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  • 1.
    Ahmed, Hesham M.
    KTH, School of Industrial Engineering and Management (ITM), Materials Science and Engineering, Materials Process Science.
    Investigations of the Kinetics of Reduction and Reduction/Carburization of NiO-WO3 Precursors.2010Doctoral thesis, comprehensive summary (Other academic)
    Abstract [en]

    Kinetic studies of reduction of the mixtures of NiO and WO3 having different Ni/(Ni+W) molar ratios in flowing hydrogen gas were investigated by means of Thermo Gravimetric Analysis (TGA), Fluidized Bed (FB) technique as well as Thermal diffusivity measurements under isothermal conditions. In the case of TGA, the reaction progress was monitored by mass loss, while evolved gas analysis by a gas chromatograph was the indicator of the reaction progress in the case of FB. The results indicate that the reduction reaction proceeds through three consecutive steps, viz.

    NiO-WO3 Ni-WO3 Ni-WO2 Ni-W

    The present results show that the fluidized bed technique can be successfully utilized in bulk production of intermetallics containing W and a transition metal (or a composite material) wherein the process conditions would have a strong impact on the particle size of the end product.

    During the investigations, it was found that there was a delay in the reaction during the hydrogen reduction of NiO-WO3 mixed oxides in a fluidized bed reactor. In order to understand the same, a theoretical model was developed to estimate the apparent reaction rate constant for the reduction reaction from the intrinsic chemical reaction rate constant. Appropriate differential mass balance equations based on intrinsic chemical reaction rate constants and thermodynamic equilibria were developed. The proposed model was successfully applied in predicting the overall reaction kinetics of a fluidized bed reactor. This model is also suitable for scale-up calculations.

    SEM images showed that the particle size of the final product was dependent on the Ni/(Ni+W) molar ratio; smaller particles were formed at higher nickel contents. X-ray diffractions of the reduced precursors exhibited slight shift of Ni peaks from the standard one indicating the dissolution of W into Ni.

    A new method for studying kinetics of the hydrogen reduction of NiO-WO3 precursors was developed in which the reaction progress was monitored by following the change of thermal diffusivity of the precursors. Activation energies of reduction as well as sintering were calculated. This method is considered unique as it provides information regarding the physical changes like sintering, change of porosity and agglomeration along with the chemical changes occurring during the gas/solid reaction.

    As a continuation of the kinetic studies, Ni-W-C ternary carbides were synthesized by simultaneous reduction–carburization of Ni-W-O system using H2-CH4 gas mixtures by TGA. The results showed that the reduction of the oxide mixture was complete before the carburization took place. The nascent particles of the metals formed by reduction could react with the gas mixture with well-defined carbon potential to form a uniform product of Ni-W-C. The above-mentioned experiments were conducted in such a way to ensure that the reaction was controlled by the chemical reaction. The activation energies of the reduction as well as carburization processes at different stages were calculated accordingly.

    The present dissertation demonstrates the potential of the investigations of gas/solid reactions towards tailoring the process towards materials with optimized properties as for example introduction of interstitials. The present process design is extremely environment-friendly with reduced number of unit processes and the product being H2O.

  • 2.
    Ahmed, Hesham M.
    et al.
    KTH, School of Industrial Engineering and Management (ITM), Materials Science and Engineering, Materials Process Science.
    El-Geassy, A. H. A.
    Seetharaman, Seshadri
    KTH, School of Industrial Engineering and Management (ITM), Materials Science and Engineering, Materials Process Science.
    Kinetics of Reduction of NiO-WO3 Mixtures by Hydrogen2010In: Metallurgical and materials transactions. B, process metallurgy and materials processing science, ISSN 1073-5615, E-ISSN 1543-1916, Vol. 41, no 1, p. 161-172Article in journal (Refereed)
    Abstract [en]

    The kinetics of reduction of the oxide mixtures of Ni-W with different Ni/(Ni-W) molar ratios within the range of 923 K to 1173 K in flowing hydrogen gas was investigated by means of thermogravimetric analysis under isothermal conditions. The products were examined by X-ray diffraction, scanning electron microscope (SEM), and electron dispersion spectroscopy (EDS) analyses. Five different oxide mixtures apart from the pure oxides were studied in the present work. The results indicate that the reduction reaction proceeds through three consecutive steps that are as follows: NiO-WO3 -> Ni-WO3 -> Ni-WO2 -> Ni-W From the experimental results, the Arrhenius activation energies of the three steps were evaluated for all of the studied compositions. The activation energy for the first step was calculated to be approximately 18 kJ/mol. For the second and third stages, the activation energy values varied from 62 to 38 kJ/mol for the second stage and 51 to 34 kJ/mol for the third stage depending on the Ni/(Ni + W) molar ratio in the precursors; the activation energy increased with increasing ratios. SEM images showed that the grain size of the final product was dependent on the Ni/(Ni + W) molar ratio; smaller grains were formed at higher nickel contents.

  • 3.
    Ahmed, Hesham M.
    et al.
    KTH, School of Industrial Engineering and Management (ITM), Materials Science and Engineering.
    El-Geassy, Abdel-Hady A.
    Viswanathan, Nurni Neelakantan
    Seetharaman, Seshadri
    KTH, School of Industrial Engineering and Management (ITM), Materials Science and Engineering.
    Kinetics and Mathematical Modeling of Hydrogen Reduction of NiO-WO(3) Precursors in Fluidized Bed Reactor2011In: ISIJ International, ISSN 0915-1559, E-ISSN 1347-5460, Vol. 51, no 9, p. 1383-1391Article in journal (Refereed)
    Abstract [en]

    In the present work, Fluidized bed reduction of NiO-WO(3) precursors was investigated isothermally at temperatures 973-1 273 K. The reaction progress was monitored by analysis of H(2)O evolved during the reaction process using a gas chromatograph instrument. A theoretical model based on intrinsic chemical reaction rate constants and thermodynamic equilibria was developed to estimate the apparent reaction rate constant for the reduction reaction. In developing the model, the particles are considered to be in a completely mixed condition and gas flow is described as plug flow. The proposed model is also suitable for scale-up calculations. The interfacial chemical reaction model was found to fit the experimental results. The apparent activation energy values of the reduction process at different stages were calculated accordingly. The present investigation proved that the fluidized bed technique can be successfully utilized in bulk production of intermetallics containing W and a transition metal (or a composite material) wherein the process conditions would have a strong impact on the particle size of the end product.

  • 4.
    Ahmed, Hesham M.
    et al.
    KTH, School of Industrial Engineering and Management (ITM), Materials Science and Engineering, Materials Process Science.
    El-Geassy, Abdel-Hady
    Seetharaman, Seshadri
    KTH, School of Industrial Engineering and Management (ITM), Materials Science and Engineering, Materials Process Science.
    Kinetic Studies of the Hydrogen Reduction of NiO-WO3 precursors in a Fluidized-bed reactorIn: Metallurgical and materials transactions. B, process metallurgy and materials processing science, ISSN 1073-5615, E-ISSN 1543-1916Article in journal (Other academic)
  • 5.
    Ahmed, Hesham M.
    et al.
    KTH, School of Industrial Engineering and Management (ITM), Materials Science and Engineering.
    Seetharaman, Seshadri
    KTH, School of Industrial Engineering and Management (ITM), Materials Science and Engineering.
    Isothermal dynamic thermal diffusivity studies of the reduction of NiO and NiWO(4) precursors by hydrogen2011In: International Journal of Materials Research - Zeitschrift für Metallkunde, ISSN 1862-5282, E-ISSN 2195-8556, Vol. 102, no 11, p. 1336-1344Article in journal (Refereed)
    Abstract [en]

    Thermal diffusivity measurements of uniaxially cold pressed NiO and NiWO(4) were carried out in a dynamic mode in order to monitor the kinetics of hydrogen reduction of the above-mentioned materials using a laser flash unit. The calculated activation energy was found to be higher than that for chemically-controlled reaction obtained earlier by thermogravimetry. The difference has been attributed to physical changes occurring along with the chemical reaction. The activation energy of sintering of the products was evaluated to be 33 and 36 kJ.mol(-1) for NiO and NiWO(4), respectively. Thermal conductivities were calculated taking into consideration the change in heat capacity considering the compositional and the structural changes with the progress of the reaction. The potentiality of the laser-flash method as a complementary technique to thermogravimetry in understanding the mechanism of gas solid reactions is discussed.

  • 6.
    Ahmed, Hesham M.
    et al.
    KTH, School of Industrial Engineering and Management (ITM), Materials Science and Engineering, Materials Process Science.
    Seetharaman, Seshadri
    KTH, School of Industrial Engineering and Management (ITM), Materials Science and Engineering, Materials Process Science.
    Reduction-Carburization of NiO-WO3 Under Isothermal Conditions Using H2-CH4 Gas Mixture2010In: Metallurgical and materials transactions. B, process metallurgy and materials processing science, ISSN 1073-5615, E-ISSN 1543-1916, Vol. 41, no 1, p. 173-181Article in journal (Refereed)
    Abstract [en]

    Ni-W-C ternary carbides were synthesized by simultaneous reduction–carburization of NiO-WO3 oxide precursors using H2-CH4 gas mixtures in the temperature range of 973 to 1273 K. The kinetics of the gas–solid reaction were followed closely by monitoring the mass changes using the thermogravimetric method (TGA). As a thin bed of the precursors were used, each particle was in direct contact with the gas mixture. The results showed that the hydrogen reduction of the oxide mixture was complete before the carburization took place. The nascent particles of the metals formed by reduction could react with the gas mixture with well-defined carbon potential to form a uniform product of Ni-W-C. Consequently, the reaction rate could be conceived as being controlled by the chemical reaction. From the reaction rate, Arrhenius activation energies for reduction and carburization were evaluated. Characterization of the carbides produced was carried out using X-ray diffraction and a scanning electron microscope (SEM) combined with electron dispersion spectroscopy (SEM-EDS) analyses. The grain sizes also were determined. The process parameters, such as the temperature of the reduction–carburization reaction and the composition of the gas mixture, had a strong impact on the carbide composition as well as on the grain size. The results are discussed in light of the reduction kinetics of the oxides and the thermodynamic constraints.

  • 7.
    Ahmed, Hesham M.
    et al.
    KTH, School of Industrial Engineering and Management (ITM), Materials Science and Engineering, Materials Process Science.
    Viswanathan, N. N.
    Seetharaman, Seshadri
    KTH, School of Industrial Engineering and Management (ITM), Materials Science and Engineering, Materials Process Science.
    On The Kinetics of Hydrogen Reduction of NiO-WO3 Precursors in Fluidized Bed- A Modeling Approach2011In: ISIJ International, ISSN 0915-1559, E-ISSN 1347-5460, Vol. 51, no 9, p. 1383-1391Article in journal (Refereed)
    Abstract [en]

    In the present work, Fluidized bed reduction of NiO-WO3 precursors was investigated isothermally at temperatures 973-1 273 K. The reaction progress was monitored by analysis of H2O evolved during the reaction process using a gas chromatograph instrument. A theoretical model based on intrinsic chemical reaction rate constants and thermodynamic equilibria was developed to estimate the apparent reaction rate constant for the reduction reaction. In developing the model, the particles are considered to be in a completely mixed condition and gas flow is described as plug flow. The proposed model is also suitable for scale-up calculations. The interfacial chemical reaction model was found to fit the experimental results. The apparent activation energy values of the reduction process at different stages were calculated accordingly. The present investigation proved that the fluidized bed technique can be successfully utilized in bulk production of intermetallics containing W and a transition metal (or a composite material) wherein the process conditions would have a strong impact on the particle size of the end product.

  • 8.
    Ahmed, Hesham M.
    et al.
    KTH, School of Industrial Engineering and Management (ITM), Materials Science and Engineering.
    Viswanathan, Nurini N.
    Seetharaman, Seshadri
    KTH, School of Industrial Engineering and Management (ITM), Materials Science and Engineering.
    Dynamic Thermal Diffusivity Measurements - A Tool for Studying Gas-Solid Reactions2011In: DIFFUSION IN SOLIDS AND LIQUIDS VI, PTS 1 AND 2, 2011, p. 217-222Conference paper (Refereed)
    Abstract [en]

    In the present work, the thermal diffusivity measurements of uniaxially cold pressed NiWO(4) has been carried out. The measurements were performed isothermally at temperatures between 973 and 1273 K under H(2) gas using the laser flash technique. The experimental thermal diffusivity values were found to increase with the reduction progress as well as with increasing temperature. The calculated activation energy was found to be higher than that for chemically controlled reaction. The difference has been attributed to factors like agglomeration of the product as well as sintering of the precursor along with the chemical reaction. In order to sort out the sintering effect on the thermal diffusivity values, complementary experiments have been done on pressed NiWO(4) and Ni-W, produced by the reduction of NiWO(4) at 1123K, under Argon gas. The porosity change and its effect on thermal diffusivity values have been studied.

  • 9.
    Ahmed, Hesham
    et al.
    KTH, School of Industrial Engineering and Management (ITM), Materials Science and Engineering.
    Mis, Michal
    KTH, School of Industrial Engineering and Management (ITM), Materials Science and Engineering.
    El-Geassy, Abdel-Hady
    KTH, School of Industrial Engineering and Management (ITM), Materials Science and Engineering.
    Seethararnan, Seshadri
    KTH, School of Industrial Engineering and Management (ITM), Materials Science and Engineering.
    Reduction-Carburization of the Oxides of Ni and W Towards the Synthesis of Ni-W-C Carbides2010In: ADVANCED MATERIALS FORUM V, PT 1 AND 2  / [ed] Rosa LG; Margarido F, 2010, Vol. 636-637, p. 952-962Conference paper (Refereed)
    Abstract [en]

    Ternary Ni-W-C cemented carbides were synthesized directly from mixture powder of NiO-WO3 by simultaneous reduction-carburization in mixed H-2-CH4 gas environment in a thin bed reactor in the temperature range 973-1273K. The kinetics of the reaction was closely followed by monitoring the mass change using thermogravimetric method (TGA). The nascent particles of the metals formed by reduction could react with the gas mixture with well-defined carbon potential to form a uniform product of Ni-W-C. The gas mixture ratio was adjusted in such a way that the Ni-W-C formed was close to the two phase tie line. In view of the fact that each particle was in direct contact with the gas mixture, the reaction rate could be conceived as being controlled by the combined reduction-carburization reaction. From the reaction rate, the Arrhenius activation energies were evaluated. Characterization of the carbides produced was carried out by using X-ray diffraction, SEM-EDS as well as high resolution electron microscope (HREM). The grain sizes were also determined. Correlations were found between the carbide composition as well as grain size and the process parameters such as temperature of the reduction-carburization reaction as well as the composition of the gas mixture. The results are discussed in the light of the kinetics of the reduction of oxides and the thermodynamic constraints.

1 - 9 of 9
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