Complex Metal Borohydrides: From Laboratory Oddities to Prime Candidates in Energy Storage Applications
Abstract
:1. Introduction
2. Hydrogen Storage Options: Physical vs. Chemical Storage
2.1. Physical Storage of Hydrogen
2.2. Chemical Storage of Hydrogen
3. General Synthesis Strategies for Metal Borohydrides M(BH4)x
3.1. Solid-State—Mechanochemical Synthesis
3.2. Wet Chemistry—Solvent-Assisted Synthesis
3.3. Nanoconfined Hydrides
3.4. Derivatives—Formation of Adducts of M(BH4)x
4. Structural Considerations of M(BH4)x
4.1. Framework and Crystal Structure
4.2. Stability of MBH
4.3. Multi-Cationic Borohydrides
4.4. Anion Substitution of MBH: From Light to Heavy Halides and Pseudo-Halide Substitution
4.5. Stabilization of M(BH4)x by Coordination of Neutral Molecules (NH3, N2H4, H2O, (CH3)2S)
5. Physical and Chemical Properties of M(BH4)x
5.1. Electrochemistry of Metal Hydrides and M(BH4)x: Electrodes, Electrolytes (Li+, Mg2+, Ca2+), Complex Metal Hydrides
5.2. Optical and Magnetic Properties
5.3. M(BH4)x as Semi- and Superconductors
5.4. CO2 Capture
6. M(BH4)x as Hydrogen Storage Materials
6.1. Thermodynamic Properties of MBH
6.2. Destabilizing Methods for Complex Metal Borohydrides
System | Catalyst | td (°C) | Obs. | Reference |
---|---|---|---|---|
LiBH4–LiNH2 | - via metastable Li2[BH4][NH2] and Li4[BH4][NH2]3 | 95melt-160onset-315peak, 230mean | 5.8 wt.%H2; H2 major; small traces of NH3 (TPD-MS data) | [310] |
LiBH4-2LiNH2 | - (LiH possible intermediate) | 249 | 7.8 wt.%H2 LiBH4: 75 kJ/molH2; LiBH4-2LiNH2: 23 kJ/molH2 | [314] |
x NaBH4–NaNH2 (x = 1,2,3,4) | - via α-/β- Na2[BH4][NH2] | 265onset-350peak,297 (2:1); 400 (1:1) | 8 wt.% | [311] |
γ- Mg(BH4)2-0.5LiH | - | 380–420 | 15.5 wt.%exp., 14.78 wt.% (theoretical) * * higher wt.% exp. due to usage of solvated γ- Mg(BH4)2 | [315] |
Ca(BH4)2–4 LiNH2 | - | 250onset-320peak (288mean) | 8 wt.% | [312,313] |
Ca(BH4)2–4LiNH2-5 wt.% CoCl2 | Co2+ (CoCl2) | 150onset-207peak (178mean) | >7 wt.% | [312] |
Ca(BH4)2-2Mg(NH2)2 | - | 220–480 (270, 290 and 310–multistep) | 8.3 (8.8 wt.% theoretical) not reversible (50-bar H2, 20–300 °C) | [309] |
Ca(BH4)2-2Ca(NH2)2 | - | 220–480 (270, 290 and 310–multistep) | 6.8 (7.5 wt.% theoretical) not reversible (50-bar H2, 20–300 °C) | [309] |
5Ca(BH4)2-2LiBH4 | - | 83 | 6.7 wt.% * * theoretical | [306] |
5Mg(BH4)2-2LiBH4 | - | −29 | 8.4 wt.%* * theoretical | [306] |
2Mg(BH4)2-Ca(BH4)2 | - | 272, 326, 346, 398 (rehydrogenation at 288onset, 273peak) | 10.5 wt.% * * theoretical | [316,317,318] |
5Mg(BH4)2-Ca(BH4)2 | - | −18 °C (p = 1atm) * * predicted based on DFT calculations; 150 °C | 7.73 wt.%H2 * * predicted based on DFT calculations | [306]* [316,317] |
LiBH4 + 0.2 MgCl2 + 0.1 TiCl3; LiBH4 + 0.076 MgCl2 + 0.047 TiCl3 | MgCl2, TiCl3 | 60onset-400peak | 5 wt.%H2 | [319,320] |
LiBH4 + 0.09 TM oxides (TiO2, V2O3) | TiB2-possible active intermediate | 200 | 7–9 wt.%H2; reversible | [319] |
LiBH4 + 0.2 M (M = Mg, Al) | Mg/Al | 60–300fast-600 | 9 wt.%H2; Al-based yields material probably volatile, only recharges to 3.5 wt.% capacity | [320] |
LiBH4 + 0.0897 Al | Al | 450 | 12.4 wt.%, partially reversible | [321] |
7. Model Systems for Hydrogen Storage of MBH and Other RMH (Reactive Metal Hydrides): Nanoconfinement vs. Bulk Behavior for Improved Thermodynamics and Kinetics
7.1. LiBH4
7.2. LiBH4 + MgH2
7.3. NaBH4
7.4. Mg(BH4)2
7.5. Ca(BH4)2
7.6. Ammonia Borane NH3BH3
8. Conclusions and Outlook
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Conflicts of Interest
References
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Metal Borohydride | Decomposition Temperature (°C) | Rehydrogenation Temperature (°C) | Space Group | Crystal System | Reference |
---|---|---|---|---|---|
o-LiBH4 | (mp = 277); | 600 | Pnma | Orthorhombic | [30,31,32,33,34,35,36,37,38,164] |
h-LiBH4 | (107) | 600 | P63mc | Hexagonal | [30,31,32,33,34,35,36,37,38] |
α-NaBH4 | 535 | 270–400 (2NaH/ MgH2) | Cubic | [165,166,167,168,169] | |
Be(BH4)2 | (mp = 91.3) td = 123 | Explosive decomp. in air/moisture | I41/cd | Tetragonal; helical polymeric chains BeH2BH2BeH2BH2 and terminal bidentate BH4 groups | [170] |
α-Mg(BH4)2 (6 known polymorphs) | ~300 | (390 °C, 90-bar H2, 72 h) (400 °C, 80-bar D2) RT stable | P6122 | Hexagonal | [106,171] |
β-Mg(BH4)2 | ~300 | HT polymorph; RT metastable | Fddd | Orthorhombic | [172,173] |
γ-Mg(BH4)2 | ~300 | RT metastable | Ia3d | Cubic; 3D network of interpenetrated channels (1st borohydride with permanent porosity, S = 1505 m2/g) | [158] |
α-Ca(BH4)2 (4 known polymorphs) | 347–387 °C, 397–497 °C (2-step process) | RT stable | F2dd | Orthorhombic | [146,147,148,149,150,151] |
β-Ca(BH4)2 | β-Ca(BH4)2 | RT, metastable, HT polymorph | Tetragonal | [146,147,148,149,150,151,157] | |
α-Al(BH4)3 | <100 | −123 | C2/c | Monoclinic | [83,84,85,86,87,88] |
β-Al(BH4)3 | <100 | −78 | Pna21 | Orthorhombic | [83,84,85,86,87,88] |
α-Y(BH4)3 (β-Y(BH4)3 is the HT polymorph) | 190, 270 | 180 °C (α-to-β phase transition) | Cubic | [67,68,69,70,71,72,73] | |
α-Mn(BH4)2 (4 known polymorphs) | 130 | RT stable | P3112 | Hexagonal | [174,175,176,177,178,179,180] |
LiSc(BH4)4 | 400 | (400), irreversible hydrogen storage in Li-Sc-B-H system | 2c | Tetragonal | [181,182,183] |
NaZn(BH4)3 | >85 °C (at 110 °C NaBH4 reacts with Na2ZnCl4 to form Zn and NaCl) | stable RT | P21c | Monoclinic | [41,184] |
NaZn2(BH4)5 | unstable, converts at low temp. to NaZn(BH4)3 | unstable at RT or −32 °C | P21c | Monoclinic | [41,184] |
Compound | Experimental Conditions/Observations | Reference | |
---|---|---|---|
LiBH4 | 2 ∙ 10−3 | 107 °C | [261] |
LiBH4·H2O | 4.89 ∙ 10−4 | t = 45 °C | [264] |
LiBH4·x NH3 | 2.21 ∙ 10−3 | ; | [265,266] |
LiBH4·x NH3@Li2O | 5.4 ∙ 10−4 | 0.67 < x < 0.8; 20 °C; max for 78 wt.% Li2O | [267] |
LiBH4·x NH3BH3 | 1.47 ∙ 10−5–4.04 ∙ 10−4 | ½ < x < 1; highest for x = 1 | [268] |
LiBH4·NH3BH3 | 10−1 | t = 55 °C; record value for Li+ | [263] |
Li2B12H12 | 10−1 | 110 °C | [257] |
Li2B10H10 | 3 ∙ 10−2 | 81 °C | [258] |
Na2B10H10 | 3 ∙ 10−2 | RT | [258] |
Na2B12H12 | 10−1 | 256 °C | [259] |
LiBH4-nano | 10−3 | RT; nanoconfined electrolyte | [260] |
Mg(BH4)2 | <10−12 | t = 30 °C | [269] |
Mg(BH4)(NH2) | 10−6 | t = 150 °C | [270] |
Mg3(BH4)4(NH2)2 | 4.1 ∙ 10−5 | 100 °C | [271] |
Mg(BH4)2·en en = NH2CH2CH2NH2 | 6 ∙ 10−5 | 70 °C, crucial role of [BH4−], Mg(en)2X2 showed σ very low | [268,272] |
Mg(BH4)2·1/2dy dy = diglyme | 2 ∙ 10−5 | 80 °C; chelating of flexible dy ligand | [273] |
Mg(BH4)2·x NH3 | 3.3 ∙ 10−4 | x = 1,2,3 6; t = 80 °C; pas-de-deux mechanism proposed | [274] |
Mg(BH4)2·1.6NH3 | 2.2 ∙ 10−3 | t = 55 °C | [275] |
Metal (M) | M(BH4)x | td [°C] | Reference | |||
---|---|---|---|---|---|---|
Li | LiBH4 | 0.98 | 798.1 | 524.95 | −147.074 | [30,31,32,33,34,35,36,37,38,196,199] |
Na | NaBH4 | 0.93 | 836.01 | 562.86 | −159.509 | [165,168,169] |
K | KBH4 | 0.82 | 922.51 | 649.36 | −186.866 | [165,166,168] |
Cu | CuBH4 | 1.9 | 257.56 | −15.59 | 81.73 | [113] forms at 253 K, dec.at 261–273 K |
Rb | RbBH4 | 0.82 | 922.51 | 649.36 | −186.866 | [167] |
Ag | AgBH4 | 1.93 | 244.94 | −28.21 | 89.191 | [114]; forms at 193 K, dec. at 243 K |
Cs | CsBH4 | 0.79 | 946.84 | 673.69 | −194.327 | [165] |
AuI | AuBH4 | 2.54 | 57.15 | −216 | 240.898 | [115] * unstable |
AuIII | Au(BH4)3 | 2.54 | 57.15 | −216 | 240.898 | [116] |
Be | Be(BH4)2 | 1.57 | 417.2 | 144.05 | −0.341 | [170] |
Mg | Mg(BH4)2 | 1.31 | 569.96 | 296.81 | −65.003 | [106,158,171,172,173,189,190,191,192,193,194,195] |
Ca | Ca(BH4)2 | 1 | 783.19 | 510.04 | −142.1 | [146,147,148,149,150,151,157] |
Cr | Cr(BH4)2 | 1.66 | 369.86 | 96.71 | 22.042 | [28,29] |
Mn | Mn(BH4)2 | 1.55 | 428.1 | 154.95 | −5.315 | [175,189,190,191,224] |
Fe | Fe(BH4)2 | 1.83 | 288.22 | 15.07 | 64.321 | [192,193] |
Ni | Ni(BH4)2 | 1.91 | 253.32 | −19.83 | 84.217 | [195] * as heteroleptic complex |
Co | Co(BH4)2 | 1.88 | 266.14 | −7.01 | 76.756 | [194] * presumed, but unstable |
Zn | Zn(BH4)2 | 1.65 | 374.98 | 101.83 | 19.555 | [119,120,121,122] |
Sr | Sr(BH4)2 | 0.95 | 820.74 | 547.59 | −154.535 | [147,148] |
Ba | Ba(BH4)2 | 0.89 | 866.97 | 593.82 | −169.457 | [148] |
Cd | Cd(BH4)2 | 1.69 | 354.71 | 81.56 | 29.503 | [149] |
Hg | Hg(BH4)2 | 2 | 216.74 | −56.41 | 106.6 | [151] * failed attempts |
Al | Al(BH4)3 | 1.61 | 395.81 | 122.66 | 9.607 | [83,84,85,86,87,88] |
Sc | Sc(BH4)3 | 1.36 | 538.74 | 265.59 | −52.568 | [182,183,295,296,297,298,299] |
TiIII | Ti(BH4)3 | 1.54 | 433.61 | 160.46 | −7.802 | [176,177,178,179,206] * Ti(IV) is reduced in situ to Ti(III) |
V | V(BH4)3 | 1.63 | 385.32 | 112.17 | 14.581 | [66] |
Ga | Ga(BH4)3 | 1.81 | 297.29 | 24.14 | 59.347 | [84,85] * as GdH(BH4)2 (volatile, 203K) and GdH2(BH4) (unstable) |
Y | Y(BH4)3 | 1.22 | 628.38 | 355.23 | −87.386 | [65,66,68,69,70,71,72,73] |
Nb | Nb(BH4)3 | 1.6 | 401.1 | 127.95 | 7.12 | [180] * no homoleptic form; as complex |
In | In(BH4)3 | 1.78 | 311.17 | 38.02 | 51.886 | [86] |
La | La(BH4)3 | 1.1 | 710.71 | 437.56 | −117.23 | [212] |
Ce | Ce(BH4)3 | 1.12 | 696.64 | 423.49 | −112.256 | [212] |
Nd | Nd(BH4)3 | 1.14 | 682.7 | 409.55 | −107.282 | [69] |
SmII | Sm(BH4)2 | 1.13 | 689.65 | 416.5 | −109.769 | [213,214] |
SmIII | Sm(BH4)3 | 1.13 | 689.65 | 416.5 | −109.769 | [214] |
Pr | Pr(BH4)3 | 1.13 | 689.65 | 416.5 | −109.769 | [64] |
EuII | Eu(BH4)2 | 1.2 | 641.75 | 368.6 | −92.36 | [213] |
EuIII | Eu(BH4)3 | 1.2 | 641.75 | 368.6 | −92.36 | [70,148] |
Gd | Gd(BH4)3 | 1.2 | 641.75 | 368.6 | −92.36 | [68,71,72,214] |
Tb | Tb(BH4)3 | 1.22 | 628.38 | 355.23 | −87.386 | [73,214] |
Dy | Dy(BH4)3 | 1.23 | 621.75 | 348.6 | −84.899 | [68] |
Ho | Ho(BH4)4 | 1.24 | 615.15 | 342 | −82.412 | [69] |
Er | Er(BH4)3 | 1.24 | 615.15 | 342 | −82.412 | [214] |
Tm | Tm(BH4)3 | 1.25 | 608.59 | 335.44 | −79.925 | [73] |
YbII | Yb(BH4)2 | 1.1 | 710.71 | 437.56 | −117.23 | [215] |
YbIII | Yb(BH4)3 | 1.1 | 710.71 | 437.56 | −117.23 | [215] |
Lu | Lu(BH4)3 | 1.27 | 595.57 | 322.42 | −74.951 | [73] |
Th | Th(BH4)4 | 1.3 | 576.31 | 303.16 | −67.49 | [78,206,207] |
Pa | Pa(BH4)3 | 1.5 | 455.99 | 182.84 | −17.75 | [78] |
U | U(BH4)4 | 1.38 | 526.49 | 253.34 | −47.594 | [78,80,208,209] |
Np | Np(BH4)4 | 1.36 | 538.74 | 265.59 | −52.568 | [79,80,210] |
PuIII | Pu(BH4)3 | 1.28 | 589.12 | 315.97 | −72.464 | [78,80] |
PuIV | Pu(BH4)4 | [79] | ||||
TlI | TlBH4 | 1.62 | 390.55 | 117.4 | 12.094 | [87] |
TlIII | Tl(BH4)3 | 1.62 | 390.55 | 117.4 | 12.094 | [88] * failed attempts; as TlCl(BH4)2 (dec. at 178 K) |
Ge | Ge(BH4)4 | 2.01 | 212.86 | −60.29 | 109.087 | no conclusive reports |
Zr | Zr(BH4)4 | 1.33 | 557.37 | 284.22 | −60.029 | [203,204] |
Sn | Sn(BH4)4 | 1.96 | 232.65 | −40.5 | 96.652 | no conclusive reports |
Hf | Hf(BH4)4 | 1.3 | 576.31 | 303.16 | −67.49 | [205] |
Binary System | Ea (kJ/mol) | A × 10−9 (min−1) | k × 102 (min−1) | Reference |
---|---|---|---|---|
Ca(BH4)2-2Mg(NH2)2 | 132.7 | 15 | 1.2 | [309] |
Ca(BH4)2-2Ca(NH2)2 | 119.3 | 3.2 | 4.3 | [309] |
Compound | DSC Peak 1; Polymorphic Transformation o-LiBH4→h-LiBH4 | DSC Peak 2; Melting Point | DSC Peak 3; DehyDrogenation (MgH2) | DSC Peak 4; DehyDrogenation (LiBH4) |
---|---|---|---|---|
2LiBH4-MgH2@RF-CA21nm | 113 °C | 267 °C | 332 °C | 351 °C |
2LiBH4-MgH2-bulk | 117 °C | 290 °C | 364 °C | 462 °C |
Substance | Scaffold | Scaffold Pore | Loading (wt.%) | td (°C) | Ea (kJ/mol) | ΔH (kJ/mol) | Ref. |
---|---|---|---|---|---|---|---|
NH3BH3 | - | - |