Topic
Temperature-programmed reduction
About: Temperature-programmed reduction is a research topic. Over the lifetime, 2924 publications have been published within this topic receiving 97092 citations.
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TL;DR: In this paper, a three-stage mechanism for the reduction of various iron oxides in hydrogen and carbon monoxide atmospheres has been investigated by temperature programmed reduction (TPR H2 and TPR CO ), thermo-gravimetric and differential temperature analysis (TG-DTA-MS), and conventional and in situ XRD methods.
Abstract: The reduction of various iron oxides in hydrogen and carbon monoxide atmospheres has been investigated by temperature programmed reduction (TPR H2 and TPR CO ), thermo-gravimetric and differential temperature analysis (TG-DTA-MS), and conventional and “ in situ ” XRD methods Five different compounds of iron oxides were characterized: hematite α-Fe 2 O 3 , goethite α-FeOOH, ferrihydrite Fe 5 HO 8 ·4H 2 O, magnetite Fe 3 O 4 and wustite FeO In the case of iron oxide-hydroxides, goethite and ferrihydrite, the reduction process takes place after accompanying dehydration below 300 °C Instead of the commonly accepted two-stage reduction of hematite, 3 α-Fe 2 O 3 → 2 Fe 3 O 4 → 6 Fe, three-stage mechanism 3Fe 2 O 3 → 2Fe 3 O 4 → 6FeO → 6Fe is postulated especially when temperature of reduction overlaps 570 °C Up to this temperature the postulated mechanism may also involve disproportionation reaction, 3Fe 2+ ⇌ 2Fe 3+ + Fe, occurring at both the atomic scale on two-dimensional interface border Fe 3 O 4 /Fe or stoichiometrically equivalent and thermally induced, above 250 °C, phase transformation—wustite disproportionation to magnetite and metallic iron, 4FeO ⇌ Fe 3 O 4 + Fe Above 570 °C, the appearance of wustite phase, as an intermediate of hematite reduction in hydrogen, was experimentally confirmed by “ in situ ” XRD method In the case of FeO–H 2 system, instead of one-step simple reduction FeO → Fe, a much more complex two-step pathway FeO → Fe 3 O 4 → Fe up to 570 °C or even the entire sequence of three-step process FeO → Fe 3 O 4 → FeO → Fe up to 880 °C should be reconsidered as a result of the accompanying FeO disproportionation wustite ⇌ magnetite + iron manifesting its role above 150 °C and occurring independently on the kind of atmosphere—inert argon or reductive hydrogen or carbon monoxide The disproportionation reaction of FeO does not consume hydrogen and occurs above 200 °C much easier than FeO reduction in hydrogen above 350 °C The main reason seems to result from different mechanistic pathways of disproportionation and reduction reactions The disproportionation reaction wustite ⇌ magnetite + iron makes simple wustite reduction FeO → Fe a much more complicated process In the case of thermodynamically forced FeO disproportionation, the oxygen sub-lattice, a closely packed cubic network, does not change during wustite → magnetite transformation, but the formation of metallic iron phase requires temperature activated diffusion of iron atoms into the region of inter-phase FeO/Fe 3 O 4 Depending on TPR H2 conditions (heating rate, velocity and hydrogen concentration), the complete reduction of hematite into metallic iron phase can be accomplished at a relatively low temperature, below 380 °C Although the reduction behavior is analogical for all examined iron oxides, it is strongly influenced by their size, crystallinity and the conditions of reduction
532 citations
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TL;DR: In this paper, a simplified mechanism for the catalytic oxidation of formaldehyde (HCHO) over 1% Pt/TiO2 was proposed, based on the behavior of adsorbed species on the surface at room temperature using in situ DRIFTS.
Abstract: The performance of TiO2 supported noble metal (Pt, Rh, Pd and Au) catalysts was examined and compared for the catalytic oxidation of formaldehyde (HCHO). Among them, the Pt/TiO2 was the most active catalyst. The effects of Pt loading and gas hourly space velocity (GHSV) on Pt/TiO2 activity for HCHO oxidation were investigated at a room temperature (20 degrees C). The optimal Pt loading is 1 wt.%. At this loading, HCHO can be completely oxidized to CO2 and H2O over the Pt/TiO2 in a GHSV of 50,000 h(-1) at 20 degrees C. The 1% Pt/TiO2 was characterized using BET, XRD, high resolution (HR) TEM and temperature programmed reduction (TPR) methods. The XRD patterns and HR TEM image show that Pt particles on TiO2 are well dispersed into a size smaller than 1 nm, an important feature for the high activity of the 1% Pt/TiO2. The mechanism of HCHO oxidation was studied with respect to the behavior of adsorbed species on Pt/TiO2 surface at room temperature using in situ DRIFTS. The results indicate that surface formate and CO species are the main reaction intermediates during the HCHO oxidation. The formate species could decompose into adsorbed CO species on the catalyst surface without the presence Of O-2, and the CO was then oxidized to CO, with the presence of O-2. Based on these results, a simplified mechanism for the catalytic oxidation of HCHO over 1% Pt/TiO2 was proposed. (c) 2006 Elsevier B.V. All rights reserved.
502 citations
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TL;DR: In this paper, the success or otherwise of catalyst preparation or modification depends on the availability of suitable characterization techniques to determine the condition of the catalyst, and none of these techniques has proved to be wholly reliable or generally applicable to the characterization of catalysts under working conditions.
Abstract: The success or otherwise of catalyst preparation or modification depends on the availability of suitable characterization techniques to determine the condition of the catalyst. There are many techniques available for this purpose including x-ray powder diffraction, electron microscopy, photoelectron spectroscopy, and infrared spectroscopy. However, none of these techniques has proved to be wholly reliable or generally applicable to the characterization of catalysts under working conditions.
467 citations
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TL;DR: The results showed that PdO is finely dispersed on the supports with high surface area DRIFTS of CO adsorption further indicated that both Pd 2+ and Pd 0 species coexist in Pd/CeO 2, while only pd 0 is detected in Pdr 0 and Pdr 1 species in C CeO 2 and CeO 0 as mentioned in this paper, which may indicate that the special Pd-Ce-Ti interaction is favorable for the reduction of Pd o 2 and interfacial O 2 species.
439 citations
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TL;DR: In this paper, a Ni/olivine catalyst, previously developed for biomass gasification and tar removal during fluidized bed steam gasification of biomass, was tested in a fixed bed reactor in toluene steam reforming as a tar destruction model reaction.
Abstract: A Ni/olivine catalyst, previously developed for biomass gasification and tar removal during fluidized bed steam gasification of biomass, was tested in a fixed bed reactor in toluene steam reforming as a tar destruction model reaction. The influence of the catalyst preparation parameters (nickel precursor, calcination temperature and nickel content) and operating parameters (reaction temperature, steam to carbon S/C ratio and space-time) on activity and selectivity was examined showing a high toluene conversion and a low carbon formation compared to olivine alone. The steam reforming of toluene was found to be of zero order for water and first order for toluene. Activation energy required for Ni/olivine was determined to be about 196 kJ mol−1 in accordance with literature. Catalyst activity and stability and its resistance against carbon formation were discussed on the basis of X-ray diffraction (XRD), transmission electron microscopy (TEM) and temperature programmed oxidation (TPO) results. Characterization before test (XRD, temperature programmed reduction (TPR), Mossbauer spectroscopy) have shown the presence of NiO–MgO solid solution, formed on the surface of olivine support, which explains the efficiency of the catalyst calcined at 1100 °C. After test, Ni–Fe alloys were observed (TEM, Mossbauer spectroscopy). It was suggested that magnesium oxide enhanced steam adsorption, facilitating the gasification of surface carbon and that Ni–Fe alloys prevented carbon deposition by dilution effect.
408 citations