ナノハイブリッド材料の創製
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- たみえ なかきむら
- 7 years ago
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1 1
2 α-fe2o3 α-fe2o3 α-fe2o3 α-fe2o3 2µm 2µm 2µm 10µm CdS CdS Cu2O 0.5µm 1µm 0.5µm 2
3 Ni-Zn 3
4 4
5 5
6 Ni-Zn 6
7 7
8 (T. Sugimoto, Adv. Colloid Interface Sci. 28, 65 (1987).) 8
9 LaMer 9
10 10
11 11
12 O 12
13 13
14 α-fe2o3 -FeOOH α-fe 2 O 3 14
15 1 mol/l 1/100 mol/l 15
16 16
17 17
18 100 Fe(OH)3 3 hours β-feooh 6 days α-fe2o3 18
19 2µm 19
20 Ni(OH)2 With PEG 50,, 12 hours NaH2PO2 0.1 M Ni(OH) M NaH 2 PO wt% PEG 400,000 20
21 2M - : 0.5 M : 1.0 M 21
22 Reservoir of M Cd(OH)2 or Metal chelates 2+ M(NH3)n M + S Reservoir of S 2- TAA Gelatin 22
23 (TAA: CH3CSNH2) 23
24 0.30 M M(CH 3 COO) M Chelating agent A or 0.33 M Chelating agent B (TMD, DMED, DETA, TETA, AA, NTA) (TAEA, EDTA) 2.6 M NH 3 NaOH or CH 3 COOH ph at 25 1 wt% Gelatin Total = 20 ml 25 or M TAA 1 wt% Gelatin Total =5 ml Product 24
25 Amines Trimethylenediamine (TMD) H2NCH2CH2CH2NH2 N,N-Dimethylethylenediamine (DMED) H2NCH2CH2N CH3 CH3 Diethylenetriamine (DETA) H2NCH2CH2NHCH2CH2NH2 Triethylenetetramine (TETA) H2NCH2CH2NHCH2CH2NHCH2CH2NH2 Tris (2-aminoethyl) amine (TAEA) Amino Acids L-Aspartic Acid (AA) Nitrilotriacetic Acid (NTA) Ethylenediamine-N,N,N,N - tertaacetic Acid (EDTA) N CH2CH2NH2 CH2CH2NH2 CH2CH2NH2 HOOCCH2CH(NH2)COOH N HOOCH2C HOOCH2C CH2COOH CH2COOH CH2COOH NCH2CH2N CH2COOH CH2COOH 25
26 logk1 or logk1k2 at 25 or 20 Cd 2+ Zn 2+ Pb 2+ Cu 2+ Ni 2+ TMD (K 1 K 2 ) 16.9 DMED (K 1 K 2 ) 16.0 DETA (K 1 K 2 ) 13.8 (14.4) (21.3) (29.6) TETA 13.9 (K 1 K 2 ) 11.9 (K 1 ) 11.4 (K 1 ) 20.1 (K 1 ) 14.1 (K 1 ) TAEA (K 1 ) (12.3) (14.7) (18.8) (14.8) AA (K 1 K 2 ) 15.2 NTA (15.5) (K 1 K 2 ) 9.18 (K 1 ) (11.4) (K 1 ) 13.2 (K 1 ) 16.2 (K 1 K 2 ) EDTA (K 1 ) *Stability constants bound by ( ) are those at 20. K [ ML] [ ML ] = ; K = 2 ; KK 1 2 = [M][L] [ML][L] 1 2 [ ML ] 2 [M][L] 2 26
27 T T N T A A N D D D A N E CdS ZnS PbS Yield (%) T N N T N A T N D D E 0 T A N N E E E E D: DETA T: TETA A: TAEA N: NTA E: EDTA 25, 2 min 25, 1 h 60, 8 h log K1 or log K1K2 27
28 Role of NH3 on the Nucleation and Growth Without Ammonia With Ammonia Cd 2+ Cd(NH3)n 2+ Cd-EDTA Cd-EDTA Nucleation Nucleation 2+ [Free Cd ] Renucleation Growth Dissociation Critical Supersaturation Level Dissociation CdS CdS Growth 28
29 29
30 A B,C B CeO 2 1.0x10-3 mol/l Ce(SO 4 ) 2 4.0x10-2 mol/l H 2 SO
31 31
32 32
33 2.0x10-2 mol dm -3 FeCl 3 and 4.5x10-4 KH 2 PO 4 at 100 o C M. Ocana, M. Morales, and C.J. Serna: J. Colloid Interface Sci. 171 (1995) 85. M. Ocana, R. Rodriguez-Clemente, C.J. Serna: Adv. Mater. 7 (1995)
34 0 hour 8 hours 2 day 4 day 7 day β-feooh α-fe 2 O 3 34
35 35
36 Run 1 Run2 Run3 36
37 37
38 CuO 38
39 CuO LaMer Matijevic CuO Lee, S.H., Her, Y.S., and Matijevic E., J. Colloid Interface Sci. 186, 193 (1997) 39
40 Cu(NO 3 ) 2 :0.20 mol dm -3, NaOH: 0.40 mol dm 3, 40 40
41 Cu(NO 3 ) 2 :0.20 mol dm -3, NaOH: 0.40 mol dm 3, 40 41
42 Cu(NO 3 ) 2 : mol dm -3, NaOH: mol dm 3, 40 42
43 Cu(NO 3 ) 2 : mol dm -3, NaOH: mol dm 3, 40 43
44 Cu(NO 3 ) mol dm -3 Cu(NO 3 ) mol dm -3 NaOH NaOH 0.40 mol dm mol dm 3 Aging (40, 6 ) Aging (40, 1 ) CuO 44
45 CuO Cu 2 O 0.5 mol dm -3 CuO 0.5 mol dm -3 hydrazine (N 2 H 4 ) at ph 9.3, 30 o Cfor 3 hours Cu 2 O 45
46 CuO Cu 2 O 46
47 47
48 [Cu 2+ ] ph 48
49 Dissolution 1. CuO = Cu 2+ Reduction 2. Cu 2+ + N2H4 = Cu + Hydrolysis 3. Cu + + H2O = Cu2O Dissolution 4. Cu2O = Cu + Reduction 5. Cu + + N2H4 = Cu Dissolution 1. CuO = Cu 2+ Reduction 2. Cu 2+ + N2H4 = Cu 49
50 Ni-Zn 50
51 Ni-Zn 51
52 Ni-Zn 2- Zn Ni Ni Ni 2+ BH 4 Ni Ni Ni only Ni Zn 2+ Zn Ni Ni-Zn Zn 2+ Ni BH 4 Ni Zn 2+ Ni Ni B Zn Ni Zn Ni B B 52
53 10 9 m = 1 nm m 53
54 54 1m 10cm 1cm 1mm 100 m 10 m 1 m 100nm 10nm 1nm m 10 m 1 m 1nm 100nm 10nm
55 55
56 56
57 57
58 nm 58
59 Ni-Zn 2- Ni-Zn Zn Ni Ni-Zn B 5 10 nm 59
60 Ni Zn, 118, p (2002) 60
61 61
62 62
63 63
64 64
65 65
66 Ni-Zn 66
67 67
68 68
69 H, CO H, CO Pt 69
70 nm Pt 3~5% 70
71 71
72 72
73 73
74 74
75 Pt Pt Cl Cl Cl OH OH Cl Pt 4+ Pt4+ Cl OH OH Cl H 2 O H 2 O 100, 2 Pt nm 20 wt% 20 30% 75
76 ph Pt(OH) wt%, ~1nm 76
77 Selective Deposition [ ] = 2.0 mm (HAuCl 4 ; RuCl 3, RhCl 3, PdCl 2, H 2 IrCl 6, H 2 PtCl 6 ) (, 24 h) NaOH = 1.6 g dm -3 (30 min) 100, 48 h Au, Ru, Rh, Pd, Ir, Pt 77
78 78
79 100 Au 80 Au hydroxides Yield (%) Initial ph = 6.24; Final ph = Time (h) Metallic Au 79
80 100 Au/ Metallic Au 80 Yield (%) Supernatant Au 20 Au hydroxides Initial ph = 5.98; Final ph = Time (h) 80
81 Au ph Au : 2.0 mm 81
82 ph>7 ph UV ph 82
83 ph 6 ph 6 ph 7 HAuCl 4 AuCl H + HAuCl 4 + 4OH - Au(OH) 3 + 4Cl - + H 2 O HAuCl 4 + 4OH - Au(OH) 3 + 4Cl - + H 2 O HAuCl 4 + 5OH - Au(OH) Cl - + H 2 O 83
84 Au 4Au(OH) 3 4Au + 6H 2 O + 3O 2 Au(OH) 3 Au(OH) 3 OH - Au 3+ Au 84
85 Au Table 2. Produced metallic Au deposited on hematite particles and oxygen in various forms in a concentrated system Reduced product Oxidized products Au ClO ClO 3 ClO 4 - O x x x x x 10 3 Initial conditions: [HAuCl 4 ] = 2.0 x 10 2 Μ, NaOH = 8.0 x 10 2 Μ, ph = 6.55 [α-fe 2 O 3 ] = 2.0 x 10 1 mol dm 3 (polycrystalline ellipsoids) 100, 72 h 2[O] 3[Au total 3] + 2[O2] = = 0 ] 2 [ClO ] + 3[ClO3] + 4[ClO 0 3 [Au ] Au(OH) Au + O2 + H2O G = 318kJ/mol (mol dm 3 ) =1 85
86 Au/ ESCA Arbitrary Unit (-) Au/ Au/ (0.02M HCl ) Au Binding Energy (ev)
87 α-fe 2 O 3 α-fe 2 O 3 α-fe 2 O 3 α-fe 2 O 3 87
88 Support Particles Table 1 Used Support Particles Size (µm) Structure BET Surface Area (m 2 /g) α Fe 2 O 3, ellipsoids (A) polycrystal 136 α Fe 2 O 3, ellipsoids (B) single crystal 21.8 α Fe 2 O 3, cubes 0.09 single crystal 15.9 α Fe 2 O 3, platelets single crystal 0.70 α FeOOH, needles single crystal 41.0 β FeOOH, needles single crystal 112 ZrO 2 (A), spheres (rough surfaces) single crystal 153 ZrO 2 (B), spheres (smooth surfaces) single crystal 118 TiO 2, ellipsoids single crystal 88
89 89
90 90
91 α-feooh β-feooh ZrO 2 (A) Rough surfaces ZrO 2 (B) TiO 2 Smooth surfaces 91
92 -FeOOH -FeOOH ZrO 2 (A) ZrO 2 (B) TiO 2 92
93 Table 3. Deposited amounts of Au(OH)3 and Au 0 and the mean size of Au 0 particles Support Particles Size (µm) Structure Deposited amount (mol %) Particle size of Au (nm) Au(OH) 3 Au 0 α Fe 2 O 3, ellipsoids (A) polycrystal α Fe 2 O 3, ellipsoids (B) single crystal α Fe 2 O 3, cubes 0.09 single crystal α Fe 2 O 3, platelets single crystal α FeOOH, needles single crystal β FeOOH, needles single crystal ZrO 2 (A), spheres (rough surfaces) single crystal ZrO 2 (B), spheres (smooth surfaces) single crystal TiO 2, ellipsoids single crystal
94 94
95 Effect of ph on yields of Pt precursor (100, 2days) 100 -Fe 2 O TiO
96 Effect of ph on adsorption of Pt ions (25, 2days) TiO 2 -Fe 2 O
97 Pt TiO 2 97
98 Pt 1- (m 2 g -1 ) (wt%) (H/M) (nm) (% TiO 2, ellipsoid (anatase) Fe 2 O 3, ellipsoid (A)* SiO2 (Stober ) ZrO2 (B)** Al2O3 156 ALO
99 Ni-Zn 99
100 Ni 100
101 101
102 Ni Well-defined as 2-102
103 Ni-Zn Zn 103
104 Ni-Zn/TiO 2 2- [Ni(AA) 2 ] = mol/l TiO 2 Zn/Ni = 0.1 [NaBH 4 ] = mol/l 30 = 2.5 g/l Ni 12wt% 2- Ni-Zn/TiO 2 104
105 - / [Ni(AA) 2 ] = mol/l Zn/Ni TiO 2 [NaBH 4 ] = mol/l TiO 2 = 2.5 g/l (Ni 12wt% ) 3-way ball valve 2Ni BH + 4 2Ni B 2H Ni 2 H Ni-Zn/TiO 2 gas gas H 2 2 N 2 heating mantle 105
106 TiO 2 TiO 2 Sugimoto : 43m 2 /g T. Sugimoto, M. Okada, and H. Itoh: J. Colloid Interface Sci. 193 (1997)
107 Zn 107
108 / (ICP )
109 Ni-Zn/TiO 2 (Zn/Ni=0.1) 109
110 Zn Ni Ni-Zn (Zn/Ni=0.1) 10 nm 110
111 2 - (2) 10nm 10n m Zn/Ni=0.2 Zn/Ni=
112 / 0.2 Ni(Metal) TiO 2 (Anatase) 112
113 ESCA (Zn/Ni=0.2) Ni Ni( ) Ni(Metal) Zn N(E)/E Binding Energy(eV) Ni 0 2 Ni/TiO 2 Zn B 26.7% B Ni 73.3% Zn Ni-Zn/TiO % 55.1% 5.6% 113
114 1 1-Octene C 8 H 16 H 2 cat n-octane C 8 H 18 H 2 5cm mol/h 30 4 Ni-Zn/TiO 2 in 2-propanol(50ml) 1-Octene 114
115 1- (1) Ni-Zn/TiO 2 (Zn/Ni=0.2) Ni Ni-Zn Ni/TiO 2 (Zn/Ni=0.2) 115
116 Ni-Zn/TiO 2 Ni/TiO Ni-Zn
117 1- (2) 117
118 Ni/TiO 2 Zn Zn B.G. Zn/Ni nm 118
119 Ni-Zn 119
120 120
121 1 121
122 FeSbO 4 ) etc FeSbO 4 ) 122
123 1000 ( ) 500 FeSbO : FeCl 3 +SbCl 5 123
124 124
125 The Gel-Sol Method The gel acts as a protective matrix against the coagulation of the growing particles as well as a reservoir of precursor ion. Gel network Monomer Growing particle 125
126 FeCl 3 +SbCl 5 NaOH Fe,Sb Fe 3+ ] 0 =[Sb 5+ ] 0 = 0.5M : H= (FeSbO 4 ) 126
127 8 FeSbO 3 FeSbO nm
128 ph ( ) nm 1.0 FeSbO 4 +Sb 2 O < < 6.0 (FeSbO 4 ) 6.0 FeSbO 4 Fe-Sb 128
129 nm 129
130 (TEOA) TEOA: N(C 2 H 4 OH) nm TEOA {100} TEOA TEOA 130
131 13 TEOA 2 131
132 g C 2 H 5 OH/O 2 /N 2 =5.8/18.8/ ( 2C 2 H 5 OH + O 2 2CH 3 CHO + 2H 2 O 132
133 1) 2) 1) (%/m 2 ) (m 2 /g) 0.15(g= ) 2) FeSbO FeSbO 4 {100} 133
134 134
135 TiO 2 135
136 CS 2 UV-visible TiO 2 TiS 2 CS , 1 136
137 137
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2 3 10 9 m = 1 nm m 4 5 100 m 1m 10cm 100 m 1cm 1mm 10 m 1 m 100nm 10nm 1nm 1 10 m 1 m 1nm 100nm 10nm 10 8 6 1 nm 10 8 7 9 10 11 12 13 14 15 17 18 19 20 21 nm Ni-Zn 2- Ni-Zn Zn Ni Ni-Zn B 5 10 nm 23
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