材料科学与技术 ›› 2017, Vol. 33 ›› Issue (12): 1433-1447.DOI: 10.1016/j.jmst.2017.09.011
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收稿日期:2016-11-15修回日期:2017-01-29出版日期:2017-12-20发布日期:2018-01-30
Hydrogen transport in metals: Integration of permeation, thermal desorption and degassing
Galindo-Nava E.I.a, Basha B.I.Y.a, Rivera-Díaz-del-Castillo P.E.J.b*(
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- aDepartment of Materials Science and Metallurgy, University of Cambridge, 27 Charles Babbage Road, Cambridge CB3 0FS, UK
bDepartment of Engineering, Lancaster University, Lancaster LA1 4YW, UK
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Received:2016-11-15Revised:2017-01-29Online:2017-12-20Published:2018-01-30 -
Contact:Rivera-Díaz-del-Castillo P.E.J.
引用本文
. [J]. 材料科学与技术, 2017, 33(12): 1433-1447.
Galindo-Nava E.I., Basha B.I.Y., Rivera-Díaz-del-Castillo P.E.J.. Hydrogen transport in metals: Integration of permeation, thermal desorption and degassing[J]. J. Mater. Sci. Technol., 2017, 33(12): 1433-1447.
Fig. 1. Schematic representation of the (a) energy and (b) concentration landscape for hydrogen transport in the traps.
Fig. 1. Schematic representation of the (a) energy and (b) concentration landscape for hydrogen transport in the traps.
Fig. 2. Schematic representation of a (a) cylindrical and (b) plate geometry.
Fig. 2. Schematic representation of a (a) cylindrical and (b) plate geometry.
Table 1 Binding energies of the traps tested in this work.
| Trap | Eb (kJ/mol) | This work (kJ/mol) | Ref. |
|---|---|---|---|
| Dislocations | 25-60 | 26.8 | [ |
| Grain boundaries | 17-50 | 17.2 | [ |
| Cementite | 33-60 | 30 | [ |
| Pearlitic cementite | 33-60 | 43 | [ |
| M2C | 25-30 | 30 | [ |
| M4C3 | 6-116 | 35 | [ |
Table 1 Binding energies of the traps tested in this work.
| Trap | Eb (kJ/mol) | This work (kJ/mol) | Ref. |
|---|---|---|---|
| Dislocations | 25-60 | 26.8 | [ |
| Grain boundaries | 17-50 | 17.2 | [ |
| Cementite | 33-60 | 30 | [ |
| Pearlitic cementite | 33-60 | 43 | [ |
| M2C | 25-30 | 30 | [ |
| M4C3 | 6-116 | 35 | [ |
Table 2 Chemical composition (in wt%) of the materials tested in this work.
| Steel | Fe | C | Mn | Si | Cr | Ni | Al | Mo | V | Ref. |
|---|---|---|---|---|---|---|---|---|---|---|
| Ferritic A | Bal. | - | - | - | - | - | - | - | - | [ |
| Ferritic B | Bal. | 0.002 | 0.12 | 0.005 | - | 0.02 | 0.21 | - | - | [ |
| Ferritic C | Bal. | 0.004 | 0.078 | - | - | - | 0.046 | - | - | [ |
| Ferritic D | Bal. | - | - | - | - | - | - | - | - | [ |
| Martensitic A | Bal. | 0.45 | - | - | - | - | - | 1.5 | - | [ |
| Martensitic B | Bal. | 0.38 | 0.5 | 0.12 | 1.34 | 3.12 | - | 0.43 | 0.2 | [ |
| Mart/Pearl | Bal. | 0.82 | 0.78 | 0.23 | 0.18 | - | - | - | - | [ |
| Pearlitic A | Bal. | 0.84 | 0.73 | 0.25 | - | - | - | - | - | [ |
| Pearlitic B | Bal. | 0.82 | 0.77 | 0.12 | - | - | - | - | - | [ |
| 100Cr6 | Bal. | 0.974 | 0.276 | 0.28 | 1.38 | 0.184 | 0.042 | 0.056 | - | This study |
| 100Cr6+0.5V | Bal. | 0.974 | 0.28 | 0.27 | 1.42 | 0.01 | 0.003 | 0.093 | 0.55 | This study |
| 100CrMnMoSi8-4-6 | Bal. | 1 | 0.9 | 0.45 | 2 | 0.15 | 0.5 | 0.5 | - | This study |
| TWIP | Bal. | 0.6 | 18 | - | - | - | - | - | - | [ |
| AISI 310 | Bal. | 0.05 | 0.88 | 0.56 | 25.54 | 19.09 | - | 0.24 | - | [ |
| AISI 301 | Bal. | 0.05 | 1.28 | 0.48 | 17.1 | 7.25 | - | 0.24 | - | [ |
| Nickel A | - | - | - | - | - | Bal. | - | - | - | [ |
| Nickel B | - | - | - | - | - | Bal. | - | - | - | [ |
| Nickel C | - | - | - | - | - | Bal. | - | - | - | [ |
Table 2 Chemical composition (in wt%) of the materials tested in this work.
| Steel | Fe | C | Mn | Si | Cr | Ni | Al | Mo | V | Ref. |
|---|---|---|---|---|---|---|---|---|---|---|
| Ferritic A | Bal. | - | - | - | - | - | - | - | - | [ |
| Ferritic B | Bal. | 0.002 | 0.12 | 0.005 | - | 0.02 | 0.21 | - | - | [ |
| Ferritic C | Bal. | 0.004 | 0.078 | - | - | - | 0.046 | - | - | [ |
| Ferritic D | Bal. | - | - | - | - | - | - | - | - | [ |
| Martensitic A | Bal. | 0.45 | - | - | - | - | - | 1.5 | - | [ |
| Martensitic B | Bal. | 0.38 | 0.5 | 0.12 | 1.34 | 3.12 | - | 0.43 | 0.2 | [ |
| Mart/Pearl | Bal. | 0.82 | 0.78 | 0.23 | 0.18 | - | - | - | - | [ |
| Pearlitic A | Bal. | 0.84 | 0.73 | 0.25 | - | - | - | - | - | [ |
| Pearlitic B | Bal. | 0.82 | 0.77 | 0.12 | - | - | - | - | - | [ |
| 100Cr6 | Bal. | 0.974 | 0.276 | 0.28 | 1.38 | 0.184 | 0.042 | 0.056 | - | This study |
| 100Cr6+0.5V | Bal. | 0.974 | 0.28 | 0.27 | 1.42 | 0.01 | 0.003 | 0.093 | 0.55 | This study |
| 100CrMnMoSi8-4-6 | Bal. | 1 | 0.9 | 0.45 | 2 | 0.15 | 0.5 | 0.5 | - | This study |
| TWIP | Bal. | 0.6 | 18 | - | - | - | - | - | - | [ |
| AISI 310 | Bal. | 0.05 | 0.88 | 0.56 | 25.54 | 19.09 | - | 0.24 | - | [ |
| AISI 301 | Bal. | 0.05 | 1.28 | 0.48 | 17.1 | 7.25 | - | 0.24 | - | [ |
| Nickel A | - | - | - | - | - | Bal. | - | - | - | [ |
| Nickel B | - | - | - | - | - | Bal. | - | - | - | [ |
| Nickel C | - | - | - | - | - | Bal. | - | - | - | [ |
Table 3 Geometry of the samples tested in this work.
| Steel | Geometry | w (mm) | h (mm) | R (mm) | L (mm) |
|---|---|---|---|---|---|
| Ferritic A | Cylindrical | - | - | 10 | 0.1 |
| Ferritic B | Cylindrical | - | - | 2.5 5 | |
| Ferritic C | Plate | 1 | 12.6 | - | 12 |
| Ferritic D | Cylindrical | - | - | 4 | 15 |
| Martensitic A | Cylindrical | - | - | 20 | 1.1 |
| Martensitic B | Cylindrical | - | - | 2.5 | 25 |
| Mart/Pearl (Mart) | Cylindrical | - | - | 7.5 | - |
| Mart/Pearl (Pearl) | Cylindrical | - | - | 3.25 | - |
| Pearlitic A | Cylindrical | - | - | 2.5 | 20 |
| Pearlitic B | Plate | 5 | 5 | 0 | 5 |
| 100Cr6 | Cylindrical | - | - | 4 | 2 |
| 100Cr6+0.5V | Cylindrical | - | - | 4 | 2 |
| 100CrMnMoSi8-4-6 | Cylindrical | - | - | 4.25 | 8.8 |
| TWIP | Cylindrical | - | - | 10 | 1.4 |
| AISI 310 | Plate | 1 | 4.8 | - | 5 |
| Nickel A | Cylindrical | - | - | 20 | 0.1 |
| Nickel B | Plate | - | - | - | 0.18 |
| Nickel C | Plate | - | - | - | 0.35 |
Table 3 Geometry of the samples tested in this work.
| Steel | Geometry | w (mm) | h (mm) | R (mm) | L (mm) |
|---|---|---|---|---|---|
| Ferritic A | Cylindrical | - | - | 10 | 0.1 |
| Ferritic B | Cylindrical | - | - | 2.5 5 | |
| Ferritic C | Plate | 1 | 12.6 | - | 12 |
| Ferritic D | Cylindrical | - | - | 4 | 15 |
| Martensitic A | Cylindrical | - | - | 20 | 1.1 |
| Martensitic B | Cylindrical | - | - | 2.5 | 25 |
| Mart/Pearl (Mart) | Cylindrical | - | - | 7.5 | - |
| Mart/Pearl (Pearl) | Cylindrical | - | - | 3.25 | - |
| Pearlitic A | Cylindrical | - | - | 2.5 | 20 |
| Pearlitic B | Plate | 5 | 5 | 0 | 5 |
| 100Cr6 | Cylindrical | - | - | 4 | 2 |
| 100Cr6+0.5V | Cylindrical | - | - | 4 | 2 |
| 100CrMnMoSi8-4-6 | Cylindrical | - | - | 4.25 | 8.8 |
| TWIP | Cylindrical | - | - | 10 | 1.4 |
| AISI 310 | Plate | 1 | 4.8 | - | 5 |
| Nickel A | Cylindrical | - | - | 20 | 0.1 |
| Nickel B | Plate | - | - | - | 0.18 |
| Nickel C | Plate | - | - | - | 0.35 |
Table 4 Microstructures of the materials tested in this work.
| Steel | ρ (m-2) | Dg (μm) | fθ (%) | rθ (nm) | fp (%) | rp (nm) | Carbide |
|---|---|---|---|---|---|---|---|
| Ferritic A | 2.5 × 1014 | - | - | - | - | - | - |
| Ferritic B | 1.8 × 1013-1.8 × 1014 | - | - | - | - | - | - |
| Ferritic C | 7.6-13.6 × 1013 | 130 | - | - | - | - | - |
| Ferritic D | 1.5 × 1015 | - | - | - | - | - | - |
| Martensitic A | 3.25 × 1014 | - | - | - | 1.2 | 30 | M2C |
| Martensitic B | 5.5 × 1014 | 8 | 4 | 20 | 0.5 | 10 | M4C3 |
| Mart/Pearl (Mart) | 3.4 × 1014 | 15 | 10 | 10 | - | - | |
| Mart/Pearl (Pearl) | 3 × 1014 | 15 | - | 75(*) | - | - | |
| Pearlitic A | 6 × 1014 | 20 | - | 75(*) | - | - | |
| Pearlitic B | 2 × 1014 | 20 | - | 75(*) | - | - | |
| 100Cr6 | 9.8 × 1015 | 20 | 10 | 10 | - | - | - |
| 100Cr6+0.5V | 9.8 × 1015 | 20 | 10 | 10 | 0.9 | 5 | M4C3 |
| 100CrMnMoSi8-4-6 | 5 × 1014 | 20 | 10 | 25 | - | - | - |
| TWIP | 1010 | 10 | - | - | - | - | - |
| AISI 310 | 1010 | - | - | - | - | - | - |
| AISI 301 | 6 × 1013(γ), 6 × 1014(α′), | - | - | - | - | - | |
| Nickel A | 1011 | 10 | - | - | - | - | - |
| Nickel B | - | 0.12-168 | - | - | - | - | - |
| Nickel C | 1015 | - | - | - | - | - | - |
Table 4 Microstructures of the materials tested in this work.
| Steel | ρ (m-2) | Dg (μm) | fθ (%) | rθ (nm) | fp (%) | rp (nm) | Carbide |
|---|---|---|---|---|---|---|---|
| Ferritic A | 2.5 × 1014 | - | - | - | - | - | - |
| Ferritic B | 1.8 × 1013-1.8 × 1014 | - | - | - | - | - | - |
| Ferritic C | 7.6-13.6 × 1013 | 130 | - | - | - | - | - |
| Ferritic D | 1.5 × 1015 | - | - | - | - | - | - |
| Martensitic A | 3.25 × 1014 | - | - | - | 1.2 | 30 | M2C |
| Martensitic B | 5.5 × 1014 | 8 | 4 | 20 | 0.5 | 10 | M4C3 |
| Mart/Pearl (Mart) | 3.4 × 1014 | 15 | 10 | 10 | - | - | |
| Mart/Pearl (Pearl) | 3 × 1014 | 15 | - | 75(*) | - | - | |
| Pearlitic A | 6 × 1014 | 20 | - | 75(*) | - | - | |
| Pearlitic B | 2 × 1014 | 20 | - | 75(*) | - | - | |
| 100Cr6 | 9.8 × 1015 | 20 | 10 | 10 | - | - | - |
| 100Cr6+0.5V | 9.8 × 1015 | 20 | 10 | 10 | 0.9 | 5 | M4C3 |
| 100CrMnMoSi8-4-6 | 5 × 1014 | 20 | 10 | 25 | - | - | - |
| TWIP | 1010 | 10 | - | - | - | - | - |
| AISI 310 | 1010 | - | - | - | - | - | - |
| AISI 301 | 6 × 1013(γ), 6 × 1014(α′), | - | - | - | - | - | |
| Nickel A | 1011 | 10 | - | - | - | - | - |
| Nickel B | - | 0.12-168 | - | - | - | - | - |
| Nickel C | 1015 | - | - | - | - | - | - |
Table 5 Charging and desorption conditions of the materials tested in this work.
| Steel | I (A/m2) | tcharg (h) | ? (°C/h) | tdegas (h) | Solution | n0 (wppm A-1/2 m) |
|---|---|---|---|---|---|---|
| Ferritic A | 1-10 | 1 | - | - | 0.1N NaOH | 9.4 × 107 |
| Ferritic B | 5 | - | - | - | 3% NaCl + 0.3% NH4SCN | 4.7 × 108 |
| Ferritic C | 1 | 12 | 100 | 0.25 | 3% NaCl + 0.3% NH4SCN | 4.7 × 108 |
| Martensitic A | 200 | 5 | - | 6 | 1M H2SO4 | - |
| Martensitic B | 100 | 100 | - | 200 | 0.1N NaOH | 9.4 × 107 |
| Mart/Pearl | 10 | 48 | 100 | - | 0.1N NaOH + 3% NaCl + 0.3% NH4SCN | 4.7 × 108 |
| Pearlitic A | - | 24-120 | 100 | - | 0.2M NH4SCN | 7.5 × 108 |
| 100Cr6 | 10 | 24 | 100 | 72 | 3% NaCl + 0.3% NH4SCN | 4.7 × 108 |
| 100Cr6+0.5V | 10 | 24 | 100 | 24 | 3% NaCl + 0.3% NH4SCN | 4.7 × 108 |
| 100CrMnMoSi8-4-6 | 10 | 48, 72 | 100 | 168 | 3% NaCl + 0.3% NH4SCN | 4.7 × 108 |
| AISI 310 | 1 | 60 | 360 | - | 1N H2SO4 + 0.002% CH2N2S | 9.2 × 1019 |
| Nickel B | 200 | 0.16-0.5 | - | 0.16-0.4 | - | - |
Table 5 Charging and desorption conditions of the materials tested in this work.
| Steel | I (A/m2) | tcharg (h) | ? (°C/h) | tdegas (h) | Solution | n0 (wppm A-1/2 m) |
|---|---|---|---|---|---|---|
| Ferritic A | 1-10 | 1 | - | - | 0.1N NaOH | 9.4 × 107 |
| Ferritic B | 5 | - | - | - | 3% NaCl + 0.3% NH4SCN | 4.7 × 108 |
| Ferritic C | 1 | 12 | 100 | 0.25 | 3% NaCl + 0.3% NH4SCN | 4.7 × 108 |
| Martensitic A | 200 | 5 | - | 6 | 1M H2SO4 | - |
| Martensitic B | 100 | 100 | - | 200 | 0.1N NaOH | 9.4 × 107 |
| Mart/Pearl | 10 | 48 | 100 | - | 0.1N NaOH + 3% NaCl + 0.3% NH4SCN | 4.7 × 108 |
| Pearlitic A | - | 24-120 | 100 | - | 0.2M NH4SCN | 7.5 × 108 |
| 100Cr6 | 10 | 24 | 100 | 72 | 3% NaCl + 0.3% NH4SCN | 4.7 × 108 |
| 100Cr6+0.5V | 10 | 24 | 100 | 24 | 3% NaCl + 0.3% NH4SCN | 4.7 × 108 |
| 100CrMnMoSi8-4-6 | 10 | 48, 72 | 100 | 168 | 3% NaCl + 0.3% NH4SCN | 4.7 × 108 |
| AISI 310 | 1 | 60 | 360 | - | 1N H2SO4 + 0.002% CH2N2S | 9.2 × 1019 |
| Nickel B | 200 | 0.16-0.5 | - | 0.16-0.4 | - | - |
Fig. 3. (a) Effect of the charging density in the permeation profile of cold-rolled Ferritic A. (b) Permeation/degassing profile in Martensitic A. (c) Hydrogen concentration as function of the dislocation density in Ferritic B. (d) Effect of the sample radius in the time for saturation and hydrogen concentration in deformed ferrite.
Fig. 3. (a) Effect of the charging density in the permeation profile of cold-rolled Ferritic A. (b) Permeation/degassing profile in Martensitic A. (c) Hydrogen concentration as function of the dislocation density in Ferritic B. (d) Effect of the sample radius in the time for saturation and hydrogen concentration in deformed ferrite.
Fig. 4. (a) Charging and (b) degassing profiles in pearlite. (c) Charging/degassing profiles in Martensitic B and (d) the relative contribution of various microstructural features to the total concentration.
Fig. 4. (a) Charging and (b) degassing profiles in pearlite. (c) Charging/degassing profiles in Martensitic B and (d) the relative contribution of various microstructural features to the total concentration.
Fig. 5. (a) Thermal desorption results in Ferritic C for various dislocation densities. (b) Comparison in the desorption profiles between martensite and pearlite in Mart/Pearl. (c) Effect of charging time in the desorption profiles in a Pearlitic A. (d) Variation in the peak temperature as function of the heating rate in Ferritic D.
Fig. 5. (a) Thermal desorption results in Ferritic C for various dislocation densities. (b) Comparison in the desorption profiles between martensite and pearlite in Mart/Pearl. (c) Effect of charging time in the desorption profiles in a Pearlitic A. (d) Variation in the peak temperature as function of the heating rate in Ferritic D.
Fig. 6. (a) Thermal desorption spectroscopy in 100CrMnMoSi8-4-6. Predicted concentration profile during charging (b) and (c) degassing prior the desorption tests. (d) Effect of vanadium in 100Cr6 series.
Fig. 6. (a) Thermal desorption spectroscopy in 100CrMnMoSi8-4-6. Predicted concentration profile during charging (b) and (c) degassing prior the desorption tests. (d) Effect of vanadium in 100Cr6 series.
Fig. 7. Hydrogen transport in austenitic steels: (a) permeation when charging at various temperatures in a TWIP steel. (b) Concentration profile during charging and (c) thermal desorption results in AISI 310. (d) Variation in the diffusion coefficient of AISI 301 as function on the martensite volume fraction.
Fig. 7. Hydrogen transport in austenitic steels: (a) permeation when charging at various temperatures in a TWIP steel. (b) Concentration profile during charging and (c) thermal desorption results in AISI 310. (d) Variation in the diffusion coefficient of AISI 301 as function on the martensite volume fraction.
Fig. 8. Hydrogen transport in pure nickel: (a) permeation/degassing at various temperatures in Nickel A; (b) current density saturation profiles for various grain sizes in Nickel B; (c) variation in the effective diffusion coefficient during permeation as function of the grain size. (d) Thermal desorption results for various sample thicknesses in Nickel C.
Fig. 8. Hydrogen transport in pure nickel: (a) permeation/degassing at various temperatures in Nickel A; (b) current density saturation profiles for various grain sizes in Nickel B; (c) variation in the effective diffusion coefficient during permeation as function of the grain size. (d) Thermal desorption results for various sample thicknesses in Nickel C.
Fig. 9. Parametric analysis in martensitic steels: effect of dislocations, cementite and vanadium carbides in (a) hydrogen concentration, (b) apparent diffusion coefficient, (c) permeation coefficient and (d) peak temperature during thermal desorption spectroscopy.
Fig. 9. Parametric analysis in martensitic steels: effect of dislocations, cementite and vanadium carbides in (a) hydrogen concentration, (b) apparent diffusion coefficient, (c) permeation coefficient and (d) peak temperature during thermal desorption spectroscopy.
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