Scaled up production of ceramic membranes for oxyfuel capture - - PowerPoint PPT Presentation

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Scaled up production of ceramic membranes for oxyfuel capture - - PowerPoint PPT Presentation

Aug 16, 2022 115 likes •310 views

Scaled up production of ceramic membranes for oxyfuel capture Marie-Laure Fontaine (SINTEF), Christelle Denonville (SINTEF), Adam Stevenson (Saint Gobain CREE), Christian His (Saint Gobain CREE), Emmanuel Mercier (Saint Gobain CREE), Caroline

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SLIDE 1

Scaled up production of ceramic membranes for oxyfuel capture

Marie-Laure Fontaine (SINTEF), Christelle Denonville (SINTEF), Adam Stevenson (Saint Gobain CREE), Christian His (Saint Gobain CREE), Emmanuel Mercier (Saint Gobain CREE), Caroline Tardivat (Saint Gobain CREE), Marijke Jacobs (VITO), Frans Snijkers (VITO), Falk Schulze-Küppers (FZJ), Wilhelm Meulenberg (FZJ), Wen Xing (SINTEF), Zuoan Li (SINTEF) Jonathan Polfus (SINTEF), Ove Paulsen (SINTEF), Paul Inge Dahl (SINTEF), Partow Henriksen (SINTEF), Rune Bredesen (SINTEF)

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Efficient Tubular Membranes for Oxy-Combustion

  • EU FP7 (2011-2016): Demonstration project
  • Coordinator: RISOE DTU (DK)
  • Partners: Air Liquide (FR), INABENZA (SP), Saint-Gobain Cree (FR), FZJ (DE), VITO (BE), SINTEF (NO), IKTS (DE)
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SLIDE 3

CaTi0.85-xFe0.15MnxO3-δ, x = 0.0-0.4

  • Low creep rate
  • Low cost
  • Stable in large oxygen partial pressure

gradient and in CO2 atmosphere

  • No phase transition from RT→ sintering T
  • Fairly good sinterability (1300°C – 1400°C)
  • TEC about 13. 10‐6 K‐1 (RT – 900 °C)

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SLIDE 4

Scaling up CaTi1-xFexO3-d asymmetric membrane

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Step 1: Length ≤ 25cm

  • Powder production
  • Tubular supports
  • Thin film membranes
  • Porous catalytic layers
  • Sealing (several partners)

Quality control parameters :

  • Thickness,
  • Porosity,
  • Straightness, roundness,
  • Leak tightness at RT
  • Flux data

Step 2: 25cm < L ≤ 50cm

  • Powder production
  • Tubular supports
  • Thin film membranes
  • Porous catalytic layers
  • Sealing

Step 3: 70 cm ++

  • Powder +Tubular supports
  • Thin film membranes
  • Porous catalytic layers
  • Sealing

Infrastructure up- grade (coating tools, furnaces, mixers …)

50 microns

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SLIDE 5

Production line

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Powder production (100 kg++) Slurries and pastes preparation Extrusion

  • f supports

Dip- coating Sintering Pre- annealing 45 cm Calendaring

  • f caps

Sintering Sealing Up to 1 m long

Clean room class 7 Clean room class 7

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SLIDE 6

Scaling up of membranes

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25cm < L ≤ 50cm

Expected porosity versus volume

  • f pore former: 45%

Samples Open porosity (%) SG1 45.2 SG011 40.8 HT21 40.0 HT31 40.2

0.1 1 10 100 0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0

Log Differential Intrusion (mL/g) Pore size Diameter (um) SG1 SG2 SG11 Small layer

SG1 SG2 SG11 HT21

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SLIDE 7

X-ray computational tomography

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A 753*753*1411 µm3 (800x800x1500 pixels) volume

Pore size distribution Average size: 7.5 µm

  • St. deviation:

2.8 µm Porosity and tortuosity Porosity in central volume: 45 % Tortuosity: 1.7

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SLIDE 8

Sealing : glass ceramic

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CTF Seal

Steel

CTF

TEC transfer

  • Dr. Falk Schulze-Küppers

Stability of seal tested in operation for 6 months at ambient pressure Leak rate: 6.10-4 mbar.l/s Leak rate: 1.10-7 mbar.l/s

50 microns 100 microns

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SLIDE 9

Flux measurements for the first scaling up

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* Reference case for transfer: 45 microns thick CTF membranes

Adjustment of procedures for heat treatment and coating for long membranes improve flux

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SLIDE 10

Scaling up at SG membranes: 70 cm ≤ Membrane

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  • Thickness of the dense CTF layer: ca. 45 microns from top to bottom
  • Thickness of porous support: ca. 0.9 mm

100 microns 100 microns

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SLIDE 11

Scaling up at SG membranes: 70 cm ≤ OTM

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Bubble test at 0.5 bar

  • ver pressure: no leak

Gradient Air/Vacuum: Leak rate: 0.24 ml/min i.e. ca 1% leak rate for a flux of 0.1 ml/min.cm2

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SLIDE 12

Activation layer by spray-coating

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7-8 µm CTF coating on short membrane

  • Air and Ar flow of 50 ml/min
  • Effective membrane surface

areas: 9-10 cm2

50 microns

Jacobs M. et al, Journal of Membrane Science 477 (2015) 58-64

30 cm

6-9 µm CTF coating on 70cm long membrane

10 microns

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SLIDE 13

Testing of 70 cm membrane

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Sweep gas supply; there is a similar inside feed gas supply tube

Cooling system Furnace Base ProbostatTM

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SLIDE 14
  • xygen purity above 99%

Flux as function of T and pO2

14 0.0 0.2 0.4 0.6 0.8 1.0 0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8

pO2 (atm) J (O2) (mL/min cm

2)

T=1000°C, inner sweep Ar (400 mL/min), feed (600 mL/min) T=950°C, inner sweep Ar (400 mL/min), feed (600 mL/min) T=900°C, inner sweep Ar (400 mL/min), feed (400 mL/min) T=850°C, outer sweep Ar (500 mL/min), feed (400 mL/min) T=850°C, inner sweep Ar (200 mL/min), feed (400 mL/min) T=800°C, inner sweep Ar (200 mL/min), feed (200 mL/min)

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SLIDE 15

Summary

  • Manufacturing protocol for CTF based tubular asymmetric membranes developed
  • Protocol transfer from SINTEF to SG CREE achieved
  • Further scaling-up of membranes to 70 cm by SG achieved
  • Scaling-up of activation layer at VITO achieved
  • Protocol transfer from SINTEF to FZJ on sealing technology achieved

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SLIDE 16

This work has been supported by the EC within the 7th framework programme under grant agreement

  • no. FP7-ENERGY-268165

Acknowledgements

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SLIDE 17

HETMOC

  • Line 1: Air/vacuum stability
  • Line 2: CO2, steam stability

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