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Chapter E: Hydrogen embrittlement and permeation Belfast – January 25, 2013

Chapter E: Hydrogen embrittlement and permeation Belfast – January 25, 2013 Hervé Barthélémy – Air Liquide. HYDROGEN EMBRITTLMENT AND PERMEATION. INTRODUCTION - GENERALITIES. REPORTED ACCIDENTS AND INCIDENTS ON HYDROGEN EQUIPMENT. TEST METHODS. PERMEATION TESTS. HYDROGEN EMBRITTLMENT

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Chapter E: Hydrogen embrittlement and permeation Belfast – January 25, 2013

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  1. Chapter E: Hydrogen embrittlement and permeation Belfast – January 25, 2013 Hervé Barthélémy – Air Liquide

  2. HYDROGEN EMBRITTLMENT AND PERMEATION INTRODUCTION - GENERALITIES REPORTED ACCIDENTS AND INCIDENTS ON HYDROGEN EQUIPMENT TEST METHODS PERMEATION TESTS

  3. HYDROGEN EMBRITTLMENT AND PERMEATION PARAMETERS AFFECTING HYDROGEN EMBRITTLEMENT OF STEELS - Environment, Design and Material HYDROGEN EMBRITTLEMENT OF OTHER MATERIALS HYDROGEN ATTACK CONCLUSION - RECOMMENDATION

  4. GENERALITIES • Internal hydrogen embrittlement • External hydrogen embrittlement

  5. 2 - IN METALLIC SOLUTION : GENERALITIES 1 - COMBINED STATE : Hydrogen attack Gaseous hydrogen embrittlement

  6. T  200°C Hydrogen embrittlement T  200°C Hydrogen attack GENERALITIES • Important parameter : THE TEMPERATURE

  7. CRITICAL CONCENTRATION AND DECOHESION ENERGY GENERALITIES • Reversible phenomena • Transport of H2 by the dislocations • H2 traps

  8. FAILURE OF A HYDROGEN TRANSPORT VESSEL IN 1980 REPORTED ACCIDENTS AND INCIDENTS

  9. FAILURE OF A HYDROGEN TRANSPORT VESSEL IN 1983. HYDROGEN CRACK INITIATED ON INTERNAL CORROSION PITS REPORTED ACCIDENTS AND INCIDENTS

  10. REPORTED ACCIDENTS AND INCIDENTS HYDROGEN CYLINDER BURSTS INTERGRANULAR CRACK

  11. REPORTED ACCIDENTS AND INCIDENTS VIOLENT RUPTURE OF A HYDROGEN STORAGE VESSEL

  12. REPORTED ACCIDENTS AND INCIDENTS H2 VESSEL. HYDROGEN CRACK ON STAINLESS STEEL PIPING

  13. Constant strain rate • Dynamic Fatigue TEST METHODS • Static (delayed rupture test)

  14. Fracture mechanic (CT, WOL, …) • Tensile test • Disk test • Other mechanical test (semi-finished products) • Test methods to evaluate hydrogen permeation and trapping TEST METHODS

  15. Vessel head • Specimen • O-rings • Vessel bottom • Gas inlet – Gas outlet • Torque shaft • Load cell • Instrumentation feed through • Crack opening displacement • gauge • Knife • Axis • Load application Fracture mechanics test with WOL type specimen TEST METHODS

  16. Specimens for compact tension test TEST METHODS

  17. Air Liquide/CTE equipment to perform fracture mechanic test under HP hydrogen (up to 1 000 bar) TEST METHODS

  18. 10-4 10-5 10-6 10-7 30 25 20 10-8 TEST METHODS Influence of hydrogen pressure (300, 150, 100 and 50 bar) - Crack growth rate versus K curves

  19. da mm/cycle dN 152 bar 41 bar 1 bar 165 bar X K, MPa Vm TEST METHODS 10-2 Influence of hydrogen pressure by British Steel 10-3 H2 10-4 N2 10-5 10 20 30 40 60 80 100 N2

  20. TEST METHODS Tensile specimen for hydrogen tests (hollow tensile specimen) (can also be performed with specimens cathodically charged or with tensile spencimens in a high pressure cell)

  21. I = (% RAN - % RAH) / % RAN I = Embrittlement index RAN = Reduction of area without H2 RAH = Reduction of area with H2 TEST METHODS

  22. TEST METHODS Pseudo Elliptic Specimen Cell for delayed rupture test with Pseudo Elliptic Specimen

  23. TEST METHODS Inner notches with elongation measurement strip Tubular specimen for hydrogen assisted fatigue tests

  24. Disk testing method – Rupture cell for embedded disk-specimen TEST METHODS • Upper flange • Bolt Hole • High-strength steel ring • Disk • O-ring seal • Lower flange • Gas inlet

  25. TEST METHODS Example of a disk rupture test curve

  26. I m (MPa) Hydrogen embrittlement indexes (I) of reference materials versus maximum wall stresses (m) of the corresponding pressure vessels TEST METHODS

  27. TEST METHODS Fatigue test - Principle

  28. TEST METHODS Fatigue test - Pressure cycle

  29. nN2 Cr-Mo STEEL 6 nH2 Pure H2 H2 + 300 ppm O2 F 0.07 Hertz 5 4 3 2 1 Delta P (MPa) 0 4 5 6 7 8 9 10 11 12 13 Fatigue tests, versus  P curves nN2 nH2 TEST METHODS

  30. TEST METHODS Fatigue test Principle to detect fatigue crack initiation

  31. TESTS CHARACTERISTICS Type of hydrogen embrittlement and transport mode

  32. TESTS CHARACTERISTICS Practical point of view

  33. TESTS CHARACTERISTICS Interpretation of results

  34. PERMEATION TESTS 4.1. Definition 4.2. Important parameter: temperature

  35. Permeability is the result of gas solution and gas diffusion Permeability coefficient is defined as follows : Pe = S × D. Permeation in polymers is a molecular permeation 4.1.Definition

  36. 2 e <<A P P P P A M M M M e e e P P P P V V V V J J J 4.1.Definition The permeability coefficient is defined as the product of the diffusion and solubility coefficients of the gas for this material. When Henry’s law is satisfied, the flow at steady state, for a given temperature, is given by: J: flow of molecules going through a surface A, at steady state (permeability flow rate) e: thickness of the sample PM: partial pressure of the gas on the upstream side PV: partial pressure of the gas on the downstream side Pe: permeability coefficient of the gas

  37. 4.2.Important parameter: Temperature • According to Arrhenius • Permeability investigated mainly for elastomer • and plastic materials • Hydrogen permeability of metals is several order • of magnitude lower than permeability of polymers

  38. PERMEATION CELL BY GASEOUS CHARGING • Reference electrode (S.C.E.) • Argon (inlet) • Argon (outlet) • Auxiliary electrode (Pt) • Teflon cell • Disk (working electrode)  58 mm and e = 0,75 mm

  39. PERMEATION TEST BY CATHODIC CHARGING - PRINCIPLE • Battery • Recorder • Potentiostat • Reference electrodes • Solution • Auxiliary electrodes (Pt) • Membrane • Charging solution

  40. PERMEATION AND DEGASSING CURVES - PRINCIPLE • Hydrogen flow • Theorical curve (with D0) • 2nd permeation • Stop in charging • Calculation • 2nd permeation • Beginning • 1st permeation • Beginning (charging)

  41. PARAMETERS AFFECTING HYDROGEN EMBRITTLEMENT OF STEELS 5.1.Environment 5.2. Material 5.3. Design and surface conditions

  42. Hydrogen purity • Hydrogen pressure • Temperature • Stresses and strains • Time of exposure 5.1. Environment or “operating conditions”

  43. 5.1. Environment or “operating conditions” • Hydrogen purity Influence of oxygen contamination

  44. 5.1. Environment or “operating conditions” • Hydrogen purity Influence of H2S contamination

  45. 5.1. Environment or “operating conditions” • Hydrogen pressure Influence of H2S partial pressure for AISI 321 steel

  46. Influence of temperature - Principle 5.1. Environment or “operating conditions” • Temperature

  47. Influence of temperature for some stainless steels 5.1. Environment or “operating conditions” • Temperature

  48. 5.1. Environment or “operating conditions” • Hydrogen purity • Hydrogen pressure • Temperature • Stresses and strains • Time of exposure

  49. Microstructure • Chemical composition • Heat treatment and mechanical properties • Welding • Cold working • Inclusion 5.2. Material

  50. 5.2. Material • Heat treatment and mechanical properties

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