Properties of polyamide 6 and thermoplastic polyurethane blends containing modified montmorillonites

In this paper are reported some experimental data related to the influence of preparation regimes and characteristics of exfoliated graphite based sorbents produced by thermal expansion of H₂SO₄-graphite intercalation compounds (H₂SO₄-GICs) on their sorption properties. Investigations involving X-ray diffraction analyses, surface area, bulk density and oil sorption capacity measurements, have been performed. Sorption capacity was discussed as a function of bulk density, total pore volume and surface area. Some empirical correlation between studied characteristics of exfoliated graphite have been found. The differences among the obtained samples, as a consequence of synthesis conditions, were also put in evidence by thermal analysis (TG, DTG and DTA) performed after their exposure to oil sorption.It was found that thermal analysis method could provide information about the exfoliated graphite pore system related to the sorbed oil oxidation rate. The capacity for oil uptake was also discussed in the case of graphite oxide soot.     

Thermal exfoliation of electrochemically synthesized graphite intercalation compound with perrhenic acid

In present work, we describe the synthesis of graphite intercalation compounds with perrhenic acid (HReO₄-GIC) through the anodic oxidation of graphite in aqueous perrhenic acid solution and their thermal exfoliation. Due to electrochemical treatment of graphite in perrhenic acid solution, ReO₄⁻ ions are intercalated into interlayer spaces of graphite. Anodic oxidation of graphite in HReO₄ solution leads to the formation of 3-stage GIC. Simultaneously, some amount of perrhenic acid becomes deposited on the graphite surface and edges. In the next step, thermal treatment of the previously synthesized GIC was performed, causing both the exfoliation of graphitic structure and transformation of perrhenic acid into rhenium oxides on the surface of graphene layers. The yielded product was exfoliated graphite-ReO₂/ReO₃ composite. The obtained composite was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and Raman spectroscopy. Additionally, specific surface area of the exfoliated materials was measured.

     

Studies on Thermal Stability of Titanium Substituted Iron Molybdenum Spinel Oxide

The thermal stability of the solid solutions of Fe₂Mo_1–xTi_xO₄ for x=0.0 to 1.0 in air, had been investigated in the temperature range 303–1173 K using differential thermal analysis and thermogravimetry (DTA and TG). The products obtained by heating the sample in air, at different temperatures, have been characterized by X-ray diffraction and IR-studies. The results show that all the ferrite samples undergo surface oxidation during initial heating. On heating to 823 K, the samples undergo oxidation of the octahedral site cations only and forma cation deficient spinel phase. On further heating in air, the ferrites undergo complete oxidation. This revised version was published online in July 2006 with corrections to the Cover Date.     

PtPd-nanoparticles supported by new carbon materials

Nanocomposites based on PtPd nanoparticles with chemical ordering like disordered solid solution on surface of multilayer graphene have been prepared through thermal shock of mechanically obtained mixture of double complex salt [Pd(NH₃)₄][PtCl₆] and different carbon materials–exfoliated graphite, graphite oxide and graphite fluoride. An effect of original carbon precursors on formation of PtPd bimetallic nanoparticles was studied using X-ray absorption spectroscopy (XAFS), transmission electron microscopy (TEM) and X-ray photoelectron spectroscopy (XPS). It was shown that the distribution of bimetallic nanoparticles over the multilayer graphene surface as well as the particles size distribution is controlled by the graphene precursors. For all nanocomposites, the surface of the nanoparticles was found to be Pd-enriched. In case when the thermal exfoliated graphite and graphite oxide were used as the graphene precursors a thin graphitized layer covered the nanoparticles surface. Such a graphitized layer was not observed in the nanocomposite, which used the fluorinated graphite as the precursor.     

Formation,dissociation and expansion behavior of platinum group metal oxides (PdO,RuO2, IrO2)

The oxidation behavior of palladium, ruthenium and iridium powders of different grain sizes was investigated by TG, DTA and X-ray methods. The solid oxides formed during heating up (PdO, RuO₂, IrO₂) show different stability and decomposition temperatures depending on the oxygen pressure. The kinetics of the reaction MeO_x → Me+x/2 O₂ is discussed. High temperature X-ray studies confirmed the strong anisotropy of thermal expansion in the case of RuO₂ and IrO₂. The thermal expansion behavior of these oxides is compared to that of other rutile-type oxides.     

氧化环境和比例对改性Hummers法制备GO的影响

以鳞片石墨(GR)为原料,采用改性Hummers法液相氧化方法制备氧化石墨,通过超声剥离的方法剥离出片状的氧化石墨烯(GO),探讨了H₂SO₄环境与H₂SO₄+H₃PO₄混酸环境和KMnO₄与GR的比例对GO制备的影响。采用FTIR、UV、TG、XRD、SEM和XPS等分析手段对制备的GO进行分析。结果表明：GO外貌是呈褶皱片状,在片层上主要有C=O、C-OH、-COOH和C-O-C等官能团,以共价键形式存在石墨层间;通过TG与XPS数据分析表明在H₂SO₄ H₃PO₄混酸环境下制备的GO含氧官能团较多,并且(KMnO₄)与鳞片石墨的最佳比例是1:4。     

The activity of dispersed oxides on natural and exfoliated graphite surfaces

Experimental data obtained indicate that ion exchange on the graphite surface can be attributed to impurity oxides. During exfoliated graphite oxidation reactions, inorganic oxides act as catalysts (Fe₂O₃, Cr₂O₃), inhibitors (B₂O₃, Al₂O₃) or are inert.     

Studies on thermal decomposition of electrochemically oxidized glass-like carbon

Glass-like carbon (GC) tiles were electrochemically oxidized in 1 mol·dm^?3 H₂SO₄ solution at a potential of 2.3 V/SCE. The surfaces of the oxidized samples were examined by scanning electron microscopy (SEM). The solid oxidation products were studied by derivatographic (TG, DTG and DTA) and elemental analyses. The solid products of electrochemical oxidation of GC, with the general formula C₈O_4.2H_2.3 were thermolabile and revealed properties similar to those of graphite oxide. They are hydrophylic and their thermal decomposition proceeds in three steps: (i) evaporation of-chemisorbed water (320–400 K), (ii) exothermic decomposition of graphite oxide (370–430 K), and (iii) gradual decomposition of the oxidation products (>430 K).     

Catalytic effect analysis of metallic additives on light crude oil by TG and DSC tests

This research aimed at the investigation of the effect of different metallic additive on the combustion and kinetic behavior of crude oil. For this purpose, the thermal behavior of the oil-only and oil–metallic salts mixtures were studies by the thermogravimetry (TG)/derivative thermogravimetry and differential scanning calorimetry (DSC) on heating rate at 10 °C min^?1. The result shows that Dagang crude oil exhibited apparent low temperature oxidation (LTO), fuel deposition, and high temperature oxidation processes. With the addition of metallic salts, the LTO process has been shortened and samples added CuSO₄, CrCl₃·6H₂O, and AlCl₃·6H₂O achieved a much lower peak temperature than that of oil. Based on the Arrhenius model, metallic additives were proven to have obvious influence on the combustion activation energy. And, by comprehensive analysis of TG/DSC profile and activation energy, ZnSO₄ exhibited a positive influence on light crude oil combustion during the high pressure air injection process.     

A thermal analysis investigation of new insulator compositions based on EPDM and phenolic resin

New rocket insulator compositions have been studied by adding various types and amounts of fillers, such as graphite and asbestos fibres, Al₂O₃, MgZrO₂, Cr₂O₃, SiC, carbon powders and phenolic resin to the base EPDM gum and graphite, kevlar,E type glass fibres to the base phenolic resin in order to improve thermal and ablative efficiency. The degradation of the insulators has been investigated by thermogravimetry (TG) analysis to 900°C and DSC analysis to 500°C. Conversion curves of the insulators at different heating rates were performed and maximum degradation temperatures were found as 646 and 661°C for EPDM P and phenolic resin, respectively. The kinetic parameters for degradation have been evaluated and the lifetime of the rocket insulators has been estimated. Thermal analysis has been conducted on the insulators and the indepth temperature distribution was evaluated in order to find optimum insulation thickness.     

Solid—liquid phase diagrams of mixtures containing substituted phenols and amine mixtures

The thermal decomposition of CaCO₃ was studied under high vacuum by means of both TG and the more recently developed constant decomposition rate thermal analysis (CRTA) which allows the monitoring of both reaction rate and the residual pressure over the sample. The reliability of the kinetic results seems to be much higher with the latter technique which actually allows the reduction of the reaction rate and therefore the heat and mass transfer effects over a broad range of sample size. For instance, it was necessary, by conventional TG started under a vacuum of 2 10^?6 torr with a heating rate of 0.5 K min^?1, to lower the amount of sample to 2 mg in order to obtain the same activation energy as that calculated from CRTA with various samples weighing up to 50 mg. The TG experimental conditions quoted above (and which are upper limits of mass and heating rate) are beyond the limit of sensitivity of most available conventional TG equipment.     

Effect of atmosphere and heating rate on mechanism of MoSi<Subscript>2</Subscript> formation during self-propagating high-temperature synthesis

To study the effect of atmospheric type and heating rate on formation mechanism of MoSi₂, the Mo + 2Si powder mixture was exposed to simultaneous thermal analysis (STA) in air atmosphere at different heating rates (10, 15, and 20 °C/min). To further study the changes, thermal analyses of molybdenum powders and consumed silicon were also performed separately. An amount of aluminum powder (5 wt.%) was also added to Mo + 2Si powder mixture and exposed to thermal analysis at different heating rates (10, 15, and 20 °C/min) to study the effect of the presence of active elements (like aluminum) on the trend of the performance of changes. To perform phase studies on the products of the thermal analysis at a later stage, each product was separately tested by an X-ray diffraction (XRD) method. Contrary to expectations, the XRD patterns showed that the trends of changes during thermal analysis were not in the direction of MoSi₂, and the DTA–TG peaks obtained from these analyses were in fact related to other changes. Ultimately, the results showed that the peaks on the DTA curves resulted from the oxidation of molybdenum particles; and the (MoO₃) melt of the product, and in continuation of the reduction of a part of this oxide, it resulted during the silicothermic and aluminothermy reactions. The results of this research also showed that with regard to the presence of intensive oxidation tendency of molybdenum particles, there is no chance for the formation of MoSi₂ by heating the powder mixture of Mo + 2Si in air atmosphere and at low heating rates.     

ZrB<Subscript>2</Subscript>/HfB<Subscript>2</Subscript>–SiC Ultra-High-Temperature Ceramic Materials Modified by Carbon Components: The Review

The review has been made of recent publications on modification of ZrB₂/HfB₂–SiC ultra-hightemperature ceramic composite materials (UHTC) by carbon components: amorphous carbon, graphite, graphene, fibers, and nanotubes. Available data have been presented on some aspects of oxidation of such materials at temperatures ≥1500°C and both at the atmospheric pressure and at the reduced oxygen partial pressure; structural features of the formed multilayer oxidized regions have been noted. It has been considered how the type and content of the carbon component and the conditions (first of all, temperature) of UHTC production affect the density, flexural strength, hardness, fracture toughness, and thermal and oxidation resistance of the modified ceramic composites.     

Thermal Behaviour of Tin(II) Complex With 8-hydroxyquinolinate in the Solid State

Tin(II) complexes with 8-hydroxyquinolinate in solid state have been obtained by adding aqueous ammonium to a solution containing stannous chloride and 8-hydroxiquinoline in medium of HCl and acetone up to pH 5 and 9, respectively. The products obtained show the same composition, Sn(C₉H₆ON)₂; however there are some differences regarding both the thermal behaviour in an oxidant atmosphere and morphology. These products were characterised by elemental and complexometric analysis, TG and DTA curves, infrared and X-ray diffractometry. TG curves show, above 448 K, the partial oxidation on air atmosphere of Sn(II) complexes to Sn(IV) complexes, SnO(C₉H₆ON)₂. This behaviour does not depend only on pH in which the compounds were obtained but also on the heating rate in TG curves. Sn(II) complexes volatilise almost completely on nitrogen atmosphere and partially on air atmosphere depending on the oxidation degree of the compound. This revised version was published online in July 2006 with corrections to the Cover Date.     

Polyethylene/graphite nanocomposites obtained by in situ polymerization

The synthesis of polyethylene/graphite nanocomposites by in situ polymerization was achieved using the catalytic system Cp₂ZrCl₂ (bis(cyclopentadienyl)zirconium(IV) dichloride)/methylaluminoxane (MAO). Graphite with nano dimensions, previously treated with MAO, was added into the reactor as filler at percentages of 1, 2, and 5% (w/w). XRD analysis showed that the chemical and thermal treatments employed preserve the structure of the graphite sheets. The formation of graphite nanosheets and nanocomposites was confirmed by TEM and AFM. TEM micrographics showed that the polyethylene grew between the graphene nanosheets, giving intercalated and exfoliated graphite nanocomposites. © 2009 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 48: 692–698, 2010     

Evaluation of PCM/diatomite composites using exfoliated graphite nanoplatelets (xGnP) to improve thermal properties

This paper deals with the thermal performances of shape-stabilized phase change materials (SSPCM) for energy saving in various fields. This study enhanced thermal properties of SSPCM using exfoliated graphite nanoplatelets (xGnP). SSPCM, which contains the xGnP, was prepared by mixing and melting techniques for high dispersibility, thermal conductivity, and latent heat storage. In the experiment, we used hexadecane, octadecane, and paraffin as phase change materials (PCMs), and they have 254.7, 247.6, and 144.6 J g^?1 of latent heat capacity, and melting points of 20.84, 30.4, and 57.09 °C, respectively. The characteristics of SSPCMs were determined using SEM, DSC, FTIR, TG, TCi, and Energy simulation. SEM morphology showed homogenous dispersion of PCM and xGnP in the porous diatomite. DSC analysis results showed the latent heat capacity of SSPCM and SSPCM/xGnP composites, and TG analysis results showed the thermal reliability of the samples. Also, we checked the thermal conductivity of the SSPCM that contains xGnP, by TCi analysis.     

Thermodegradation of poly(4-vinylpyridine-co-crotonic acid-co-divinylbenzene) and N-oxide derivatives

Copolymer networks based on 4-vinylpyridine (4VPy)/crotonic acid (CrA)/divinylbenzene (DVB) and their N-oxide derivatives have been investigated by thermogravimetric analysis (TG) to evaluate their thermal stability in nitrogen atmosphere at fixed heating rate. Thermal stability was determined from TG curves to investigate the influence of 4VPy content and introduction of N-oxide groups. The TG and DTG curves of unmodified copolymers clearly show two thermodegradation stage and the same kinetic pathway. The decomposition temperatures do not depend on the 4VPy content. The copolymers modified by oxidation present lower thermostability than unmodified showing that the introduction of N-oxide groups modifies their kinetic pathways. A kinetic model Ozawa was used to determine the kinetic parameters. The apparent thermal decomposition activation energies (ΔE_d) of the unmodified copolymer under nitrogen was higher than that in modified copolymer. Also, the characterizations of copolymer networks were done by Fourier transform infrared spectroscopy (FTIR).     

Thermodynamic analysis of radioactive graphite reprocessing by incineration in air and oxidation in molten salt

Reactor graphite waste of nuclear industry contains various radionuclides. This study deals with the behaviour of radioactive elements during thermal treatment of waste. Two thermal processes were simulated: incineration of graphite in air and oxidation of graphite in a molten salt, containing Na₂CO₃ + K₂CO₃ + 20 mass% PbO. Carbon oxides CO and CO₂, containing radioactive ¹⁴C, are the main components of the gaseous phase with partial pressures approximately 10⁴ Pa in both cases. More gaseous radionuclides are observed during incineration of graphite in air than during oxidation of graphite in the molten salt. In the latter case radionuclides are in the condensed state in the melt of sodium and potassium carbonates.     

Thermal studies on the starch-g-copolymers prepared from two terpene acrylate monomers under oxidative conditions

The simultaneous thermal studies (TG/DTG/DSC) coupled with the FTIR analysis of the gaseous decomposition products created under oxidative heating of starch-g-poly(neryl acrylate) and starch-g-poly(geranyl acrylate) copolymers have been presented. To these studies, the copolymers with the following grafting percents (G) were selected: starch-g-poly(neryl acrylate) copolymers: 36.6?±?0.3%, 40.3?±?0.4%, 42.8?±?0.4% and starch-g-poly(geranyl acrylate) copolymers: 28.9?±?0.2%, 32.4?±?0.6%, 35.6?±?0.4%. The performed tests proved that the thermal resistance of the copolymers was strongly dependent on their G values, despite a small difference in the G values between the samples. The slight increase (ca. 6.2–6.7%) in the G value caused the significant drop of the thermal stability of all the studied materials. The TG/DTG/DSC studies confirmed at least three-stage decomposition mechanism of the copolymers where simultaneous pyrolysis, oxidation, dehydration and decarboxylation processes took place. The TG/FTIR analyses showed the emission of various structure fragments; among them, one can mention the creation of some organic fragments such as aldehyde, acid, alkene, alkane, furan fragments, CH₄ and inorganic species (CO₂, CO, H₂O) as a result of the oxidative decomposition processes of the studied copolymers. In addition, the conducted studies demonstrated similar decomposition course and mechanism for both types of the copolymers, regardless of the monomer type used to the graft process.

     

Thermoanalytical study of heavier trivalent lanthanides fumarates

Solid-state heavier lanthanides fumarates compounds have been synthesized, and the compounds were characterized by employing simultaneous thermogravimetry and differential thermal analysis (TG–DTA), differential scanning calorimetry (DSC), Fourier transform infrared spectroscopy (FTIR), TG coupled to FTIR, elemental analysis, and complexometry. On heating, the dehydration occurs in a single and two consecutive steps and the thermal decomposition of the anhydrous compounds occurs in consecutive and/or overlapping steps, with formation of the respective oxides: Tb₄O₇ and Ln₂O₃ (Ln=Dy to Lu). The results also led to information about composition, thermal behavior, and the type of coordination of the isolated compounds.