nanocomposites prepared by ultrasonic spray … prepared by ultrasonic spray pyrolysis and their...
TRANSCRIPT
![Page 1: Nanocomposites Prepared by Ultrasonic Spray … Prepared by Ultrasonic Spray Pyrolysis and their Applications Rongbo Zheng Southwest Forestry University, China ICMAT 2011 D NANOFORMULATION](https://reader033.vdocuments.us/reader033/viewer/2022042801/5ac2e8c07f8b9aa0518bb111/html5/thumbnails/1.jpg)
Nanocomposites Prepared by Ultrasonic
Spray Pyrolysis and their Applications
Rongbo Zheng
Southwest Forestry University, China
ICMAT 2011 DNANOFORMULATION 2011
![Page 2: Nanocomposites Prepared by Ultrasonic Spray … Prepared by Ultrasonic Spray Pyrolysis and their Applications Rongbo Zheng Southwest Forestry University, China ICMAT 2011 D NANOFORMULATION](https://reader033.vdocuments.us/reader033/viewer/2022042801/5ac2e8c07f8b9aa0518bb111/html5/thumbnails/2.jpg)
1. Introduction
http://www.scs.uiuc.edu/suslick/suslickresearchdescription
•One step
•Rapidly
•Continuous
•Scalable
![Page 3: Nanocomposites Prepared by Ultrasonic Spray … Prepared by Ultrasonic Spray Pyrolysis and their Applications Rongbo Zheng Southwest Forestry University, China ICMAT 2011 D NANOFORMULATION](https://reader033.vdocuments.us/reader033/viewer/2022042801/5ac2e8c07f8b9aa0518bb111/html5/thumbnails/3.jpg)
K. S. Suslick, J. Am. Chem. Soc., 2006, 128, 12642.
Porous Carbon
Precursor:
Alkali metal chloroacetate
or dichloroacetate
![Page 4: Nanocomposites Prepared by Ultrasonic Spray … Prepared by Ultrasonic Spray Pyrolysis and their Applications Rongbo Zheng Southwest Forestry University, China ICMAT 2011 D NANOFORMULATION](https://reader033.vdocuments.us/reader033/viewer/2022042801/5ac2e8c07f8b9aa0518bb111/html5/thumbnails/4.jpg)
Magnetic luminescent mesostructured silica Microspheres
J. F. Wang, Adv. Funct. Mater., 2008,18, 2956.
![Page 5: Nanocomposites Prepared by Ultrasonic Spray … Prepared by Ultrasonic Spray Pyrolysis and their Applications Rongbo Zheng Southwest Forestry University, China ICMAT 2011 D NANOFORMULATION](https://reader033.vdocuments.us/reader033/viewer/2022042801/5ac2e8c07f8b9aa0518bb111/html5/thumbnails/5.jpg)
2. Nanocomposites prepared by USP
USP
Different carbon precursor
Glucose
Citrate acid
Sodium citrate
Li-ion battery
ElectrophoreticDisplays
Schematic of the ultrasonic spray pyrolysis (USP) synthesis of nanocomposites
![Page 6: Nanocomposites Prepared by Ultrasonic Spray … Prepared by Ultrasonic Spray Pyrolysis and their Applications Rongbo Zheng Southwest Forestry University, China ICMAT 2011 D NANOFORMULATION](https://reader033.vdocuments.us/reader033/viewer/2022042801/5ac2e8c07f8b9aa0518bb111/html5/thumbnails/6.jpg)
2.1 Rattle-type carbon hollow spheres and their application in Li-ion battery
� Definition: Rattle-type hollow spheres (denoted as A@B)
refer to hollow shells with a solid particle core and interstitial
hollow space in between.
![Page 7: Nanocomposites Prepared by Ultrasonic Spray … Prepared by Ultrasonic Spray Pyrolysis and their Applications Rongbo Zheng Southwest Forestry University, China ICMAT 2011 D NANOFORMULATION](https://reader033.vdocuments.us/reader033/viewer/2022042801/5ac2e8c07f8b9aa0518bb111/html5/thumbnails/7.jpg)
� Conventional route to A@B
I Inside-to-outside routeII Outside-to-inside route
![Page 8: Nanocomposites Prepared by Ultrasonic Spray … Prepared by Ultrasonic Spray Pyrolysis and their Applications Rongbo Zheng Southwest Forestry University, China ICMAT 2011 D NANOFORMULATION](https://reader033.vdocuments.us/reader033/viewer/2022042801/5ac2e8c07f8b9aa0518bb111/html5/thumbnails/8.jpg)
Sn@Carbon
SEM and TEM images of Sn@carbon obtained via USP of aqueous solutions containing SnCl4 and sodium citrate
R. B. Zheng, J. Phys. Chem. C, 2009, 113, 11065
![Page 9: Nanocomposites Prepared by Ultrasonic Spray … Prepared by Ultrasonic Spray Pyrolysis and their Applications Rongbo Zheng Southwest Forestry University, China ICMAT 2011 D NANOFORMULATION](https://reader033.vdocuments.us/reader033/viewer/2022042801/5ac2e8c07f8b9aa0518bb111/html5/thumbnails/9.jpg)
Formation mechanism
SEM images of carbon hollow spheres obtained by USP of sodium citrate aqueous solutions
![Page 10: Nanocomposites Prepared by Ultrasonic Spray … Prepared by Ultrasonic Spray Pyrolysis and their Applications Rongbo Zheng Southwest Forestry University, China ICMAT 2011 D NANOFORMULATION](https://reader033.vdocuments.us/reader033/viewer/2022042801/5ac2e8c07f8b9aa0518bb111/html5/thumbnails/10.jpg)
TEM images of Sn@carbon solids (A) collected withoutwater at 700 °C and (B) collected with water at 500 °C.
![Page 11: Nanocomposites Prepared by Ultrasonic Spray … Prepared by Ultrasonic Spray Pyrolysis and their Applications Rongbo Zheng Southwest Forestry University, China ICMAT 2011 D NANOFORMULATION](https://reader033.vdocuments.us/reader033/viewer/2022042801/5ac2e8c07f8b9aa0518bb111/html5/thumbnails/11.jpg)
Illustration of the M@carbon obtained via USP of aqueous solutions containing metal salts and sodium citrate
(1): Sn NPs; capillary force; sodium citrate outer shell(2): Carbonization(3): Removing of water-soluble byproduct
![Page 12: Nanocomposites Prepared by Ultrasonic Spray … Prepared by Ultrasonic Spray Pyrolysis and their Applications Rongbo Zheng Southwest Forestry University, China ICMAT 2011 D NANOFORMULATION](https://reader033.vdocuments.us/reader033/viewer/2022042801/5ac2e8c07f8b9aa0518bb111/html5/thumbnails/12.jpg)
Other M@Carbon by USP
20 30 40 50 60 70 80
B
311
22020
0
111
22011
1
200
Inte
nsity
(a.u
.)
2θ (degree)
A
XRD and TEM of (A) Pt@carbon and (B) Ag@Carbon obtained via USP of aqueous solutions containing metal salts and sodium citrate
![Page 13: Nanocomposites Prepared by Ultrasonic Spray … Prepared by Ultrasonic Spray Pyrolysis and their Applications Rongbo Zheng Southwest Forestry University, China ICMAT 2011 D NANOFORMULATION](https://reader033.vdocuments.us/reader033/viewer/2022042801/5ac2e8c07f8b9aa0518bb111/html5/thumbnails/13.jpg)
The applications of Sn@C in Li-ion battery
0 20 40 60 80 1000
300
600
900
1200
1500 discharge charge
0.55mA/cm2
0.25mA/cm20.15mA/cm2
Cap
acity
(mA
h/g)
Cycle number
A
The cycling performance in the 0 mV-3 V (vs. Li+/Li) voltage window at different rate of Sn@carbon (46 wt % Sn).
![Page 14: Nanocomposites Prepared by Ultrasonic Spray … Prepared by Ultrasonic Spray Pyrolysis and their Applications Rongbo Zheng Southwest Forestry University, China ICMAT 2011 D NANOFORMULATION](https://reader033.vdocuments.us/reader033/viewer/2022042801/5ac2e8c07f8b9aa0518bb111/html5/thumbnails/14.jpg)
2.2 Magnetic carbon hollow spheres
Reactant: aqueous solutions containing FeCl2 and citrate acid
Iron citrate
Citrate acid solution
(1) (2) (3)
Fe3O4 nanoparticles
Carbon
Formation mechanism
![Page 15: Nanocomposites Prepared by Ultrasonic Spray … Prepared by Ultrasonic Spray Pyrolysis and their Applications Rongbo Zheng Southwest Forestry University, China ICMAT 2011 D NANOFORMULATION](https://reader033.vdocuments.us/reader033/viewer/2022042801/5ac2e8c07f8b9aa0518bb111/html5/thumbnails/15.jpg)
20 30 40 50 60 70 80
533
440
511
42240
0
311
Inte
nsity
(a.u
.)
2θ/degree
220
XRD patterns of Fe3O4-C magnetic hollow spheres obtained by USP of aqueous solutions containing FeCl2 and citrate acid.
Face-centered cubic Fe3O4
(JCPDS file No. 48–1487) or γγγγ-Fe2O3
![Page 16: Nanocomposites Prepared by Ultrasonic Spray … Prepared by Ultrasonic Spray Pyrolysis and their Applications Rongbo Zheng Southwest Forestry University, China ICMAT 2011 D NANOFORMULATION](https://reader033.vdocuments.us/reader033/viewer/2022042801/5ac2e8c07f8b9aa0518bb111/html5/thumbnails/16.jpg)
0 200 400 600 800 100070
75
80
85
90
95
100
TG (%
)
Temperature (oC)
TGA of Fe3O4-C magnetic hollow spheres
•Increasing in mass between 180 and 280 °C
•Fe3O4 is oxidized to form Fe2O3
![Page 17: Nanocomposites Prepared by Ultrasonic Spray … Prepared by Ultrasonic Spray Pyrolysis and their Applications Rongbo Zheng Southwest Forestry University, China ICMAT 2011 D NANOFORMULATION](https://reader033.vdocuments.us/reader033/viewer/2022042801/5ac2e8c07f8b9aa0518bb111/html5/thumbnails/17.jpg)
TEM images of Fe3O4-C magnetic hollow spheres obtained by USP of aqueous solutions containing FeCl2 and citrate acid
R. B. Zheng, Eur. J. Inorg. Chem., 2009, 20, 3003
![Page 18: Nanocomposites Prepared by Ultrasonic Spray … Prepared by Ultrasonic Spray Pyrolysis and their Applications Rongbo Zheng Southwest Forestry University, China ICMAT 2011 D NANOFORMULATION](https://reader033.vdocuments.us/reader033/viewer/2022042801/5ac2e8c07f8b9aa0518bb111/html5/thumbnails/18.jpg)
TEM images of porous hollow carbon spheres obtained by acid treatment of Fe3O4-C magnetic hollow spheres in concentrated HCl (12 M) for 12 h.
Porous hollow carbon spheres
![Page 19: Nanocomposites Prepared by Ultrasonic Spray … Prepared by Ultrasonic Spray Pyrolysis and their Applications Rongbo Zheng Southwest Forestry University, China ICMAT 2011 D NANOFORMULATION](https://reader033.vdocuments.us/reader033/viewer/2022042801/5ac2e8c07f8b9aa0518bb111/html5/thumbnails/19.jpg)
Acid-durability
-20000 -10000 0 10000 20000-40
-30
-20
-10
0
10
20
30
40
M (e
mu/
g)
H (Oe)
A
Ms: 35.9 emu/g
Mr: 2.1 emu/g
Hc: 34 Oe
(A) The M–H hysteresis loop and (B) TEM image of MCHMsafter acid treatment (pH = 1) at room temperature for 10 d.
![Page 20: Nanocomposites Prepared by Ultrasonic Spray … Prepared by Ultrasonic Spray Pyrolysis and their Applications Rongbo Zheng Southwest Forestry University, China ICMAT 2011 D NANOFORMULATION](https://reader033.vdocuments.us/reader033/viewer/2022042801/5ac2e8c07f8b9aa0518bb111/html5/thumbnails/20.jpg)
Good dispersibility in various solvents
4000 3500 3000 2500 2000 1500 1000 500
Tran
smitt
ance
(a.u
.)
Wavenumber (cm-1)
O-H
C-H
C=C
Fe3O4
A
FTIR spectrum of sample HC 2; (B): photographs of sample HC 2 suspensions in methanol, ethanol and tetrachloroethylene.
![Page 21: Nanocomposites Prepared by Ultrasonic Spray … Prepared by Ultrasonic Spray Pyrolysis and their Applications Rongbo Zheng Southwest Forestry University, China ICMAT 2011 D NANOFORMULATION](https://reader033.vdocuments.us/reader033/viewer/2022042801/5ac2e8c07f8b9aa0518bb111/html5/thumbnails/21.jpg)
2.3 Carbon–Iron Oxide Microspheres’Black Pigments and their application in Electrophoretic Displays
� Carbon black: density, 0.8 g/cm3
� Tetrachloroethylene:density, 1.6 g/cm3
B. Comiskey, et al., Nature, 1998, 394, 253
![Page 22: Nanocomposites Prepared by Ultrasonic Spray … Prepared by Ultrasonic Spray Pyrolysis and their Applications Rongbo Zheng Southwest Forestry University, China ICMAT 2011 D NANOFORMULATION](https://reader033.vdocuments.us/reader033/viewer/2022042801/5ac2e8c07f8b9aa0518bb111/html5/thumbnails/22.jpg)
�����
�������GlucoseFeCl2
USP
Doping-eroding route
![Page 23: Nanocomposites Prepared by Ultrasonic Spray … Prepared by Ultrasonic Spray Pyrolysis and their Applications Rongbo Zheng Southwest Forestry University, China ICMAT 2011 D NANOFORMULATION](https://reader033.vdocuments.us/reader033/viewer/2022042801/5ac2e8c07f8b9aa0518bb111/html5/thumbnails/23.jpg)
4000 3000 2000 1000 0
Fe2O
3
Tran
smitt
ance
(a.u
.)
�Wavemumber (cm-1)
O-H
C-H C=C Fe3O
4
FT-IR spectrum of carbon-iron oxide
2.2 g/cm3, 1.7 g/cm3, 1.5 g/cm3
Carbon-iron oxide with (from left to right 0, 1, 12 h) etching time aredispersed in tetrachloroethylene.
X. W. Meng, R.B. Zheng, et al, Nanoscale Res Lett 2010, 5,1664.
![Page 24: Nanocomposites Prepared by Ultrasonic Spray … Prepared by Ultrasonic Spray Pyrolysis and their Applications Rongbo Zheng Southwest Forestry University, China ICMAT 2011 D NANOFORMULATION](https://reader033.vdocuments.us/reader033/viewer/2022042801/5ac2e8c07f8b9aa0518bb111/html5/thumbnails/24.jpg)
Black-white e-paper
![Page 25: Nanocomposites Prepared by Ultrasonic Spray … Prepared by Ultrasonic Spray Pyrolysis and their Applications Rongbo Zheng Southwest Forestry University, China ICMAT 2011 D NANOFORMULATION](https://reader033.vdocuments.us/reader033/viewer/2022042801/5ac2e8c07f8b9aa0518bb111/html5/thumbnails/25.jpg)
2.4 Silver porous hollow spheres
GlucoseAgNO3
USP
SEM of SPHS prepared via USP of aqueous solutions containing glucose and AgNO3
Glucose worked as reducing agent and pore-forming directing agent
R.B. Zheng, Applied surface sci., 2011, 257, 2367
![Page 26: Nanocomposites Prepared by Ultrasonic Spray … Prepared by Ultrasonic Spray Pyrolysis and their Applications Rongbo Zheng Southwest Forestry University, China ICMAT 2011 D NANOFORMULATION](https://reader033.vdocuments.us/reader033/viewer/2022042801/5ac2e8c07f8b9aa0518bb111/html5/thumbnails/26.jpg)
Vis-NIR spectrum of SPHS (A) and silver solid spheres (B) fabricated via USP.
400 600 800 1000 1200
Abs
optio
n (a
.u.)
Wavelength (nm)
A
B
480 nm
![Page 27: Nanocomposites Prepared by Ultrasonic Spray … Prepared by Ultrasonic Spray Pyrolysis and their Applications Rongbo Zheng Southwest Forestry University, China ICMAT 2011 D NANOFORMULATION](https://reader033.vdocuments.us/reader033/viewer/2022042801/5ac2e8c07f8b9aa0518bb111/html5/thumbnails/27.jpg)
Thanks for your attention!!!