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The chemical reduction progression behaviour of transition metals (Mo, Zr, W, Ce, and Co) doped on NiO was studied using temperature programmed reduction (TPR) analysis. A wet impregnation method was applied to synthesise the doped NiO series catalysts. The reduction progress of the catalysts was attained by using a reductant gas at the concentration of 40% v/v CO/N2. X-ray diffraction (XRD) was employed to determine the composition of the reduced phases. Undoped NiO was reduced at 384℃ to obtain a cubic phase of NiO. It was observed that Ce/NiO exhibited the lowest reduction temperature of 370℃ among all catalysts. This phenomenon might be due to a higher surface area of Ce/NiO compared to undoped NiO, which facilitated a faster reduction reaction. The rest of the doped NiO series catalysts (Co/NiO, Mo/NiO, W/NiO and Zr/NiO) demonstrated a higher reduction temperature compared to undoped NiO. New peaks in the XRD pattern were observed only for the reduced catalysts of Mo/NiO and W/NiO, which were associated with monoclinic MoO2 and WO2.72 phases, respectively. The formation of new compounds or more stable nickel alloys led to a slower reduction reaction than undoped NiO. Therefore, Ce/NiO was the most efficient catalyst in promoting the formation of Ni under the CO atmosphere.

Temperature programmed reduction (TPR) analysis was applied to investigate the chemical reduction progression behavior of molybdenum oxide (MoO3) catalyst. The composition and morphology of the reduced phases were characterized by X-ray diffraction spectroscopy (XRD), X-ray photoelectron spectroscopy (XPS), and field emission scanning electron microscopy (FE-SEM). The reduction progression of MoO3 catalyst was attained with different reductant types and concentration (10% H2/N2, 10% and 20% CO/N2 (%, v/v)). Two different modes of reduction process were applied. The first approach of reduction involved non-isothermal mode reduction up to 700 °C, while the second approach of reduction involved the isothermal mode reduction for 60 min at 700 °C. Hydrogen temperature programmed reduction (H2-TPR) results showed the reduction progression of three-stage reduction of MoO3 (Mo6+ → Mo5+ → Mo4+ → Mo0) with Mo5+ and Mo4+. XRD analysis confirmed the formation of Mo4O11 phase as an intermediate phase followed by MoO2 phase. After 60 min of isothermal reduction, peaks of metallic molybdenum (Mo) appeared. Whereas, FESEM analysis showed porous crater-like structure on the surface cracks of MoO2 layer which led to the growth of Mo phase. Meanwhile, the reduction of MoO3 catalyst in 10% carbon monoxide (CO) showed the formation of unstable intermediate phase of Mo9O26 at the early stage of reduction. Furthermore, by increasing 20% CO led to the carburization of MoO2 phase, resulted in the formation of Mo2C rather than the formation of metallic Mo, as confirmed by XPS analysis. Therefore, the presented study shows that hydrogen gave better reducibility due to smaller molecular size, which contributed to high diffusion rate and achieved deeper penetration into the MoO3 catalyst compared to carbon monoxide reductant. Hence, the reduction of MoO3 in carbon monoxide atmosphere promoted the formation of Mo2C which was in agreement with the thermodynamic assessment.

The purposes of this study are to reduce Fe2O3 using hydrogen (H2) and carbon monoxide (CO) gases at a high temperature zone (500 °C–900 °C) by focusing on the influence of reduction gas concentrations. Reduction behavior of hematite (Fe2O3) at high temperature was examined using temperature programmed reduction (TPR) under non-isothermal conditions with the presence of 10% H2/N2, 20% H2/N2, 10% CO/N2, 20% CO/N2 and 40% CO/N2. The TPRCO results indicated that the first and second reduction peaks of Fe2O3 at a temperature below 660 °C appeared rapidly when compared to TPRH2. However, TPRH2 exhibited a better reduction in which Fe2O3 entirely reduced to Fe at temperature 800 °C (20% H2) without any remaining of wustite (FeO) whereas a temperature above 900 °C is needed for a complete reduction in 10% H2/N2, 10% and 20% CO/N2. Furthermore, the reduction of hematite could be improved when increasing CO and H2 concentrations since reduction profiles were shifted to a lower temperature. Thermodynamic calculation has shown that enthalpy change of reaction (ΔHr) for all phases transformation in CO atmosphere is significantly lower than in H2. This disclosed that CO is the best reductant as it is a more exothermic, more spontaneous reaction and able to initiate the reduction at a much lower temperature than H2 atmosphere. Nevertheless, the reduction of hematite using CO completed at a temperature slightly higher compared to H2. It is due to the presence of an additional carburization reaction which is a phase transformation of wustite to iron carbide (FeO → Fe3C). Carburization started at the end of the second stage reduction at 600 °C and 630 °C under 20% and 40% CO, respectively. Therefore, reduction by CO encouraged the formation of carbide, slower the reduction and completed at high temperature. XRD analysis disclosed the formation of austenite during the final stage of a reduction under further exposure with high CO concentration. Overall, less energy consumption needed during the first and second stages of reduction by CO, the formation of iron carbide and austenite were enhanced with the presence of higher CO concentration. Meanwhile, H2 has stimulated the formation of pure metallic iron (Fe), completed the reduction faster, considered as the strongest reducing agent than CO and these are effective at a higher temperature. Proposed iron phase transformation under different reducing agent concentrations are as followed: (a) 10% H2, 20% H2 and 10% C; Fe2O3 → Fe3O4 → FeO → Fe, (b) 20% CO; Fe2O3 → Fe3O4 → FeO → Fe3C → Fe and (c) 40% CO; Fe2O3 → Fe3O4 → FeO → Fe3C → Fe → F,C (austenite).

The physical and chemical behaviour of bulk tungsten oxide (WO3) and Ni doped tungsten oxide (15% Ni/WO3) were examined by performing a temperature-programmed reduction (TPR) technique. The chemical composition, morphology, and surface composition of both samples before and after reduced were analysed by X-ray diffraction (XRD), scanning electron microscopy (FESEM), and X-ray photoelectron spectroscopy (XPS) analysis. The XRD pattern of calcined Ni doped tungsten oxide powder comprised of WO3 and nickel tungstate (NiWO4) phases. The reduction behaviour was investigated by a non-isothermal reduction up to 900 °C achieved under (10 and 20% v/v) hydrogen in nitrogen (H2 in N2) and (20 and 40% v/v) carbon monoxide in nitrogen (CO in N2) atmospheres. The H2-TPR were indicated the reduction of bulk WO3 and 15% NiWO3 proceed in three steps (WO3 → WO2 → WO2 + W) and (WO3 → WO2 → W + Ni4W) respectively under 20% H2. Whereas, the reduction of 15% WO3 under 40% CO involves of two following stages: (i) low temperature ( 800 °C) transformation of WO2 → W → WC. Furthermore, NiWO4 alloy phase was transformed according to the sequence NiWO4 → Ni + WO2.72 → Ni + WO2 → Ni + W → Ni4W + W at temperature >700 °C and >800 °C in H2 and CO atmospheres, respectively. It can be concluded that the reduction behaviour of WO3 is matched with the thermodynamic data. In addition, the reduction under H2 is more favourable and have better reducibility compared to the CO gas. It is due to the small molecule size and molecule mass of H2 that encourages the diffusion of H2 molecule into the internal surface of the catalyst compared to CO. Moreover, Ni additive had improved the WO3 reducibility and enhancing the CO adsorption and promotes the formation of tungsten carbide (WC) by carburisation reaction. Besides, the formation of Ni during the reduction of 15% Ni/WO3 under CO reductant catalysed the Boudouard reaction to occur, which disproportionated the carbon monoxide to carbon dioxide and carbon (CO → CO2 + C).

Temperature-programmed reduction (TPR) was used to observe the chemical reduction behaviour of molybdenum trioxide (MoO3) and zirconia (Zr)-doped MoO3 catalyst by using carbon monoxide (CO) as the reductant. The characterisation of catalysts was performed by X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET) and transmission electron microscopy (TEM) analyses. The reduction performance were examined up to 700°C and reduction was continued for 60 min at 700°C in a stream of 20 vol. % CO in nitrogen. The TPR profile showed that the doped MoO­3 catalyst was slightly moved to a higher temperature (580°C) as compared to the undoped MoO3 catalyst, which began at around 550°C. The interaction between zirconia and molybdenum ions in doped MoO3 catalyst led to an increase in the reduction temperature. According to characterisation of the reduction products by using XRD, it revealed that the reduction behaviour of pure MoO3 to MoO2 by CO reductant involved two reduction stages with the formation of Mo4O11 as the intermediate product. Meanwhile, MoO3 catalyst doped with zirconia caused a delay in the reduction process and was proven by the presence of Mo4O11 species at the end of reactions. Physical analysis by using BET showed a slight increase in surface area of 3% Zr-MoO3 from 6.85 m2/g to 7.24 m2/g. As for TEM analysis, black tiny spots located around MoO3 particles revealed that the zirconia was successfully intercalated into MoO3 particles. This confirmed that formation of intermetallic between Zr-MoO3 catalyst will give new chemical and physical properties which has a remarkable chemical effect by disturbing the reduction progression of MoO3 catalyst.

Surface modification of Fe2O3 by adding BeO was synthesized and calcined at different temperatures of 200-600 °C. The adsorbents were characterized by using XRD, N2 adsorption-desorption isotherm prior to performing CO2 adsorption and desorption studies. The CO2 adsorption data were analyzed using adsorption isotherm models such as Langmuir, Freundlich, Temkin, and Dubinin-Radushkevich. BeO/Fe2O3-300 that calcined at 300 °C showed the most efficient adsorbent with physisorption and chemisorption were measured at 5.85 and 45.88 mg/g respectively. The CO2 adsorption notably best fitted with Freundlich isotherm with R2 = 0.9897 and calculated adsorption capacity closest to experimental data. This implies the CO2 adsorption process was governed by multilayer adsorption on the heterogeneous surface of the adsorbent. The mean free energy of adsorption (E=3.536 kJ/mol) from Dubinin-Radushkevich and heat of adsorption (bT=3.219 kJ/mol) from the Temkin model support that the adsorption process is physical phenomena.

The reduction behaviour of cobalt doped with nickel oxide and undoped nickel oxide (NiO) by hydrogen (H2) in nitrogen (20%, v/v) and carbon monoxide (CO) in nitrogen (40%, v/v) atmospheres have been investigated by temperature programmed reduction (TPR). The phases formed of partially and completely reduced samples were characterized by X-ray diffraction spectroscopy (XRD). TPR results indicate that the reduction of Co doped and undoped nickel oxide in both reductants proceed in one step reduction (NiO → Ni) without intermediate. TPR results also suggested that by adding Co metal into NiO, the reduction to metallic Ni by both reductant gaseous give different intensity of the peak. The reduction process of Co and undoped NiO become faster when H2 was used as a reductant. Furthermore, in H2 atmosphere, Co-NiO give complete reduction to metallic Ni at 700 °C. Meanwhile, XRD analysis indicated that NiO without Co composed better crystallite phases of NiO with higher intensity.

The reduction behavior of nickel oxide (NiO) and zirconia (Zr) doped NiO (Zr/NiO) was investigated using temperature programmed reduction (TPR) using carbon monoxide (CO) as a reductant and then characterized using X-ray diffraction (XRD), nitrogen absorption isotherm using BET technique and FESEM-EDX. The reduction characteristics of NiO to Ni were examined up to temperature 700 °C and continued with isothermal reduction by 40 vol. % CO in nitrogen. The studies show that the TPR profile of doped NiO slightly shifts to a higher temperature as compared to the undoped NiO which begins at 387 °C and maximum at 461 °C. The interaction between ZrO2 with Ni leads to this slightly increase by 21 to 56 °C of the reduction temperature. Analysis using XRD confirmed, the increasing percentage of Zr from 5 to 15% speed up the reducibility of NiO to Ni at temperature 550 °C. At this temperature, undoped NiO and 5% Zr/NiO still show some crystallinity present of NiO, but 15% Zr/NiO shows no NiO in crystalline form. Based on the results of physical properties, the surface area for 5% Zr/NiO and 15% Zr/NiO was slightly increased from 6.6 to 16.7 m2/g compared to undoped NiO and for FESEM-EDX, the particles size also increased after doped with Zr on to NiO where 5% Zr/NiO particles were 110 ± 5 nm and 15% Zr/NiO 140 ± 2 nm. This confirmed that the addition of Zr to NiO has a remarkable chemical effect on complete reduction NiO to Ni at low reduction temperature (550 °C). This might be due to the formation of intermetallic between Zr/NiO which have new chemical and physical properties.

The aims of this study are to produce Fe3O4 from Fe2O3 using hydrogen (H2) and carbon monoxide (CO) gases by focusing on the influence of these gases on reduction of Fe2O3 to Fe3O4 at low temperature (below 500 °C). Low reduction temperature behavior was investigated by using temperature programmed reduction (TPR) with the presence of 20% H2/N2, 10% CO/N2, 20% CO/N2 and 40% CO/N2. The TPR results indicated that the first reduction peak of Fe2O3 at low temperature appeared faster in CO atmosphere compared to H2. Furthermore, reducibility of first stage reduction could be improved when increasing CO concentration and reduction rate were followed the sequence as: 40% CO > 20% CO > 10% CO > 10% H2. All reduction peaks were shifted to higher temperature when the CO concentration was reduced. Although, initial reduction by H2 occurred slower (first peak appeared at higher temperature, 465 °C) compared to CO, however, it showed better reduction with Fe2O3 fully reduced to Fe at temperature below 800 °C. Meanwhile, complete reduction happened at temperature above 800 °C in 10% and 20% CO/N2. Thermodynamic calculation revealed that CO acts as a better reducer than H2 as the enthalpy change of reaction (ΔHr) is more exothermic than H2 and the change in Gibbs free energy (ΔG) at 500 °C is directed to more spontaneous reaction in converting Fe2O3 to Fe3O4. Therefore, formation of magnetite at low temperature was thermodynamically more favorable in CO compared to H2 atmosphere. XRD analysis explained the formation of smaller crystallite size of magnetite by H2 whereas reduction of CO concentration from 40, 20 to 10% enhanced the growth of highly crystalline magnetite (31.3, 35.5 and 39.9 nm respectively). All reductants were successfully transformed Fe2O3 → Fe3O4 at the first reduction peak except for 10% CO/N2 as there was a weak crystalline peak due to remaining unreduced Fe2O3. Overall, less energy consumption needed in reducing Fe2O3 to Fe3O4 by CO. This proved that CO was enhanced the formation of magnetite, encouraged formation of highly crystalline magnetite in more concentrated CO, considered better reducing agent than H2 and these are valid at lower temperature.

During the monsoon season, a wild-termite mushroom Termitomyces heimii RFES 230662 (THR2) was successfully isolated from Negeri Sembilan, Malaysia. The mushroom was morphologically labelled based on its stipe, pileus, and the budding mycelia from the termites nest. Genetic component of THR2 (300 bp) was sequenced and found to be 99% identical to Termitomyces sp. strain. The evolutionary distance (Knuc) of the isolate justified THR2 as T. heimii species. Two THR2 extracts were prepared from fruiting body (FB) and mycelial biomass (MB) for antimicrobial responses. THR2 was cultivated in a submerged-fermentation (SF) producing 8.55 g/L of MB, 0.80 g/L of endopolysaccharide (ENS) and 1.44 g/L of exopolysaccharide (EPS), respectively. For THR2-FB, two ENS extracts were obtained using hot (3.20 g/L) and cold-water (1.36 g/L) treatments. FTIR spectra analysis verified all polysaccharide as β-glucan when compared to laminarin standard. Those β-glucan possess antibacterial properties with highest response shown by s-glucan-FB compared to s-glucan-MB extracts. These findings serve as the blueprint for the production of β-glucan from a rare termite mushroom.

Chemical reduction behaviour of 3% chromium doped (Cr–Fe2O3) and undoped iron oxides (Fe2O3) were investigated by using temperature programmed reduction (TPR). The reduced phases were characterized by X-ray diffraction spectroscopy (XRD). The reduction processes were achieved with 10% H2 in nitrogen (%, v/v), 10% and 20% of carbon monoxide (CO) in nitrogen (%, v/v). In hydrogen atmosphere, the TPR results indicate that the reduction of Cr–Fe2O3 and Fe2O3 proceed in three steps (Fe2O3 → Fe3O4 → FeO → Fe) with Fe3O4 and FeO as intermediate states. A complete reduction to metallic iron for both samples occurred at 900 °C. As for CO reductant, the profiles show the reduction of Fe2O3 also proceeded in three steps with a complete reduction occurs at 900 °C in 10% CO with no sign of carbide formation. Nevertheless, a 20% CO was able to reduce the completely at lower temperature at 700 °C and there is a formation of iron carbide at 500 °C but the carbide disappeared as the reduction temperature increase. Meanwhile in 10% CO atmosphere, Cr–Fe2O3 shows a better reducibility compared to Fe2O3 with a complete reduction at 700 °C, which is 200 °C lower than Fe2O3. A Cr dopant in the Fe2O3 can lead to formation of various forms of iron carbides such as F2C, Fe5C2, Fe23C6 and Fe3C as the CO concentration was increased to 20%. The transformation profile of iron phases during carburization follows the following forms, Fe2O3 → Fe3O4 → iron carbides (FexC). The XRD pattern shows the diffraction peaks of Cr–Fe2O3 are more intense with improved crystallinity for the characteristic peaks of Fe2O3 compare to undoped Fe2O3. No visible sign of chromium particles peaks in the XRD spectrum that indicates the Cr particles loaded onto the iron oxide are well dispersed. The uniform dispersion with no sign of sintering effects of the Cr dopant on the Fe2O3 was confirmed by FESEM. The study shows that Cr dopant gives a better reducibility of iron oxide but promotes the formation of carbides in an excess CO concentration.

The reduction of pure WO3 and Ce/WO3 has been studied by using temperature programmed reduction (TPR), X-ray diffraction (XRD), and FESEM analysis. The reduction behavior were examined by non-isothermal reduction up to 900 oC then continued with isothermal reduction at 900 oC for 45 min under (40% v/v) carbon monoxide in nitrogen (CO in N2) atmosphere. The TPR results shows that reduction peak of Ce/WO3 were shifts to lower temperature as compared with to the pure WO3. In addition, TPR results indicate that addition with ceria give better reducibility compared to pure WO3. Based on the characterization of the reduction products after hold 45 min using XRD, pure WO3 were completely converted to WO2 and W metal phases. While, after addition of Ce to the WO3, the reduction was enhanced to W phases and some suboxide W5O14 and W3O5 with no WO2 phase remained and carbide observed. This is associated to the formation of alloy complex Ce2WO6 which gave remarkable effect to the reduction.

This study was undertaken to investigate the effect of carburization of metallic Fe by (20%,v/v) carbon monoxide (CO). Carburization of Fe by carbon monoxide was examined by using temperature-programmed reduction (TPR), X-Ray powder diffractometry (XRD) and Carbon Hydrogen Nitrogen Sulfur (CHNS) technique. Based on a thermodynamic calculation, the free energy Gibb’s value to produce carbon is-8.08 kcal/mol which are favorable. However, production of iron carbide from the same reaction, the free energy Gibb’s value is +9.24 kcal/mol which is not feasible. From the XRD results, shows that after carburization of Fe, the peak appears only for Fe but there is a broad peak between 20 – 30°. The peak might be indicated as carbon in amorphous form. This finding is supported by the percent of carbon content in CHNS analysis which are increasing when the temperature is increased. This shows that after carburization the carbon content is increasing with increasing in temperature due to carbon deposited on metallic iron. In this research, three different temperatures were used which are 300°C, 500°C and 700°C.

The reduction behavior of silver doped molybdenum trioxide (Ag/MoO3) and undoped MoO3 by using carbon monoxide, CO were investigated by using temperature programmed reduction (TPR). The reduced phases were characterized by X-ray diffraction (XRD). In the carbon monoxide atmosphere, the XRD results indicated that the reduction of Ag/MoO3 and undoped MoO3 to MoO2 phase proceed in two steps (MoO3 → Mo4O11 → MoO2) with Mo4O11 present as an intermediate state. A complete reduction to metallic molybdenum for both samples cannot occurred since in an excess CO atmosphere, MoO2 is promoted to form carbides rather than reduce to metallic molybdenum. Nevertheless, addition of silver to modified MoO3 shows the better reducibility compared to MoO3 alone by lower the reducing temperature of MoO3. TPR results show that the reduction peak of Ag/MoO3 is slightly shifts to lower temperature as compared with the undoped MoO3. The interaction between silver and molybdenum ions leads to this slightly decrease of the reduction temperature of silver doped MoO3. It can be seen that doping with silver has a remarkable influence in the reduction process of the MoO3 catalyst.

Reduction of iron oxide is one of the most studied topics owing to the importance of iron/steel industry and also has been used as a precursor and active component in a number of important chemical processes. The interaction between iron oxide and other metal additive have gained interest in the past two decades due to the ability on enhancing the reduction performance of the iron oxide. Therefore, this study was undertaken to investigate the influence of cerium on the reduction behaviours of iron oxide by (10%, v/v) carbon monoxide in nitrogen. The cerium doped (Ce-Fe2O3) and non-doped iron oxide reduction behaviour and the kinetic studies have been studied by temperature programmed reduction (TPR) and the phases formed of partially and completely reduced samples were characterized by X-ray diffraction spectroscopy (XRD) while the activation energy values were calculated from Arrhenius equation using Wimmer’s method. TPR results indicate that the reduction of doped and undoped iron oxide proceeds in three steps reduction (Fe2O3 ? Fe3O4 ? FeO ? Fe), while doped iron oxide showed a large shifted towards lower temperature especially in the transition steps of FeO ? Fe. Furthermore, TPR results also suggested that by adding Ce metal into iron oxide the reduction of metal iron completed at lower temperature (700 ?C) compared to non-doped iron oxide (900 ?C). Meanwhile, XRD analysis indicated that doped iron oxide composed of Fe2O3 and a small amount of FeCe2O4. The increase in the rates of iron oxide reduction may relate to the presence of cerium species in the formed of FeCe2O4 and was confirmed by the decrease in the activation energy regarding to all transition phases (Fe2O3 ? Fe3O4 ? FeO ? Fe) during the reduction process

Depletion of fossil fuels resources has triggered more research on finding potential alternative sources that are more sustainable such as biomass waste. However, deconstruction of the complex biomass waste into desired products is too challenging and usually require a strong catalyst with a great hydrolysing property. Common acids such as sulphuric acid, hydrochloric acid and nitric acid were the most studies for biomass conversion. These liquid acids catalysts suffer low recovery and recyclability that can be overcome by a solid acid catalyst. Heteropoly acid (HPA) catalyst is the preferred choice to replace these common acid catalysts as it is known to have a strong Bronsted acid site with an oxidizing property that allows this catalyst to hydrolyse and oxidize in one-step reaction. Furthermore, heteropoly acid (HPA) catalyst can be modified into heterogenous type of catalyst by solidifying HPA to increase the surface area and recyclability. Future work of this research is necessary to improvise the previous method of the catalyst preparation and to suppress the by-products after the catalytic process. In this review, we summarize the use of HPA catalyst in the complex reaction process of biomass conversion to valuable chemical products.

The reduction behaviour of 3% cerium doped (Ce-Fe2O3) and undoped iron oxide (Fe2O3) by hydrogen in nitrogen (10%,v/v) and carbon monoxide in nitrogen (10%,v/v) atmospheres have been investigate by temperature programmed reduction (TPR). The phases formed of partially and completely reduced samples were characterized by X-ray diffraction spectroscopy (XRD). TPR results indicate that the reduction of Ce doped and undoped iron oxide in both reductants proceed in three steps reduction (Fe2O3 → Fe3O4 → FeO → Fe) with Fe3O4 and FeO were the intermediate. TPR results also suggested that by adding Ce metal into iron oxide the reduction to metallic Fe by using both reductant gaseous give better reducibility compare to the undoped Fe2O3. The reduction process of Ce and undoped Fe2O3 become faster when CO was used as a reductant instead of H2. Furthermore, in CO atmosphere, Ce-Fe2O3 give complete reduction to metallic iron at 700 0C which about 200 0C temperature lower than other samples. Meanwhile, XRD analysis indicated that Ce doped iron oxide composed better crystallite phases of Fe2O3 with higher intensity and a small amount of FeCe2O4.

The reduction behavior of molybdenum trioxide (MoO3) by carbon monoxide (CO) has been studied using temperature programmed reduction (TPR) and was characterized using X-ray diffraction spectroscopy (XRD). The TPR result shows that the first reduction peak of MoO3 under 20 vol. % CO in nitrogen started at 530 °C and second reduction peaks observed was at 700 °C. The XRD technique was employed to identify the changes in the sample. It was found that after non-isothermal reduction up to 700 °C, the intermediate phases Mo4O11 were observed. Completed reduction to MoO2 achieved after continued reduction with isothermal mode at 700 °C for 60 minutes. Based on the XRD analysis, it is confirmed that the reduction of MoO3 to MoO2 in CO atmosphere consists of two reduction stages, i) Mo6+ → Mo5+ and ii) Mo5+ → Mo4+. While, CO excess have resulted the formation of molybdenum carbide (Mo2C) rather than formation of metallic molybdenum (Mo).

The reduction behaviour of tungsten oxide has been studied by using temperature programmed reduction (TPR) and X-ray diffraction (XRD). The reduction behavior were examine by nonisothermal reduction up to 900 oC then continued with isothermal reduction at 900 oC for 45 min time under (40% v/v) carbon monoxide in nitrogen (CO in N2) atmosphere. The TPR signal clearly shows one peak attributed to formation of suboxide W18O49 (more) and WO2 (less) observed at 80 min. The reduction product was investigated by varying the holding reaction time. Based on the characterization of the reduction products by using XRD, it was found that, nonisothermal reduction of WO3 at temperature 900 oC partially converted to some W18O49 and WO2 phases. However, after increased the reaction holding time for 45 min, WO3 phases disappeared and converted to WO2 and W metal phases. It is obviously shows that by hold the reduction time could improve the reducibility of the sample oxide. Furthermore, it is suggested that reduction by using CO as reducing agent follows the consecutives steps WO3 → WO2.92 → W18O49 → WO2 → W.

Tungsten (VI) oxide (WO3) reduction by carbon monoxide were examined using temperature-programmed reduction (TPR) and X-ray powder diffractometry (XRD) studies. Results show that WO3 start to reduce at 20% (CO in N2) at temperature 900 °C and the intermediate phases WO2.9 and WO2.83 were observed. The WO3 was reduced and transformed the completely to the WO2.72. As comparison, reduction by using 10% (H2 in N2), WO3 was reduced completely toWO2. The WO3 is a stable oxide because the reduction agent used to promote the reduction was not sufficient enough to reduce to zero metal tungsten.

A metallic molybdenum is formed by a two-stage process that was carburized MoO2 with carbon monoxide followed by heat treatment. XRD techniques were employed to identify the phase’s changes in the sample. It was found that by the present of carbon monoxide during carburization process until 900 °C, Mo2C is formed first, compared to metallic molybdenum, due to the high thermodynamic barrier for formation of metallic molybdenum. In the second stage, Mo2C further reacts with the remaining MoO2 at 900 °C to produce metallic molybdenum.