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Nanoscaled Metal Borides and Phosphides: Recent Developments Review pubs.acs.org/CR Nanoscaled Metal Borides and Phosphides: Recent Developments and Perspectives Sophie Carenco,†,‡,§,∥,⊥ David Portehault,*,†,‡,§ Cedrić Boissiere,̀†,‡,§ Nicolas Mezailles,́ ∥,# and Clement́ Sanchez*,†,‡,§ † Chimie de la Matierè Condenseé de Paris, UPMC Univ Paris 06, UMR 7574, Collegè de France, 11 Place Marcelin Berthelot, 75231 Paris Cedex 05, France ‡ Chimie de la Matierè Condenseé de Paris, CNRS, UMR 77574, Collegè de France, 11 Place Marcellin Berthelot, 75231 Paris Cedex 05, France § Chimie de la Matierè Condenseé de Paris, Collegè de France, 11 Place Marcellin Berthelot, 75231 Paris Cedex 05, France ∥ Laboratory Heteroelements and Coordination, Chemistry Department, Ecole Polytechnique, CNRS-UMR 7653, Palaiseau, France 2.5.3. Metal−Metalloid Bonds: From Cova- lency to Ionicity K 2.5.4. Electrical Behavior of Bulk MBs and MPs L 2.6. From Bulk to Nanoscale MPs and MBs: Characterization Tools L 2.6.1. Chemical Analysis M 2.6.2. X-ray and Neutron Diffraction M 2.6.3. Electron Microscopy N 2.6.4. X-ray Photoelectron Spectroscopy (XPS), Auger Electron Spectroscopy (AES), and X-ray Absorption Spectroscopy (XANES, EXAFS) N 2.6.5. Electron Energy Loss Spectroscopy CONTENTS (EELS) O 2.6.6. Nuclear Magnetic Resonance (NMR) 1. Introduction C Spectroscopy and ab Initio Calculations O 2. Introductory Background D 3. Nanoscaled Metal Borides Q 2.1. Nomenclature D 3.1. Variety of Boron Precursors R 2.2. Instructive Genesis of Metal Phosphides and 3.1.1. Metal−Boron Alloys and Metal Borides R Metal Borides D 3.1.2. Elemental Boron R 2.2.1. Metal Borides: A Challenging Topic in 3.1.3. Boranes R Materials Synthesis D 3.1.4. Borohydrides S 2.2.2. Metal Phosphides: Materials from the 3.1.5. Boron Halogenides S New Era of Chemistry F 3.1.6. Boron−Oxygen Species (Boron Oxide 2.3. Metal Boride and Metal Phosphide Crystallo- and Boric Acid) S graphic Structures G 3.1.7. Molecular Single Source T 2.3.1. Metal Boride Crystallographic Structures G 3.2. Deposition from a Reactive Vapor Phase T 2.3.2. Metal Phosphide Crystallographic Struc- 3.2.1. General Considerations on the Thermal tures H Decomposition of Boranes T 2.4. Quest for Original Structures: Latest Devel- 3.2.2. Boriding Metal Films T opments I 3.2.3. Non-Nanostructured Thin Films U 2.4.1. New Developments for Bulk Metal 3.2.4. CVD for Growth of 1D Nanostructures V Borides I 3.2.5. CVD, PLD, and HPCVD for MgB2 Nano- 2.4.2. New Developments for Bulk Metal structures X Phosphides I 3.2.6. Alternative Processes toward Other 2.4.3. Contribution of Calculations: Thermody- Nanostructured Films Z namics, New Phases, and Properties J 3.3. Solid State Syntheses AA 2.5. Bonding and Electronic Structure in Metal 3.3.1. Reduction of Nanostructured Metal Borides and Phosphides J Oxides AA 2.5.1. Case in Point: Cobalt Monoboride and Monophosphide J 2.5.2. Metal−Metal and Metalloid−Metalloid Bonds K Received: January 16, 2013 © XXXX American Chemical Society A dx.doi.org/10.1021/cr400020d | Chem. Rev. XXXX, XXX, XXX−XXX Chemical Reviews Review 3.3.2. Solid State Reactions under Autogenic 4.6. Alternative to TOP: Other Alkyl- and Pressure AB Arylphosphines AW 3.3.3. Mechanosynthesis AD 4.7. Elemental Phosphorus AW 3.4. Preceramic Routes AE 4.7.1. White Phosphorus P4 AX 3.4.1. Carboreduction in Physical Mixtures of 4.7.2. Red Phosphorus AY Metal Oxide, Boron Oxide or Boric Acid, 4.8. Alternative Phosphorus Sources AZ and Carbon AE 4.9. Alternative Processes AZ 3.4.2. Carboreduction in Mixtures of Metal 4.10. Summary for Nanoscaled Metal Phos- Oxides and B-Containing Polymers AE phides AZ 3.4.3. Carboreduction in Metal and Boron 5. Properties of Nanoscaled Metal Borides and Hybrid Oxo-Gels AE Metal Phosphides BA 3.5. Liquid Phase Syntheses in High Temper- 5.1. Li-Ion Batteries BA ature (>1000 °C) Flux AF 5.1.1. Overview BA 3.6. Liquid Phase Syntheses under Autogenous 5.1.2. Major Advances in the Field: The Case of Pressure AF Metal Phosphides BA 3.6.1. Salt Melts under Autogenous Pressure AF 5.1.3. Nanostructuration of the Electrodes BA 3.6.2. Organic Solvents under Autogenous 5.2. Alkaline Aqueous Batteries BA Pressure AG 5.2.1. Primary Alkaline Batteries BA 3.6.3. Liquid Reactants under Autogenous 5.2.2. Secondary Alkaline Batteries BB Pressure AG 5.3. Catalysis BB 3.7. Low Temperature and Atmospheric Pressure 5.3.1. Hydrogenation: A Driving Force toward Colloidal Syntheses of Crystalline Metal Metal Boride and Metal Phosphide Boride Nanostructures AG Nanoparticles BB 3.7.1. Salt Melts under Atmospheric Pressure AH 5.3.2. Hydrotreating Reactions BD 3.7.2. Organic Solvents under Atmospheric 5.3.3. Hydrogen Generation BF Pressure AJ 5.3.4. Other Dissociative Reactions BG 3.8. Low Temperature Colloidal Syntheses of 5.3.5. Associative Reactions BG Amorphous Metal Borides AJ 5.4. Electrochemical and Photoelectrochemical 3.8.1. Synthesis of Amorphous Metal Boride Devices BH Nanoparticles in Water AJ 5.5. Initiation of Nanotubes and Nanowires 3.8.2. Synthesis of Amorphous Metal Boride Growth BH Nanoparticles in Organic Solvents AK 5.6. Electronics BH 3.8.3. Nature of the Amorphous Boride Nano- 5.7. Optics BI particles AL 5.8. Magnetism BI 3.8.4. Tuned Nanostructures of Amorphous 5.9. Mechanical Properties BJ Metal Boride Alloys AM 5.10. Biology, Medicine, Toxicology, and Envi- 3.8.5. Borane Adducts: Beyond Borohydrides ronmental Applications BJ for the Production of Nanostructures of 5.11. Metal Phosphides and Metal Borides as Amorphous Metal Borides AN Fortuitous Compounds and Other Less 3.8.6. Supported Systems AO Defined Compounds BJ 3.9. Summary for Nanoscaled Metal Borides AO 6. Conclusive Perspectives BK 4. Nanoscaled Metal Phosphides AO 6.1. Toward New Compositions and Crystal 4.1. From Bulk to Nanoscaled Metal Phosphides AO Structures BK 4.2. Short Historic Introduction: Why MP Nano- 6.1.1. Amorphous State versus Crystalline particles? AO State BK 4.2.1. Beyond III−V Semiconductors AP 6.1.2. Control of the Stoichiometry BK 4.2.2. Quantum Effects in III−V Semiconduc- 6.1.3. Control of Polymorphism BL tors: Toward Nanoscaled Metal Phos- 6.2. P and B Sources: An Essential Struggle BL phides AP 6.2.1. Oxidation Degree of the Phosphorus 4.3. Colloidal Syntheses from Single-Source Source BL Precursors AQ 6.2.2. Oxidation Degree and Reactivity of the “ ” 4.4. Substitutes for PH3 as Safer P Donors AQ Boron Source BM 4.4.1. In Situ and ex Situ PH3 Generation AQ 6.3. Toward Advanced Morphologies and Com- 4.4.2. P(SiMe3)3 as a Highly Reactive Alter- plex Nanostructures BM native to PH3 AQ 6.3.1. Reactivity of the P Source for the 4.5. Tri-n-octylphoshine (TOP): A Versatile “P” Preparation of Advanced Morphologies BM Source AS 6.3.2. Toward Complex Structures: Janus 4.5.1. Reaction of TOP with M(0) Precursors AS Nanoparticles as an Example of the 4.5.2. Widening the Scope of the Reactivity of Power of Colloidal Synthesis BN TOP AS 6.3.3. Homogeneous versus Heterogeneous 4.5.3. Knowledge or Know-How? AU Nucleation: A “Trick” To Overcome 4.5.4. Recent Mechanistic Studies AU Boron Lack of Reactivity BN B dx.doi.org/10.1021/cr400020d | Chem. Rev. XXXX, XXX, XXX−XXX Chemical Reviews Review 6.4. Surface State, Surface Oxidation, and Other Chemical colloidal routes toward nanophosphides are Surface Passivation BO currently developed, and the resulting nanoparticles reach a 6.5. Mechanistic Studies and Trails for the high degree of sophistication in terms of composition, crystal Design of New Synthetic Routes BO structure, monodispersity, and morphology, as exemplified by − 6.5. Novel Properties and Fields of Applied the ones using tri-n-octylphopshine as a “P” source.41 48 Many Research: The Potential Fate of Nanostruc- innovative approaches have been and still are being explored, tured MBs and MPs as Nanomaterials BO including the choice of highly reactive metal and phosphorus Author Information BP precursors.49,50 However, a sound understanding of reaction Corresponding Author BP pathways is still missing, although it is mandatory to trigger a Present Addresses BP rational improvement of these routes and to identify new levers Notes BP for an accurate control of the resulting materials. In Biographies BP comparison, nanoborides seem still in their infancy: colloidal Acknowledgments BQ routes have addressed amorphous nanoparticles, but very few − References BQ attain nanocrystalline state.51 56 Therefore, materials chemists are relying on more expensive approaches involving hard-to- handle gaseous precursors,57 pressurized vessels,34 high energy 1. INTRODUCTION ball-milling,58 etc. Besides cost issues, one of the main The quest for nanoscaling has extended beyond traditional ffi − di culties of these methods is the challenge of tuning the metal oxides1 4 and metal(0),5 as exemplified by the huge final nanomaterial characteristics. Indeed, the key experimental development of “quantum dots” chalcogenide nanoparticles, in levers are not readily accessible and cannot be easily adjusted, 6−9 terms of both preparative methods and applications. During thus resulting in mainly sub-micrometer-size particles. Although the past decade, less common nanoscaled nitrides and carbides these systems are not strictly nanoscaled (many of them do not were also investigated. Their tremendous catalytic properties bear any dimension below 100 nm), they will be considered in were a driving force for innovative research targeting novel 10 this review, because they are the object of most current nanomaterials, which resulted from original fabrication routes.
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