Nano-particle prepared from sol-gel method 1. TiO2 Polyethylene glycol Titanium...

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Nano-particle prepared from sol-gel method 1. TiO2 Polyethylene glycol Titanium tetra-iso-propoxide diethanolamine Solution I with Polyethylene glycol Solution II without Polyethylene glycol SiO 2 substrate

Transcript of Nano-particle prepared from sol-gel method 1. TiO2 Polyethylene glycol Titanium...

Page 1: Nano-particle prepared from sol-gel method 1. TiO2 Polyethylene glycol Titanium tetra-iso-propoxidediethanolamine Solution I with Polyethylene glycol Solution.

Nano-particle prepared from sol-gel method1. TiO2

Polyethylene glycol

Titanium tetra-iso-propoxide diethanolamine

Solution I with Polyethylene glycolSolution II without Polyethylene glycol

SiO2 substrate

Page 2: Nano-particle prepared from sol-gel method 1. TiO2 Polyethylene glycol Titanium tetra-iso-propoxidediethanolamine Solution I with Polyethylene glycol Solution.

Solution IParticle size 10~15nm.Space with a width of several nanometers existed between the crystallites.Anatase phase transforms to rutile above 650oC

Solution IIDense structure,Particle size ~15nm and connected each other.Particle size increases to ~50nm heated above 650oC and the crystallites had connected hard each other.

Page 3: Nano-particle prepared from sol-gel method 1. TiO2 Polyethylene glycol Titanium tetra-iso-propoxidediethanolamine Solution I with Polyethylene glycol Solution.

amorphous

Anatase powder

The relatively high intensities indicates that a significant amount of the crystallites arranged with c axis perpendicular to the surface

Page 4: Nano-particle prepared from sol-gel method 1. TiO2 Polyethylene glycol Titanium tetra-iso-propoxidediethanolamine Solution I with Polyethylene glycol Solution.

2. Au-SiO2

TEOS+C2H5OH HAuCl4·4H2O+H2

O

+C2H5OH+HCl

mixing and stirring vigorously at room temp for 5mins, then kept tightly in container at 40oC for

various of time prior to dip-coating

TEOS : H2O :C2H5OH: Au =1:2~10:0.4:2:0.028

r= H2O/TEOS

Dip-coated film is transparent and almost colorless, film is heated at 500oC for 10mins, the film exhibits red to purple color

Page 5: Nano-particle prepared from sol-gel method 1. TiO2 Polyethylene glycol Titanium tetra-iso-propoxidediethanolamine Solution I with Polyethylene glycol Solution.
Page 6: Nano-particle prepared from sol-gel method 1. TiO2 Polyethylene glycol Titanium tetra-iso-propoxidediethanolamine Solution I with Polyethylene glycol Solution.
Page 7: Nano-particle prepared from sol-gel method 1. TiO2 Polyethylene glycol Titanium tetra-iso-propoxidediethanolamine Solution I with Polyethylene glycol Solution.
Page 8: Nano-particle prepared from sol-gel method 1. TiO2 Polyethylene glycol Titanium tetra-iso-propoxidediethanolamine Solution I with Polyethylene glycol Solution.

MAE: monoethanolamine NHC2H4OH

227nm and 314nm are assigned to 1Ag1g→1E1u and 1Ag1g→1E2u.The changes of the intensities of the peaks suggest the change in the coordination state in the gold complex

Page 9: Nano-particle prepared from sol-gel method 1. TiO2 Polyethylene glycol Titanium tetra-iso-propoxidediethanolamine Solution I with Polyethylene glycol Solution.

Effects of the exposure of the gel film to MEA vapor prior to heat-treatment1. Decrease the size of gold particle to 5nm.2. Increase the amount of trapped gold particles in silica matrix.Possible reasons1. The pore size of silica matrix is smaller.2. Precipitation of gold hydroxide, smaller gold hydroxide particles are fixed in the gel.3. Change the coordination state of Au+3.

Page 10: Nano-particle prepared from sol-gel method 1. TiO2 Polyethylene glycol Titanium tetra-iso-propoxidediethanolamine Solution I with Polyethylene glycol Solution.

Journal ofCrystal Growth 144 (1994) 141—149

TEOS, C2H5OH, H2O,HCl in molar 1:1:1:0.27

C2H5OH, NH4OHin molar 4: 1.25 : 0.005

hydrated cadmium acetate C4H6CdO4·2H2O CH3OH0.05: 1

Dried in ovenDried gelGel Heat treatment

Heat treated in H2S at 200oC for 2hrs

3. CdS in SiO2 gel

Page 11: Nano-particle prepared from sol-gel method 1. TiO2 Polyethylene glycol Titanium tetra-iso-propoxidediethanolamine Solution I with Polyethylene glycol Solution.

Journal of solid state chemistry 118, 1-5 (1995)

Dimethyl sulfoxide (CH3)2SO

Heat treated to various temp

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Photonics and Nanostructures – Fundamentals and Applications 5 (2007) 156–163

Page 13: Nano-particle prepared from sol-gel method 1. TiO2 Polyethylene glycol Titanium tetra-iso-propoxidediethanolamine Solution I with Polyethylene glycol Solution.

CdS01 TEOS:Cd=1:0.5Particle size 1.66nmCdS02 TEOS:Cd=1:1Particle size 2.99nmAbsorption peak for CdS bulk at 520nm

Page 14: Nano-particle prepared from sol-gel method 1. TiO2 Polyethylene glycol Titanium tetra-iso-propoxidediethanolamine Solution I with Polyethylene glycol Solution.

(Ti(OCH(CH3)2)4(5ml) +C2H5OH(25ml) stirred at 0oC

Add C2H5OH(25ml)+ H2O(0.5ml) +0.1MHCl(0.5ml) at 15oC

After 60 s at 15oC the resulting mixture turned milky white (sol formation).

alumina template membrane was immediately dipped into this solution for an immersion time that was varied between 5 and 60 s. dried in air for 30 min at room temperature.

placed in a tube furnace (in air), and the temperature was ramped (50 °C h-1) to 400 °C. The membranes were heated at this temperature for 6 h, and the temperature was ramped back down (30 °C h-1) to room temperature.

TiO2 tubules and fibrils

Page 15: Nano-particle prepared from sol-gel method 1. TiO2 Polyethylene glycol Titanium tetra-iso-propoxidediethanolamine Solution I with Polyethylene glycol Solution.

氧化鋁濾膜 AnodiscTM13(0.2m, 膜厚 50 m)

正面 反面 剖面

Page 16: Nano-particle prepared from sol-gel method 1. TiO2 Polyethylene glycol Titanium tetra-iso-propoxidediethanolamine Solution I with Polyethylene glycol Solution.

Electron Microscopy. SEM images of the 200 nm diameter tubules and fibrils wereobtained as follows: One surface layer was removed, and the membrane was glued to apiece of paper towel. The membrane was glued with the polished face up. The resulting composite was immersed into 6 M aqueous NaOH for 10 min in order to dissolve thealumina.

When the sol was 5 °C, thin-walled tubules were obtained even at long immersion times (1 min). In contrast, when the sol was maintained at 20 °C, solid TiO2 fibrils were obtained even after very brief (5 s) immersion times.

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Bundles of the TiO2 nanostructures were observed. The bundle sizes observedranged from as small as 2-4 fibrils to as large as 10 or more fibrils. The main feature in figure that runs diagonally across the image consists of two bundles of fibrils, one on the right edge of the main feature and one on the left edge. In this case thebundles consist of approximately 3-4 fibrils. A second set of two bundles is observed below this main feature; this second set of bundles also proceeds diagonally across the image but at a smaller angle.

TEM image for TiO2 Fibrils Prepared in the membrane with 22 nm diameter pores. It shows a bundle of 15 nm diameter TiO2 fibrils.

Page 18: Nano-particle prepared from sol-gel method 1. TiO2 Polyethylene glycol Titanium tetra-iso-propoxidediethanolamine Solution I with Polyethylene glycol Solution.

To 20 mL of ethanol was added 0.35 g of zinc acetate, and the resulting mixture was boiled until a clear solution was obtained (ca. 30 min). The volume was returned to 20 mL with ethanol, and 0.06 g of LiOH·H2O was added. The resulting solution was ultrasonicated until a white suspension was obtained (ca. 1 h). The alumina membranewas immersed into this sol for 1 min, removed, and allowed to dry in air at room temperature for 30 min. The membrane was then heated in air at 120 °C for 6 h.

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(a) Cross-sectional FE-SEM image of AgI/Ag embedded inside the AAO membrane.( b) FE-SEM top-view image.

Nano-battery

AgI-Ag nanowires

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The ionic conductivity of single AgI/Ag was estimated to be on theorder of 1.5–8.0 × 10–3 (-cm)–1 Compared with that of room-temperature bulk polycrystallineAgI (ca. 10–5–10–6 (-cm)–1 an enhancement by two to three orders of magnitude was demonstrated. This enhanced ionic conductivity may be attributed to interfacial defects and mesoscopic multiphase effects as a result of stacking-fault arrangements.

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