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Christian Hess - One of the best experts on this subject based on the ideXlab platform.

  • Monitoring Silica Supported Molybdenum Oxide Catalysts at Work: A Raman Spectroscopic Study
    Chemphyschem : a European journal of chemical physics and physical chemistry, 2012
    Co-Authors: Jörg P. Thielemann, Christian Hess
    Abstract:

    The structure of silica SBA-15-supported Molybdenum Oxide catalysts is investigated during selective oxidation of propylene at 500 °C using operando Raman spectroscopy. The active catalysts contain mixtures of dispersed Molybdenum Oxide species exhibiting monooxo and dioxo structure. An increase in Molybdenum Oxide loading results in a decrease of the ratio of dioxo and monooxo species from 3.8 to 1.9, as determined by quantitative analysis of Raman spectra. Additional in situ Raman studies at 500 °C reveal that the dioxo/monooxo ratio increases in the presence of steam at higher Molybdenum Oxide loadings. The observed structural changes are assigned to shifts in the equilibrium between dioxo and monooxo species resulting from hydration/dehydration of the catalyst. This study demonstrates that the detailed structure of nanostructured Molybdenum Oxide catalysts depends on temperature, gas-phase composition, and Molybdenum Oxide loading.

  • Controlled Synthesis and Characterization of Highly Dispersed Molybdenum Oxide Supported on Silica SBA‐15
    ChemCatChem, 2011
    Co-Authors: Jörg P. Thielemann, Gisela Weinberg, Christian Hess
    Abstract:

    Silica-supported Molybdenum Oxide catalysts with high densities of disperse Molybdenum Oxide species of up to 3.5 atoms nm−2 were prepared by using a novel synthesis approach on the basis of functionalized mesoporous SBA-15. As revealed by using Raman spectroscopy and thermal analysis, the synthesis mechanism consists of an ion exchange of heptamolybdate ions (Mo7O246−) into the porous functionalized framework and decomposition of the intact precursor into smaller fragments during final calcination. The amount of dispersed Molybdenum Oxide as well as the ratio of dispersed to crystalline Molybdenum Oxide was determined in detail for Mo densities of 0–13.0 atoms nm−2 by using a combination of X-ray fluorescence (XRF), energy-dispersive X-ray analysis (EDX), and Raman spectroscopy. Up to 3.5 atoms nm−2 dehydrated Molybdenum Oxide is present exclusively as dispersed species. At higher densities, additional Mo is introduced as crystalline MoO3, and the amount of dispersed species remains unchanged. The structure of the supported Molybdenum Oxide under ambient conditions largely resembles that of heptamolybdate ions. Dehydration leads to the formation of grafted monomeric and connected Molybdenum Oxide surface species. Detailed X-ray photoelectron spectroscopy (XPS) analysis revealed an increase in the Mo/Si ratio as well as a positive binding energy shift upon dehydration, indicative of an increase in the dispersion of the supported Molybdenum Oxide. The combination of Raman and XPS analyses establishes a correlation of the changes in structure and dispersion of the supported Molybdenum Oxide species

  • structure of Molybdenum Oxide supported on silica sba 15 studied by raman uv vis and x ray absorption spectroscopy
    Applied Catalysis A-general, 2011
    Co-Authors: Jörg P. Thielemann, Thorsten Ressler, Anke Walter, Genka Tzolovamuller, Christian Hess
    Abstract:

    Abstract The structure of Molybdenum Oxide supported by silica SBA-15 has been studied by visible Raman spectroscopy, diffuse reflectance UV–Vis spectroscopy and X-ray absorption spectroscopy in the dehydrated state obtained after thermal treatment at elevated temperatures (≥350 °C). No dependence of the Molybdenum Oxide structure on preparation procedure or loading has been observed within the range of loadings studied in detail (0.2–0.8 Mo/nm2). X-ray absorption spectroscopy (XAS) reveals that the dehydrated state consists of a mixture of monomeric and connected Molybdenum Oxide centres. While the presence of crystalline MoO3 can be excluded by Raman spectroscopy, tetrahedrally and octahedrally coordinated MoO4 and MoO6 units are identified by XAS. The MoO6 units possess connectivity similar to that of MoO3 building blocks, whereas the MoO4 units are isolated or connected to other MoxOy units. These results are supported by UV–Vis spectra showing intensity at wavelengths (>300 nm) typical for dimeric and/or oligomeric species.

  • Synthesis, Characterization and in situ Catalysis of Silica SBA-15 Supported Molybdenum Oxide Model Catalysts
    2011
    Co-Authors: Jörg P. Thielemann, Christian Hess, Robert Schlögl, Reinhard Schomäcker
    Abstract:

    This work describes the synthesis, the structural characterization and the catalytic testing of silica SBA-15 supported Molybdenum Oxide model catalysts. Additionally, a solvent induced washing effect during the SBA-15 synthesis and its scale up on the SBA-15 structure was studied. The MoxOy/SBA-15 catalysts were prepared with a Mo loading between 1.0 and 21.1 wt.% Mo (0.2 to 9.8 Mo/nm2) by a grafting/ion exchange procedure and incipient wetness impregnation. The catalyst structure was analyzed with Raman-, UV/Vis-, Photoelectron-, X-ray absorption- and IR spectroscopy. Furthermore, the catalyst structure was studied under reaction conditions in presence of propylene/oxygen and steam in an in situ Raman-MS setup, which was constructed in the course of this work. The study of washing SBA-15 with two solvents (water and ethanol) with nitrogen adsorption and XRD revealed that the surface area can be increased by 25% to 800 m2/g compared to washing with a single solvent. Moreover, it was found that huge solvent quantities for washing should be avoided, as they induce hydrolysis reactions, which alter the SBA-15 structure and lead to a widening and narrowing of certain mesopore sections. This decreases the surface area and pore volume of the support. The effect decreases with up-scaling of the synthesis. For the MoxOy/SBA-15 catalysts the Molybdenum Oxide was observed on the support in a dispersed state up to a loading of 12.1 wt.% Mo (3.5 Mo/nm2). Above this loading crystalline -MoO3 and as minority phase-MoO3 are formed. In this loading region the fraction of dispersed Molybdenum Oxide was almost constant at 12 to 13 wt.% Mo. Regarding the dispersed Molybdenum Oxide two structurally different states were observed. The hydrated state exists in the presence of moisture at room temperature, whereas the dehydrated state is obtained after treatment over 350°C in synthetic air. The Molybdenum Oxide structure in the hydrated state can be described as preferentially octahedral centres, which also exhibit connections and form di- or oligomers beside monomers. Comparing the XPS data of the dehydrated and the hydrated state showed that the Molybdenum Oxide was higher dispersed in the dehydrated state. UV/Vis spectroscopy supported this finding and showed that beside monomeric also di- or oligomeric species were present at Mo densities in the range of dispersed Molybdenum Oxide (≤3.5 Mo/nm2). Connections between neighbouring Molybdenum Oxide centres were detected by EXAFS and IR Spectroscopy using nitric Oxide as probe molecule. Furthermore, a octahedral to tetrahedral ratio of 1 : 3 was found by a XANES fit. Therefore, the Molybdenum Oxide structure of the dehydrated state can be described as dispersed tetrahedral and octahedral Molybdenum Oxide centres, which coexist as monomers and connected di- or oligomers on the silica support surface. Moreover, the size distribution of the dispersed Molybdenum Oxide species in the hydrated and dehydrated state seems to be independent of the loading. MoxOy/SBA-15 was catalytically tested in the selective oxidation of propylene and propane. Whereas propylene was oxidized selectively to propionaldehyde, acetone and acrolein as major products, the oxidation of propane led unselectively to COx. In situ Raman investigations reveal that during the propylene oxidation or in the presence of steam, the structure of the catalyst largely resembles the structure of dehydrated dispersed Molybdenum Oxide.

Jörg P. Thielemann - One of the best experts on this subject based on the ideXlab platform.

  • Monitoring Silica Supported Molybdenum Oxide Catalysts at Work: A Raman Spectroscopic Study
    Chemphyschem : a European journal of chemical physics and physical chemistry, 2012
    Co-Authors: Jörg P. Thielemann, Christian Hess
    Abstract:

    The structure of silica SBA-15-supported Molybdenum Oxide catalysts is investigated during selective oxidation of propylene at 500 °C using operando Raman spectroscopy. The active catalysts contain mixtures of dispersed Molybdenum Oxide species exhibiting monooxo and dioxo structure. An increase in Molybdenum Oxide loading results in a decrease of the ratio of dioxo and monooxo species from 3.8 to 1.9, as determined by quantitative analysis of Raman spectra. Additional in situ Raman studies at 500 °C reveal that the dioxo/monooxo ratio increases in the presence of steam at higher Molybdenum Oxide loadings. The observed structural changes are assigned to shifts in the equilibrium between dioxo and monooxo species resulting from hydration/dehydration of the catalyst. This study demonstrates that the detailed structure of nanostructured Molybdenum Oxide catalysts depends on temperature, gas-phase composition, and Molybdenum Oxide loading.

  • Controlled Synthesis and Characterization of Highly Dispersed Molybdenum Oxide Supported on Silica SBA‐15
    ChemCatChem, 2011
    Co-Authors: Jörg P. Thielemann, Gisela Weinberg, Christian Hess
    Abstract:

    Silica-supported Molybdenum Oxide catalysts with high densities of disperse Molybdenum Oxide species of up to 3.5 atoms nm−2 were prepared by using a novel synthesis approach on the basis of functionalized mesoporous SBA-15. As revealed by using Raman spectroscopy and thermal analysis, the synthesis mechanism consists of an ion exchange of heptamolybdate ions (Mo7O246−) into the porous functionalized framework and decomposition of the intact precursor into smaller fragments during final calcination. The amount of dispersed Molybdenum Oxide as well as the ratio of dispersed to crystalline Molybdenum Oxide was determined in detail for Mo densities of 0–13.0 atoms nm−2 by using a combination of X-ray fluorescence (XRF), energy-dispersive X-ray analysis (EDX), and Raman spectroscopy. Up to 3.5 atoms nm−2 dehydrated Molybdenum Oxide is present exclusively as dispersed species. At higher densities, additional Mo is introduced as crystalline MoO3, and the amount of dispersed species remains unchanged. The structure of the supported Molybdenum Oxide under ambient conditions largely resembles that of heptamolybdate ions. Dehydration leads to the formation of grafted monomeric and connected Molybdenum Oxide surface species. Detailed X-ray photoelectron spectroscopy (XPS) analysis revealed an increase in the Mo/Si ratio as well as a positive binding energy shift upon dehydration, indicative of an increase in the dispersion of the supported Molybdenum Oxide. The combination of Raman and XPS analyses establishes a correlation of the changes in structure and dispersion of the supported Molybdenum Oxide species

  • structure of Molybdenum Oxide supported on silica sba 15 studied by raman uv vis and x ray absorption spectroscopy
    Applied Catalysis A-general, 2011
    Co-Authors: Jörg P. Thielemann, Thorsten Ressler, Anke Walter, Genka Tzolovamuller, Christian Hess
    Abstract:

    Abstract The structure of Molybdenum Oxide supported by silica SBA-15 has been studied by visible Raman spectroscopy, diffuse reflectance UV–Vis spectroscopy and X-ray absorption spectroscopy in the dehydrated state obtained after thermal treatment at elevated temperatures (≥350 °C). No dependence of the Molybdenum Oxide structure on preparation procedure or loading has been observed within the range of loadings studied in detail (0.2–0.8 Mo/nm2). X-ray absorption spectroscopy (XAS) reveals that the dehydrated state consists of a mixture of monomeric and connected Molybdenum Oxide centres. While the presence of crystalline MoO3 can be excluded by Raman spectroscopy, tetrahedrally and octahedrally coordinated MoO4 and MoO6 units are identified by XAS. The MoO6 units possess connectivity similar to that of MoO3 building blocks, whereas the MoO4 units are isolated or connected to other MoxOy units. These results are supported by UV–Vis spectra showing intensity at wavelengths (>300 nm) typical for dimeric and/or oligomeric species.

  • Synthesis, Characterization and in situ Catalysis of Silica SBA-15 Supported Molybdenum Oxide Model Catalysts
    2011
    Co-Authors: Jörg P. Thielemann, Christian Hess, Robert Schlögl, Reinhard Schomäcker
    Abstract:

    This work describes the synthesis, the structural characterization and the catalytic testing of silica SBA-15 supported Molybdenum Oxide model catalysts. Additionally, a solvent induced washing effect during the SBA-15 synthesis and its scale up on the SBA-15 structure was studied. The MoxOy/SBA-15 catalysts were prepared with a Mo loading between 1.0 and 21.1 wt.% Mo (0.2 to 9.8 Mo/nm2) by a grafting/ion exchange procedure and incipient wetness impregnation. The catalyst structure was analyzed with Raman-, UV/Vis-, Photoelectron-, X-ray absorption- and IR spectroscopy. Furthermore, the catalyst structure was studied under reaction conditions in presence of propylene/oxygen and steam in an in situ Raman-MS setup, which was constructed in the course of this work. The study of washing SBA-15 with two solvents (water and ethanol) with nitrogen adsorption and XRD revealed that the surface area can be increased by 25% to 800 m2/g compared to washing with a single solvent. Moreover, it was found that huge solvent quantities for washing should be avoided, as they induce hydrolysis reactions, which alter the SBA-15 structure and lead to a widening and narrowing of certain mesopore sections. This decreases the surface area and pore volume of the support. The effect decreases with up-scaling of the synthesis. For the MoxOy/SBA-15 catalysts the Molybdenum Oxide was observed on the support in a dispersed state up to a loading of 12.1 wt.% Mo (3.5 Mo/nm2). Above this loading crystalline -MoO3 and as minority phase-MoO3 are formed. In this loading region the fraction of dispersed Molybdenum Oxide was almost constant at 12 to 13 wt.% Mo. Regarding the dispersed Molybdenum Oxide two structurally different states were observed. The hydrated state exists in the presence of moisture at room temperature, whereas the dehydrated state is obtained after treatment over 350°C in synthetic air. The Molybdenum Oxide structure in the hydrated state can be described as preferentially octahedral centres, which also exhibit connections and form di- or oligomers beside monomers. Comparing the XPS data of the dehydrated and the hydrated state showed that the Molybdenum Oxide was higher dispersed in the dehydrated state. UV/Vis spectroscopy supported this finding and showed that beside monomeric also di- or oligomeric species were present at Mo densities in the range of dispersed Molybdenum Oxide (≤3.5 Mo/nm2). Connections between neighbouring Molybdenum Oxide centres were detected by EXAFS and IR Spectroscopy using nitric Oxide as probe molecule. Furthermore, a octahedral to tetrahedral ratio of 1 : 3 was found by a XANES fit. Therefore, the Molybdenum Oxide structure of the dehydrated state can be described as dispersed tetrahedral and octahedral Molybdenum Oxide centres, which coexist as monomers and connected di- or oligomers on the silica support surface. Moreover, the size distribution of the dispersed Molybdenum Oxide species in the hydrated and dehydrated state seems to be independent of the loading. MoxOy/SBA-15 was catalytically tested in the selective oxidation of propylene and propane. Whereas propylene was oxidized selectively to propionaldehyde, acetone and acrolein as major products, the oxidation of propane led unselectively to COx. In situ Raman investigations reveal that during the propylene oxidation or in the presence of steam, the structure of the catalyst largely resembles the structure of dehydrated dispersed Molybdenum Oxide.

Israel E. Wachs - One of the best experts on this subject based on the ideXlab platform.

  • Catalytic Properties of Supported Molybdenum Oxide Catalysts: In Situ Raman and Methanol Oxidation Studies
    The Journal of Physical Chemistry, 1995
    Co-Authors: Israel E. Wachs
    Abstract:

    The oxidation of methanol was studied over supported Molybdenum Oxide catalysts as a function of the specific Oxide support (TiO2,ZrO2, Nb2O5, and A1203) and Molybdenum Oxide loading (surface coverage). The surface Molybdenum Oxide species were selective for the production of formaldehyde, and the Oxide support sites yielded dimethyl ether (alumina and niobia) and methyl formate (zirconia) or were relatively inactive (titania). The turnover frequency (TOF) for the selective oxidation of methanol to formaldehyde varied by a factor of 2-4 with surface Molybdenum Oxide coverage and a factor of approximately 10 with the specific Oxide support at monolayer coverage. The molecular structures of the surface Molybdenum Oxide species (isolated, tetrahedral at low coverages and polymerized, octahedralketrahedral at high coverages) did not affect the reaction selectivity but did appear to influence the slight increase in TOF with surface coverage. The order of magnitude variation in TOF with the specific Oxide support correlated with the reducibility of the support and suggests that the Mo-0-support bond is critical in controlling the TOF. In situ Raman studies during methanol oxidation revealed that the supported Molybdenum Oxide species were 100% dispersed up to monolayer coverage. The percent reduction of the surface Molybdenum Oxide species, reflected by the decrease in the Raman intensity of the Mo-0 bond, during methanol oxidation was not a strong function of surface coverage and the specific Oxide support. This suggests that the order of magnitude variation in the TOF with the specific Oxide support is primarily related to the activity per site of the surface Molybdenum Oxide species rather than variation in the number of participating sites.

  • Molecular Structures and Reactivity of Supported Molybdenum Oxide Catalysts
    Journal of Catalysis, 1994
    Co-Authors: Du Soung Kim, Israel E. Wachs, Kohichi Segawa
    Abstract:

    Supported Molybdenum Oxide catalysts were prepared by an equilibrium adsorption method. The molecular structures of the Molybdenum Oxide overlayers on different Oxide supports (Al{sub 2}O{sub 3}, TiO{sub 2}, ZrO{sub 2}, SiO{sub 2}, and MgO), under in situ conditions, were investigated by Raman spectroscopy. The Molybdenum Oxide species on TiO{sub 2}, ZrO{sub 2}, and Al{sub 2}O{sub 3} possess a highly distorted, octahedrally coordinated surface Molybdenum Oxide species with one short Mo=O bond regardless of the Molybdenum Oxide content. The MoO{sub 3}/SiO{sub 2} catalysts primarily contain crystalline MoO{sub 3} because of the lower density and reactivity of the silica surface OH groups. The MoO{sub 3}/MgO catalysts possess MgMoO{sub 4} and CaMoO{sub 4} compounds due to the high aqueous solubility of MgO and CaO (an impurity in the MgO support) and the strong acid-base interaction between Molybdenum Oxide and MgO/CaO. The methanol oxidation reaction studies revealed that the MoO{sub 3}/TiO{sub 2} (anatase and rutile) and MOO{sub 3}/ZrO{sub 2} catalysts are the most active catalysts and that their activities (TOFs) are at least 1-2 orders of magnitude higher than those of the MoO{sub 3}/Al{sub 2}O{sub 3}, MoO{sub 3}SiO{sub 2}, and MoO{sub 3}/MgO catalysts. It was also found that the catalytic activities correlate with themore » reducibility of the surface Molybdenum Oxide species on the Oxide supports as well as their surface morphology (e.g., Molybdenum Oxide dispersion and molybdate compound formation). These studies demonstrate that the specific Oxide support controls the reactivity of the supported Molybdenum Oxide phases. 55 refs., 6 figs., 2 tabs.« less

  • Surface Structures of Supported Molybdenum Oxide Catalysts under Ambient Conditions
    Journal of Catalysis, 1992
    Co-Authors: Du Soung Kim, Koichi Segawa, Tomotsune Soeya, Israel E. Wachs
    Abstract:

    Two sets of supported Molybdenum Oxide catalysts, wet (dried at room temperature) and calcined (calcined at 773 K) samples, were prepared by an equilibrium adsorption method at different pH values of the impregnating solution. The adsorbed amounts of Molybdenum Oxide species onto the Oxide support are strongly dependent on the pH of the impregnating solution and increase with decreasing pH. The Raman spectroscopic studies reveal that the surface Molybdenum Oxide species under ambient conditions, wet and calcined, are hydrated and essentially in an aqueous medium. Furthermore, the surface structures of Molybdenum Oxide species on the Oxide support were found to depend on the net surface pH at point of zero charge (PZC) under ambient conditions. The net surface pH at PZC under ambient conditions is determined by the specific Oxide support and surface Molybdenum Oxide coverage. The surface Molybdenum Oxide structures in the wet, uncalcined, samples are not only dependent on the net surface pH at PZC but also on the number of NH4+ cations which coordinate to the surface Molybdenum Oxide species for compensation of net charge: Mo7O246− species in NH4+-rich concentrations (high pH region) favor formation of (NH4)6Mo7O24 · 4H2O. Upon calcination, the NH4+ ions are removed and the surface Molybdenum Oxide species become rehydrated upon exposure to air by adsorbing moisture. Consequently, the structures of surface Molybdenum Oxide species in the calcined samples which have been exposed to ambient are also dependent on the net surface pH at PZC.

Du Soung Kim - One of the best experts on this subject based on the ideXlab platform.

  • Molecular Structures and Reactivity of Supported Molybdenum Oxide Catalysts
    Journal of Catalysis, 1994
    Co-Authors: Du Soung Kim, Israel E. Wachs, Kohichi Segawa
    Abstract:

    Supported Molybdenum Oxide catalysts were prepared by an equilibrium adsorption method. The molecular structures of the Molybdenum Oxide overlayers on different Oxide supports (Al{sub 2}O{sub 3}, TiO{sub 2}, ZrO{sub 2}, SiO{sub 2}, and MgO), under in situ conditions, were investigated by Raman spectroscopy. The Molybdenum Oxide species on TiO{sub 2}, ZrO{sub 2}, and Al{sub 2}O{sub 3} possess a highly distorted, octahedrally coordinated surface Molybdenum Oxide species with one short Mo=O bond regardless of the Molybdenum Oxide content. The MoO{sub 3}/SiO{sub 2} catalysts primarily contain crystalline MoO{sub 3} because of the lower density and reactivity of the silica surface OH groups. The MoO{sub 3}/MgO catalysts possess MgMoO{sub 4} and CaMoO{sub 4} compounds due to the high aqueous solubility of MgO and CaO (an impurity in the MgO support) and the strong acid-base interaction between Molybdenum Oxide and MgO/CaO. The methanol oxidation reaction studies revealed that the MoO{sub 3}/TiO{sub 2} (anatase and rutile) and MOO{sub 3}/ZrO{sub 2} catalysts are the most active catalysts and that their activities (TOFs) are at least 1-2 orders of magnitude higher than those of the MoO{sub 3}/Al{sub 2}O{sub 3}, MoO{sub 3}SiO{sub 2}, and MoO{sub 3}/MgO catalysts. It was also found that the catalytic activities correlate with themore » reducibility of the surface Molybdenum Oxide species on the Oxide supports as well as their surface morphology (e.g., Molybdenum Oxide dispersion and molybdate compound formation). These studies demonstrate that the specific Oxide support controls the reactivity of the supported Molybdenum Oxide phases. 55 refs., 6 figs., 2 tabs.« less

  • Surface Structures of Supported Molybdenum Oxide Catalysts under Ambient Conditions
    Journal of Catalysis, 1992
    Co-Authors: Du Soung Kim, Koichi Segawa, Tomotsune Soeya, Israel E. Wachs
    Abstract:

    Two sets of supported Molybdenum Oxide catalysts, wet (dried at room temperature) and calcined (calcined at 773 K) samples, were prepared by an equilibrium adsorption method at different pH values of the impregnating solution. The adsorbed amounts of Molybdenum Oxide species onto the Oxide support are strongly dependent on the pH of the impregnating solution and increase with decreasing pH. The Raman spectroscopic studies reveal that the surface Molybdenum Oxide species under ambient conditions, wet and calcined, are hydrated and essentially in an aqueous medium. Furthermore, the surface structures of Molybdenum Oxide species on the Oxide support were found to depend on the net surface pH at point of zero charge (PZC) under ambient conditions. The net surface pH at PZC under ambient conditions is determined by the specific Oxide support and surface Molybdenum Oxide coverage. The surface Molybdenum Oxide structures in the wet, uncalcined, samples are not only dependent on the net surface pH at PZC but also on the number of NH4+ cations which coordinate to the surface Molybdenum Oxide species for compensation of net charge: Mo7O246− species in NH4+-rich concentrations (high pH region) favor formation of (NH4)6Mo7O24 · 4H2O. Upon calcination, the NH4+ ions are removed and the surface Molybdenum Oxide species become rehydrated upon exposure to air by adsorbing moisture. Consequently, the structures of surface Molybdenum Oxide species in the calcined samples which have been exposed to ambient are also dependent on the net surface pH at PZC.

Oh-shim Joo - One of the best experts on this subject based on the ideXlab platform.

  • Electrosynthesis of Molybdenum Oxide thin films onto stainless substrates
    Electrochemistry Communications, 2006
    Co-Authors: Habib M. Pathan, Sun-ki Min, Kwang-deog Jung, Oh-shim Joo
    Abstract:

    The electrodeposition of uniform, nanocrystalline and highly oriented Molybdenum Oxide thin films was investigated at room temperature onto stainless steel substrates using citric acid as a complexing agent. The electrodeposition process of Molybdenum Oxide thin films from molybdic acid of various concentrations onto stainless steel substrate were studied by utilizing the electrochemical techniques. The prepared films were characterized for their structural, surface morphological and compositional properties by means of X-ray diffraction, scanning electron microscopy, transmission electron microscopy and energy dispersive X-ray analysis. X-ray diffraction and transmission electron microscopy experiment reveals that the films are of crystallized size. XRD experiment showed that the crystallized product is composed of Molybdenum Oxide with dominant orientations of MoO3.