Ceramic Membranes for Oxyfuel Power Plants

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1 Mitglied der Helmholtz-Gemeinschaft Ceramic Membranes for Oxyfuel Power Plants May 19, 2009 Michael Betz, Stefan Baumann, Wilhelm A. Meulenberg Forschungszentrum Jülich GmbH Institute for Energy Research IEF-1: Materials Synthesis and Processing

2 Outline 1. Introduction 2. Sample preparation of asymmetric structures 3. Permeation experiments 4. Conclusion and outlook May 19, 2009 slide 2

3 1 Introduction Development of a O 2 /N 2 -separation membrane for application in Oxyfuel power plants. Different conditions for the membrane are possible that require different materials (vacuum, CO 2 -sweep, etc.). Ba 0,5 Sr 0,5 Co 0,8 Fe 0,2 O 3-δ (BSCF) is a highly oxygen permeable mixed ionic and electronic conductor (MIEC). BSCF can be a suitable material for conditions without flue gas contact of the membrane - e.g. vacuum (CO 2 Carbonates, SO 2 Sulfates). Satisfying the demanded permeation rate of at least j=3 ml/(min cm 2 ) a decrease of the layer thickness is favorable. May 19, 2009 slide 3

4 1 Introduction Diffusion controlled transport according to Wagner-Equation j = K T L ln p h σ iσ e σ + σ ln p l ln PO 2 Below a characteristic thickness L c the Wagner-Equation does not apply any more. Surface kinetics take control of the permeation rate. i e d Thin membrane layers (<100 µm) need to be mechanically supported. Differences in TEC and shrinkage behavior can lead to cracked structures May 19, 2009 slide 4

5 1 Introduction TEC [10-6 K -1 ] BSCF Inconel 625 (fcc) LSCF Crofer APU 22 (bcc) 8YSZ Not matching expansion behavior due to chemical expansion of BSCF Chemical compatibility has to be provided Temperature [ C] first approach: same support material BSCF May 19, 2009 slide 5

6 2 Sample preparation Porous support via Tape Casting Slurry preparation BSCF (d 50 =1,7 µm) + 20 wt-% rice starch (2-8 µm) as pore forming material + solvent, dispersing agent, binder and plasticizers are homogeneously mixed and degassed Tape casting h (doctor blade)= 1,9 mm h (tape green state) 1 mm Casting speed = 200 mm/min Doctor Blades Reservoir SLURRY Carrier Relative Carrier Motion May 19, 2009 slide 6

7 2 Sample preparation Porous support Tape casting facilities small tapes (width around 14 cm) large tapes (width up to 50 cm) Slow debinding of organic matter (24 h) Presintering step at 900 C/3h with a shrinkage of 13% May 19, 2009 slide 7

8 2 Sample preparation Porous support Permeability (D s = cm 2 according to DIN 51058) Average pore size = 1,1 µm (Hgporosimetry) Porosity of 23 Vol-% (optical analysis) 25 Permeability measurement 40 50µm SEM picture Porosity [%] 0 1E-3 0,01 0, May 19, 2009 slide Average pore size (APS) 1,1 μm Pore size [μm] Relative volume [%]

9 2 Sample preparation Dense layer via Screen Printing BSCF-powder is mixed with ethyl cellulose binder, dispersing agent and terpineol as transport media. Homogenization with 3 roller mill and characterization of pastes. Multiple printing with wet layer thickness of 95 µm per step. 100 Viscosity Viskosität [Pa s] Shear rate [1/s] Scherrate [1/s] May 19, 2009 slide 9

10 2 Sample preparation Asymmetric membrane Sintering at 1100 C/5h with subsequent characterization Layer thickness: 120 µm Substrate thickness: 860 µm Machined to Ø15mm by cylindrical grinding He-Leak rate: mbar l /cm 2 s 200µm May 19, 2009 slide 10

11 3 Permeation measurement Setup and parameters Quartz glass recipient Membrane: Ø 15 mm Dense layer on feed side Sealing with gold rings Ar Temperature controlled by thermocouple Air/O 2 Feed: Air-O 2 -mixture F=250 ml/min Sweep: Argon F= ml/min Permeate concentration measured by mass spectrometry May 19, 2009 slide 11

12 Permeation rate [ml/min cm 2 ] 3 Permeation measurement Temperature 2,5 2,0 1,5 1,0 0,5 0,0 asymm. (120µm) bulk (1mm) Temperature [ C] Feed (Air): F=250 Nml/min Sweep (Ar): F=50 Nml/min Dense layer on feed side + 27% Decrease in thickness leads to higher permeation Bulk: j =1,53 ml/min cm 2 Asymm.: j =1,94 ml/min cm 2 According to Wagner: (T=900 C) May 19, 2009 slide 12 j O L(bulk) L(asymm.) 1 2 L = 1000 µm 120 µm = 8, 3

13 3 Permeation measurement Sweep flow rate Permeation rate [ml/min cm 2 ] 3,5 3,0 2,5 2,0 1,5 1,0 0,5 0,0 L=1mm T=900 C Feed (Air): 250Nml/min Variation of F(Ar) Low driving force: F(Ar)=50 Nml/min p l *= 0,041 atm j(o 2 )= 1,74 ml/min cm 2 High driving force: F(Ar)=2000 Nml/min p l *= 0,002 atm j(o 2 )= 3,21 ml/min cm 2 Argon flow rate [Nml/min] + 85% May 19, 2009 slide 13

14 Permeation rate [ml/min cm 2 ] 3 Permeation measurement Partial pressure gradient Feed 84% O 2 Feed 20% O ln (p h /p l ) L=1 mm F(Air/O 2 )=250 Nml/min F(Ar)= Nml/min 1 p j ln L pl May 19, 2009 slide 14 h different permeation rates for same ratio of partial pressures absolute values of partial pressures have influence

15 Permeation rate [ml/min cm 2 ] 3 Permeation measurement Partial pressure gradient Asymm Bulk ln (p h /p l ) Feed 84% O 2 Feed 20% O 2 F(Air/O 2 )=250 Nml/min F(Ar)= Nml/min Difference more evident for asymmetric structures Oxygen partial pressure (p) at the surface not detectable measurement of the oxygen partial pressure in the permeate gas stream (p*) May 19, 2009 slide 15

16 3 Permeation measurement Partial pressure gradient Substrate changes oxygen partial pressure measured p l * Ar F(Air/O 2 )=250 Nml/min F(Ar)= Nml/min Difference more evident for asymmetric structures real p l p h Air Oxygen partial pressure (p) at the surface not detectable measurement of the oxygen partial pressure in the permeate gas stream (p*) May 19, 2009 slide 16

17 Permeation rate [ml/min cm 2 ] 3 Permeation measurement Partial pressure gradient Asymm Bulk * * ln (p h /p l ) Feed 84% O 2 Feed 20% O 2 F(Air/O 2 )=250 Nml/min F(Ar)= Nml/min Difference more evident for asymmetric structures Oxygen partial pressure (p) at the surface not detectable measurement of the oxygen partial pressure in the permeate gas stream (p*) May 19, 2009 slide 17

18 4 Conclusion and outlook Gas tight asymmetric membrane structures of BSCF can be prepared via tape casting and screen printing. Increase in permeation rates but no Wagner relation. Substrate (feed/sweep, porosity) Gas flow conditions (sweep/vacuum) Permeation j Surface exchange kinetics (p h /p l, catalytic layers) May 19, 2009 slide 18

19 4 Conclusion and outlook high p(o 2 ): Air (O 2 /N 2 ) 2 e - O 2- Membrane Layer Catalytic Layer Catalytic Layer Substrate O 2 low p(o 2 ): Vacuum (50 mbar) For high flux membrane structures the dependencies need to be clarified and quantified. May 19, 2009 slide 19

20 Thank you for your attention. Work funded by: BMWi in the framework of the OXYMEM-project ( B) May 19, 2009 slide 20

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