be responsible for the increase in the ionic conductivity, whereas complex 3 formation might decrease the ionic conductivity. An activated carbon‐based supercapacitor has been fabricated using SPEs and characterized by cyclic voltammetry, galvanostatic ‘charge–discharge’ behavior, and impedance spectroscopic analysis. POLYM. ENG. SCI., 55:1536–1545, 2015. © 2015 Society of Plastics Engineers     

Comparison of the performance of copper oxide and yttrium oxide nanoparticle based hydroxylethyl cellulose electrolytes for supercapacitors

Biodegradable solid polymer electrolyte (SPE) systems composed of hydroxylethyl cellulose blended with copper(II) oxide (CuO) and yttrium(III) oxide (Y₂O₃) nanoparticles as fillers, magnesium trifluoromethane sulfonate salt, and 1‐ethyl‐3‐methylimidazolium trifluoromethane sulfonate ionic liquid were prepared, and the effects of the incorporation of CuO and Y₂O₃ nanoparticles on the performance of the SPEs for electric double‐layer capacitors (EDLCs) were compared. The X‐ray diffraction results reveal that the crystallinity of the SPE complex decreased upon inclusion of the Y₂O₃ nanoparticles compared to CuO nanoparticles; this led to a higher ionic conductivity of the Y₂O₃‐based SPE [(3.08 ± 0.01) × 10^?4 S/cm] as compared to CuO [(2.03 ± 0.01) × 10^?4 S/cm]. The EDLC performances demonstrated that the cell based on CuO nanoparticles had superior performance in terms of the specific capacitance, energy, and power density compared to the Y₂O₃‐nanoparticle‐based cell. However, Y₂O₃‐nanoparticle‐based cell displayed a high cyclic retention (91.32%) compared to the CuO‐nanoparticle‐based cell (80.46%) after 3000 charge–discharge cycles. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134 , 44636.     

Synthesis and characterization of SrBi4Ti4O15ferroelectric filler based composite polymer electrolytes for lithium ion batteries

Composite polymer electrolytes (CPEs) based on poly (ethylene oxide) (PEO) (Mol.Wt ∼6×10⁵) complexed with LiN(CF₃SO₂)₂ lithium salt and SrBi₄Ti₄O₁₅ ferroelectric ceramic filler have been prepared as films. Citrate gel technique and conventional solid state technique were employed for the synthesis of the ferroelectric fillers in order to study the effect of particle size of the filler on ionic conductivity of the polymer electrolyte. Characterization techniques such as X-ray diffraction (XRD), differential thermal analysis (DTA), scanning electron microscopy (SEM) and temperature dependant DC conductivity studies were taken for the prepared polymer composite electrolytes. The broadening of DTA endotherms on addition of ceramic fillers to the polymer salt complex indicated the reduction in crystallinity. An enhancement in conductivity was observed with the addition of SrBi₄Ti₄O₁₅ as filler to the (PEO)₈-LiN(CF₃SO₂)₂ polymer salt complexes. Among the investigated samples (PEO)₈-LiN(CF₃SO₂)₂ +10 wt% SrBi₄Ti₄O₁₅ (citrate gel) polymer composite exhibits a maximum conductivity.     

Influence of molar mass on the thermal properties,conductivity and intermolecular interaction of poly(ethylene oxide) solid polymer electrolytes

The sample preparation pathway of solid polymer electrolytes (SPEs ) influences their thermal properties, which in turn governs the ionic conductivity of the materials especially for systems consisting of a crystallizable constituent. Majority of poly(ethylene oxide) (PEO)‐based SPEs with molar masses of PEO well above 10⁴ g mol^?1 (where PEO is crystallizable and should reach an asymptote in thermal behaviour) display molar mass dependence of the thermal properties and ionic conductivities in non‐equilibrium conditions, as reported in the literature. In this study, PEO of different viscosity‐molar masses (M _η = 3 × 10⁵, 6 × 10⁵, 1 × 10⁶, 4 × 10⁶ g mol^?1) and LiClO₄ salt (0 to 16.7 wt%) were used. The SPEs were thermally treated under inert atmosphere above the melting temperature of PEO and then cooled down for subsequent isothermal crystallization for sufficient experimental time to develop morphology close to equilibrium conditions. The thermal properties (e.g. glass transition temperature, melting temperature, crystallinity) according to differential scanning calorimetry and the ionic conductivity obtained from impedance spectroscopy at room temperature (σ _DC ～ 10^?6 S cm^?1) demonstrate insignificant variation with respect to the molar mass of PEO at constant salt concentration. These findings are in agreement with the PEO crystalline structures using X‐ray diffraction and ion ? dipole interaction by Fourier transform infrared results. © 2017 Society of Chemical Industry     

In Situ synthesis of inorganic filler‐filled polyethylene using polyethersulfone‐supported TiCl4 catalyst system

In situ ethylene polymerizations with inorganic fillers were performed using catalyst based on titanium tetrachloride supported on polyethersulfone. The inorganic fillers used were MgO, TiO₂, and CaCO₃, which were pretreated with cocatalyst (methylaluminoxine) for better dispersion onto the polymer matrix. The formation of polyethylene (PE) within the whole matrix was confirmed by Fourier transform infrared studies. The wide‐angle X‐ray diffraction profile of the synthesized PEs indicated the presence of crystalline region. It was found that the nature of inorganic filler did not have any remarkable effect on the melting characteristics of the polymer, but the degree of crystallinity of PE was found to be higher for TiO₂‐filled PE. The amount of filler incorporated into the matrix was also evaluated through thermogravimetric analysis, where TiO₂‐filled PE showed ～ 49% of filler material, which was also reflected in the higher productivity obtained by this system. The morphology of the filler‐filled PEs was different, whereas the elemental dispersion was found to be uniform on the surface as elucidated through energy‐dispersive X‐ray spectroscopy. © 2010 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Structural characterization of new poly(ethylene oxide)-based alkaline solid polymer electrolytes

A new class of alkaline solid polymer electrolytes (SPEs) based on poly(ethylene oxide) (PEO), potassium hydroxide (KOH), and water was investigated. The structure of the SPEs was studied by differential scanning calorimetry, thermogravimetric analysis (TGA), X-ray diffraction, and optical microscopy techniques. The existence of a crystalline complex between PEO, KOH, and H₂O was evidenced for some compositions, depending on the O/K ratio. A possible structure was proposed, and a schematic phase diagram was established for this PEO–KOH–H₂O system. The first conductivity measurements also revealed the great interest of these systems, with conductivity values up to 10^-3 S/cm. © 1997 John Wiley & Sons, Inc. J Appl Polym Sci 65:601–607, 1997     

A Novel Top‐Seeded Infiltration Growth Technique for Fabricating Y–Ba–Cu–O Single‐Grain Superconductor Nano‐Composites

Top‐seed infiltration and growth technique (TSIG) is proposed to fabricate Y–Ba–Cu–O (YBCO) single‐grain superconductor nano‐composites, in which a solid source composition of nano‐Y₂O₃ + BaCuO₂ and a liquid source composition of Y₂O₃ + 10BaO + 16CuO are employed. As can be seen, this novel technique uses just one source of precursor powder of BaCuO₂, so it is more simplified and efficient. Microstructural observation indicates that fine Y₂BaCuO₅ (Y‐211) inclusions with a size from dozens of nanometers to about one hundred nanometers are successfully introduced in YBa₂Cu₃O_7?x (Y‐123) superconducting matrix, which can act as more effective pinning centers for improving the bulk performance. Superconducting property measurement shows that, a maximum trapped field of 0.36044 T is present at the center of the sample after magnetization by a permanent magnet (B = 0.5 T). These results prove that our proposed TSIG technique is a practical method for fabricating YBCO bulk superconductor nano‐composites with high performance.     

Design and fabrication of electro‐conductive polymer nanocomposites with mechanical and thermal resistance

The commencement of the industrial revolution paved the way for the fabrication of flexible polymers with high‐strength metalloceramics as novel materials of all kinds. Fabricating metal–ceramic/polymer conductive composites is one such dimension followed for the present research work making use of the properties of the three components. Electroless deposition, for permanent metallic coating, was performed to coat Al₂O₃ with metallic Cu followed by the inclusion of the Cu–Al₂O₃ filler into a poly(vinyl chloride) (PVC) matrix. X‐ray diffraction and energy‐dispersive X‐ray studies predicted a prominent growth of metallic Cu crystallites onto Al₂O₃ with an increased average size and variation in elemental composition, respectively, when compared to pristine Al₂O₃. Morphological behaviour via scanning electron microscopy also envisioned uniform Cu coating onto Al₂O₃ and a homogeneous dispersion throughout the polymer matrix. When incorporated into PVC, electrical conductivity analysis highlighted a distinct variation in composite phases from insulating (7.14 × 10^?16 S cm^?1) to semiconducting behaviour (8.33 × 10^?5 S cm^?1) as a function of Cu–Al₂O₃ filler. Mechanical behaviour (tensile strength, Young's modulus and elongation at break) and thermal properties of the prepared composites also indicated a substantial improvement in material strength with Cu–Al₂O₃ incorporation. The enhanced electrical conductivity along with improved thermomechanical status with significant filler–matrix interaction permits the potential usage of such novel composites in a range of state‐of‐the‐art semiconducting electronic devices. © 2018 Society of Chemical Industry     

Significant Improvement of Superconducting Properties in Nano‐NiFe2O4‐Doped Y–Ba–Cu–O Single‐Grain Superconductor

Introduction of refined second‐phase particles in superconducting YBa₂Cu₃O_7?x (Y‐123) matrix is known to be an effective route to improve the δl‐type pinning and the performance of Y–Ba–Cu–O (YBCO) single‐grain superconductors, while the δT_c‐type pinning induced by spatial fluctuations in matrix composition is also important and contributes to the in‐field J_c performance and high‐field applications of bulk superconductors. In this communication, chemical doping of nano‐sized NiFe₂O₄ (mean size 50 nm) in single‐grain YBCO superconductor is performed using a novel top‐seeded infiltration growth (TSIG) technique based on a solid source pellet (SSP) of nano‐Y₂O₃ + BaCuO₂. The results indicate that, significant improvement of bulk performances including levitation force (33.93 N) and trapped field (0.3628 T) has been observed in the 0.2 wt% nano‐NiFe₂O₄‐doped sample, which are much higher than the undoped sample (28.81 N and 0.2754 T). T_c measurement indicates that, a decreased onset T_c of about 87.5 K and a broadened transition width of about 5 K are observed in the NiFe₂O₄‐doped sample, indicating appearance of weak superconducting regions in superconducting matrix caused by Ni and Fe substitutions in Y‐123 crystal lattice. This study supplies a practical approach to increase the YBCO bulk performance significantly.     

Morphological characterization of γ-LiAlO2-filled composite polymer electrolytes containing LiPF6

Morphological properties of composite polymer electrolytes based on blends of polyethylene oxide (PEO) and a perfluorinated polyphosphazene (PPz) containing LiPF₆ as lithium salt and a finely divided ceramic filler, γ-LiAlO₂, were studied by using polarizing optical microscopy and differential scanning calorimetry (DSC). A parallel study was performed on propylene carbonate plasticized composite polymer electrolytes. Results indicate that both the morphology and the thermal properties depend upon the composition of the polymer host, a result not observed in composite polymer electrolytes having the same polymer composition containing LiCF₃SO₃ as lithium salt. The incorporation of the ceramic filler at the lower concentration tested (10% by wt) has practically no effect on the thermal behavior of the samples; whereas, differences were clearly distinguished at a concentration of ceramic material of 20 wt %. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 73: 1023–1030, 1999     

Fabrication and characterization of PEO/PPC polymer electrolyte for lithium‐ion battery

A new poly(propylene carbonate)/poly(ethylene oxide) (PEO/PPC) polymer electrolytes (PEs) have been developed by solution‐casting technique using biodegradable PPC and PEO. The morphology, structure, and thermal properties of the PEO/PPC polymer electrolytes were investigated by scanning electron microscopy, X‐ray diffraction, and differential scanning calorimetry methods. The ionic conductivity and the electrochemical stability window of the PEO/PPC polymer electrolytes were also measured. The results showed that the T_g and the crystallinity of PEO decrease, and consequently, the ionic conductivity increases because of the addition of amorphous PPC. The PEO/50%PPC/10%LiClO₄ polymer electrolyte possesses good properties such as 6.83 × 10^?5 S cm^?1 of ionic conductivity at room temperature and 4.5 V of the electrochemical stability window. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Nanocomposite polymer electrolytes for solid-state lithium-ion batteries with enhanced electrochemical properties

Solid-state polymer electrolytes (SPEs) have attracted significant attention owing to their improvement in high energy density and high safety performance. However, the low lithium-ion conductivity of SPEs at room temperature restricts their further application in lithium-ion batteries (LIBs). Herein, we propose a novel poly (ethylene oxide) (PEO)-based nanocomposite polymer electrolytes by blending boron-containing nanoparticles (BNs) in the PEO matrix (abbreviated as: PEO/BNs NPEs). The boron atom of BNs is sp²-hybridized and contains an empty p-orbital that can interact with the anion of lithium salt, promoting the dissociation of the lithium salts. In addition, the introduction of the BNs could reduce the crystallinity of PEO. And thus, the ionic conductivity of PEO/BNs NPEs could reach as high as 1.19 × 10⁻³ S cm⁻¹ at 60°C. Compared to the pure PEO solid polymer electrolyte (PEO SPEs), the PEO/BNs NPEs showed a wider electrochemical window (5.5 V) and larger lithium-ion migration number (0.43). In addition, the cells assembled with PEO/BNs NPEs exhibited good cycle performance with an initial discharge capacity of 142.5 mA h g⁻¹ and capacity retention of 87.7% after 200 cycles at 2 C (60°C).     

Preparation of nano‐reinforced thermal conductive natural rubber composites

Natural rubber (NR) composites highly filled with nano‐α‐alumina (nano‐α‐Al₂O₃) modified in situ by the silane coupling agent bis‐(3‐triethoxysilylpropyl)‐tetrasulfide (Si69) were prepared. The effects of various modification conditions and filler loading on the properties of the nano‐α‐Al₂O₃/NR composites were investigated. The results indicated that the preparation conditions for optimum mechanical (both static and dynamic) properties and thermal conductivity were as follows: 100 phr of nano‐α‐Al₂O₃, 6 phr of Si69, heat‐treatment time of 5 min at 150°C. Furthermore, two other types of fillers were also investigated as thermally conductive reinforcing fillers for the NR systems: (1) hybrid fillers composed of 100 phr of nano‐α‐Al₂O₃ and various amounts of the carbon black (CB) N330 and (2) nano‐γ‐Al₂O₃, the particles of which are smaller than those of nano‐α‐Al₂O₃. The hybrid fillers had better mechanical properties and dynamic performance with higher thermal conductivity, which means that it can be expected to endow the rubber products serving under dynamic conditions with much longer service life. The smaller sized nano‐γ‐Al₂O₃ particles performed better than the larger‐sized nano‐α‐Al₂O₃ particles in reinforcing NR. However, the composites filled with nano‐γ‐Al₂O₃ had lower thermal conductivity than those filled with nano‐α‐Al₂O₃ and badly deteriorated dynamic properties at loadings higher than 50 phr, both indicating that nano‐γ‐Al₂O₃ is not a good candidate for novel thermally conductive reinforcing filler. POLYM. COMPOS., 37:771–781, 2016. © 2014 Society of Plastics Engineers     

Degradation of Nextel™ 610‐based oxide‐oxide ceramic composites by aluminum oxychloride decomposition products

Nextel? 610 alumina fibers and alumina‐YAG (yttrium‐aluminum garnet) matrices were used to make oxide‐oxide ceramic matrix composites (CMCs) with and without monazite (LaPO₄) fiber‐matrix interfaces. Twelve sequential aluminum oxychloride (AlOCl) infiltrations with 1 hour heat treatments at 1100°C and a final 1 hour heat treatment at 1200°C were used for matrix densification. This matrix processing sequence severely degraded CMC mechanical properties. CMC tensile strengths and interlaminar tensile (ILT) strengths were less than 10 MPa and 1 MPa, respectively. Axial fracture of Nextel? 610 fibers was observed after ILT testing, highlighting the extreme degradation of fiber strength. Extensive characterization was done to attempt to determine the responsible degradation mechanisms. Changes in Nextel? 610 fiber microstructure after CMC processing were characterized by optical microscopy, SEM, and extensively by TEM. In AlOCl degraded fibers, grain boundaries near the fiber surface were wetted with a glass that contained Y₂O₃/SiO₂ or Y₂O₃/La₂O₃/P₂O₅/SiO₂, and near‐surface pores were partially filled with Al₂O₃. This glass must also contain some Al₂O₃ and initially some chlorine. AlOCl decomposition products were predicted using the FactSage^® Thermochemical code, and were characterized by mass spectrometry. Effects of AlOCl precursors on monazite coated and uncoated Nextel? 610 fibers tow and filament strength were evaluated. A mechanism for the severe degradation of the oxide‐oxide CMCs and Nextel? 610 fibers that involves subcritical crack growth promoted by release of chlorine containing species during breakdown of intergranular glasses in an anhydrous environment is proposed.     

Polyvinylidene fluoride‐based novel polymer electrolytes for magnesium‐rechargeable batteries with Mg(CF3SO3)2

Magnesium trifluoromethanesulfonate (Mg (CF₃SO₃)₂)‐based polymer electrolytes (PEs) have been prepared with polyvinylidene fluoride (PVdF) as a host matrix. Tetraglyme and tetrabutyl ammonium chloride (TBACl) were used as plasticizer and filler, respectively, in the matrix by solution‐casting technique. The electrolyte containing 5 wt % TBACl exhibits the conductivity of 0.442 mS cm^?1 at ambient temperature. X‐ray diffraction study reveals the amorphous nature of the PE. Linear sweep voltammetry was also performed to evaluate the decomposition potential of the electrolyte. The morphological features were analyzed by scanning electron microscope. The activation energy has also been calculated, which corroborates the ionic conductivity results. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Fabrication,characterization, and properties of poly(ethylene‐co‐vinyl acetate)/magnetite nanocomposites

Poly(ethylene‐co‐vinyl acetate) (EVA)/magnetite (Fe₃O₄) nanocomposite was prepared with different loading of Fe₃O₄ nanoparticles. The mixing and compounding were carried out on a two‐roll mixing mill and the sheets were prepared in a compression‐molding machine. The effect of loading of nanoparticles in EVA was investigated thoroughly by different characterization technique such as transmission electron microscopy (TEM), X‐ray diffraction (XRD), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), limiting oxygen index (LOI), and technological properties. TEM analysis showed the uniform dispersion of filler in the polymer matrix and the dispersion of filler decreased with increase in filler content. XRD of the nanocomposite revealed the more ordered structure of the polymer chain. An appreciable increase in glass transition temperature was observed owing to the restricted mobility of Fe₃O₄‐filled EVA nanocomposite. TGA and flame resistance studies indicated that the composites attain better thermal and flame resistance than EVA owing to the interaction of filler and polymer segments. Mechanical properties such as tensile strength, tear resistance, and modulus were increased for composites up to 7 phr of filler, which is presumably owing to aggregation of Fe₃O₄ nanoparticle at higher loading. The presence of Fe₃O₄ nanoparticles in the polymer matrix reduced the elongation at break and impact strength while improved hardness of the composite than unfilled EVA. The change in technological properties had been correlated with the variation of polymer–filler interaction estimated from the swelling behavior. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40116.     

Preparation and characterization of nano‐Sb2O3/poly(butylene terephthalate) composite powders based on high‐energy ball milling

In this work, a kind of composite powders with good dispersion and distribution of nano‐Sb₂O₃ particles in poly(butylene terephthalate) (PBT) was prepared by the high‐energy ball milling (HEBM). The effects of the milling time on the structure, morphology, particle size distribution, and thermal behavior of the nano‐Sb₂O₃/PBT composite powders were characterized by Fourier transform infrared spectroscopy, scanning electron microscope, laser diffraction particle size analyzer, and thermal analysis (TGA, DTG and DSC) techniques. The results showed that the regular shape of PBT powders was converted into flakes and the nano‐Sb₂O₃ particles were well deagglomerated and better dispersed in the PBT matrix during the HEBM process. The mechanochemical activation that was provided by the HEBM process caused a reduction in the molecular weight of PBT, which result in favoring the first step of thermal degradation. Furthermore, two T_g’s were obtained in the case of the nanocomposite powders when the milling time was over 3 h, one of them being slightly higher than that of the pure PBT, which indicated that there was a special interaction between PBT and nano‐Sb₂O₃ particles. However, the HEBM process leaded to a decreasing of the PBT crystallinity. J. VINYL ADDIT. TECHNOL., 25:91–97, 2019. © 2018 Society of Plastics Engineers