Fabrication of a monoclinic/hexagonal junction in WO3 and its enhanced photocatalytic degradation of rhodamine B

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1 Cinese Journal of Catalysis 37 (2016) 催化学报 2016 年第 37 卷第 3 期 available at journal oepage: Article (Invited Article fro te Awardee of Catalysis Counity in Cina) Fabrication of a onoclinic/exagonal junction in WO3 and its enanced potocatalytic degradation of rodaine B Yuanyuan Lu a, Guo Liu a, Jing Zang a, *, Zaoci Feng b, Can Li b, Zi Li c a College of Ceistry, Ceical Engineering and Environental Engineering, Liaoning Siua University, Fusun , Liaoning, Cina b State Key Laboratory of Catalysis, Dalian Institute of Ceical Pysics, Cinese Acadey of Sciences, Dalian , Liaoning, Cina c Key Laboratory of Potoceical Conversion and Optoelectronic Materials, Tecnical Institute of Pysics and Ceistry, Cinese Acadey of Sciences, Beijing , Cina A R T I C L E I N F O Article istory: Received 25 Noveber 2015 Accepted 27 Noveber 2015 Publised 5 Marc 2016 Keywords: Tungsten oxide Pase junction Teral decoposition etod Potocatalysis Rodaine B A B S T R A C T A series of WO3 saples wit different crystalline pases were prepared by te teral decoposition etod fro aoniu tungstate ydrate. X ray diffraction (XRD), scanning electron icroscopy (SEM), ig resolution transission electron icroscopy (HRTEM), X ray potoelectron spectroscopy, and N2 adsorption desorption were used to caracterize te crystalline pase, orpology, particle size, ceical coposition, and surface area of te WO3 saples. Te foration of exagonal ( WO3) and onoclinic ( WO3) crystal structures of WO3 at different teperatures or different ties was confired by XRD. WO3 is fored at 600 C, wile WO3 starts to transfor into WO3 at 800 C. However, WO3, wic fors at 800 C, ay transfor into WO3 by increasing te calcination teperature to 1000 C. SEM results indicate tat WO3 particles exibit a bulky sape wit eavy aggregates, wile WO3 particles exibit a rod like sape. Moreover, WO3 crystals are sporadically patced on te surface of te WO3 rod like particles, resulting in te exposure of bot WO3 and WO3 on te surface. It is observed tat te onoclinic pase ( WO3)/exagonal pase ( WO3) junction was fabricated by tuning te calcination teperature and calcination tie. Te relative ratios between WO3 and WO3 in te pase junction can readily be tailored by control of te calcination tie. Te potocatalytic activities of WO3 wit different crystalline pases were evaluated by te potocatalytic degradation of rodaine B as a odel pollutant. A iger potocatalytic activity was observed in te WO3 saple wit te WO3/ WO3 junction as copared wit te saple wit only WO3. Te iproveent of potocatalytic activity can be attributed to te reduction of te electron ole recobination rate owing to te foration of te pase junction, wose presence as been confired by HRTEM and potoluinescence spectra. 2016, Dalian Institute of Ceical Pysics, Cinese Acadey of Sciences. Publised by Elsevier B.V. All rigts reserved. 1. Introduction Potocatalysis as been intensively investigated as it as potential for exploitation in environental reediation (pollutant degradation) and clean energy production (H2 production, CO2 reduction) [1 3]. Te etal oxide seiconductors, suc as * Corresponding autor. Tel: ; Fax: ; E ail: Tis work was supported by te National Natural Science Foundation of Cina ( ), te Liaoning Provincial Natural Science Foundation ( ), te Progra for Liaoning Excellent Talents in University (LJQ ), te Scientific Researc Foundation for te Returned Overseas Cinese Scolars, State Education Ministry ([2013]1792), te Opening Project of Key Laboratory of Potoceical Conversion and Optoelectronic Materials, TIPC, CAS, and te Opening Project of State Key Laboratory of Catalysis, DICP, CAS (N 09 06) DOI: /S (15) ttp:// Cin. J. Catal., Vol. 37, No. 3, Marc 2016

2 350 Yuanyuan Lu et al. / Cinese Journal of Catalysis 37 (2016) TiO2, tungsten oxide (WO3), Bi2O3, and ZnO, ave been sown to be efficient as potocatalysts in different processes [4 6]. Aong tese etal oxides, WO3 is of great interest because of its attractive properties suc as sall energy band gap (fro 2.4 to 2.8 ev), stable pysicoceical properties, non toxicity, and resistance to potocorrosion [7]. However, a ig carge recobination rate of poto induced electron ole pairs is a critical drawback in te developent of WO3 as an efficient potocatalyst [8]. Several etods ave been developed to iprove te potocatalytic activity of WO3. Zang et al. [9] syntesized onoclinic WO3 nanoplates by a one step teplate free ydroteral route troug a topoceical conversion process of H2WO4 nanoplates. Te as prepared WO3 nanoplate exibited a superior potocatalytic activity for te degradation of rodaine B (RB) under visible ligt irradiation. Lin et al. [10] odified WO3 wit an ionic liquid [Bi]I troug a facile ipregnation etod. Te presence of a surface bound iidazoliu ring was deonstrated to effectively suppress te recobination of potoexcited electron ole pairs. Additionally, it as been sown tat proper junctions fored in seiconductor based potocatalysts could lead to enanced activity. O et al. [11] prepared WO3/MWCNT TiO2 coposites using a odified sol gel etod. It is found tat te WO3/MWCNT TiO2 potocatalyst sowed efficient carge separation during UV irradiation. Our previous work [12] indicated tat te pase junction fored between te anatase and rutile TiO2 could greatly enance potoexcited carge igration between te two pases tat, in turn, enanced te carge separation. Recently, Jaroniec et al. [13] proposed a new surface eterojunction concept to explain te difference in te potocatalytic activity of anatase TiO2 wit co exposed (001) and (101) facets. Te pase junction enanced carge separation and tus iproved potocatalytic efficiency, and as been deonstrated for a variety of aterials. α Ga2O3/β Ga2O3 [14], α Bi2O3/β Bi2O3 [15], and WO3/WO3 H2O [16] pase junction structures ave been successfully syntesized and exibit ig potocatalytic activity for H2 production and RB degradation. Terefore, te foration of te pase junction becoes an efficient way to produce seiconductor etal oxides exibiting ig potocatalytic activity. WO3 exists ainly in four polyorps, wic are onoclinic, triclinic, ortorobic, and tetragonal, along wit a exagonal pase [17]. Aong tese crystalline pases, te onoclinic pase as been reported as te ost stable pase [18]. Te onoclinic ( WO3) and exagonal ( WO3) pases of WO3 ave attracted te ost attention because te WO3 is an attractive candidate for potocatalytic applications and WO3 exibits an open tunnel structure and ric intercalation ceistry [19]. We are interested in deterining if we can fabricate te pase junction fored between WO3 and WO3 by a siple etod, as well as understanding if te pase junction in WO3 enances its potocatalytic activity. However, te relationsip between te pase junction in WO3 and te potocatalytic activity is not well understood. Generally, a aterial wit different crystalline pases possesses a different band gap and flat band. Terefore, a pase junction could be built between different crystal pases given te two pases are in close contact, wic will lead to efficient electron ole separation and iger catalytic reactivity [20]. Jing Zang (born in 1980) is currently a Professor in College of Ceistry, Ceical Engineering and Environental Engineering, Liaoning Siua University. Supervised by Prof. Can Li, Jing Zang obtained er PD degree in pysical ceistry fro Dalian Institute of Ceical Pysics, Cinese Acadey of Sciences in During te PD, se as been investigating te effect of surface crystalline pase of TiO2 on its potocatalytic activity and firstly presented tat te pase junction in TiO2 wic is beneficial for iproving te efficiency of te carge separation of potoexcited electrons and oles in potocatalysis. Rational design and fabrication of pase junctions is terefore deonstrated to be an attractive strategy for te developent of efficient potocatalysts. Te corresponding results were publised in J. Pys. Ce. B wit 410 citations and Angew. Ce. Int. Ed. wit 525 citations, and also igligted by Ceical & Engineering News (C&E NEWS). Wit te accoplisents of above researc work, se was awarded as te Second Prize of National Natural Science Award (ranking te 3rd). In 2007, se joined Liaoning Siua University, were er researc interest includes UV Raan spectroscopy, control and tunes te surface crystalline pase of etal oxides, fabrication of oojunction and eterojunction aterials in potocatalysis. Se extended postdoctoral researc on bioass conversion (developing te effective catalyst for te conversion of fructose in water pase and delineating te critical olecular level reactions involved in te catalytic breakdown of glucose, fructose to produce feedstock ceicals) at Nortwestern University. Jing Zang was prooted as full professor in 2014 and was selected as distinguised professor of Liaoning Province in After tat, se is launcing project of constructing Key Laboratory of Advanced Clean Energy Materials Ceistry enrolling 8 10 young teacing stuff upon te university policy support. Se as publised ore tan 30 peer reviewed journal articles in Angew. Ce. Int. Ed., Appl. Catal. B, ACS Catal., J. Pys. Ce. C., etc., wit over 1500 citations and one book capter, and delivered over 20 presentations in scientific eetings and congresses. In recognition of er acieveents in pase junction in potocatalysis and bioass conversion researc, se was granted as a Young Scientists of te 15t International Congress on Catalysis and te Catalysis Rising Star Award in 2012 presented by Te Catalysis Society of Cina.

3 Yuanyuan Lu et al. / Cinese Journal of Catalysis 37 (2016) According to Ref. [21], te valence band position and conduction band position of WO3 are lower tan tose of WO3, wic iplies tat a pase junction could be establised between WO3 and WO3. Terefore, tis study attepts to fabricate a pase junction in a WO3 potocatalyst, and ten to investigate te effect of te pase junction in te WO3 potocatalyst on its potocatalytic activity. Te teral decoposition etod was used to fabricate a pase junction in WO3 by tuning te calcination teperature and te calcination tie, and te pase junction ( WO3/ WO3) fored between exagonal and onoclinic WO3 deonstrated an enanced potocatalytic activity for RB degradation. 2. Experiental 2.1. Saple preparation Aoniu tungstate ydrate (H40N10O41W12 xh2o, APT) was of analytical grade and used witout furter purification. For te teral decoposition etod, te wite APT powder was calcined at C for 4 in a static atospere of air, and ten was naturally cooled to roo teperature. Te obtained saples were labeled as WO3 T, were T represents te calcination teperature ( C) used to obtain te saples. APT powders were also calcined at 800 C for different ties fro 8 to 30 and were denoted as WO3 t, were t represents calcination tie () Saple caracterization Terogravietry and differential teral analysis (TG DTA) was perfored using a TG/DTA 6300 teral analyzer at te rate of 10 C/in under air atospere (60 L/in). Te structure caracterization was carried out by powder X ray diffraction (XRD) using a Rigaku MiniFlex diffractoeter wit a Cu K radiation source. Te orpologies of te saples were investigated using scanning electron icroscopy (SEM, Quanta 200 F) and ig resolution transission electron icroscopy (HETRM, JEOL, JEM 2100). X ray potoelectron spectra (XPS) were obtained using a Tero ESCALAB 250Xi X ray potoelectron spectroeter. Te BET surface area was deterined by N2 adsorption desorption isoters using a NOVA 4200e surface area and pore size analyzer fro Quantacroe. A Hitaci F 4500 spectropotofluoroeter was used to record te potoluinescence spectra (PL) using an excitation wavelengt of 350 n Potocatalytic reaction A set of potocatalytic degradation experients were perfored wit te following procedure. Potodegradation of RB was carried out in a 100 L Pyrex reactor filled wit de ionized water (60 L) containing RB (10 g/l) and te WO3 saple. Te suspension was stirred for 30 in in te dark to obtain adsorption desorption equilibriu of te dye before illuination. After irradiation wit a 125 W Hg lap (λ = 365 n, Sangai Feilipu Yaing Ligting Co.), a 3 L aliquot was taken every 30 in and iediately centrifuged. Te RB concentration in te clear solution was analyzed by optical caracteristic absorption (22PC spectropotoeter, Sangai Lengguang Tecnology Co., Ltd.) at a wavelengt of 553 n for a RB solution. Te blank experients witout a ercury lap and witout catalysts in te RB solution under te sae conditions are also copared. Te blank study sows tat ere potolysis can be ignored for RB. 3. Results and discussion Fig. 1 sows TG DTA curves of APT in a dynaic atospere of air. Te TG curve sows five ain ass loss steps wit a total of 11.8% loss of te original ass of APT. Four ass loss steps totaling 10.6% (2.2% + 2.1% + 1.2% + 5.1% = 10.6%) and four ain endoteric peaks at 84, 130, 208, and 275 C could be observed in te DTA curve, wic are attributed to te loss of absorbed water, crystal water, structural water, and loss of aonia. In addition, two exoteric peaks are observed at 355 and 440 C. Te peak at 440 C can be attributed to crystallization of te aorpous pase of WO3 [22]. In tis study, calcination teperatures iger tan 600 C were cosen to prepare WO3, wic facilitated a ig degree of crystallinity. Fig. 2 sows te XRD patterns of APT calcined at different teperatures. Wen te WO3 saple was calcined at 600 C, diffraction peaks at 2θ = 23.1, 23.6, 24.3, and 34.1 were observed, wic represent te indices of te (002), (020), (200), and (202) planes of WO3 (PDF # ), respectively. Tese results indicate tat te WO3 600 C saple is in te onoclinic pase. Moreover, te XRD peaks are strong and sarp, indicating tat te WO3 600 C saple exibits ig crystallinity. Te XRD pattern of te WO3 700 C saple is alost te sae as tat for te WO3 600 C saple. On eating to 800 C, tree weak peaks appear at 2θ = 14.0, 28.2, and 36.6, wic arise fro WO3 (PDF # ), in addition to te typical peaks of te onoclinic pase. Tis iplies te co existence of exagonal and onoclinic pases in te WO3 800 C saple, wile WO3 is te ain constituent in te crystalline pase. Mass (%) % % % 440 Exo % % Teperature ( o C) Fig. 1. TG DTA curves of APT in a dynaic atospere of air DTA ( V)

4 352 Yuanyuan Lu et al. / Cinese Journal of Catalysis 37 (2016) Intensity (a.u.) (a) : Monoclinic : Hexagonal WO o C WO o C WO o C WO o C WO o C Intensity (a.u.) (b) WO C WO C WO C WO C WO C /( o ) Fig. 2. XRD patterns of APT calcined at different teperatures /( o ) Martínez de la Cruz et al. [23] prepared WO3 particles by te precipitation etod using APT as te starting aterial and PEG as te teplate and steric stabilizer. It was also found tat a long calcination tie prooted te foration of te exagonal structure of WO3 in addition to WO3. Te XRD peaks of WO3 ardly canged for te WO3 saple calcined at teperatures up to 900 C. However, te intensities of te typical peaks of WO3 were decreased for te WO C saple (Fig. 2(b)). (a) (c) (b) (d) -WO 3 Te orpologies and particle sizes of te WO3 T saples were investigated by SEM (Fig. 3). As sown in Fig. 3(a) and (b), te WO3 600 C saple consists of dispersed large and fine particles wit irregular polyedral sapes. Bulky coponents wit diensions up to 10 were observed, and te sizes of te fine particles were approxiately n for te WO3 600 C saple. It is obvious tat te rod like coponents (circled by a dased line in Fig. 3), assigned to te exagonal pase, appear in te WO3 800 C saple (Fig. 3(c) and (d)). Tis sows te co existence of te onoclinic and exagonal pases in te WO3 800 C saple, wic is in agreeent wit te results fro XRD (Fig. 2). Moreover, it can be seen tat WO3 and WO3 particles are in close contact, and WO3 particles are located on te surface of WO3 particles wit a rod like sape. Crucial inforation on te spatial distribution of te WO3 and WO3 particles was furter provided by HRTEM (Fig. 4). Te HRTEM iage of WO3 800 C sows an exaple of te intiate contact between WO3 and WO3 pases. As sown in Fig. 4, te sall particles and rod like particles exibit fringes wit a lattice spacing of and Å, respectively, wic can be indexed into te (020) atoic plane of WO3 and (100) atoic plane of WO3, respectively. HRTEM and SEM results (Fig. 3) reveal tat te pase junction can be built between te WO3 particles and WO3 nanorods. Fro Fig. 3, no apparent canges in te orpology of te WO3 particles were observed in te WO C saple, as (e) (f) a 6.361Å [100] -WO 3 -WO 3 b a b -WO Å [020] Fig. 3. SEM iages of WO3 600 C (a, b), WO3 800 C (c, d), and WO C (e, f). Fig. 4. HRTEM iage of WO3 800 C.

5 Yuanyuan Lu et al. / Cinese Journal of Catalysis 37 (2016) copared wit te WO3 800 C saple. However, te saples obtained after calcination at 1000 C sowed a inor tendency to for large aggloerates, as sown in Fig. 3(e). Moreover, it sould be noted tat it is not easy to observe rod like particles in te WO C saple, and te nuber of rod like particles decreased for WO C as copared wit te WO3 800 C saple, fro te SEM iage. Tis result is in agreeent wit tat fro XRD (Fig. 2). It is reported tat triangular and exagonal cannels are fored along te structure in WO3 bronzes owing to te special arrangeent of corner saring WO6 octaedra [24]. Alkaline (Na +, K +, Cs + and so fort) or NH4 + ions are tougt to be located in exagonal cannels [25]. Szilágyi et al. [24] studied te foration of WO3 during te annealing of exagonal aoniu tungsten bronze (HATB), wic is obtained by eating APT ((NH4)10[H2W12O42] 4H2O) in H2. Tey proposed tat, in general, soe ions or olecules were needed in te exagonal cannels to aintain a exagonal tungsten oxide structure. Moreover, residual NH4 + and NH3 (fro APT) in te exagonal cannels seeed to be vital for stabilizing WO3: wen NH4 + and NH3 were copletely released, te exagonal fraework collapsed in an exoteric reaction into WO3. Tus, cobined wit te results fro previous studies, WO3, wic fors at 800 C, ay transfor into WO3 by increasing te calcination teperature to 1000 C because of te release of NH4 + ions and NH3 olecules (fro APT starting aterial) in te exagonal cannels at ig teperature. Tus, te aount of rod like WO3 decreased for WO C fro Fig. 2. Furter work is in progress to study te ecanis of te pase transforation between WO3 and WO3 in our lab. To furter cange te pase coposition in te WO3 saple, te APT powder was calcined at 800 C for different ties. Fig. 5 displays te XRD patterns of te WO3 t saples. It can be seen tat te ixed pases of WO3 and WO3 were obtained for all te WO3 t saples. WO3 8 saple is ainly coposed of WO3 wit a sall aount of WO3. More intense peaks of WO3 appeared wen te annealing tie was increased fro 8 to 12 (Fig. 5(b)), suggesting an increase of WO3 content in te ixed pases. However, te diffraction peaks of WO3 gradually decreased in intensity after calcination for 12. Wit a furter increase of te calcination tie up to 24 30, WO3 saples were again ainly coposed of WO3 wit a sall aount of WO3. Te XPS tecnique was used to deterine te ceical states of WO3 saples. Te overview XPS spectru of te WO3 12 saple in Fig. 6(a) sows te corresponding peaks of O 1s, C 1s, and W 4f, confiring te existence of W and O eleents in te WO3 12 saple. Te fine spectru in Fig. 6(b) (a) WO 3-30 (b) WO 3-30 Intensity (a.u.) WO 3-24 WO 3-16 WO 3-12 Intensity (a.u.) WO 3-24 WO 3-16 WO 3-12 WO 3-8 WO /( o ) 2 /( o ) Fig. 5. XRD patterns of APT calcined at 800 C for different ties. (a) O 1s (b) W 4f 7/2 (c) O 1s Intensity (a.u.) W 4s W 4p W 4d C 1s W 4f W 4f 5/ Binding energy (ev) Binding energy (ev) Fig. 6. XPS spectra of te WO3 12 saple. (a) Survey spectru; (b) W 4f; (c) O 1s Binding energy (ev)

6 354 Yuanyuan Lu et al. / Cinese Journal of Catalysis 37 (2016) (a) (c) (e) (b) (d) (f) displays two peaks at 35.4 and 37.5 ev, wic suggests tat te W exists in te W 6+ for [26]. Tese two peaks are attributed to te spin orbit splitting of te W 4f coponents (W 4f7/2 and W 4f5/2). For O 1s XPS (Fig. 6(c)), a peak at ev was found, wic can be assigned to lattice oxygen O 2 of WO3 [27]. According to XPS studies, te W/O atoic ratio was estiated to be 1:3, wic is consistent wit tungsten(vi) trioxide. Terefore, te XPS results agree well wit te results fro te XRD pattern of te WO3 12 saple. Te orpologies of te WO3 t saples were deterined by te SEM analysis and are sown in Fig. 7. Te WO3 particles exibit a bulky sape wit eavy aggregates, wile WO3 particles exibit a rod like sape. Terefore, substances containing WO3 and WO3 can be identified siply by te particle orpology. Te WO3 8 saple (Fig. 7(a)) is coposed of WO3 particles and soe WO3 particles. As copared wit te WO3 8 saple, te nuber of rod like particles obviously increases for te WO3 12 saple, wic is in accordance wit te XRD results (Fig. 5). It is sown tat WO3 particles can be easily observed in te WO3 16 saple altoug te nuber of WO3 particles decreases wit an increase of te calcination tie to 16. Wit a furter increase in te calcination tie to 30, te WO3 products are coposed of a large nuber of WO3 particles coupled wit a sall nuber of WO3 particles, as sown in Fig. 7(g). Te results fro XRD, SEM, and HRTEM deonstrate tat well defined WO3/ WO3 pase junctions of WO3 can be fabricated by te pase transforation between WO3 and WO3. It is observed tat te ratio of WO3 and WO3 in te WO3 products is ainly controlled by te calcination tie. Moreover, fro SEM and HRTEM iages, it can be seen tat WO3 crystals are sporadically patced on te surface of te WO3 rod like particles, resulting in te exposure of bot WO3 and WO3 on te surface. RB was used as a representative organic substance to investigate and copare te potocatalytic activity of te WO3 saples (Fig. 8). Te degradation of RB could be described by te first order kinetics of ln(ct/c0) versus reaction tie (t): ln(ct/c0) = kapt, were kap is te apparent reaction rate constant, and C0 and Ct are te initial concentration and te concentration at reaction tie t of RB, respectively. After 180 in of irradiation, 41% and 30% of RB were degraded by te WO3 600 C and WO3 700 C catalysts, respectively. Te lower degradation ability ay be ascribed to te decrease of te surface area fro to /g wit increasing calcination teperature fro 600 to 700 C. Fro Table 1, WO3 600 C, WO3 700 C, WO3 800 C, WO3 900 C, and WO C saples exibit a potocatalytic perforance wit kap deterined as , , , , and in 1. It is observed tat te potocatalytic activity increases wit increasing calcination teperature to 800 C. Te WO3 900 C saple exibits te igest potocatalytic activity altoug te surface area of te WO3 900 C saple ( /g) is lower tan tose of WO3 600 C and WO3 700 C. Terefore, we concluded tat te enanceent in te potocatalytic activity of te WO3 800 C and WO3 900 C saples arose fro te pase junction between WO3 and WO3, te presence of wic is confired by SEM and HRTEM results dark UV ligt (g) () C/C WO o C WO o C WO o C WO o C WO o C Fig. 7. SEM iages of WO3 8 (a, b), WO3 12 (c, d), WO3 16 (e, f), and WO3 30 (g, ) Tie (in) Fig. 8. Potocatalytic activity of te degradation of RB on te WO3 calcined at different teperatures.

7 Yuanyuan Lu et al. / Cinese Journal of Catalysis 37 (2016) Table 1 First order rate constants (kap) and relative coefficients (R 2 ) for te degradation of RB under UV ligt irradiation for different calcination teperatures and different calcination ties. Catalyst kap (in 1 ) R 2 WO3 600 C WO3 700 C WO3 800 C WO3 900 C WO C WO WO WO WO WO Te foration of te pase junction ay iprove te carge separation efficiency of potoexcited electrons and oles in te WO3 800 C and WO3 900 C saples. Tus, WO3 800 C and WO3 900 C saples sow a iger potocatalytic activity tan WO3 600 C and WO3 700 C containing te onoclinic pase. By furter increasing te calcination teperature to 1000 C, te potocatalytic activity of WO C (surface area is /g) decreased. However, te WO C saple sows a coparable potocatalytic activity to WO3 600 C altoug te potocatalytic activity of WO C decreases copared wit tat of WO3 800 C and WO3 900 C. Fro te above discussion, te decrease of te potocatalytic activity for WO C arises fro te decrease in te aount of WO3 wen te calcination teperature is raised to 1000 C, wic decreases te aount of te exposed WO3/ WO3 pase junction. To furter confir te pase junction effect of WO3, te potocatalytic activities of WO3 t saples tat were calcined at 800 C for different ties were investigated (Fig. 9) because te WO3 and WO3 pase coposition can be carefully controlled by calcination at 800 C for different ties. Wen te APT powder was calcined at 800 C for 8 30, all saples are in te ixed pases of WO3 and WO3 fro XRD results (Fig. 5), and all te above saples sow iger potocatalytic C/C WO WO 3-12 WO 3-16 WO WO 3-30 WO o C Irradiation tie (in) Fig. 9. Potocatalytic activity of degradation of RB by te WO3 t potocatalysts and WO3 600 C. activities copared wit WO3 600 C containing WO3 (Fig. 9). Moreover, te potocatalytic activities were iproved by gradually increasing te calcination tie range fro 8 to 12. Te increase in te potocatalytic activity ay ainly arise fro te extent of te pase junction wen te calcination tie is increased fro 8 to 12 because te XRD results indicate tat te aount of WO3 increases gradually wit increasing calcination tie. Fro Table 1, te WO3 12 saple exibits te igest potocatalytic activity wit kap of in 1. Wit furter increases of te calcination tie to 24 and 30, te potocatalytic activity decreases. A ecanis for electron ole separation and transport of an WO3/ WO3 pase junction is proposed and is sown in Fig. 10. Te valence and conduction band potentials of WO3 were found to be 3.18 and 0.41 ev [21], wereas tese values for WO3 were 3.37 and 0.80 ev, respectively [28]. Te conduction band (CB) of WO3 is lower tan tat of WO3, tus te poto induced electrons on te conduction band of WO3 transfer easily to WO3 troug te well developed interface, and te potogenerated oles ove in te opposite direction fro te electrons. Terefore, te pase junction of WO3/ WO3 could act as an active center for indering te rapid recobination of poto induced electron ole pairs. Te electrons accuulated on te CB of WO3 can be scavenged by O2 to produce a superoxide radical ( O2 ) and ydrogen peroxide (H2O2), wic can interact to produce a powerful oxidant (ydroxyl radical, OH) to decopose RB. Te oles accuulated in te VB of WO3 take part in te oxidation process to ake OH or H2O species to produce reactive ydroxyl radicals [29 31]. To furter investigate te effect of te pase junction, PL analysis was applied to reveal te diffusion and recobination process of potogenerated electron ole pairs. Fig. 11 sows te PL spectra of WO3 600 C, WO3 800 C, and WO3 12 saples. A ain peak at approxiately 469 n and several peaks in te range of n were observed in te PL spectru of WO3 600 C, wic is in agreeent wit te results fro Ref. [32]. In te case of WO3 800 C and WO3 12 wit an WO3/ WO3 junction, te sape of te curves is siilar to tat of WO3 600 C, wereas te peak intensities significantly decrease. Potential (V) NHE CB = 0.41 ev VB = 3.18 ev OH E g = 2.77 ev H 2 O(OH ) -WO 3 e - e - e - e - e - e - e - e - CB = 0.80 ev VB = 3.37 ev O 2 -WO 3 E g = 2.57 ev O 2 Fig. 10. A proposed ecanis for te carge transfer and separation in te WO3/ WO3 pase junction.

8 356 Yuanyuan Lu et al. / Cinese Journal of Catalysis 37 (2016) PL intensity (a.u.) WO o C WO o C properties of WO3, togeter wit teir relationsips wit te potocatalytic degradation of RB, reveal tat a pase junction between WO3 and WO3 of WO3 was fabricated by a teral decoposition strategy to inibit te recobination of carriers. Te prootion of te potocatalytic perforance is ainly ascribed to te enanced carge separation originating fro te pase junction between WO3 and WO3. Tis work provides a siple etod to design and fabricate te effective WO3 based potocatalyst. References WO Wavelengt (n) Fig. 11. PL eission of different potocatalysts under UV radiation. Generally, a iger PL intensity indicates a iger recobination rate of potoexcited electron ole, and a lower PL intensity expresses a lower recobination rate of potoexcited electrons and oles [33,34]. Tis indicates tat te interaction between WO3 and WO3 in te WO3 800 C and WO3 12 saples is favorable for interfacial carge transfer, and tus reduces te recobination rate of electron ole pairs under ligt irradiation. Moreover, it can be seen tat te PL intensity of te peak at 469 n of WO3 12 is weaker tan tat of te WO3 800 C saple. Tis result indicates tat WO3 12 exibits a lower electron ole recobination rate tan tat of WO3 800 C. Tus, WO3 12 exibits iger potocatalytic activity tan WO3 800 C. 4. Conclusions WO3 potocatalysts wit different crystalline pases were prepared by teral decoposition of APT at C for 4 and 800 C for Caracterization of crystal structure, orpology, ceical coposition, surface area, and optical [1] C. G. Feng, H. R. Sang, X. Liu, Cin. J. Catal., 2014, 35, [2] P. Zou, J. G. Yu, M. Jaroniec, Adv. Mater., 2014, 26, [3] H. H. Cen, Y. M. Xu, RSC Adv., 2015, 5, [4] L. Q. Jing, Z. Wei, G. H. Tian, H. G. Fu, Ce. Soc. Rev., 2013, 42, [5] R. Asai, T. Morikawa, T. Owaki, K. Aoki, Y. Taga, Science, 2001, 293, [6] R. G. Li, Y. X. Weng, X. Zou, X. L. Wang, Y. Mi, R. F. Cong, H. X. Han, C. Li, Energy Environ. Sci., 2015, 8, [7] L. Li, M. Krissanasaeranee, S. W. Pattinson, M. Stefik, U. Wiesner, U. Steiner, D. Eder, Ce. Coun., 2010, 46, [8] K. Jotivenkatacala, S. Prabu, A. Nitya, K. Jeganatan, RSC Adv., 2014, 4, [9] H. L. Zang, J. Q. Yang, D. Li, W. Guo, Q. Qin, L. J. Zu, W. J. Zeng, Appl. Surf. Sci., 2014, 305, [10] J. J. Liu, S. Q. Han, J. Li, J. Lin, RSC Adv., 2014, 4, [11] L. Zu, Z. D. Meng, W. C. O, Cin. J. Catal., 2011, 32, [12] J. Zang, Q. Xu, Z. C. Feng, M. J. Li, C. Li, Angew. Ce. Int. Ed., 2008, 47, [13] J. G. Yu, J. X. Low, W. Xiao, P. Zou, M. Jaroniec, J. A. Ce. Soc., 2014, 136, [14] X. Wang, Q. Xu, M. R. Li, S. Sen, X. L. Wang, Y. C. Wang, Z. C. Feng, J. Y. Si, H. X. Han, C. Li, Angew. Ce. Int. Ed., 2012, 51, [15] Y. F. Qiu, M. L. Yang, H. B. Fan, Y. Z. Zuo, Y. Y. Sao, Y. J. Xu, X. X. Yang, S. H. Yang, Mater. Lett., 2011, 65, [16] Y. Liu, Q. Li, S. A. Gao, J. K. Sang, CrystEngCo, 2014, 16, Grapical Abstract Cin. J. Catal., 2016, 37: doi: /S (15) Fabrication of a onoclinic/exagonal junction in WO3 and its enanced potocatalytic degradation of rodaine B -WO3 O O 2 2 Yuanyuan Lu, Guo Liu, Jing Zang *, Zaoci Feng, Can Li, Zi Li Liaoning Siua University; Dalian Institute of Ceical Pysics, Cinese Acadey of Sciences; Tecnical Institute of Pysics and Ceistry, Cinese Acadey of Sciences Degradation product OH CB VB E g = 2.77 ev e - e - e - e - e - e - e - e - CB VB H -WO3 2 O(OH ) E g = 2.57 ev A onoclinic pase ( WO3)/exagonal pase ( WO3) coposite as been fabricated by tuning te calcination teperature and tie in te teral decoposition etod. Te WO3/ WO3 pase junction deonstrates enanced potocatalytic activity for RB degradation. RB -WO3 -WO3

9 Yuanyuan Lu et al. / Cinese Journal of Catalysis 37 (2016) [17] X. Liu, F. Y. Wang, Q. Wang, Pys. Ce. Ce. Pys., 2012, 14, [18] H. D. Zeng, J. Z. Ou, M. S. Strano, R. B. Kaner, A. Mitcell, K. Kalantar zade, Adv. Funct. Mater., 2011, 21, [19] D. B. Hernandez Uresti, D. Sáncez Martínez, A. Martínez de la Cruz, S. Sepúlveda Guzán, L. M. Torres Martínez, Cera. Int., 2014, 40, [20] Y. Y. Sun, W. Z. Wang, L. Zang, Z. J. Zang, Ce. Eng. J., 2012, , [21] I. Asla, C. B. Cao, M. Tanveer, W. S. Kan, M. Tair, M. Abid, F. Idrees, F. K. Butt, Z. Alia, N. Maood, New J. Ce., 2014, 38, [22] M. S. Marasi, J. Vadati Kaki, S. M. Zebarjad, Int. J. Refract. Met. Hard Mater., 2012, 30, [23] E. Luévano Hipólito, A. Martínez de la Cruz, Q. L. Yu, H. J. H. Brouwers, Cera. Int., 2014, 40, [24] I. M. Szilágyi, J. Madarász, G. Pokol, P. Király, G. Tárkányi, S. Saukko, J. Mizsei, A. L. Tót, A. Szabó, K. Varga Josepovits, Ce. Mater., 2008, 20, [25] E. Lassner, W. D. Scubert, Tungsten: Properties, Ceistry, Tecnology of te Eleent, Alloys, and Ceical Copounds, Springer, New York, [26] G. Lu, X. Y. Li, Z. P. Qu, Q. D. Zao, H. Li, Y. Sen, G. H. Cen, Ce. Eng. J., 2010, 159, [27] A. H. Yan, C. S. Xie, F. Huang, S. P. Zang, S. L. Zang, J. Alloys Copd., 2014, 610, [28] S. F. Cen, L. Ji, W. M. Tang, X. L. Fu, Dalton Trans., 2013, 42, [29] S. Q. Wei, Y. Y. Cen, Y. Y. Ma, Z. C. Sao, J. Mol. Catal. A, 2010, 331, [30] R. L. Liu, H. Y. Ye, X. P. Xiong, H. Q. Liu, Mater. Ce. Pys., 2010, 121, [31] S. L. Bai, H. Y. Liu, J. H. Sun, Y. Tian, S. Cen, J. L. Song, R. X. Luo, D. Q. Li, A. F. Cen, C. C. Liu, Appl. Surf. Sci., 2015, 338, [32] Q. H. Huang, L. S. Wang, M. Wang, J. M. Nan, J. Alloys Copd., 2011, 509, [33] J. Cao, B. D. Luo, H. L. Lin, B. Y. Xu, S. F. Cen, Appl. Catal. B, 2012, , [34] W. J. Li, D. Z. Li, Y. M. Lin, P. X. Wang, W. Cen, X. Z. Fu, Y. Sao, J. Pys. Ce. C, 2012, 116, WO 3 中单斜相 / 六方相异相结的构建及提高光催化降解罗丹明 B 活性 卢圆圆 a, 刘果 a, 张静 a,*, 冯兆池 b, 李灿 b c, 李智 a 辽宁石油化工大学化学化工与环境学部化学与材料科学学院, 辽宁抚顺 b 中国科学院大连化学物理研究所催化基础国家重点实验室, 辽宁大连 c 中国科学院北京理化技术研究所光化学转换与光电材料重点实验室, 北京 摘要 : 光催化技术被认为有可能成为解决环境污染和能源危机的有效手段之一, 引起了各国政府和科学家的极大兴趣. 以 TiO 2, WO 3 和 Bi 2 O 3 等半导体为催化剂的光催化反应受到广泛关注. WO 3 是一种典型的 n 型半导体材料, 具有电致变色 气敏和光催化等性能, 在电致变色器件 气敏传感器和光催化剂等方面有着广泛应用前景. 由于 WO 3 具有高的太阳能利用率 良好的可见光响应性和较强的抗光腐蚀性, 是一种极具开发潜力的半导体光催化材料, 所以在光解水制氢及催化降解有机污染物等领域中得到广泛应用. 然而, WO 3 半导体表面上较高的光生电子 - 空穴复合效率是影响其光催化性能的主要因素之一, 从而限制了 WO 3 在光催化领域的工业应用. 研究发现, TiO 2 材料在从锐钛矿向金红石转变的过程中, 通过精细调变焙烧温度, 可以在两种晶相的界面形成 TiO 2 异相结. 形成的锐钛矿 - 金红石异相结能有效促进电子 - 空穴分离. 目前, 构建异相结已成为改善光催化剂电子 - 空穴分离效率的有效方法之一. 近年来, 人们先后成功构建了 -Ga 2 O 3 / -Ga 2 O 3, -Bi 2 O 3 / -Bi 2 O 3 和 WO 3 /WO 3 H 2 O 等异相结, 这些异相结催化剂在光催化降解水产氢和降解污染物反应中显示了比单一晶相更高的光催化活性. WO 3 是一种多晶相材料, 具有正交 六方 单斜和四方等多种晶体结构, 其中六方晶相 (-WO 3 ) 由于具有开放结构而在气体传感器和电池电极等领域显示了突出性能, 而单斜晶相 (-WO 3 ) 具有合适的带宽和良好的可见光响应性, 因而广泛应用在光催化领域. 而且, -WO 3 的导带和价带均低于 -WO 3 的导带和价带, 所以在 WO 3 材料中有可能通过构建单斜 / 六方异相结 (-WO 3 /-WO 3 ) 来提高 WO 3 的光催化性能. 本文借鉴半导体异相结概念, 采用固相热分解法, 试图通过调节焙烧温度和焙烧时间以构建 -WO 3 /-WO 3 异相结催化剂. 利用 X 射线衍射 (XRD) 高分辨透射电镜(HRTEM) 扫描电镜(SEM) X 射线光电子能谱仪 (XPS) 和 N 2 吸附 - 脱附等方法对 WO 3 样品的晶相结构 形貌和元素组成等进行了表征. 以光催化降解罗丹明 B(RB) 为模型, 研究了不同晶相 WO 3 材料的光催化性能, 考察了 WO 3 晶相和异相结对其光催化性能的影响, 从而为 WO 3 材料中异相结的构建提供思路 方法和理论指导. 结果表明, 采用偏钨酸铵固相热分解制备 WO 3 的过程中, 焙烧温度为 C 时, 样品为单斜晶相, 随着焙烧温度升高至 800 C 时, 样品中开始出现六方晶相. 随着焙烧温度升高, -WO 3 的含量没有明显变化, 当温度升至 1000 C 时, -WO 3 的含量有所减少. SEM 和 HRTEM 结果验证了 -WO 3 /-WO 3 异相结的形成, 小的 -WO 3 粒子分布在棒状 -WO 3 上, 并且两者紧密接触. 为了进一步证实 WO 3 的异相结效应, 将偏钨酸铵在 800 C 焙烧不同时间 (8 30 ). 结果表明, 通过改变焙烧时间可有效控制 -WO 3 和 -WO 3 混合晶相比例, 800 C 焙烧 8 时 -WO 3 为主要晶相, 焙烧 12 时 -WO 3 含量明显增加, 当焙烧时间延长至 24 和 30 时 -WO 3 含量减少. SEM 结果同样显示, 在 800 C 焙烧 12 样品中棒状 -WO 3 显著增多, 与小的 -WO 3

10 358 Yuanyuan Lu et al. / Cinese Journal of Catalysis 37 (2016) 粒子接触几率增大, 即 -WO 3 /-WO 3 异相结数量增加. 不同晶相 WO 3 样品光催化降解 RB 的结果表明, 具有 -WO 3 /-WO 3 异相结结构的 WO 3 催化剂具有较高光催化活性. 荧光光谱结果表明, 单斜相 / 六方相异相结的形成提高了电子 - 空穴分离效率, 从而提高了其光催化降解 RB 的活性. 而在具有 -WO 3 /-WO 3 异相结结构的 WO 3 催化剂中, 随着焙烧温度升高或焙烧时间延长, -WO 3 含量有所减少, 从而导致暴露的 -WO 3 /-WO 3 异相结数量减少, 因而使得活性有所降低. 本文采用固相热分解法通过调变焙烧温度构建了 -WO 3 /-WO 3 异相结光催化剂, 显著提高了光催化降解 RB 的活性, 这对设计合成高效 WO 3 基光催化剂具有一定借鉴. 关键词 : 氧化钨 ; 异相结 ; 热分解法 ; 光催化 ; 罗丹明 B 收稿日期 : 接受日期 : 出版日期 : * 通讯联系人. 电话 : ; 传真 : (024) ; 电子信箱 : 基金来源 : 国家自然科学基金 ( ); 辽宁省自然科学基金 ( ); 辽宁省高等学校优秀人才支持计划 (LJQ ); 教育部留学回国人员科研启动基金 ( 教外司留 [2013]1792 号 ); 中国科学院北京理化技术研究所光化学转换与光电材料重点实验室和中国科学院大连化学物理研究所催化基础国家重点实验室开放课题 (CAS, N-09-06). 本文的英文电子版由 Elsevier 出版社在 ScienceDirect 上出版 (ttp://

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