Temperature-Programmed Reduction Reaction between h-MoO3 and H2 to Prepare Ultrafine Mo Powder AITranslate
Abstract AITranslate
Molybdenum metal powder with suitable size，morphology，purity，and dispersityis of immense importance for alloy preparation by powder metallurgy. In the work，the temperature-programmed reduction （TPR）reaction between hexagonal-shaped h-MoO3 and high-purity H2 was investigated in the range of room temperature to 1273 K，and various technologies such as Thermogravimetry-differential thermal analysis （TG-DTA），X-ray diffraction （XRD）and field emission scanning electronic microscope （FESEM）were adopted to analyze the phase transition law and morphological evolution behavior during the reaction process. The results of TG curves showed that there were five main stages in the whole reaction process，among those the mass loss produced by Stages I and II was 5.84%，which was independent of the reducing atmosphere，and the mass loss in the two stages were mainly due to the removal of adsorbed water and ammonium ion existed on the sample surface. The mass loss of Stages III and IV was 12.32%，which was close to the theoretical mass loss of the reduction of MoO3 to MoO2 （11.1%），that was，the main reaction took place in the stages was the transformation of MoO3 to MoO2. The mass loss of Stage V was 20.65%，which was close to the theoretical mass loss of MoO2 to Mo （22.22%），so the main reaction took place in the stage was the transition from MoO2 to Mo. In addition，it was found that the required temperature for each mass loss stage was increased with the increase of heating rate，and the main reason was due to the hysteresis phenomenon produced by the high heating rate. The results of DTA curves also supported this view. When the reaction extent （defined as the ratio of the instantaneous mass loss to the maximum mass loss）was less than α3=0.1443，the existed phase in the sample was still h-MoO3. When the reaction extent increased to α4=0.2510，the residual sample was transformed into the mixture of α-MoO3 and Mo4O11，further increased the reaction extent to α5=0.3088，the reaction product was still composed of α-MoO3 and Mo4O11；however，the content of Mo4O11 in the sample at this time was significantly higher than that at α4=0.2510. When the reaction extent was increased to α6=0.4129，it could be found that α-MoO3 disappeared completely and MoO2 began to be generated，and the obtained products were mainly composed of Mo4O11 and MoO2. While when the reaction extent was increased to α7=0.4753，the reaction product was only MoO2. With the continuous increase of reaction temperature，the reduction reaction of MoO2 to Mo began，and during the following stage，the content of MoO2wasgradually decreased，while that of metallic Mo gradually increased. When the reaction reached a plateau，the reaction product was only metallic Mo. The total reaction paths of h-MoO3→α-MoO3+Mo4O11→MoO2→Mo was concluded. According to FESEM images，it was found that the original sample first changed from a smooth hexagonal prismatic structure to a rough step-like structure，then to a smooth and irregular layered shape，and finally evolved into fine smooth particles，with the continue process of the reaction. In this case，the average particle size of the as-prepared Mo powder was measured to be 369.81 nm. The work also found that the chemical vapor phase transport mechanism dominated during the reduction process of MoO3 to MoO2；as to the reduction process ofMoO2 to Mo，however，the pseudomorphic transformation mechanism dominated，and the obtained metallic Mo basically maintained the same sheet morphology as MoO2.
KeyWords AITranslate
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Basic Information:
DOI：10.13373/j.cnki.cjrm.XY24010004
Chinese Library Classification Number:TF841.2
Citation Information:
Molybdenum metal powder with suitable size，morphology，purity，and dispersityis of immense importance for alloy preparation by powder metallurgy. In the work，the temperature-programmed reduction （TPR）reaction between hexagonal-shaped h-MoO3 and high-purity H2 was investigated in the range of room temperature to 1273 K，and various technologies such as Thermogravimetry-differential thermal analysis （TG-DTA），X-ray diffraction （XRD）and field emission scanning electronic microscope （FESEM）were adopted to analyze the phase transition law and morphological evolution behavior during the reaction process. The results of TG curves showed that there were five main stages in the whole reaction process，among those the mass loss produced by Stages I and II was 5.84%，which was independent of the reducing atmosphere，and the mass loss in the two stages were mainly due to the removal of adsorbed water and ammonium ion existed on the sample surface. The mass loss of Stages III and IV was 12.32%，which was close to the theoretical mass loss of the reduction of MoO3 to MoO2 （11.1%），that was，the main reaction took place in the stages was the transformation of MoO3 to MoO2. The mass loss of Stage V was 20.65%，which was close to the theoretical mass loss of MoO2 to Mo （22.22%），so the main reaction took place in the stage was the transition from MoO2 to Mo. In addition，it was found that the required temperature for each mass loss stage was increased with the increase of heating rate，and the main reason was due to the hysteresis phenomenon produced by the high heating rate. The results of DTA curves also supported this view. When the reaction extent （defined as the ratio of the instantaneous mass loss to the maximum mass loss）was less than α3=0.1443，the existed phase in the sample was still h-MoO3. When the reaction extent increased to α4=0.2510，the residual sample was transformed into the mixture of α-MoO3 and Mo4O11，further increased the reaction extent to α5=0.3088，the reaction product was still composed of α-MoO3 and Mo4O11；however，the content of Mo4O11 in the sample at this time was significantly higher than that at α4=0.2510. When the reaction extent was increased to α6=0.4129，it could be found that α-MoO3 disappeared completely and MoO2 began to be generated，and the obtained products were mainly composed of Mo4O11 and MoO2. While when the reaction extent was increased to α7=0.4753，the reaction product was only MoO2. With the continuous increase of reaction temperature，the reduction reaction of MoO2 to Mo began，and during the following stage，the content of MoO2wasgradually decreased，while that of metallic Mo gradually increased. When the reaction reached a plateau，the reaction product was only metallic Mo. The total reaction paths of h-MoO3→α-MoO3+Mo4O11→MoO2→Mo was concluded. According to FESEM images，it was found that the original sample first changed from a smooth hexagonal prismatic structure to a rough step-like structure，then to a smooth and irregular layered shape，and finally evolved into fine smooth particles，with the continue process of the reaction. In this case，the average particle size of the as-prepared Mo powder was measured to be 369.81 nm. The work also found that the chemical vapor phase transport mechanism dominated during the reduction process of MoO3 to MoO2；as to the reduction process ofMoO2 to Mo，however，the pseudomorphic transformation mechanism dominated，and the obtained metallic Mo basically maintained the same sheet morphology as MoO2.
quote
| GB/T 7714-2015 | [1] Hongxiao Li, Lu Wang, Zhengliang Xue. Temperature-Programmed Reduction Reaction between h-MoO3 and H2 to Prepare Ultrafine Mo Powder[J]. Chinese Journal of Rare Metals, 2025, 49(5): 726-736. DOI:10.13373/j.cnki.cjrm.XY24010004. |
| MLA | [1] Hongxiao Li, et al., "Temperature-Programmed Reduction Reaction between h-MoO3 and H2 to Prepare Ultrafine Mo Powder." Chinese Journal of Rare Metals, vol. 49, no. 5, 2025, pp. 726-736, https://doi.org/10.13373/j.cnki.cjrm.XY24010004. |
| APA | [1] Hongxiao Li, Lu Wang, & Zhengliang Xue. (2025). Temperature-Programmed Reduction Reaction between h-MoO3 and H2 to Prepare Ultrafine Mo Powder. Chinese Journal of Rare Metals, 49(5), 726-736. https://doi.org/10.13373/j.cnki.cjrm.XY24010004 |
| IEEE | [1] Hongxiao Li, Lu Wang, and Zhengliang Xue, "Temperature-Programmed Reduction Reaction between h-MoO3 and H2 to Prepare Ultrafine Mo Powder," Chinese Journal of Rare Metals, vol. 49, no. 5, pp. 726-736, 2025, doi: 10.13373/j.cnki.cjrm.XY24010004. keywords: {ultrafine Mo powder;h-MoO;H;temperature-programmed reduction;reaction mechanism} |