New Nano-structured Semiconductor Photocatalysts for Photocatalytic Solar Hydrogen Production
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1 2010 The 7th Korea-USA Nano Forum New Nano-structured Semiconductor Photocatalysts for Photocatalytic Solar Hydrogen Production JIN-OOK BAEG Jin-Ook Baeg Korea Research Institute of of Chemical Technology
2 Photocatalyst Application Environmental Remediation - Pollutant Treatment - Deodorization - Sterilization h Solar Energy Conversion - Water Splitting - H 2 S Splitting Energy Photo-induced reaction Pollutant (organic comp.) +O 2 G<0 (down hill) E G<0 The reaction irreversibly proceeds. degradation CO 2 + H 2 O + etc. Energy Light energy conversion reaction H 2 O Water splitting H 2 + O 2 G>0 (up hill) A back reaction easily proceeds.
3 Solar Energy Conversion for Hydrogen Production Photocatalytic Water Splitting for H 2 Production Solar light H 2 O Photocatalyst PV / hybrid H 2
4 Solar Energy h Solar Energy 1.74 x 10 5 TW Global l need 15.7 TW in ,000 times of Current world demands (~ 0.1% of the Earth s surface : 10% conversion efficiency )
5 Photocatalytic Water Splitting for Hydrogen Production h Conduction Band H 2 O O Valence Band h 2H 2 O 2H 2 + O 2 H 2 O H 2 Potent tial + h CB Band gap VB e - h + + H + / H2 0V O2/ H2O V
6 Energy Requirement for Overall Water Splitting 2 H 2 O 2H 2 + O 2 G = 237kJ/mol(E = - G /nf = -1.23V) Overpotentials for photo-splitting of water Reaction type Energy required ev Electron transfer at a cathode 0.2 Hole transfer at an anode 0.2 H 2 overpotential ti at a cathode 0.1 O 2 overpotential at an anode 0.5 Band bending for efficient charge separation at an anode 0.2 Total 1.2
7 2400 Solar Spectrum 물광분해반응의열역학적고찰 Spectral Irradienc ce (W/m 2 / m) Air Mass 0 Air Mass 1.5 AM1.5 ~ 100mW/cm Wavelength ( m) 0% 0.5% 3.5% 46% Wavelength (nm) UV VIS IR 510 nm 1008 nm 3.10eV (400nm) 2.43eV 1.55eV (800nm) 1.23eV
8 Band Gap Energy and Band Edge Position of Photocatalysts
9 Photocatalysts for Water Splitting (UV Light) TiO 2 Photocatalyst TiO 2 - h Pt H 2 O H 2 H 2 O + O 2 RuO 2 TiO 2 : E g = 3.2 ev, g = 388 nm Catalyst H 2 (μmol/h) Pt/TiO 2 2 Pt/TiO 2 /RuO J. C. Escudero et al., J. Catal., 1990, 123, 319.
10 Perovskite Photocatalyst (UV Light) Water splitting mechanism of K 4 Nb 6 O 17 h A [M n-1 Nb n O 3n+1 ] Ⅰ Ⅱ Ⅰ Ⅱ O 2 h + e - H 2 O Ni Ni e - h e + - e - h + H 2 H 2 O h + h + Ni e - Ni h + h + H 2 O O 2 NbO 6 h + e - h H + 2 O A (Alkali Metals) Ⅰ Ni Ni H e- = K, Rb, Cs, etc. 2 e - h + M (Alkali Earth Metals) = Ca, St, etc. e - h
11 Perovskite Photocatalyst (UV Light) X Catalyst Rate of Gas evolution (μmol/h) H 2 O Ni-K 4 Nb 6 O Ni-K 4Ta 2Nb 6O Ni-K 4 Ta 3 Nb 6 O Ni-K 4 Ta 4 Nb 6 O A [M n-1 Nb n O 3n+1 ] 0 Ni-Rb 4 Nb 6 O Ni-Rb 4 Ta 2 Nb 4 O 17 Ni-Rb 4 Ta 3 Nb 4 O 17 Ni-Rb 4 Ta 4 Nb 4 O 17 Ni-Rb 4 Ta 6 Nb 4 O Ni-Rb 4 Ta 6 Nb 4 O wt% nickel was loaded. d Catalyst, t 1 g; distilled d water, 350 ml; high pressure Hg lamp (400 W); inner irradiation cell (quartz). - K. Domen et al., Catal. Today, 1996, 28, 175.
12 Summary of Quantum Efficiency of Overall Water Splitting Under UV Light NiO-SrTiO 3 1% (300nm) Ni-Rb 4 Nb 6 O 17 10% (300nm) NiO-NaTaO3 :La 56% (270nm) NiO-Ni- Rb 2 La 2 Ti 3 O 10 30% (300nm)
13 Photocatalyst for Water Splitting (Visible Light) CdS : Eg = 2.4eV, g = 517nm - CdS has ideal band gap & band edge position for water splitting for H 2 production under visible light irradiation. h h CdS - TiO 2 - Support H 2 But it undergoes photocorrosion! H + H 2 yield, μmol Pt Catalyst Calcination Temp.( C) h Pt/TiO 2 /SiO CdS/SiO Pt/TiO H 2 /SiO CdS/SiO H + Pt/TiO 2 /SiO CdS/SiO Pt/TiO 2 /SiO Pt CdS/SiO Pt/TiO 2 /SiO CdS/SiO Interparticle electron transfer: (A) Mediated by the conduction band of TiO 2 ; (B) Direct electron transfer to separately supported platinum. - J. M. White et al., J. Phys. Chem., 1987, 91, a Reaction conditions: 10 mg of TiO 2 /SiO 2 ; 0.4 wt% Pt (in situ photoplatinization); 10 ml of 1:1 H 2 O-MeOH 0.01 M KOH; light source: 450W Xe lamp, 420 nm cut-off filter
14 ZnCuS Photocatalyst ZnS Zn Cu S E g = 3.7eV E g = 2.5eV g = 335nm g = 496nm b.units Absorban nce / ar ZnS Zn Cu S CuS * Quantum yield: 37%( 3.7% > 420 nm) (Photocorrosion) * Rate of H 2 revolution: 430 mol/g.cat.hr (0.5M Na 2 SO 3 ) Wavelength/nm - A. Kudo et al. Catal Letter, 1999, 58, 241.
15 Rh 2 O 3 : Cr 2 O 3 /(Ga 1-x Zn x )(N 1-x O x ) Photocatalyst for Water Splitting ( = 420~ nm; ph=4.5) QY: 2.5% Catalyst: 0.3 g, Rh 2 O 3 : Cr 2 O 3 5 wt.%, Domen, et. al., Nature, 440, 295 (2006).
16 CdIn 2 S 4 Nanotube and Marigold Nanostructure Photocatalyst Cubic spinel nanostructured CdIn 2 S 4 Marigold(aq.) : 3~5 μm CdIn 2 S 4 - Nanotubs Nanotube(MeOH) : 25nm X 780nm Density of states (DOS) for CdIn 2 S 4 (Calc. Eg = 1.90 ev) VB (S 3p) ; CB (In 5s, 5p major & Cd 5s, 5p) Advanced Functional Materials, 2006,16, 1349.
17 CdIn 2 S 4 Nanotube and Marigold Nanostructure Photocatalyst CdIn 2 S 4 Photocatalyst for Hydrogen production 1.8 A bs (b) (c) (d) (a) Eg = 2.19 ev (570 nm) High quantum yield! - Nanotube(MeOH) : 17.1% (@ = 500 nm) - Marigold(aq.) : 16.8% (@ = 500 nm) Quantum yield (%) = [Number of H 2 molecules evolved x 2] [Number of incident photons] X Rate of H 2 revolution: wavelength(nm) - Nanotube : 3480 mol/hr - Marigold : 3476 mol/hr Diffuse Reflection Spectra s (a) aqueous (b) methanol (c) ethylene glycol (d) polyethylene glycol (5%) mediated CdIn 2S 4. Advanced Functional Materials, 2006,16, 1349.
18 Nano-CdS Q.D. Photocatalyst in Glass Matrix Procedure of Preparation for Powder of Q-CdS in glass matrix SiO2 + Na2O + K2O + ZnO, B2O3 + TiO2 + BaO & CdS(0.5 wt%) Ball-milled mixing for 6h a b Reaction at 1500~1600 o C for 3h Annealing at o C (Tg = ) 580) for 72h Grinding Typical photographs of glass matrix, a) host glass b) after crystal growth of Q-CdS Powder of Q-CdS in glass matrix Journal of Material Chemistry, 2007, 17, 4297.
19 Nano-CdS Q.D. Photocatalyst in Glass Matrix Photocatalytic Activity for H 2 Production (Visible ) Q-CdS (1% amount ) has 300% higher photocatalytic activity than bulk CdS!! High quantum yield (@ = 470 nm)!! - Q-CdS-glass: 17.5% (1g of powder contains 0.005g of Q-CdS) - CdS: 5.5% (0.5 g of CdS) Quantum yield (%) = [Number of H 2 molecules evolved x 2] [Number of incident photons] X 100 Journal of Material Chemistry, 2007, 17, 4297.
20 Octahedrally Coordinated d 0 Transition Metal Oxide Photocatalysts Octahedrally Coordinated d 0 Transition Metal Oxide Photocatalysts TiO 2, SrTiO 3, A 2 Ti 6 O 13 (A = Na, K, Rb) BaTi 4 O 9, A 2 La 2 Ti 3 O 10 (A = K, Rb, Cs) K 2 Ti 4 O 9, Na 2 Ti 3 O 7 Ti 4+ V Cr ZrO 2 Zr 4+ Nb 5+ Mo Hf Ta 5+ W Ta 2 O 5, ATaO 3 (A = Na, K) A 4 Nb 6 O 17 (A=K, Rb) MTa 2 O 6 (M = Ca, Sr, Ba) Sr 2 Nb 2 O 7 Sr 2 Nb 2 O 7
21 Density of States of TiO 2 by First Principle Calculation O - TiO 2 Conduction Band h Ti + Valence Band Density of states of TiO 2 TiO 2
22 Density of States of ZnBiGaO 2 by First Principle Calculation Zn 2 GaO 4 Eg = 3.82 ev ZnBiGaO 4 Eg = 1.92 ev
23 Photocatalytic 물Activities 광분해반응의 of New 열역학적 Photocatalysts 고찰 (Visible) Photocatalytic H 2 Production System(Visible ) Catalyst Band gap energy (ev) H 2 evolution rate a ( mol/hr) ZnBiGaO (440nm) 3,030 CdBiGaO (510nm) 2,454 a Catalyst 0.5g, 250mL(H 2 O) + KOH(0.5M), H 2 S(2.5mL/min), Xe lamp(450w), light filter(>420nm).
24 Development of Synthetic Method for New Metal Oxide Photocatalyst Low temperature economical photocatalyst preparation method! Procedure of Preparation for ZnBiVO 4 by Solid State Method Procedure of Preparation for ZnBiVO 4 by Hydrothermal Method Zn(II)-oxide Bi(III)-oxide V(III)-oxide Zn(NO 3 ) 2 5H 2 O + Bi(NO3) 3 6H 2 O Mixing & Tableting NH 4 VO (b) (b) hydrothermal Urea & water Reaction at 670 o C for 15h Grinding Abs (a) (a) solid state Reaction at 130 o C for 60-72h Reaction at 725 o C for 12h Grinding ZnBiVO (Eg = 2.30eV: 539nm) wavelength(nm) Specific surface Area BET (m 2 /g) : 0.27 Wash & Dry at 250 o Cfor5h Specific surface ZnBiVO Area BET (m 2 4 /g) : 2.50
25 Preparation of Visible Light Photocatalyst by N-doping Procedure of Preparation for Nb 2 Zr 6 O 17-x N x ZrO 2 Nb 2 O 5 Mixing & Tableting Reaction at 1300 o C for 24h Grinding Nb 2 Zr 6 O 17 NH 3 /20mL/min Reaction at 800 o C for 2h Grinding Nb 2 Zr 6 O 17-x N x
26 New Visible Light Photocatalyst Synthesis by Molten Salt Method Procedure of Preparation for Ga 2 Pb 2 Nb 2 O 7 Pb(II)-oxide Ga(III)-oxide Nb(V)-oxide Mixing & Tableting NaCl (10eq.) Reaction at 1093 o K for 4h Grinding & Washing Reaction at 1473 o C for 12h Grinding Ga 2 Pb 2 Nb 2 O 7
27 Present Statust Conclusions Quantum efficiency (UV) : ~ 56%(270nm: H 2 O) Quantum efficiency (Visible) : ~ 5.2%(410nm: H 2 O) Quantum efficiency (Visible) : ~ 20%(500nm: H 2 S) Future target Quantum efficiency (Visible) : 30% ( 600nm) Hydrogen production rate (1 km 2 ) : 16,500Nm 3 /h Photoreactor t H 2 Solar Hydrogen Production System Purification Storage
28 Thank you!
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