机械力固相法制备纳米α-FeOOH及其光催化性能研究
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摘要
采用机械力固相法以FeCl_3和Fe(NO_3)_3分别作为铁源。在铁源与碱1∶5摩尔比的条件下,先球磨3 h,再经过60℃水浴陈化得到纳米针铁矿(α-Fe OOH)。用X-射线衍射仪(XRD)、场发射扫描电子显微镜(FE-SEM)、比表面和孔隙度分析仪(BET)、紫外-可见分光光度计以及电化学工作站对其物相、微观形貌、比表面、光催化和光电化学性能进行表征。结果表明:不同铁源的阴离子会诱导合成形貌和性能差异的纳米针铁矿,以Fe Cl3为原料合成的纳米α-Fe OOH粒径较小、比表面积及孔容较大、对有机染料罗丹明B的降解率较以Fe(NO3)3为原料的α-Fe OOH提高了48. 7%。
Using mechanical force solid phase method,FeCl_3 and Fe(NO_3)_3 were used as iron source respectly. Under the condition of a molar ratio of iron source to base of 1∶ 5,the nano-goethite( α-Fe OOH) was obtained by ball milling for 3 h and then aged in a 60 ℃ water bath. The phase,morphology,photocatalytic and photoelectric performance influenced by the various anions of the iron source were characterized using X-ray diffraction( XRD),field emission scanning electron microscopy( FE-SEM), accelerated specific surface and porosimetry system( BET), UV-vis spectrophotometer and electrochemical testing. The results show that different anions of the iron source can induce nano-goethite with different morphology and performance. Nano α-Fe OOH synthesized with raw materials of Fe Cl3 has smaller particle size,larger specific surface area and larger pore volume,and its photocatalytic degradation of Rhodamine B is better than that of nano α-Fe OOH synthesized with Fe( NO3)3. The degradation efficiency increases 48. 7% compared to that of α-Fe OOH synthesized with the raw materials of Fe( NO3)3.
Using mechanical force solid phase method,FeCl_3 and Fe(NO_3)_3 were used as iron source respectly. Under the condition of a molar ratio of iron source to base of 1∶ 5,the nano-goethite( α-Fe OOH) was obtained by ball milling for 3 h and then aged in a 60 ℃ water bath. The phase,morphology,photocatalytic and photoelectric performance influenced by the various anions of the iron source were characterized using X-ray diffraction( XRD),field emission scanning electron microscopy( FE-SEM), accelerated specific surface and porosimetry system( BET), UV-vis spectrophotometer and electrochemical testing. The results show that different anions of the iron source can induce nano-goethite with different morphology and performance. Nano α-Fe OOH synthesized with raw materials of Fe Cl3 has smaller particle size,larger specific surface area and larger pore volume,and its photocatalytic degradation of Rhodamine B is better than that of nano α-Fe OOH synthesized with Fe( NO3)3. The degradation efficiency increases 48. 7% compared to that of α-Fe OOH synthesized with the raw materials of Fe( NO3)3.
引文
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[22] Zhou Y,Liu F S,Yu S T. Preparation and Photo-catalytic Activities of Fe OOH/ZnO/MMT Composite[J]. Applied Surface Science,2015,355:861-867.
[23] Tian H Y,Zhao G H,Zhang Y N,et al. Hierarchical(001)Facet Anatase/Rutile Ti O2Heterojunction Photoanode with Enhanced Photoelectrocatalytic Performance[J]. Electrochimica Acta,2013,96:199-205.
[24]李宏斌. CuO和Ti O2微/纳米材料的制备、表征及性质[D].天津:天津理工大学,2013.
[2] Xu J G,Li Y Q,Yuan B L,et al. Large Scale Preparation of Cu-dopedα-Fe OOH Nanoflowers and Their Photo-fenton-like Catalytic Degradation of Diclofenac Sodium[J]. Chemical Engineering Journal,2016,291:174-183.
[3] Gao C P,Zhang G,Wang T M,et al. Enhancing the Tribological Performance of PEEK Exposed to Water-lubrication by Filling Goethite(α-Fe OOH)Nanoparticles[J]. Rsc Advances,2016,6(56):51247-51256.
[4] Wang T Q,Jiang Z F,Chu K H,et al. X-shapedα-Fe OOH with Enhanced Charge Separation for Visible-light-driven Photocatalytic Overall Water Splitting[J]. ChemSusChem,2018,11(8):1365-1373.
[5] Wang Y,Liang M X,Fang J S,et al. Visible-light Photo-fenton Oxidation of Phenol with r GO-α-Fe OOH Supported on Al-doped Mesoporous Silica(MCM-41)at Neutral pH:Performance and Optimization of the Catalyst[J]. Chemosphere,2017,182:468-476.
[6] Fu D D,He Z Q,Su S S,et al. Fabrication ofα-Fe OOH Decorated Graphene Oxide-carbon Nanotubes Aerogel and Its Application in Adsorption of Arsenic Species[J]. Journal of Colloid and Interface Sciencec,2017,505:105-114.
[7] Budimirovic D,Velickovic Z S,Djokic V R,et al. Efficient As(V)Removal byα-Fe OOH andα-Fe OOH/α-Mn O2Embedded PEG-6-arm Functionalized Multiwall Carbon Nanotubes[J]. Chemical Engineering Research and Design,2017,119,75-86.
[8]张恩磊,武娇一,王国胜,等.磁性CuFe2O4纳米棒的合成及其芬顿反应降解刚果红性能的研究[J].材料导报,2015,29(5):43-46.
[9] Chen Z M,Wang F,Balachandran S,et al. Morphology Control of Rutile Ti O2with Tunable Bandgap by Preformedβ-Fe OOH Nanoparticles[J].Nanotechnology,2018,29(12):125602.
[10] He D L,Chen Y,Situ Y,et al. Synthesis of Ternary g-C3N4/Ag/γ-Fe OOH Photocatalyst:an Integrated Heterogeneous Fenton-like System for Effectively Degradation of Azo Dye Methyl Orange under Visible Light[J]. Applied Surface Science,2017,425:862-872.
[11] Bujan M,Sikiric M,Filipovic'-Vincekovic N,et al. Effect of Anionic Surfactants on Crystal Growth of Calcium Hydrogen Phosphate Dihydrate[J]. Langmuir,2001,17(21):6461-6470.
[12] Liu H Y,Feng Z B,Wang J,et al. Synthesis of Hollow Carbon Nanostructures Using a ZnO Template Method[J]. Carbon,2016,100:711.
[13] An Z G,Zhang J J,Pan S L,et al. Novel Peanut-likeα-Fe2O3Superstructures:Oriented Aggregation and Ostwald Ripening in a One-pot Solvothermal Process[J]. Powder Technology,2012,217:274-280.
[14] Shen N M,Xiang X M,She X C,et al. Hydrothermal Synthesis and Characterization of Single Crystalline Cu-dopedα-Fe OOH Nanowires[J].Applied Surface Science,2012,259:306-310.
[15] Hojamberdiev M,Zhu G Q,Eminov A,et al. Template-free Hydrothermal Synthesis of Hollowα-Fe OOH Urchin-like Spheres and Their Conversion toα-Fe2O3under Low-Temperature Thermal Treatment in Air[J]. Journal of Cluster Science,2013,24(1):97-106.
[16] Maiti D,Manju U,Velaga S,et al. Phase Evolution and Growth of Iron Oxide Nanoparticles:Effect of Hydrazine Addition during Sonication[J].Crystal Growth&Design,2013,13(8):3637-3644.
[17] Wang D J,Zhou C,Zhu D C,et al. Nanosized CeO2Particles Obtained by Mechanical Solid-state Reaction Combined with Sol-gel Method[J].Transaction of Indian Institute of Metals,2017,70(10):2667-2672.
[18] Khanchandani S,Kumar S,Ganguli A K. Comparative Study of Ti O2/CuS Core/shell and Composite Nanostructures for Efficient Visible-light Photocatalysis[J]. Acs Sustainable Chemistry&Engineering,2016,4(3):1487-1499.
[19]甄延忠,王杰,王丹军,等.一维Fe2O3/α-Mo O3异质结的制备及其可见光光催化性能[J].人工晶体学报,2017,46(1):55-62.
[20]王韵芳,焦爱峰,丁光月,等. CuO/SnO2/Ti O2复合光催化剂的制备及光催化性能[J].人工晶体学报,2010,39(2):401-406.
[21]次立杰,张绍岩,张玉军. BiVO4/SiO2复合材料的制备及光学性能[J].人工晶体学报,2010,39(3). 797-801.
[22] Zhou Y,Liu F S,Yu S T. Preparation and Photo-catalytic Activities of Fe OOH/ZnO/MMT Composite[J]. Applied Surface Science,2015,355:861-867.
[23] Tian H Y,Zhao G H,Zhang Y N,et al. Hierarchical(001)Facet Anatase/Rutile Ti O2Heterojunction Photoanode with Enhanced Photoelectrocatalytic Performance[J]. Electrochimica Acta,2013,96:199-205.
[24]李宏斌. CuO和Ti O2微/纳米材料的制备、表征及性质[D].天津:天津理工大学,2013.