Effect of synthesis temperature on the morphology and stability of copper(i) hydride nanoparticles

Soroka, Inna L.; Tarakina, Nadezda V.; Korzhavyi, Pavel A.; Stepanenko, Vladimir; Jönsson, Mats

doi:10.1039/c3ce41303a

Cited by 15 publications

(34 citation statements)

References 30 publications

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“…They also have the same valence shell electronic structure and can thus correlate with each other owing to their similarities in the bulk metals, a fcc (face‐centered cubic) lattice packing. Even some of the fcc ‐CuH (or silver hydride proved by theory at (>50 GPA) has been identified at high pressure (>14.4 GPA) synthesis ,…”

Section: Discussionmentioning

confidence: 99%

“…They also have the same valence shell electronic structure and can thus correlate with each other owing to their similarities in the bulk metals, a fcc (face-centered cubic) lattice packing. Even some of the fcc-CuH [32] (or silver hydride proved by theory at (> 50 GPA) [33] has been identified at high pressure (> 14.4 GPA) synthesis. [34,32] 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36 37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54 55 56 57…”

Section: Discussionmentioning

confidence: 99%

“…[8a-b] An elongated triangular orthobicupola metallic framework correlates with an elongated triangular gyrobicupola frame by rotation through 60 o on the C 3 axis. Interestingly, H 2 evolution was observed in the [Cu 32 (H) 20 {S 2 P(O i Pr) 2 } 12 ], 3 H , cluster [11]] that was produced in modest yield (41%). Similar to [Cu 20 (H) 11 Cluster 3 H is intriguing as it not only contains additional hydride (29%) compared to 4 H but also releases more H 2 (> 26%) under similar reaction conditions.…”

Section: Introductionmentioning

confidence: 99%

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Synthesis, Structural Characterization, and H₂ Evolution Study of a Spheroid‐Shape Hydride‐Rich Copper Nanocluster

et al. 2018

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This study reports on new bis‐2‐butyl dithiophosphate‐stabilized polyhydrido copper nanoclusters, [Cu32(H)20{S2P(O2Bu)2}12], 1H, and [Cu20H11{S2P(O2Bu)2}9], 2H. The clusters 1H and 2H have been characterized by a variety of techniques including multinuclear NMR (1H, 2H, 31P), electrospray ionization mass spectrometry (ESI‐MS), and low temperature X‐ray crystallography. The presence of hydride ligands was supported by the 2H NMR spectrum of the deuteride analogs [Cu32(D)20{S2P(O2Bu)2)12], 1D and [Cu20D11{S2P(O2Bu)2}9], 2D. The metal skeleton of 1H revealed that a hexacapped rhombohedron of fourteen copper atoms was sandwiched between two sets of eighteen (9x2) copper atoms in a cup shape and the entire cluster is an elongated triangular gyrobicupola. The metal core is stabilized by 20 hydride ligands via various (μ3, μ4, μ5)‐H coordination modes and 12 dithiophosphate ligands coordinated either in tetrametallic tetraconnective (η4: μ2, μ2) or trimetallic tetraconnective (η3: μ2, μ2) patterns. The structural motif of 2H showed fascinating correlations with 1H having an elongated triangular orthobicupola framework of eighteen (9x2) copper atoms with an encapsulated linear Cu2 unit along the C3 axis and protected by 11 (μ3, μ4)‐H and 9 dithiophosphate ligands in a tetrametallic tetraconnective (η4: μ2, μ2) mode. The isopropyl derivatives, [Cu32(H)20{S2P(OiPr)2}12], 3H and [Cu20(H)11{S2P(OiPr)2}9], 4H, were used to study H2 evolution under different physico‐chemical conditions and proved to be excellent models for hydrogen storage materials. Additionally, following H2 evolution under sunlight irradiation, mild thermolysis (∼60 oC) and acidification, cluster 3H converted into [Cu8(H){S2P(OiPr)2}6]+, 5H. Intriguingly 5H can react with Cu+ salt in the presence of [BH4]− and re‐form 3H. Cluster 4H also reproducibly re‐formed via the reaction between 5H and [BH4]− from which a continuous cycle of cluster conversion and H2 evolution is proposed. Rhombus‐shaped copper nanoparticles fabricated from further reductions of 3H and 4H showed the intermediary role of metal hydrides in the formation of metal nanoparticles under wet chemical methods.

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Section: Discussionmentioning

confidence: 99%

Section: Discussionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Synthesis, Structural Characterization, and H₂ Evolution Study of a Spheroid‐Shape Hydride‐Rich Copper Nanocluster

et al. 2018

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“…Cu 2 O can be applied in antiseptic, germicide, catalyst and colourant in daily life [1,2]. In the past years, many methods have been used for obtaining Cu 2 O with various morphologies [3][4][5][6][7][8][9]. Many reducing agents such as glucose [10][11][12][13][14][15], ascorbic acid [16][17][18], fructose [19], hydrazine hydrate [20][21][22][23], ureophil [3], glacial acetic acid [24], sodium borohydride [25] and polyol [26] will be introduced when copper salts (Cu 2+ ) are used as raw materials.…”

mentioning

confidence: 99%

Controllable synthesis of cuprite (Cu ₂ O) microcrystals and their shape‐dependent photocatalytic performances

Liu

Zhang

et al. 2018

Micro & Nano Letters

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Microcrystals of cuprite (Cu 2 O) samples exhibiting octahedral and spherical morphologies were synthesised via a facile chemical method and were then characterised by X-ray powder diffraction and scanning electron microscopy. It was observed that the potassium sodium tartrate (KNaC 4 H 4 O 6 •4H 2 O, PST) and gelatin addition had a prominent effect on the morphologies. The possible formation mechanism of Cu 2 O microcrystals was discussed based on the effects of PST and gelatin. Furthermore, the photocatalytic activities of the prepared Cu 2 O microcrystals were investigated by UV-vis spectrophotometry, demonstrating that their behavior was influenced by the different morphologies, and the Cu 2 O microspheres possessed the highest activity.

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“…This remains the most often used route to CuH (Warf & Feitknecht, 1950;Fitzsimons et al, 1995), although other routes have been developed including a sonochemical synthesis (Hasin & Wu, 2012), precipitation of the hydride from pyridine solutions of CuI and LiAlH 4 (Dilts & Shriver, 1968) ISSN 2052-5206 While the products from the Wü rtz and the pyridine methods have been extensively investigated (Korzhavyi et al, 2012;Soroka et al, 2013;Auer & Kohlmann, 2014;Bennett et al, 2015), that produced via equation (1) has been much less studied. This synthetic method results in an insoluble form of CuH, ('CuH/BH 4 '), that is coffee-coloured rather than the rust-red obtained from the Wü rtz synthesis.…”

Section: Introductionmentioning

confidence: 99%

Structure and spectroscopy of CuH preparedviaborohydride reduction

Bennett

Wilson

Murphy

et al. 2015

Acta Crystallogr Sect B

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Copper(I) hydride (cuprous hydride, CuH) was the first binary metal hydride to be discovered (in 1844) and is singular in that it is synthesized in solution, at ambient temperature. There are several synthetic paths to CuH, one of which involves reduction of an aqueous solution of CuSO 4 Á5H 2 O by borohydride ions. The product from this procedure has not been extensively characterized. Using a combination of diffraction methods (X-ray and neutron) and inelastic neutron scattering spectroscopy, we show that the CuH from the borohydride route has the same bulk structure as CuH produced by other routes. Our work shows that the product consists of a core of CuH with a shell of water and that this may be largely replaced by ethanol. This offers the possibility of modifying the properties of CuH produced by aqueous routes.

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Effect of synthesis temperature on the morphology and stability of copper(i) hydride nanoparticles

Cited by 15 publications

References 30 publications

Synthesis, Structural Characterization, and H₂ Evolution Study of a Spheroid‐Shape Hydride‐Rich Copper Nanocluster

Synthesis, Structural Characterization, and H₂ Evolution Study of a Spheroid‐Shape Hydride‐Rich Copper Nanocluster

Controllable synthesis of cuprite (Cu ₂ O) microcrystals and their shape‐dependent photocatalytic performances

Structure and spectroscopy of CuH preparedviaborohydride reduction

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Effect of synthesis temperature on the morphology and stability of copper(i) hydride nanoparticles

Cited by 15 publications

References 30 publications

Synthesis, Structural Characterization, and H2 Evolution Study of a Spheroid‐Shape Hydride‐Rich Copper Nanocluster

Synthesis, Structural Characterization, and H2 Evolution Study of a Spheroid‐Shape Hydride‐Rich Copper Nanocluster

Controllable synthesis of cuprite (Cu 2 O) microcrystals and their shape‐dependent photocatalytic performances

Structure and spectroscopy of CuH preparedviaborohydride reduction

Contact Info

Product

Resources

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Synthesis, Structural Characterization, and H₂ Evolution Study of a Spheroid‐Shape Hydride‐Rich Copper Nanocluster

Synthesis, Structural Characterization, and H₂ Evolution Study of a Spheroid‐Shape Hydride‐Rich Copper Nanocluster

Controllable synthesis of cuprite (Cu ₂ O) microcrystals and their shape‐dependent photocatalytic performances