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Effects of thermal treatment and fluoride ion doping on surface and catalytic properties of NiO–ZrO2 catalysts Cover

Effects of thermal treatment and fluoride ion doping on surface and catalytic properties of NiO–ZrO2 catalysts

Open Access
|Apr 2016

Figures & Tables

Fig. 1

DTA curves of Z, ZN5, ZN10, ZN15 and ZN25 gels.

Fig. 2

DTA curves of Z, ZF, ZN15 and ZN15F gels.

Fig. 3

XRD patterns of ZrO2 and NiO–ZrO2 samples calcined at 550 °C.

Fig. 4

XRD patterns of ZrO2 sample calcined at different temperatures.

Fig. 5

XRD patterns of ZN15 sample calcined at different temperatures

Table 1

Crystal structure and crystal size of undoped catalysts.

CatalystPhases detected*Major phase [%]Crystal size (D) of major phase [nm]Degree of crystallinity [a.u.]**Es [kJ_mol−1]
M(2θ = 28.2)T(2θ = 30.3)
ZIT100(T)29.5225
ZIIT100(T)38.026813.8
ZIIIT100 (T)44.5380
ZIVM+T83.8(M)49.5130300
ZN5IT100(T)19.5210
ZN10IT100(T)23.4190
ZN15IT100(T)29.5145
ZN25IT100(T)39.536
ZN15IT100(T)29.5145
ZN15IIT100(T)21.428224.89
ZN15IIIM+T+C64.1(M)31.0178195
ZN15IVM+T+C91.3(M)40.548343

* M: monoclinic ZrO2, T: tetragonal ZrO2 and C: cubic NiO.

** The peak height of the major line of each phase was taken as a measure of the degree of crystallinity of the ZrO2.

Table 2

Crystal structure and crystal size of the samples doped with fluoride ions.

CatalystPhases detected*Major phase [%]Crystal size [D] of major phase [nm]Degree of crystallinity [a.u.]**Es [kJ_mol−1]
M(2θ = 28.2)T(2 θ = 30.3)
ZFIT100 (T)30.0280
ZFIIT100 (T)36.826513.21
ZFIIIT100 (T)42.0290
ZFIVM+T86.2(M)48.5110210
ZN15FIT100 (T)18.0130
ZN15FIIT100 (T)22.021223.16
ZN15FIIIM+T+C73.6(M)30.0140118
ZN15FIVM+T+C85.5(M)41.024160

* M: monoclinic ZrO2, T: tetragonal ZrO2 and C: cubic NiO.

** The peak height of the major line of each phase was taken as a measure of the degree of crystallinity of the ZrO2.

Fig. 6

Nitrogen adsorption-desorption isotherms of some selected samples.

Table 3

Surface characteristics, acidic and catalytic properties of the investigated catalysts.

SampleSBET [m2·g−1]St [m2·g−1]Vp [ml·g−1]¯r [A˚ ]Ei [mV]N (acid sites g−1) × 10−20DHD [%]DHG [%]
ZI76.0370.50.2154.4410.7237.30
ZII58.058.20.1856.7350.68028.80
ZIII50.628.40.1372.2300.59018.40
ZIV1811.80.0996.0130.51810.40
ZN5I98.6100.20.3496.08520.57820.414.6
ZN10I127.6130.40.3871.37620.53019.220.4
ZN15I138.0144.00.34253.46700.54216.528.6
ZN25I100.098.00.15931.0780.43010.638.0
ZN15I138.0144.00.34253.46700.54216.528.6
ZN15II80.078.60.2659.8710.54216.027.8
ZN15III36.034.40.1868.53560.4526.69.6
ZN15IV20.418.00.11472.0440.3804.06.0
ZFI70.669.50.20658.3810.99468.00
ZFII50.449.00.18975.0720.7847.00
ZFIII27.831.00.1490.3630.69332.30
ZFIV12.420.40.102113660.53014.00
ZN15FI118.0117.60.30651.8980.87954.012.0
Fig. 7

Arrhenius plots of activation energy of sintering process for tested samples.

Fig. 8

DHD of isopropanol as a function of acid sites per gram for ZI sample.

DOI: https://doi.org/10.1515/msp-2016-0009 | Journal eISSN: 2083-134X (formerly 2083-124X) | Journal ISSN: 2083-1331
Language: English
Page range: 53 - 62
Submitted on: Mar 30, 2015
Accepted on: Nov 16, 2015
Published on: Apr 27, 2016
Published by: Wroclaw University of Science and Technology
In partnership with: Paradigm Publishing Services

© 2016 Reham M. Abdel Fattah, Hala A. Kiwan, Awad I. Ahmed, Mohamed R. Mostafa, published by Wroclaw University of Science and Technology
This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.