Catalytic combustion of methane over Pd/SnO2 catalysts

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1 Chinese Journal of Catalysis 38 (2017) 催化学报 2017 年第 38 卷第 8 期 available at journal homepage: Article Catalytic combustion of methane over Pd/SnO2 catalysts Zhenyang Zhao, Bowei Wang, Jian Ma, Wangcheng Zhan, Li Wang *, Yanglong Guo, Yun Guo #, Guanzhong Lu Key Laboratory for Advanced Materials and Research Institute of Industrial Catalysis, School of Chemistry and Molecular Engineering, East China University of Science and Technology, Shanghai , China A R T I C L E I N F O A B S T R A C T Article history: Received 26 March 2017 Accepted 18 May 2017 Published 5 August 2017 Keywords: Methane combustion Palladium Tin oxide Lattice match Oxygen activation SnO2 supported Pd catalysts were prepared and the effects of the support calcination temperature on the subsequent catalytic activity during methane combustion were investigated. The physicochemical properties of the Pd/SnO2 were characterized by X ray diffraction, high resolution transmission electron microscopy, X ray photoelectron spectroscopy, oxygen temperature programmed desorption and CH4 temperature programmed surface reaction. Only crystalline Pd species were found on the catalysts fabricated from the supports calcined above 800 C. It was also determined that lattice geometry matching between PdO and SnO2 in the catalyst made with a support calcined at 1200 C facilitated oxygen activation from SnO2 to vacant oxygen sites on the PdO/Pd surface via the back spillover of oxygen. This effect in turn enhanced the catalytic combustion process. The activity of this material was clearly increased compared with the catalysts that did not exhibit lattice matching between the PdO and support. 2017, Dalian Institute of Chemical Physics, Chinese Academy of Sciences. Published by Elsevier B.V. All rights reserved. 1. Introduction Methane, the main component of natural gas and a well known greenhouse gas (with 20 times the greenhouse effect of CO2), has been widely used in power generation and other industrial heating applications. The incomplete combustion of natural gas not only wastes energy but also produces atmospheric pollution such as CO, NOx, and unburned hydrocarbons. Compared with standard combustion, the catalytic combustion of CH4 may provide an environmentally friendly method of generating power with greater efficiency and lower emissions of air pollutants [1 4]. Because of the highly symmetrical structure of CH4, it is challenging to decrease the complete oxidation temperature of this compound [5 7]. However, compared with transition metal oxide catalysts, supported Pd catalysts have exhibited better performance in this regard [8,9]. It is known that the Pd particle size and chemical state as well as the support characteristics all play important roles in promoting CH4 catalytic combustion [10 12]. Hicks et al. [13,14] determined that the activity of small PdO particles was almost two orders of magnitude higher than that of large Pd crystallites, and that the respective turnover frequency values of these materials were 0.02 and 1.3 s 1, respectively. Although PdO is regarded as active for CH4 combustion [15,16], there are still contradictory data regarding this catalyst. As an example, Oh and coworkers [17,18] found that both reduced Pd species * Corresponding author. Fax: ; E mail: # Corresponding author. Fax: ; E mail: This work was supported by the National High Technology Research and Development Program of China (2015AA034603), the National Key Research and Development Program of China (2016YFC ), the National Natural Science Foundation of China ( , , ), the "Shu Guang" Project of the Shanghai Municipal Education Commission (12SG29), and the Commission of Science and Technology of Shanghai Municipality (15DZ ). DOI: /S (17)62864 X Chin. J. Catal., Vol. 38, No. 8, August 2017

2 Zhenyang Zhao et al. / Chinese Journal of Catalysis 38 (2017) in the form of Pd δ+ (0 < δ < 2) and high valence Pd 4+ atoms [19] are active during CH4 catalytic combustion. Porous supports with high specific surface areas tend to improve the dispersion of active metal species [20,21], while a support s acidity and redox properties have a more pronounced effect in terms of promoting CH4 combustion. Lou et al. [22] confirmed that the surface Brönsted acid sites on H ZSM 5 were able to anchor Pd species and modulate the morphologies of Pd structures. Cargnello et al. [23] designed a catalyst in which the close contract between Ce and Pd maximized the transformation of metallic Pd to PdOx. SnO2, which exhibited high oxygen transfer capability and thermal stability [24 26], was considered a good candidate for a support material. Sekizawa et al. [27 30] showed that the Pd/SnO2 on SnO2 calcined at 1200 C exhibited excellent catalytic activity during methane oxidation, allowing complete oxidation at 440 C. Bratan et al. [31] also found that the oxygen storage capacity and the release properties of a SnO2/TiO2 support enhanced the mobility of lattice oxygen. Improving the interactions between noble metal nanoparticles and supports can avoid the sintering and decomposition of the noble metal. Zou et al. [32] prepared well crystallized PdO nanoparticles by epitaxial growth over NiAl2O4, thus avoiding particle agglomeration and obtaining a good distribution. Matching of lattice geometry was observed in trials with Pt/MgAl2O4, and this work also demonstrated that strong electronic attractions at the interface between the support and the epitaxial metal oxide stabilize the Pt particles [33,34]. The above results prompted our own group to study Pd/SnO2. In the present work, a Pd/SnO2 catalyst was prepared by the precipitation method and the effects of the support calcination temperature on CH4 combustion were investigated. N2 adsorption desorption, X ray diffraction (XRD), inductively coupled plasma atomic emission spectroscopy (ICP AES), O2 temperature programmed desorption (O2 TPD), CH4 temperature programmed surface reaction (CH4 TPSR) and X ray photoelectron spectroscopy (XPS) were all used to characterize the physicochemical properties of the samples. By studying the structure of these Pd/SnO2 specimens, we hoped to understand the role of lattice matching between the noble metal and the support in promoting CH4 combustion. 2. Experimental 2.1. Sample preparation The SnO2 support was synthesized by a chemical precipitation method. SnCl4 5H2O (99.7%, Sinopharm Chemical Reagent Co., Ltd.) and NaNO3 (99.7%, Aladdin) were dissolved in deionized water to form a mixed solution that was subsequently heated to 150 C and refluxed for 16 h with vigorous stirring. The resulting white precipitate was filtered and washed with deionized water to remove chloride ions. After filtering, the solid powder was dried at 120 C for 12 h and calcined at 600, 800, 1000 or 1200 C for 4 h in air. The obtained SnO2 powders are denoted herein as SnO2(x), where x represents the calcination temperature. Supported Pd catalysts were prepared by impregnating these SnO2(x) powders with a CH2Cl2 (99.7%, Sinopharm Chemical Reagent Co., Ltd.) solution of Pd(CH3COO)2 (Pd 47.32%, Kunming Institute of Precious Metals). After impregnation, the catalysts were dried and calcined in air at 600 C for 4 h. The resulting catalysts are denoted as Pd/SnO2(x), where x represents the calcination temperature applied to the SnO2. The final Pd loadings were determined by ICP AES Evaluation of the catalyst The catalytic combustion of CH4 over these supported Pd catalysts was carried out in a fixed bed reactor at atmospheric pressure, using 200 mg catalyst samples (40 60 mesh) diluted with 1 g silica sand (20 40 mesh). A feed gas containing 1 vol% CH4, 20 vol% O2 and N2 as the balance flowed through the catalytic bed at a rate of 30 ml/min. The temperature of the catalyst bed was measured using a thermocouple inserted at the top of the bed. The bed heating rate was 4 C/min. An online gas chromatograph (GC, Agilent 7890) was used to monitor the composition of the outlet gas. The catalytic activity is expressed herein by the T10 and T100 values for CH4, corresponding to the reaction temperatures required for 10% CH4 and 100% CH4 conversion, respectively Catalyst characterization The specific surface areas of the catalysts were determined from N2 adsorption isotherms at 196 C using a Micromeritics ASAP 2020 analyzer. The powder XRD patterns of the samples were obtained with a Rigaku D/max 2550 VB/PC diffractometer with Cu Kα radiation operating at 40 kv and 40 ma. The intensity data were collected at room temperature over a 2θ range from 10 to 70 at a scan rate of 6 /min. The average crystallite sizes of samples were calculated using the Debye Scherrer formula based on the diffraction peaks. Transmission electron microscopy (TEM) images were obtained with a JOEL 2100 instrument operating at 200 kv. XPS was performed with an AXIS Ultra DLD spectrometer incorporating a monochromated Al Kα X ray source ( ev). The base pressure inside the analysis chamber was kpa and the XPS spectra of selected elements were acquired at a constant analyzer pass energy of 40 ev. All binding energy (BE) values were determined relative to the adventitious C 1s peak (BE = ev). CO chemisorption measurements were performed using a pulse method with a chemisorption analyzer (Micromeritics Autochem 2920). The catalysts were pre reduced under 10% H2 in Ar at 150 C for 1 h prior to testing, and the average CO to Pd molar ratio was assumed to be 1 when calculating the Pd dispersion [35]. O2 TPD was carried out in a quartz flow microreactor using a chemisorption analyzer (Micromeritics Autochem 2920) equipped with an HPR 20 QIC mass spectrometer (MS). In these trials, a 200 mg quantity of the catalyst was pretreated under 3 vol% O2 in He (50 ml/min) at 600 C for 30 min, then cooled to room temperature and allowed to absorb O2 for 1 h.

3 1324 Zhenyang Zhao et al. / Chinese Journal of Catalysis 38 (2017) After subsequent purging with He for 1 h, the sample was heated at a rate of 10 C/min from 30 to 850 C and the desorbed O2 signal (Mr/z = 32) was detected by the MS. CH4 TPSR was performed with the same reaction apparatus as used for O2 TPD. In these trials, a 100 mg quantity of the catalyst was pretreated at 400 C for 40 min in a 50 ml/min flow of 3 vol% O2 in He, after which the catalyst was cooled to room temperature. The TPSR data were acquired by heating the catalyst from 30 to 650 C at a rate of 10 C/min in 50 ml/min flow of 5 vol% CH4 in He. The release of CH4 (Mr/z = 16) and CO2 (Mr/z = 44) was determined with an online MS (HPR 20 QIC Benchtop Gas Analysis System). 3. Results and discussion 3.1. Catalytic performance The catalytic activities of the SnO2 and Pd/SnO2 during CH4 combustion are summarized in Fig. 1. The activity of the SnO2 gradually decreased with increasing calcination temperature from 600 to 1200 C (Fig. 1(a)). The SnO2(600) exhibited the highest catalytic activity, giving T10 and T100 values of 410 and 580 C, respectively. In contrast, the T10 and T100 values obtained using the SnO2(1200) were 490 and 736 C. The deposition of Pd significantly improved the CH4 combustion, as shown in Fig. 1(b), such that the T100 for Pd/SnO2(600) was 140 C lower than that for SnO2(600). Increasing the calcination temperature also lowered the temperature required for complete CH4 combustion. The T100 for Pd/SnO2(1200) was relatively low at 390 C while the value for Pd/SnO2(600) was 440 C. A stability test was also conducted and the results are presented in the insert to Fig. 1(b), showing that there was no obvious decline in activity even after 80 h at 370 C. The specific surface areas of the samples varied with the calcination temperature, and so this effect was accounted for by calculating the relative reaction rate of CH4, giving the results presented in Table 1. With increases in the calcination temperature, the reaction rate over Pd/SnO2 can be seen to have increased. The relative reaction rate of CH4 over Pd/SnO2(1200) CH4 conversion (%) CH4 conversion (%) SnO2(600) SnO2(800) SnO2(1000) SnO2(1200) Pd/SnO2(600) Pd/SnO2(800) Pd/SnO2(1000) Pd/SnO2(1200) was 36 times that over Pd/SnO2(600) at 300 C. These data also demonstrate that there was no obvious difference in the amount of Pd loading between samples, meaning that the observed variations in activity required further study BET surface area and XRD results CH4 conversion (%) The specific surface areas of samples are also provided in Pd/SnO2(1200) (a) (b) Time (h) Fig. 1. CH4 oxidation activity as a function of temperature over (a) SnO2(x) and (b) Pd/SnO2(x). Insert: the catalytic stability of Pd/SnO2(1200) at 370 C. Table 1 Summary of the characterization results for Pd/SnO2 catalysts fabricated using different SnO2 calcination temperatures. Catalyst SBET (m 2 /g) a Crystalline size (nm) b Pure SnO2 in R (10 5 mmol s 1 m 2) c Pd loading (wt%) d Pd dispersion (%) e Pd Pd diameter 4+ /Pd 2+ (%) (nm) g f Surface Pd concentration (at%) g CH4 consumption amount h O2 desorption amount i SnO2 Pd/SnO2 Pd/SnO2(600) Pd/SnO2(800) Pd/SnO2(1000) Pd/SnO2(1200) a Calculated from N2 adsorption desorption. b Crystalline size of samples was calculated using the Debye Scherrer formula. c Reaction rate of CH4 per unit specific surface area at 300 C. d As determined by ICP. e As determined by CO chemisorption at 25 C. f Average diameter calculated assuming a truncated cuboctahedral particle shape [36]. g The chemical state of Pd/SnO2 as obtained from XPS analysis. h The relative CH4 consumption amount per unit Pd atom surface area as obtained from CH4 TPSR. i The relative O2 desorption amount per unit Pd atom surface area as obtained from O2 TPD.

4 Zhenyang Zhao et al. / Chinese Journal of Catalysis 38 (2017) Table 1. The Brunauer Emmett Teller (BET) surface area of the SnO2 decreased as expected with increasing calcination temperature from 600 to 1000 C, and the surface area of the Pd/SnO2 presented the same trend. Thus, the Pd/SnO2(600) had the highest surface area (19.8 m 2 /g). Temperatures above 800 C did not affect the surface area, such that the surface area of the Pd/SnO2(1200) was almost equal to that of the Pd/SnO2(1000). The XRD patterns of the SnO2(x) and Pd/SnO2(x) are shown in Fig. 2. The SnO2 exhibits a classic rutile phase (JCPDS card ), and the SnO2 diffraction peaks intensify with increasing calcination temperature, accompanied by increases in the crystallite size from 12.6 to 72.3 nm (Table 1). The Pd/SnO2 did not generate any Pd diffractions, indicating either that the Pd species were highly dispersed on the SnO2 or that the Pd concentration was too low to be detected by XRD [37,38]. Compared with the XRD pattern of SnO2(x), a slight shift to higher 2θ values was evident in the case of the Pd/SnO2(600) and Pd/SnO2(800) (Fig. 2(b)) as the result of lattice shrinkage. This effect is due to the insertion of smaller Pd ions into the SnO2 lattice. At calcination temperatures above 1000 C, there was only a minimal shift in the diffraction peak positions. Higher calcination temperatures thus also increased the Pd particle size, in agreement with the CO adsorption analysis High resolution transmission electron microscopy HRTEM images of the Pd/SnO2(x) specimens are presented in Fig. 3. These images demonstrate that the average Pd particle size on the Pd/SnO2(600) surface was 4 nm. As the support calcination temperature was raised from 600 to 1200 C, the Pd particle size increased from 4 to 8 nm. Both PdO and SnO2 lattice fringes are clearly seen in the HRTEM image of Pd/SnO2(1000) in Fig. 3(b). The interplanar lattice spacings for PdO and SnO2 are and nm, respectively, corresponding to the PdO(101) and SnO2(101) lattice planes X ray photoelectron spectroscopy XPS was used to characterize the surface compositions and Intensity Intensity SnO 2(1200) SnO 2(1000) SnO 2(800) SnO 2(600) /( o ) /( o ) chemical states of the catalysts. The surface Pd concentrations on the Pd/SnO2(x) samples are summarized in Table 1, while the Pd 3d XPS data are shown in Fig. 4. The presence of Pd species on the Pd/SnO2(600) in two states is evident from the peaks at and ev, corresponding to Pd 2+ and Pd 4+, respectively [39 41], with a Pd 2+ /Pd 4+ atomic ratio of 2.3 (Table 1). With increases in the calcination temperature, this ratio (a) (b) SnO 2(1200) SnO 2(1000) SnO 2(800) SnO 2(600) Fig. 2. XRD patterns of SnO2(x) and Pd/SnO2(x) catalysts. (a1) (a2) (b) PdO Å (a3) (a4) SnO Å Fig. 3. TEM images of (a1) Pd/SnO2(600), (a2) Pd/SnO2(800), (a3) Pd/SnO2(1000) and (a4) Pd/SnO2(1200), and (b) an HRTEM image of Pd/SnO2(1000).

5 1326 Zhenyang Zhao et al. / Chinese Journal of Catalysis 38 (2017) Pd 3d 5/2 Pd 3d 3/2 Pd Pd/SnO 2 (1200) Intensity (a.u.) Pd/SnO 2 (1000) Pd/SnO 2 (800) Pd Pd Pd Pd Signal of O Fig. 5. O2 TPD profiles of the Pd/SnO2(x) catalysts. Pd/SnO 2 (600) Pd Binding energy (ev) decreases in the order Pd/SnO2(1200) > Pd/SnO2(1000) > Pd/SnO2(800) > Pd/SnO2(600). These data are in accordance with the activity results shown in Fig. 1(b). The XRD patterns in Fig. 2 demonstrate lattice shrinkage of the Pd/SnO2(600) and Pd/SnO2(800). The radius of Pd 4+ (61.5 pm) is smaller than that of Sn 4+ (69 pm), and so Pd 4+ readily inserts into the SnO2 lattice to generate a Sn1 xpdxo2 solid solution during the preparation process. This results in high valence Pd 4+ ions in the lattice [42,43]. In contrast, in the case of the catalyst prepared from the support calcined at high temperature (>1000 C), there is no angle shift because Pd 2+ (86 pm) is too large to enter into the lattice. Although the Pd loading amounts were almost equal, different surface Pd concentrations were determined by XPS analysis. Increases in the calcination temperature raised the Pd concentration from 0.76% to 1.56%. Considering the XRD and TEM results, this result can be explained. Varying the calcination temperature generates Pd species in different forms. The catalyst made from the supports calcined at low temperatures (< 800 C) contained agglomerated Pd particles, thus reducing the surface Pd concentration. In contrast, higher temperature calcination resulted in elevated Pd concentrations O2 temperature programmed desorption Pd Fig. 4. Pd 3d XPS spectra of the Pd/SnO2(x) catalysts. O2 activation is a crucial factor in redox reactions, and the bonding strength of oxygen species on the catalyst surface determines the catalytic activity during deep oxidation [44,45]. In this work, the relationship between oxygen activation and the Pd/SnO2 structure was investigated by obtaining O2 TPD data, as shown in Fig. 5. A broad O2 desorption peak ranging from 540 to 680 C was generated by each of the samples. The peak portion at lower temperatures ( C) is assigned to the decomposition of oxygen species on PdOx surfaces [46], while the portion in the range of C is attributed to lattice oxygen species driven from the PdO bulk phase [16,47]. With increases in the calcination temperature, the O2 desorption peak shifts to lower temperatures, which is in agreement with changes observed in the size of the PdO particles. Small PdO particles on the support tend to have stronger interactions, which shifts the O2 desorption peak to higher temperature, and vice versa. The nature of the active sites can be assessed based on the quantity of sites and their intrinsic activity [48]. The O2 consumption amounts per unit Pd surface were obtained based on the areas of the O2 desorption peaks, setting the desorption peak area for Pd/SnO2(1200) to These values are shown in Table 1. The O2 desorption amount of the Pd/SnO2(1200) was found to be three times that of the Pd/SnO2(600). The larger area of the O2 desorption peak generated by the former material implies a greater concentration of included oxygen species compared with the other catalysts CH4 temperature programmed surface reaction To further examine the performance of the PdO species during the CH4 reaction, CH4 TPSR was carried out and the results are shown in Fig. 6. A CH4 consumption peak was generated in the temperature range of 200 to 250 C and the production of CO2 was detected simultaneously. Low temperature CH4 consumption peaks (< 400 C) are typically attributed to the reaction between active oxygen species and CH4, and so reflect the reduction of PdO species [49].

6 Zhenyang Zhao et al. / Chinese Journal of Catalysis 38 (2017) Signal of CH4 Signal of CO2 (a) (b) Fig. 6. CH4 TPSR profiles of Pd/SnO2 catalysts, (a) CH4 peaks; (b) CO2 peaks. According to Carstens et al. [50], the crystalline form of PdO is more easily reduced than the amorphous forms. The HRTEM analysis (Fig. 3(b)) determined that the catalysts calcined at high temperatures (>1000 C) contained highly crystalline PdO (Fig. 3(b)). Thus, it is not difficult to understand why the O2 desorption temperatures in the O2 TPD profiles are in the same order as the reduction temperatures. The activity data presented above show that the sequences of the CH4 reduction temperatures and O2 desorption temperatures both coincide with that of the activity during methane combustion. The activities of unit Pd atoms on the surfaces of the catalysts during CH4 TPSR were characterized by calculating the amounts of CH4 consumed per unit Pd atom surface area, with the results shown in Table 1. It is evident that the CH4 consumption order follows the same trend as the O2 desorption data, although the CH4 consumption of the Pd/SnO2(1200) was 45% higher than that of the Pd/SnO2(600) Discussion The support calcination temperature had a pronounced effect on the progress of the CH4 catalytic combustion. The Pd/SnO2(1200) exhibited the highest activity, and the reaction rate during CH4 combustion over this material was 36 times that over the Pd/SnO2(600) at 300 C. Although there were differences in the Pd surface concentrations and chemical states between these two materials, it is difficult to explain the significant activity gap between them. The XRD and XPS data suggest that the catalysts made from the supports calcined at low temperatures (< 800 C) contained some Pd species adsorbed in the support because of the similar diameters of Pd 4+ and Sn 4+, while some small, amorphous Pd particles were present on the support surface. In contrast, the catalysts fabricated using the supports calcined at high temperatures (> 800 C) showed Pd species only on the catalyst surface, in the form of highly crystalline PdO. The SnO2(101) and PdO(101) lattice fringes were found to exhibit close spacing during HRTEM observations. A specific spinel oxide crystal plane family is known to interact with PdO via epitaxy [51]. In addition, intimate contact (with a small contact angle) between the PdO(110) and NiAl2O4(400) planes in Pd/0.5NiO/Al2O3 has been shown to improve the performance of the catalyst and inhibit the migration and growth of Pd particles over time [32]. This same study determined that intimate contact lowers both the O2 TPD temperature and activation energy. Cai s group [52] found that oxygen vacancies in the CeO2 lattice of Pd Ce/ZSM 5 provide a pathway for oxygen atoms to easily approach or leave from the Pd particles, implying significant oxygen transfer from the support to the metal. Martin and Duprez [53] also demonstrated exceptional mobility of both surface and bulk oxygen over CeO2, and found that the presence of metal particles on the CeO2 markedly increases the oxygen mobility between 300 and 450 C. Based on these literature data and our own experimental results, we suggest that the close spacing of the SnO2(101) and PdO(101) lattice fringes is the main factor explaining the low O2 TPD temperature and the high amount of O2 desorption associated with the Pd/SnO2(1200). The matching lattice geometries of the PdO and SnO2 allows oxygen at the Pd SnO2 interface to be activated, following which the Pd acts as an oxygen pump to drive CH4 combustion, similar to the back spillover of oxygen from CeO2 to oxygen vacancy sites on the PdO/Pd surface [54 56]. Therefore, we can reasonably conclude that the close spacing of the SnO2(101) and PdO(101) lattice fringes also explains the remarkably enhanced CH4 combustion activity of the Pd/SnO2(1200). 4. Conclusions The support calcination temperature plays a key role in the behavior of Pd/SnO2 during CH4 catalytic combustion. A catalyst prepared from SnO2 calcined at 1200 C exhibited excellent activity and stability; the reaction rate of CH4 on the Pd/SnO2(1200) specimen was 35 times higher than that over the Pd/SnO2(600), and the former remained stable over an 80 h test. Lattice matching based on the geometry of PdO and SnO2 facilitates oxygen activation from the SnO2 to vacant oxygen sites on the PdO/Pd surface via the back spillover of oxygen mechanism, which promotes CH4 catalytic combustion.

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