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Frontiers of Chemical Science and Engineering

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Front. Chem. Sci. Eng.    2020, Vol. 14 Issue (3) : 405-414    https://doi.org/10.1007/s11705-019-1886-0
RESEARCH ARTICLE
A CO and CO2 tolerating (La0.9Ca0.1)2(Ni0.75Cu0.25)O4+d Ruddlesden-Popper membrane for oxygen separation
Guoxing Chen1,3(), Marc Widenmeyer1,3, Binjie Tang3, Louise Kaeswurm3, Ling Wang3, Armin Feldhoff2, Anke Weidenkaff1,4
1. Institute of Materials Science, Technische Universität Darmstadt, 64287 Darmstadt, Germany
2. Institute of Physical Chemistry and Electrochemistry, Leibniz Universität Hannover, 30167 Hannover, Germany
3. Institute for Materials Science, Universität Stuttgart, 70569 Stuttgart, Germany
4. Fraunhofer Institute IWKS, 63457 Hanau, Germany
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Abstract

A series of novel dense mixed conducting ceramic membranes based on K2NiF4-type (La1–xCax)2 (Ni0.75Cu0.25)O4+δ was successfully prepared through a sol-gel route. Their chemical compatibility, oxygen permeability, CO and CO2 tolerance, and long-term CO2 resistance regarding phase composition and crystal structure at different atmospheres were studied. The results show that higher Ca contents in the material lead to the formation of CaCO3. A constant oxygen permeation flux of about 0.63 mL·min−1·cm−2 at 1173 K through a 0.65 mm thick membrane was measured for (La0.9Ca0.1)2 (Ni0.75Cu0.25)O4+δ, using either helium or pure CO2 as sweep gas. Steady oxygen fluxes with no sign of deterioration of this membrane were observed with increasing CO2 concentration. The membrane showed excellent chemical stability towards CO2 for more than 1360 h and phase stability in presence of CO for 4 h at high temperature. In addition, this membrane did not deteriorate in a high-energy CO2 plasma. The present work demonstrates that this (La0.9Ca0.1)2(Ni0.75Cu0.25)O4+δ membrane is a promising chemically robust candidate for oxygen separation applications.
Keywords K2NiF4 structure      oxygen permeation membrane      CO2 and CO resistances      CO2 plasma resistance      long-term robustness     
Corresponding Author(s): Guoxing Chen,Marc Widenmeyer,Anke Weidenkaff   
Just Accepted Date: 08 August 2019   Online First Date: 12 November 2019    Issue Date: 28 April 2020
 Cite this article:   
Guoxing Chen,Marc Widenmeyer,Binjie Tang, et al. A CO and CO2 tolerating (La0.9Ca0.1)2(Ni0.75Cu0.25)O4+d Ruddlesden-Popper membrane for oxygen separation[J]. Front. Chem. Sci. Eng., 2020, 14(3): 405-414.
 URL:  
https://academic.hep.com.cn/fcse/EN/10.1007/s11705-019-1886-0
https://academic.hep.com.cn/fcse/EN/Y2020/V14/I3/405
Fig.1  (a) XRD patterns of (La1–xCax)2(Ni0.75Cu0.25)O4+δ (x = 0, 0.1, 0.2, 0.3, 0.4) powders and (b) magnification of the 103 main reflection. (1) x = 0; (2) x = 0.1; (3) x = 0.2; (4) x = 0.3; (5) x = 0.4. (c) unit cell parameters a and c vs. nominal Ca2+ content.
Fig.2  TG-curves of (La1-xCax)2(Ni0.75Cu0.25)O4+δ (x = 0, 0.1, 0.2, 0.3, 0.4) bulk samples at 10 K·min−1 under flowing CO2 atmosphere. CO2 flow rate is 30 mL·min−1.
Fig.3  XRD patterns of (La1–xCax)2(Ni0.75Cu0.25)O4+δ (x = 0, 0.1, 0.2, 0.3) bulk samples after exposure to pure CO2 for 500 h at 1173 K. The CO2 flow rate was 30 mL·min−1.
Fig.4  XRD patterns of La2NiO4+δ and (La0.9Ca0.1)2 (Ni0.75Cu0.25)O4+δ bulk samples before and after exposure to pure CO for 4 h at 923 K. The CO flow rate was 50 mL·min−1.
Fig.5  (a) In situ XRD patterns of (La0.9Ca0.1)2(Ni0.75Cu0.25)O4+δ powder in air; (b) Close-up of the XRD patterns at 30°<2q<33°.
Fig.6  Rietveld refinements of XRD patterns for (La0.9Ca0.1)2 (Ni0.75Cu0.25)O4+δ powder in air at different temperatures: (a) at 303 K before heating, (b) at 1123 K and (c) at 303 K after heating.
Temperature /K Cell volume /Å3 a /Å c /Å x2
303 371.99(1) 5.4032(1) 12.7414(3) 2.90
373 373.03(1) 5.4073(1) 12.7576(3) 2.85
473 374.50(2) 5.4135(1) 12.7791(3) 2.97
573 376.05(2) 5.4201(1) 12.8008(3) 2.99
673 377.64(2) 5.4266(1) 12.8242(3) 3.01
773 379.22(2) 5.4339(2) 12.8432(4) 3.05
873 380.84(2) 5.4412(2) 12.8629(4) 2.98
973 382.45(2) 5.4486(2) 12.8828(4) 2.84
1073 384.07(2) 5.4558(2) 12.9030(4) 2.88
1123 384.92(2) 5.4596(2) 12.9138(4) 2.94
1073 384.09(2) 5.4559(2) 12.9032(4) 2.86
973 382.47(2) 5.4486(2) 12.8832(4) 3.02
873 380.83(2) 5.4412(2) 12.8631(4) 3.06
773 379.21(2) 5.4337(2) 12.8434(4) 3.12
673 379.21(2) 5.4263(1) 12.8241(4) 3.25
573 376.09(2) 5.4196(1) 12.8043(3) 3.18
473 374.48(2) 5.4128(1) 12.7815(3) 3.11
373 372.98(1) 5.4068(1) 12.7589(3) 3.05
303 372.01(1) 5.4030(1) 12.7435(3) 2.99
Tab.1  Refined structural parameters of (La0.9Ca0.1)2(Ni0.75Cu0.25)O4+δ in a space group I4/mmm at different temperatures
Fig.7  Temperature dependence of the unit cell volume and the c/a ratio of (La0.9Ca0.1)2(Ni0.75Cu0.25)O4+δ powder.
Fig.8  Oxygen permeation fluxes through a (La0.9Ca0.1)2 (Ni0.75Cu0.25)O4+δ membrane in different gas atmosphere gradients. Sweep gas flow rate: He or CO2 = 29 mL·min−1, Ne=1 mL·min−1; feed gas flow rate: synthetic air (80 vol-% N2, 20 vol-% O2) or a mixture of CO2 and synthetic air=150 mL·min−1; membrane thickness: 0.65 mm.
Fig.9  XRD patterns of the (La0.9Ca0.1)2(Ni0.75Cu0.25)O4+δ membrane after exposure to pure CO2 at 1173 K for various times. The CO2 flow rate was 30 mL·min−1. The dashed lines mark the area, where the strongest reflection of CaCO3 is expected.
Fig.10  SEM images and EDS elemental distributions of the (La0.9Ca0.1)2(Ni0.75Cu0.25)O4+δ bulk sample after exposure to pure CO2 at 1173 K for 1360 h.
Fig.11  XRD patterns of the (La0.9Ca0.1)2(Ni0.75Cu0.25)O4+δ bulk sample after different CO2 plasma treatments. Treatment 1: 30 min at 1073 K; Treatment 2: 30 min at 1273 K; Treatment 3: 6 ´ 5 min at 1073 K with 5 min breaks in between; Treatment 4: 6 ´ 5 min at 1273 K with 5 min breaks in between. The dashed lines mark the area, where the strongest reflection of CaCO3 is expected.
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