Ammonothermal Synthesis of Alkali‐Alkaline Earth Metal and Alkali‐Rare Earth Metal Carbodiimides: K5–xMx(CN2)2+x(HCN2)1–x(M= Sr, Eu) and Na4.32Sr0.68(CN2)2.68(HCN2)0.32

Mallmann, Mathias; Häusler, Jonas; Cordes, Niklas; Schnick, Wolfgang

doi:10.1002/zaac.201700238

Cited by 8 publications

(7 citation statements)

References 50 publications

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“…Synthesis of Eu(NH 2 ) 2 : Eu(NH 2 ) 2 was synthesized ammonothermally starting from Eu metal (99.99 %, smart elements). The experiment was carried out analogously to the synthesis described in literature …”

Section: Methodsmentioning

confidence: 99%

Sr₃P₃N₇: Complementary Approach by Ammonothermal and High‐Pressure Syntheses

Mallmann

Wendl

Strobel

et al. 2020

Chemistry A European J

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Nitridophosphates exhibit an intriguing structural diversity with different structuralm otifs, for example, chains, layers or frameworks. In this contribution the novel nitridophosphate Sr 3 P 3 N 7 with unprecedented dreier double chains is presented. Crystalline powders were synthesized using the ammonothermal method, while single crystals wereo btained by ah igh-pressurem ultianvil technique. The crystal structure of Sr 3 P 3 N 7 was solved and refinedf rom single-crystal X-ray diffraction and confirmed by powderX -ray meth-ods. Sr 3 P 3 N 7 crystallizes in monoclinic space group P2/c. Energy-dispersive X-ray and Fourier-transformed infrared spectroscopy were conducted to confirm the chemical composition, as well as the absence of NH x functionality. Theo ptical band gap was estimated to be 4.4 eV using diffuse re-flectanceU V/Vis spectroscopy.U pon doping with Eu 2 + , Sr 3 P 3 N 7 showsabroad deep-red to infrared emission (l em = 681 nm, fwhm % 3402 cm À1 )w ith an internal quantum efficiencyo f42%.

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Section: Methodsmentioning

confidence: 99%

Sr₃P₃N₇: Complementary Approach by Ammonothermal and High‐Pressure Syntheses

Mallmann

Wendl

Strobel

et al. 2020

Chemistry A European J

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“…[10] Furthermore, the ammonothermal methodw as used for synthesis of other nitrides, oxonitrides, and other compounds with crystallites in the mmr ange. [11][12][13] Accordingly,t he ammonothermal method could be applicable for synthesis and crystal growth of other nitrides, like phosphorus nitrides and nitridophosphates,w here single crystals are often hard to access. [14] Am ajor challenge regarding the synthesis of phosphorus nitrides and nitridophosphates is the limited thermals tability and the low decomposition temperature of P 3 N 5 (1070K).…”

Section: Introductionmentioning

confidence: 99%

Ammonothermal Synthesis, Optical Properties, and DFT Calculations of Mg₂PN₃ and Zn₂PN₃

Mallmann

Maak

Niklaus

et al. 2018

Chemistry A European J

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The phosphorus nitrides, Mg PN and Zn PN , are wide band gap semiconductor materials with potential for application in (opto)electronics or photovoltaics. For the first time, both compounds were synthesized ammonothermally in custom-built high-temperature, high-pressure autoclaves starting from P N and the corresponding metals (Mg or Zn). Alkali amides (NaNH , KNH ) were employed as ammonobasic mineralizers to increase solubility of the starting materials in supercritical ammonia through formation of reactive intermediates. Single crystals of Mg PN , with length up to 30 μm, were synthesized at 1070 K and 140 MPa. Zn PN already decomposes at these conditions and was obtained as submicron-sized crystallites at 800 K and 200 MPa. Both compounds crystallize in a wurtzite-type superstructure in orthorhombic space group Cmc2 , which was confirmed by powder X-ray diffraction. In addition, single-crystal X-ray diffraction measurements of Mg PN were carried out for the first time. To our knowledge, this is the first single-crystal X-ray study of ternary nitrides synthesized by the ammonothermal method. The band gaps of both nitrides were estimated to be 5.0 eV for Mg PN and 3.7 eV for Zn PN by diffuse reflectance spectroscopy. DFT calculations were carried out to verify the experimental values. Furthermore, a dissolution experiment was conducted to obtain insights into the crystallization behavior of Mg PN .

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“…Synthesis of Eu(NH 2 ) 2 : Eu(NH 2 ) 2 was synthesized starting from Eu metal (99.99 %, smart elements) in supercritical ammonia according to the synthesis described in literature …”

Section: Methodsmentioning

confidence: 99%

Ammonothermal Synthesis of Ba₂PO₃N – An Oxonitridophosphate with Non‐Condensed PO₃N Tetrahedra

et al. 2020

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The ortho‐oxonitridophosphate Ba2PO3N was synthesized under ammonobasic conditions (T = 1070 K, p = 120 MPa) in custom‐built high‐temperature autoclaves, starting from red phosphorus, BaO, NaN3 and KOH. Thus, single crystals of up to several hundred µm were obtained, which were used for single‐crystal X‐ray diffraction. Ba2PO3N [Pnma (no. 62), a = 7.596(2), b = 5.796(1), c = 10.212(3) Å, Z = 4] crystallizes in the β‐K2SO4 structure type with non‐condensed [PO3N]4– ions and is isotypic to its lighter homologues EA2PO3N (EA = Ca, Sr). Powder X‐ray diffraction, energy dispersive X‐ray and Fourier Transformed Infrared spectroscopy corroborate the crystal structure. The optical band gap was determined by means of diffuse reflectance UV/Vis spectroscopy to be 4.3 eV. Eu2+ doped samples show green luminescence (λem = 534 nm, fwhm = 85 nm/2961 cm–1) when irradiated with UV light (λexc = 420 nm). However, Ba2PO3N:Eu2+ shows strong thermal quenching, even at room temperature.

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Ammonothermal Synthesis of Alkali‐Alkaline Earth Metal and Alkali‐Rare Earth Metal Carbodiimides: K_5–_xM_x(CN₂)_2+x(HCN₂)_1–x(M= Sr, Eu) and Na_4.32Sr_0.68(CN₂)_2.68(HCN₂)_0.32

Cited by 8 publications

References 50 publications

Sr₃P₃N₇: Complementary Approach by Ammonothermal and High‐Pressure Syntheses

Sr₃P₃N₇: Complementary Approach by Ammonothermal and High‐Pressure Syntheses

Ammonothermal Synthesis, Optical Properties, and DFT Calculations of Mg₂PN₃ and Zn₂PN₃

Ammonothermal Synthesis of Ba₂PO₃N – An Oxonitridophosphate with Non‐Condensed PO₃N Tetrahedra

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Ammonothermal Synthesis of Alkali‐Alkaline Earth Metal and Alkali‐Rare Earth Metal Carbodiimides: K5–xMx(CN2)2+x(HCN2)1–x(M= Sr, Eu) and Na4.32Sr0.68(CN2)2.68(HCN2)0.32

Cited by 8 publications

References 50 publications

Sr3P3N7: Complementary Approach by Ammonothermal and High‐Pressure Syntheses

Sr3P3N7: Complementary Approach by Ammonothermal and High‐Pressure Syntheses

Ammonothermal Synthesis, Optical Properties, and DFT Calculations of Mg2PN3 and Zn2PN3

Ammonothermal Synthesis of Ba2PO3N – An Oxonitridophosphate with Non‐Condensed PO3N Tetrahedra

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Ammonothermal Synthesis of Alkali‐Alkaline Earth Metal and Alkali‐Rare Earth Metal Carbodiimides: K_5–_xM_x(CN₂)_2+x(HCN₂)_1–x(M= Sr, Eu) and Na_4.32Sr_0.68(CN₂)_2.68(HCN₂)_0.32

Sr₃P₃N₇: Complementary Approach by Ammonothermal and High‐Pressure Syntheses

Sr₃P₃N₇: Complementary Approach by Ammonothermal and High‐Pressure Syntheses

Ammonothermal Synthesis, Optical Properties, and DFT Calculations of Mg₂PN₃ and Zn₂PN₃

Ammonothermal Synthesis of Ba₂PO₃N – An Oxonitridophosphate with Non‐Condensed PO₃N Tetrahedra