浙江省分析测试科技计划研究项目

1EC-SPMTiO22TiO2TiO2TiO2--31-TiTiO2SPMSPM2TiO2TiTiO2TiO232O23TiO2SPMTiO24-TiO2TiO241-2TiO23-TiO251-2TiO2333TiO2431EC-SPM1-123AFM765432111-2-3-4-5-6-7-342ECControllerAFMSpisel32iconAFM3TiO2NiAg1cm20.1mol·L-1NiSO40.1mol·L-1CH3COONa25mA·cm-12510s2s10min5min11135200812,,2008,59(S1):88-921cm200.3µm0.5mol·L-1NaClORC10mV·s-1-0.30.4V251AppliedCatalysisA:General112TiO21TiO2TiTiO2TiO2100V(0.5,0.7,1.0mol·L-1.)10min20.5mol·L-190160nm2a2b2cTiO20.5mol·L-160V80V100V100V10min33abc36abc2,100V10minAFMa)0.5mol·L-1H2SO4b)0.7mol·L-1H2SO4c)1.0mol·L-1H2SO4.()3cd3d3(d)TiTiO20.5mol·L-160V6min8min10min17min44a37abcd310minAFM0.5mol·L-1H2SO4a),60Vb),80Vc),100Vd),100V.4b4c4d0.5mol·L-1H2SO4+0.4wt%NH4HF21220V30minTiO2538abcd4AFM0.5mol·L-1H2SO460Va)6minb)8minc)10mind)17min.5TiO2AFM,0.5mol·L-1H2SO4+0.4wt%NH4HF21220V30mina)b)3D.3930min3D3050nm2030nm60minTiO266TiO2AFM,0.5mol·L-1H2SO4+0.4wt%NH4HF21220V60min60min120150nm610nmJ.M.Macak1mol·L-1H2SO40.5wtHFNH4F20V15hTiO2100nm500nmTiO2J.M.MacakTi0.1mmTi1mmTiTi3(1)(2)(3)40TiTiO2++→+H4TiOOH2Ti222TiO2TiO2O27X-TiTiTiO2SPMTiO21µmSPMSPM100nmSPM4120304050607080050010001500200025003000♦Titanium♦♦♦♦♦♦♦Intensity2θ,Deg.♦7TiO2XRD2TiO2SPMTiO2CVLVPVMPTiO21H2SO41TiO2(mol/L)(V)(min)(min)380.560154CV390.560354CV400.560554CV410.560554LV420.560554MP430.5130/10()CV440.5120/10()CV450.5100/10()CV460.580/10()CV470.513010/PV480.513010/LV490.513010/MP500.513010/CV42510.5130/10(35-38)LV520.5130/10(20-39)PV530.5130/10(20-40)LV540.5130/10(10-19)MP550.5130//CV560.5130//CV570.513030/CV580.513060/CV590.51302/LV6411302/MP710.58010(20)/CV720.510010(20)/LV730.512010(20)/MP740.710010(20)/CV751.010010(20)/CV761.510010(20)//CV770.510010(20)/PV601+KF2015/CV611+KF2030/CV621+KF2060/CV631+KF2045/CV651+NH4HF22060/CV661+NH4HF22030/CV671+NH4HF22045/CV681+NH4HF22015/CV691+NH4HF22060(20)/LV701+NH4HF22030(20)/LV781+NH4HF22090(12)/LV791+NH4HF220120(12)/LV800.5+NH4HF22060(12)/CV810.5+NH4HF22030(12)/CV820.5+NH4HF22060(12)/CV830.5+NH4HF22090(12)/CV81SPMSPMTiO243383940/414243444546474849/44535455//56575859606162636465666745686970/717273/747576777879468081828381SPM838400.5mol/LH2SO460VTiO2434643444660V4759647177100140V55577176566063KFF65707879NH4HF2NH4HF2KFNH48083H2SO4H2SO4CVLVPVMP47-3EC-SPM0.5mol·L-11mol·L-1TiO2X-XRDTiO225µm20µm80150nmTiO2.10.4mmTi10min20V5030min0.5mol/LH2SO4H2SO41mol/LTiO2EC-SPMX-CHI660B37A/dm2502TiO2X-9TiTiTiO210TiO2SPM10aTiO225µm20µm10bTiO23D80150nm4820304050607080050010001500200025003000♦Titanium∇Rutile∇♦♦♦♦♦♦♦Intensity2θ,Deg.♦∇Fig.9XRDpatternofTiO2anodizedin0.5mol·L-1H2SO4+1mol·L-1MAfor10minat20Vand50(c)(b)(a)Fig.10AFMimagesofTiO2filmformedbyanodizationin0.5mol·L-1H2SO4+1mol·L-1MAfor10minat20Vand50.(a)2020µm2;(b)55µm2;(c)22µm2(3Dimage)TiO211A-0.57V-0.55V-0.99V-0.92VTiO2/Ti2O3TiO2/Ti(OH)311B11A-0.86V-0.91VTi3+Ti3+Ti3+TiO2MATiO2(MA)ad.+49H2OH+eTi(OH)3(MA)ad.+++TiO2(MA)ad.SA+Ti(OH)3(MA)ad.TiO20.0-0.2-0.4-0.6-0.8-1.0-1.2051015202530350.0-0.2-0.4-0.6-0.8-1.0-1.20.00.51.01.52.0I/mAE/V(vs.SCE)2I/mAE/V(vs.SCE)1(A)(B)Fig.11Cyclicvoltammogramsobtainedin0.5mol·L-1H2SO4forTi/TiO2electrode(1)intheabsenceand(2)inthepresenceof1mol·L-1MA.Scanrate:50mV·s-1250mA/cm25TiO2TiO2Table2GalvanostaticelectrolysisdataonthereductionofMAatnano-rodTiO2cathodeConcentrationofMA:1mol·L-1;Temperature:50No.Currentdensity(mA·cm-2)WeightofSA(g)YieldofSA(%)Currentefficiency(%)1255.668.869.92355.972.573.73506.478.679.94705.567.568.75*507.490.992.5*In-situactivationbygalvaniccycles.TiO290.992.55041-TiO2AgNi2TiTiO2TiTiO23(1)(2)(3)3TiO2TiO2Ti3+Ti3+TiO2431,,,.TiO2.,2008,24(11):2139-2142,,,..,2008,59(S1):88-92,*.TiO2.,2009,21(1):121-127,.Ti/TiO2,CN101407924200810122146511ECControllerAFMSpisel32iconAFM217218.571750210005232962.5745052506167219021SPM231520091216-2053