TiO2ナノ粒子の部分硫化による可視光応答性光触媒の開発
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- きのこ あいしま
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1
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3 2002 CdS, ZnS
4 by
5 CdS CdS, ZnS
6 CdS CdS, ZnS
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11 (a) (b) (c) (d) (e) (f) (g) (h)
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15 ev, nm 1240 nm
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18 TiO 2 =3.2eV (= 390nm)
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20 (a) (b) (c)pt
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22 1 Fe 2 O TiO 2 (rutile) 3.0 Cu 2 O 2.2 TiO 2 (anatase) 3.2 In 2 O SrTiO WO ZnO <3.3 Fe 2 TiO 3 <2.8 BaTiO PbO 2.8 CaTiO V 2 O KTaO FeTiO SnO Bi 2 O ZrO Nb 2 O 3 3.0
23 2 Si 1.1 GaAs 1.4 CdSe, n 1.7 GaP 2.25 CdS, n 2.4 ZnS, n 3.5
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26 P-1. P-2. P-3. P-4. * * P-5. N P-6. P-7.
27 P-8. P-9. TiO2 P-10. TiO2 P-11. V4+ * * * P-12. * ** ** *** **** * ********** * ** *** **** KAST***** P-13. * * P-14. Ti TiOxNy
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31 TiO 2 O S R.Asahi, T.Morikawa, T.Ohwaki, K.Aoki,, and Y. Taga, Science, 293, 269 (2001).
32 Umebayashi (TiS 2 ) T.Umebayashi T.Yamaki, S.Tanaka,, and K.Asai,, Chem. Lett., 32, 330 (2003).
33 Ohno
34 UV nm X 700 S T.Ohno, F.Tanigawa, K.Fujihara, S.Izumi,, and M.Matsumura,, J. Photochem. Photobiol., A:127, 107 (1999). T.Ohno, Y.Masaki, S.Hirayama,, and M.Matsumura,, J. Catal., 204, 163 (2001). T.Ohno, T.Mitsui,, and M.Matsumura,, Chem. Lett., 32, 364 (2003).
35
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37 TiO 2
38 TiO 2 - ST01 ST01 20nm
39 TiO 2 TiO 2
40 TiO 2 (ST01, ) 110 TiO 2 TiO Ti(OH) 4
41 TG Sample (100 Evacuation N 2 refilling CS 2 /N 2 gas flow (5/50 ml/min) Heating (1 ºC/ min) TG curve Telescope Quartz spring Thermal shield Gas inlet Water-cooled cap Sample in Electrical Quartz basket furnace Height meter Gas outlet Schematic drawing of thermobalance
42 TG curves of sulfurization of TiO 2 powders with CS 2 45 Weight change(%) Heating rate: 1 C/min Gas flow rate: CS 2 : 5 ml/min N 2 : 50 ml/min Sample: a. ST01 b. Dried ST01 c. Anatase d. Rutile e. Ti(OH) 4 TiS 2 Ti 1.08 S 2 Ti 3 S 4 a b e c d Temperature (ºC )
43 XRD patterns of sulfurized TiO 2 powders Rutile Ti 3 S 4 Ti 1.08 S 2 e. Ti(OH) 4 Intensity (a.u.) d. Rutile c. Anatase b. Dried ST01 a. ST Θ ( degrees)
44 Reactions Sulfurization TiO 2 +CS 2 TiS 2 + CO 2 Decomposition TiS 2 Ti 1.08 S 2 Ti 3 S 4 Dehydration Ti(OH) 4 TiO 2 + 2H 2 O
45 TiO 2 -ST01 TiO 2 -ST01 TG T>450 T<
46 TiO 2 XRD j. 500 C i. 450 C h. 400 C Intensity (a.u.) g. 350 C f. 300 C e. 250 C d. 200 C c. 150 C b. 100 C a. ST01 TiS 2 TiO Θ (º) 450 TiS 2
47 TiO ST C 200 C 250 C C 300 C %R C C C Wave length, nm
48 TiO 2 (a) TiO 2 (a) 100 TiO 2 (a) 150 TiO 2 (a) 200 TiO 2 (a) 250 TiO 2 (a) 300 TiO 2 (a) 350 TiO 2 (a) TiO 2 (a) TiS TiO 2 (a) TiS
49 TiO 2 ST01 500
50 SrTiO 3 n
51 Introduction SrTiO 3 Band gap energy = 3.3 ev Active for photodecomposition of the water by UV light irradiation Sr 1.15 TiS 3 Band gap energy = 0.3 ev Absorb the visible light Dissolve in water by irradiation of light Partially sulfurized SrTiO 3 : It could be chemically stable and enhance the photocatalytic activity of SrTiO 3.
52 Materials SrTiO 3 nanoparticles (SR-01) were prepared by sol-gel method. Ti(OPri) 4 were mixed with tri-ethanol amine (0.05:0.1) and maintained for 24 hours in argon atmosphere. De-carbonated water were added to complete 100 ml (stock solution). 5,3 g of Sr(OH) 2 8H 2 O were dissolved in 10ml H 2 O and mixed with 10 ml of stock solution. The formed gel was heated in autoclave at 250 for 3hrs. The powders were obtained after rinsing with water ultrasonically and centrifugal separation. The powders were dried at R.T. for 1d. Commercial SrTiO 3 were obtained from Wako Pure Chemical Co. Ltd. (SR-02) and High Purity Chemicals Co. Ltd. (SR-03).
53 TEM microphotographs of initial materials 50 nm 200 nm 200 nm SR-01 SR-02 SR-03 The particle size of SR-01 is smaller than 40 nm.
54 A cubic SrTiO 3 phase was founded in initial materials. XRD patterns for initial materials a. SR-01 Intensity/a.u. b. SR-02 c. SR-03 SrTiO 3 (Cub., JCPDS ) θ/degree
55 TG curves of initial materials in Ar atmosphere Weight change/% SR-01 SR-02 Samples: SrTiO 3 Heating rate: 5 ºC/min, in argon atmosphere Temperature/ºC SR Carbonates SR-01 only contents 3.9 % of adsorbed water and 2.83 % of OH groups.
56 TG curves of sulfurization in CS 2 30 Gas flow: N2 50 ml/min CS2 5mL/min Heating Rate: 1 C/min Weight change/% SR-01 starts to sulfurize at 280 ºC -1.9 SrTiS 3 Sr 1.05 TiS 3 Sr 1.15 TiS 3 SR-01 SR SR Temperature/ C 17.1 SR-02 and SR-03 start to sulfurize at 550 ºC SR-01 is sulfurized at lower temperatures than SR-02 and SR-03
57 XRD patterns for Sulfurized SR-02 d C Intensity/a.u. c. 750 C b. 650 C a. As-received SR-02 Sr 1.15 TiS 3 (JCPDS ) SrTiO 3 (Cub., JCPDS ) Θ/degree A hexagonal Sr 1.15 TiS 3 phase was founded as final product in SR-02.
58 XRD patterns for sulfurized SR-03 d C Intensity/a.u. c. 750 C b. 650 C a. As-received SR-03 Sr 1.15 TiS 3 (JCPDS ) SrTiO 3 (Cub., JCPDS ) /degree A hexagonal Sr 1.15 TiS 3 phase was also founded as final product in SR-03.
59 XRD patterns for Sulfurized SR-01 e C d. 750 C Intensity/a.u. c. 650 C b. 550 C a. As-prepared SR-01 Sr 1.15 TiS 3 (Hex., JCPDS ) SrTiO 3 (Cub., JCPDS ) Θ/degree However, a hexagonal Sr 1.15 TiS 3-x phase was founded in SR-01.
60 Sulfurization SR-02 and SR-03 Between 550 and 950 ºC C the sulfurization of SrTiO 3 is carried on SrTiO 3 Sr 1.15 TiS 3 Sr 1.15 SR-01 At temperature below 180 ºC C is produced the desorption of water. Between 180 and 280ºC, the adsorption of CS 2 on SrTiO 3 surface occurs. Between 280 and 850ºC, SrTiO 3 is sulfurized. At higher temperatures, the decomposition of obtained Sr 1.15 TiS 3 is produced. SrTiO 3 Sr 1.15 TiS 3 Sr 1.15 TiS Sr 1.15 Sr 1.15 TiS 3-x
61 Conclusions SrTiO 3 nanoparticles was sulfurized at low temperatures in comparison with commercial powders. The sulfurization behavior of SR-01 could be summarized as follows: Evaporation of water, adsorption of CS 2, sulfurization of SrTiO 3 and decomposition of Sr 1.15 TiS 3.
62 BaTiO 3
63 Introduction BaTiO 3 is used as Dielectric material. Supported catalyst for CO 2 reforming and partial oxidation of CH 4 at higher temperatures. Catalyst for processing of hazard pollutants by non-thermal plasma reactors. However, BaTiO 3 is unknown photocatalyst due to High band energy of 3.27 ev (378 nm). Photoactivity in UV spectra.
64 Preparation of BaTiO g TIPO* g TEA* De-carbonated water *TIPO: titanium tetra-iso-propoxide TEA: tri-ethanol-amine Solution Argon atm. Overnight Stock Solution TIPO:TEA 0.05: ml stock solution g Ba(OH) 2 10 ml de-carbonated water Stirring 30 min Gel Teflon autoclave Heating: 3 hrs T: 250 C BaTiO 3 Cleaning Centrifugation Drying at r. t. BaTiO 3
65 Partial sulfurization of BaTiO 3 BaTiO 3 Sulfurization Purification Evacuation N 2 refilling CS 2 /N 2 gas Flow rate: 5/50 ml/min Heating : 3 ºC/min T: ºC Toluene 100 ºC Vacuum Partially Sulfurized BaTiO 3 Thermocouple Electric furnace Quartz tube Gas inlet Gas outlet Quartz boat Sample:1 g BaTiO 3 Schematic drawing of reaction tube
66 Characteristics of ultrafine BaTiO 3 particles 200 nm TEM microphotograph of BaTiO 3 BaTiO 3 particles were obtained by using TIPO and TEA as precursors. Characteristics: Phase: Cubic Particle size: 95 nm Lattice parameter: Å Specific area:12.42 mg/m 2 H 2 O (%): 1.6
67 Sulfurization behavior of BaTiO BaTiS 3 Weight change/% Starting temperature of sulfurization 19.2 Gas flow: N 2 50 ml/min CS 2 5mL/min Heating Rate: 1 C/min Temperature/ C BaTiO 3 reacts slowly with CS 2 at around 400 ºC forming BaTiS 3. Reaction: BaTiO CS 2 BaTiS CO 2
68 XRD patterns for partially sulfurized BaTiO C Sulfide Sulfide 400 C Intensity/a.u. 300 C 200 C 100 C Initial Material BaTiO 3 (cub., JCPDS ) BaTiS 3 (hex., JCPDS ) Θ/degree Peaks corresponding to BaTiS 3 appears only when BaTiO 3 is sulfurized at 500ºC
69 Variation of lattice parameter 4.02 Lattice parameter a/ Å Lattice parameter : Å JCPDS Cubic BaTiO 3 Formation of hex. BaTiS Temperature/ºC Lattice parameter increases with increasing the sulfurization temperature. However, it decreases with formation of sulfide.
70 XPS of S2p 3/2 for partially sulfurized BaTiO 3 Sulfate Sulfide Intensity/a.u. 500 ºC 400 ºC 300 ºC 200 ºC Sulfite Sulfur 100 ºC Binding energy/ev From 200 and 500 ºC, a peak assigned to sulfide appears at around and ev whose intensity increases with the temperature.
71 UV-Vis Vis spectra for partially sulfurized BaTiO 3 Band gap of BaTiO 3 : 100 BaTiO nm º C R /% ºC 300 ºC 400 ºC ºC BaTiS Wave length/nm Increasing the sulfurization temperature, the absorption of visible light increases in sulfurized BaTiO 3 samples.
72 Conclusions Partially sulfurized BaTiO 3 absorbed higher visible light than initial BaTiO 3 sample. The absorption increased with increasing the temperature of sulfurization. Since sulfide as BaTiS 3 is formed above 400 ºC, it is suggested that absorption of visible light is caused by replacement of sulfur by oxygen in the initial BaTiO 3 structure.
73
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206 : 316-8511 4-12 - 1 Laser Sintering Characteristics of Silver Nanoparticle Paste for Electronics Packaging YAMASAKI Kazuhiko, MAEKAWA Katsuhiro (Received January 10, 2012) Ibaraki University, Faculty
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Authors' Abstract It in known that the method of feeding powder into split cell affects the adhesion forces of powder beds, especially in fine particle powders. But the effect of the agglomeration phenomenon
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JNC TN8430 2003-002 ) 7.878 15.138 47.155 exp( 2 ρ b ρ b κ + = κ [m 2 ] b ρ [Mg/m 3 ] * ** JNC TN8430 2003-002 March2003 Hydraulic characteristics of Buffer Material-II The influence which saline water
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CO2 Laser Treatment of Tinea Pedis Masahiro UEDA:,' Kiyotaka KITAMURA** and Yukihiro GOKOH*** Table I Specifications 1. Kind of Laser 2. Wavelength of Lasers. Power of Laser. Radiation Mode. Pulse Duration.
平成26年度 化学物質分析法開発報告書
2,2-2,2 -Iminodiethanol Diethanol amine CAS 111-42-2 C 4 H 11 NO 2 105.1356-105.0790-28 C 1) 1.0881 g/cm 3 1)
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*1 *2 *1 JIS A X TEM 950 TEM JIS Development and Research of the Equipment for Conversion to Harmless Substances and Recycle of Asbe
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Friction welding of ADC 12 aluminum alloy diecastings Kazuyoshi KATO* and Hiroshi TOKISUE* Both squeeze and gravity castings of ADC 12 aluminum alloy were friction-welded, using a brake type welding machine.
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Preparation of Functional Nonwoven Fabric KAMIKO Utilizing Wasted Tea Leaves Tetsuya Takahashi 1, Wakako Kasai 2, and Tetsuo Kondo 2 1 Faculty of Education, Shimane University, 1060, Nishikawatsu-cho,
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技術研究報告第２６号
1) 2) 3) 250Hz 500Hz RESEARCH ON THE PHYSICAL VOLUME OF THE DYNAMIC VIBRATION RESPONSE AND THE REDUCTION OF THE FLOOR IMPACT SOUND LEVEL IN FLOORS OF RESIDENTIAL HOUSING Hideo WATANABE *1 This study was
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Fig. ph Si-O-Na H O Si- Na OH Si-O-Si OH Si-O Si-OH Si-O-Si Si-O Si-O Si-OH Si-OH Si-O-Si H O 6
NMR ESR NMR 5 Fig. ph Si-O-Na H O Si- Na OH Si-O-Si OH Si-O Si-OH Si-O-Si Si-O Si-O Si-OH Si-OH Si-O-Si H O 6 Fig. (a) Na O-B -Si Na O-B Si Fig. (b) Na O-CaO-SiO Na O-CaO-B -Si. Na O-. CaO-. Si -. Al O
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Study on Application of the cos a Method to Neutron Stress Measurement Toshihiko SASAKI*3 and Yukio HIROSE Department of Materials Science and Enginee
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rectomy as the subjects of study, urinary steroid hormones were measured, and simultaneously the enzyme work and enzyme pattern related to the steroid metabolism, as proposed by Yoshida of our laboratory,
LAGUNA LAGUNA 10 p Water quality of Lake Kamo, Sado Island, northeast Japan, Katsuaki Kanzo 1, Ni
LAGUNA10 47 56 2003 3 LAGUNA 10 p.47 56 2003 1997 2001 1 2 2 Water quality of Lake Kamo, Sado Island, northeast Japan, 1997 2001 Katsuaki Kanzo 1, Niigata Prefectural Ryotsu High School Science Club, Iwao