Increase in the Surface Catalytic Ability by Addition of Palladium in C14 Metal Hydride Alloy
Abstract
:1. Introduction
2. Experimental Setup
3. Results and Discussions
3.1. Properties of Pd
3.2. Chemical Composition
3.3. XRD Analysis
3.4. SEM/EDS Analysis
3.5. PCT Analysis
3.6. Electrochemical Analysis
3.7. Magnetic Susceptibility
4. Conclusions
Acknowledgments
Author Contributions
Conflicts of Interest
Abbreviations
MH | Metal hydride |
H-storage | Hydrogen storage |
HRD | High-rate dischargeability |
AM | Arc melting |
RD | Replacement-diffusion |
MA | Mechanical alloying |
TA | Thermal annealing |
IM | Induction melting |
MS | Melt spinning |
LM | Levitation melting |
WI | Wet impregnation |
GP | Gaseous phase |
EC | Electrochemical |
Io | Surface exchange current |
XRD | X-ray diffractometer |
SEM | Scanning electron microscope |
PCT | Pressure concentration temperature |
ICP-OES | Inductively coupled plasma optical emission spectrometer |
EDS | Energy dispersive spectroscopy |
M.S. | Magnetic susceptibility |
ΔHh | Heat of hydride formation |
hcp | Hexagonal close-packed |
fcc | Face-centered-cubic |
bcc | Body-centered-cubic |
IMC | Intermetallic compound |
e/a | Average electron density |
VC14 | Unit cell volume of the C14 phase |
FWHM | Full width at half maximum |
BEI | Back-scattering electron image |
ΔSh | Change in entropy |
T | Absolute temperature |
R | Ideal gas constant |
D | Bulk diffusion coefficient |
R | Surface charge-transfer resistance |
C | Surface double-layer capacitance |
MS | Saturated magnetic susceptibility |
H1/2 | Applied magnetic field strength corresponding to half of saturated magnetic susceptibility |
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Host | Preparation | Application | Amount | Major Effect(s) of Pd | Reference |
---|---|---|---|---|---|
LaNi5 | AM | GP | 16 at % | Increased plateau pressure | [47] |
Mg2Ni | RD | GP | 8.3 at % | Increased absorption kinetics | [48] |
Mg2Ni | MA | GP | <1 wt. % | Increased absorption kinetics | [49] |
TiFe | MA | GP | <1 wt. % | Increased activation | [50] |
V3TiNi0.56 | AM | EC | 1 & 5 at % | Increased capacity | [51] |
TiFe | AM + TA | GP | 2.5 to 15 at % | Increased activation | [52] |
Ti2Ni | AM | EC | 9.6 at % | Increased HRD and cycle life | [53] |
AB2 | AM | EC | 3.3 at % | Increased cycle life | [54] |
Mg | MA | GP | 14 wt. % | Increased desorption kinetics | [55] |
AB2 | IM | EC | 1 to 4 at % | Increased HRD | [56] |
Mg2Ni | MS | EC | 5 to 20 at % | Increased capacity and cycle life | [57,58] |
MgNix | MS | EC | 10 at % | Easy amorphization | [59] |
MgNi | MA | EC | 1 to 10 at % | Increased cycle life | [60] |
MgNi | MA | EC | 10 at % | Increased cycle life | [61] |
TiFe | AM | EC | 5 to 10% | Increased EC activity | [62] |
Mg0.9Ti0.1Ni | MA | EC | 0 to 7.5 at % | Increased cycle life and Io | [63,64,65,66] |
Li3BN2 | MA | GP | 5 to 10 wt. % | Increased desorption kinetics | [67] |
Mg | MA | GP | 5 wt. % | Decreased absorption kinetics | [68] |
Mg | MA | GP | 10 wt. % | Increased desorption kinetics | [69] |
MgTix | MA | EC | 5 at % | Increased activation | [70] |
Mg6Pd7Si3 | TA | GP | 44 at % | Increased cycle life | [71] |
LaMg2Pd | TA | GP | 25 at % | Novel MH alloy | [72] |
TiVCr | AM | GP | 0 to 0.5 at % | Increased capacity and activation | [73] |
TiVCr | LM | EC | 0 to 3 at % | Increased capacity, cycle life, and activation | [74] |
TiZrNi | AM | EC | 0 to 7 at % | Increased capacity, HRD, and cycle life | [75] |
MgNi | MA | EC | 0 to 5 at % | Increased HRD and cycle life | [76] |
C | WI | GP | 0 to 6 at % | Increased capacity | [77] |
MgTi | MA | EC | 3.3 at % | Increased capacity and Io | [78] |
AB2 | AM + TA | EC | 5 to 10 wt. % | Increased HRD | [79] |
Mg2Ni | MA | EC | 10 wt. % | Increased capacity | [80] |
TiNi | IM | GP | 0 to 2.5 at % | Decreased Capacity | [81] |
MgNi | MA | EC | 3.5 at % | Increased capacity, HRD, and cycle life | [82] |
LaNi5 | AM + TA | GP | 4 to 25 at % | Increase in plateau pressure | [83] |
Mg2Ni | MA | EC | 3.3 at % | Increased capacity and cycle life | [84] |
C | WI | GP | 5 wt. % | Decreased absorption kinetics | [85] |
MgNi | MA | EC | 5 at % | Increased HRD and cycle life | [86] |
MgNi | MA | EC | 0 to 5 at % | Increased capacity and cycle life | [87] |
Mg | MA | GP | 0.1 to 5 wt. % | Increased absorption and desorption | [88] |
MgNi | MA | EC | 0 to 4 at % | Increased capacity | [89] |
LaMg2Ni | IM | GP | 5 at % | Increased absorption and desorption | [90] |
TiNi | MA | EC | 5 wt. % | Increased capacity and cycle life | [91] |
Mg2Co | MA | EC | 5 at % | Increased capacity, Io, and cycle life | [92,93] |
WMCNT | WI | GP | 5 wt. % | Increased capacity | [94] |
Na2SiO3 | TA | GP | 2.5 to 5 wt. % | Increased capacity | [95] |
Graphene | WI | GP | 5 to 10 wt. % | Increased capacity | [96] |
TiNi, Ti2Ni | MA + TA | EC | 5 wt. % | Increased capacity and cycle life | [97] |
C | WI | GP | 0 to 13 wt. % | Increased capacity | [98] |
Mg6Pd | TA | GP | 14 at % | Novel MH alloy | [99] |
TiVCr | AM | GP | 0.05 to 0.1 at % | Increased capacity | [100] |
MgCo | MA | EC | 5 at % | Increased HRD | [101] |
PdCu, PdCuAg | MA | GP | 15 to 100 at % | Increased capacity | [102] |
Property | Zr | Ti | Pd | V | Cr | Mn | Co | Ni | Al |
---|---|---|---|---|---|---|---|---|---|
Atomic Number | 40 | 22 | 46 | 23 | 24 | 25 | 27 | 28 | 13 |
Number of Outer-layer e− | 4 | 4 | 10 | 5 | 6 | 7 | 9 | 10 | 3 |
Earth Crust Abundance (%) | 0.013 | 0.66 | 6 × 10−7 | 0.019 | 0.014 | 0.11 | 0.003 | 0.009 | 8.1 |
Radius (Å) [112] | 1.771 | 1.614 | 1.521 | 1.491 | 1.423 | 1.428 | 1.385 | 1.377 | 1.582 |
Electronegativity | 1.33 | 1.54 | 2.20 | 1.63 | 1.66 | 1.55 | 1.88 | 1.91 | 1.61 |
Crystal Structure [113] | hcp | hcp | fcc | bcc | bcc | bcc | hcp | fcc | fcc |
Melting Point (°C) [114] | 1855 | 1668 | 1555 | 1910 | 1907 | 1246 | 1495 | 1455 | 660 |
ΔHh (kJ·mol−1) [11] | −94 | −67 | −20 | −35 | −8 | −8 | 15 | −3 | 3 |
Number of IMC with Ni [115] | 8 | 3 | 0 | 3 | 0 | 0 | 0 | - | 4 |
Alloy | Source | Ti | Zr | V | Cr | Mn | Co | Ni | Pd | Al | e/a | B/A |
---|---|---|---|---|---|---|---|---|---|---|---|---|
Pd0 | Design | 12.0 | 22.8 | 10.0 | 7.5 | 8.1 | 7.0 | 32.2 | 0.0 | 0.4 | 6.771 | 1.87 |
ICP | 11.9 | 22.9 | 10.0 | 7.5 | 8.0 | 7.1 | 32.2 | 0.0 | 0.4 | 6.773 | 1.87 | |
Pd1 | Design | 12.0 | 21.8 | 10.0 | 7.5 | 8.1 | 7.0 | 32.2 | 1.0 | 0.4 | 6.831 | 1.87 |
ICP | 12.0 | 21.3 | 10.3 | 7.5 | 8.5 | 7.0 | 31.9 | 1.1 | 0.4 | 6.834 | 1.91 | |
Pd2 | Design | 12.0 | 20.8 | 10.0 | 7.5 | 8.1 | 7.0 | 32.2 | 2.0 | 0.4 | 6.891 | 1.87 |
ICP | 12.0 | 20.5 | 9.9 | 7.5 | 8.6 | 6.9 | 32.2 | 2.0 | 0.4 | 6.900 | 1.90 | |
Pd3 | Design | 12.0 | 19.8 | 10.0 | 7.5 | 8.1 | 7.0 | 32.2 | 3.0 | 0.4 | 6.951 | 1.87 |
ICP | 12.0 | 19.5 | 10.1 | 7.5 | 8.6 | 7.0 | 32.1 | 2.8 | 0.4 | 6.949 | 1.92 | |
Pd4 | Design | 12.0 | 18.8 | 10.0 | 7.5 | 8.1 | 7.0 | 32.2 | 4.0 | 0.4 | 7.011 | 1.87 |
ICP | 11.9 | 18.7 | 10.1 | 7.6 | 8.7 | 7.0 | 31.9 | 3.7 | 0.4 | 6.996 | 1.92 | |
Pd5 | Design | 12.0 | 17.8 | 10.0 | 7.5 | 8.1 | 7.0 | 32.2 | 5.0 | 0.4 | 7.071 | 1.87 |
ICP | 11.9 | 17.8 | 10.2 | 7.4 | 8.6 | 7.1 | 32.0 | 4.6 | 0.4 | 7.055 | 1.92 |
Structural Property | Pd0 | Pd1 | Pd2 | Pd3 | Pd4 | Pd5 |
---|---|---|---|---|---|---|
a, C14 (Å) | 4.9739 | 4.9631 | 4.9561 | 4.9471 | 4.9394 | 4.9328 |
c, C14 (Å) | 8.1134 | 8.0915 | 8.0767 | 8.0598 | 8.0427 | 8.0254 |
a/c, C14 (Å) | 0.61305 | 0.61337 | 0.61363 | 0.61380 | 0.61415 | 0.61465 |
VC14 (Å3) | 173.83 | 172.61 | 171.81 | 170.83 | 169.93 | 169.12 |
a, C15 (Å) | 7.0121 | 6.9929 | 6.9827 | 6.9689 | 6.9550 | 6.9468 |
a, TiNi (Å) | 3.0795 | 3.0829 | 3.0846 | 3.0893 | 3.0955 | 3.0995 |
FWHM, C14 (103) | 0.237 | 0.25 | 0.249 | 0.241 | 0.234 | 0.243 |
C14 Crystallite Size (Å) | 482 | 446 | 448 | 469 | 491 | 465 |
C14 Abundance (%) | 85.4 | 72.1 | 72.7 | 72.0 | 72.4 | 59.8 |
C15 Abundance (%) | 11.2 | 12.6 | 11.0 | 7.0 | 5.5 | 13.4 |
TiNi Abundance (%) | 3.4 | 15.3 | 16.3 | 21.0 | 22.1 | 26.8 |
Alloy | Location | Ti | Zr | V | Cr | Mn | Co | Ni | Pd | Al | e/a | B/A | Phase |
---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Pd1 | Pd1-1 | 16.8 | 24.5 | 1.4 | 0.5 | 2.3 | 2.7 | 45.4 | 5.8 | 0.5 | 7.3 | 1.1 | TiNi |
Pd1-2 | 13.3 | 20.8 | 9.2 | 5.1 | 8.2 | 6.7 | 35.2 | 1.0 | 0.5 | 6.9 | 1.8 | C15 | |
Pd1-3 | 9.6 | 21.8 | 12.4 | 10.6 | 10.2 | 7.8 | 26.5 | 0.6 | 0.5 | 6.7 | 2.1 | C14 | |
Pd1-4 | 7.8 | 58.9 | 5.0 | 2.6 | 4.2 | 3.0 | 17.4 | 0.9 | 0.3 | - | - | ZrO2 | |
Pd2 | Pd2-1 | 21.6 | 19.2 | 2.1 | 0.9 | 3.6 | 4.3 | 39.6 | 8.0 | 0.7 | 7.2 | 1.0 | TiNi |
Pd2-2 | 11.6 | 20.8 | 7.2 | 4.0 | 7.1 | 5.1 | 40.9 | 2.8 | 0.5 | 7.2 | 1.8 | C15 | |
Pd2-3 | 10.0 | 20.7 | 12.4 | 9.6 | 10.1 | 8.0 | 27.7 | 1.0 | 0.5 | 6.7 | 2.2 | C14 | |
Pd2-4 | 5.7 | 69.1 | 3.3 | 2.3 | 3.0 | 2.3 | 12.5 | 1.6 | 0.3 | - | - | ZrO2 | |
Pd3 | Pd3-1 | 20.7 | 18.3 | 2.0 | 0.8 | 4.3 | 3.8 | 37.8 | 11.6 | 0.7 | 7.3 | 1.0 | TiNi |
Pd3-2 | 12.7 | 19.7 | 6.0 | 3.0 | 6.4 | 4.5 | 41.9 | 5.3 | 0.5 | 7.4 | 1.7 | C15 | |
Pd3-3 | 10.1 | 20.2 | 11.9 | 10.1 | 9.7 | 8.1 | 28.0 | 1.4 | 0.4 | 6.8 | 2.2 | C14 | |
Pd3-4 | 19.5 | 51.8 | 3.3 | 1.5 | 3.2 | 2.2 | 15.3 | 3.0 | 0.2 | - | - | ZrO2 | |
Pd4 | Pd4-1 | 19.7 | 17.2 | 2.0 | 0.8 | 5.4 | 3.4 | 35.7 | 14.9 | 0.8 | 7.4 | 0.9 | TiNi |
Pd4-2 | 10.7 | 18.9 | 7.5 | 4.2 | 6.9 | 4.8 | 40.8 | 5.7 | 0.6 | 7.4 | 1.8 | C15 | |
Pd4-3 | 9.6 | 19.0 | 12.1 | 10.9 | 10.2 | 8.1 | 27.8 | 1.8 | 0.5 | 6.8 | 2.3 | C14 | |
Pd4-4 | 3.6 | 80.1 | 1.8 | 1.0 | 1.3 | 1.3 | 7.6 | 3.2 | 0.1 | - | - | ZrO2 | |
Pd4-5 | 1.7 | 0.2 | 42.8 | 41.1 | 8.8 | 2.4 | 2.8 | 0.1 | 0.1 | - | - | BCC | |
Pd5 | Pd5-1 | 18.5 | 16.4 | 2.3 | 1.0 | 6.6 | 3.1 | 33.0 | 18.3 | 0.8 | 7.5 | 0.9 | TiNi |
Pd5-2 | 12.4 | 18.0 | 7.7 | 4.1 | 6.7 | 4.7 | 38.7 | 7.2 | 0.5 | 7.3 | 1.7 | C15 | |
Pd5-3 | 12.2 | 16.6 | 10.7 | 6.8 | 8.8 | 7.4 | 33.6 | 3.5 | 0.4 | 7.1 | 2.1 | C14 | |
Pd5-4 | 10.3 | 18.1 | 11.5 | 10.4 | 9.4 | 8.3 | 29.2 | 2.4 | 0.4 | 6.9 | 2.2 | C14 | |
Pd5-5 | 7.3 | 51.4 | 7.3 | 5.0 | 5.2 | 4.2 | 17.4 | 2.0 | 0.2 | - | - | ZrO2 |
Gaseous Phase Property | Unit | Pd0 | Pd1 | Pd2 | Pd3 | Pd4 | Pd5 |
---|---|---|---|---|---|---|---|
Maximum capacity @ 2 MPa and 30 °C | wt. % | 1.52 | 1.55 | 1.40 | 1.20 | 1.02 | 0.76 |
Reversible Capacity @ 30 °C | wt. % | 1.25 | 1.32 | 1.23 | 1.11 | 0.92 | 0.69 |
Capacity @ 0.002 MPa and 30 °C | wt. % | 0.30 | 0.23 | 0.17 | 0.10 | 0.09 | 0.06 |
Desorption Pressure @ 0.75 wt. % and 30 °C | MPa | 0.021 | 0.048 | 0.112 | 0.306 | 0.745 | 1.882 |
Slope Factor @ 30 °C | % | 78 | 81 | 78 | 66 | 53 | 44 |
Hysteresis @ 30 °C | 0.21 | 0.05 | 0.03 | 0.05 | 0.03 | 0.00 | |
−ΔHh | kJ·mol H2−1 | 41.6 | 40.5 | 35.6 | 30.9 | 28.0 | - |
−ΔSh | J·mol H2−1·K−1 | 127 | 125 | 118 | 111 | 109 | - |
Electrochemical and Magnetics Properties | Unit | Pd0 | Pd1 | Pd2 | Pd3 | Pd4 | Pd5 |
---|---|---|---|---|---|---|---|
3rd Cycle High-rate Discharge Capacity | mAh·g−1 | 300 | 335 | 327 | 285 | 226 | 143 |
3rd Cycle Full Discharge Capacity | mAh·g−1 | 376 | 349 | 330 | 288 | 228 | 150 |
3rd Cycle HRD | % | 80 | 96 | 99 | 99 | 99 | 98 |
Activation Cycle # to Achieve 92% HRD | 6 | 1 | 1 | 1 | 1 | 1 | |
Diffusion Coefficient, D | 10−10 cm2·s−1 | 2.1 | 4.4 | 6.2 | 2.0 | 4.1 | 4.5 |
Surface Reaction Current, Io | mA·g−1 | 12.8 | 24.7 | 28.8 | 25.2 | 22.1 | 17.1 |
Charge-transfer Resistance @ −40 °C | Ω·g | 158.6 | 29.1 | 28.3 | 22.9 | 15.7 | 39.9 |
Double-layer Capacitance @ −40 °C | F·g−1 | 0.18 | 0.16 | 0.15 | 0.16 | 0.13 | 0.10 |
RC Product @ −40 °C | s | 28.4 | 4.8 | 4.2 | 3.6 | 2.0 | 4.0 |
Total Saturated Magnetic Susceptibility, MS | emu·g−1 | 0.035 | 0.015 | 0.008 | 0.018 | 0.011 | 0.013 |
Applied Field @ M.S. = ½ MS, H1/2 | kOe | 0.50 | 0.47 | 0.34 | 0.61 | 0.77 | 0.36 |
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Young, K.-H.; Ouchi, T.; Nei, J.; Chang, S. Increase in the Surface Catalytic Ability by Addition of Palladium in C14 Metal Hydride Alloy. Batteries 2017, 3, 26. https://doi.org/10.3390/batteries3030026
Young K-H, Ouchi T, Nei J, Chang S. Increase in the Surface Catalytic Ability by Addition of Palladium in C14 Metal Hydride Alloy. Batteries. 2017; 3(3):26. https://doi.org/10.3390/batteries3030026
Chicago/Turabian StyleYoung, Kwo-Hsiung, Taihei Ouchi, Jean Nei, and Shiuan Chang. 2017. "Increase in the Surface Catalytic Ability by Addition of Palladium in C14 Metal Hydride Alloy" Batteries 3, no. 3: 26. https://doi.org/10.3390/batteries3030026