Ammonothermal Synthesis and Crystal Growth of the Chain‐type Oxonitridosilicate Ca1+xY1–xSiN3–xOx (x &gt; 0)

Mallmann, Mathias; Maak, Christian; Schnick, Wolfgang

doi:10.1002/zaac.202000018

Cited by 3 publications

(3 citation statements)

References 41 publications

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“…Be was reported form soluble intermediates [175] with NaN3 as the mineralizer, while C was known to be transported as an impurity with both NaNH2 [145] and KNH2 [176]. Ca formed compounds which were not reported to be transported in cases of NaN3 [177] and LiNH2 [178], whereas Cd [119] and Cr react similarly [179] in a KNH2 environment. Co shows higher corrosion resistance in a NaNH2 environment in both elemental and alloy forms [147].…”

Section: Ammonobasic Conditionsmentioning

confidence: 99%

“…More recently, cobalt-based alloys have been considered [166,304], as the system Co-Al-W provides the opportunity to harden the alloys by the precipitation of the ordered phase (γ′) in the Co solid solution matrix phase (γ), and the higher melting point of Co results in high liquidus and solidus temperatures [166]. Aiming for higher temperatures at the expense of maximum operating pressure, the molybdenum-based alloy titanium-zirconium-molybdenum (TZM) [164] and the nickel-base alloy Haynes 282 [177,186,301,305,306] have been used for ammonothermal autoclaves. For comparison, an iron-based alloy with high mechanical strength at elevated temperatures is also shown in Figure 16.…”

Section: General Design Considerationsmentioning

confidence: 99%

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Ammonothermal Crystal Growth of Functional Nitrides for Semiconductor Devices: Status and Potential

Wostatek,

Chirala,

Stoddard

et al. 2024

Materials

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The state-of-the-art ammonothermal method for the growth of nitrides is reviewed here, with an emphasis on binary and ternary nitrides beyond GaN. A wide range of relevant aspects are covered, from fundamental autoclave technology, to reactivity and solubility of elements, to synthesized crystalline nitride materials and their properties. Initially, the potential of emerging and novel nitrides is discussed, motivating their synthesis in single crystal form. This is followed by a summary of our current understanding of the reactivity/solubility of species and the state-of-the-art single crystal synthesis for GaN, AlN, AlGaN, BN, InN, and, more generally, ternary and higher order nitrides. Investigation of the synthesized materials is presented, with a focus on point defects (impurities, native defects including hydrogenated vacancies) based on GaN and potential pathways for their mitigation or circumvention for achieving a wide range of controllable functional and structural material properties. Lastly, recent developments in autoclave technology are reviewed, based on GaN, with a focus on advances in development of in situ technologies, including in situ temperature measurements, optical absorption via UV/Vis spectroscopy, imaging of the solution and crystals via optical (visible, X-ray), along with use of X-ray computed tomography and diffraction. While time intensive to develop, these technologies are now capable of offering unprecedented insight into the autoclave and, hence, facilitating the rapid exploration of novel nitride synthesis using the ammonothermal method.

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Section: Ammonobasic Conditionsmentioning

confidence: 99%

Section: General Design Considerationsmentioning

confidence: 99%

Ammonothermal Crystal Growth of Functional Nitrides for Semiconductor Devices: Status and Potential

Wostatek,

Chirala,

Stoddard

et al. 2024

Materials

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“…[4] The ammonothermal synthesis proved to be suitable for obtaining the nitridosilicates MSi 2 N 3 (M = Li, Na), MSiN 2 (M = Zn, Mg, Mn) and their solid solutions, CaGaSiN 3 as well as the oxonitridosilicate Ca 1 + x Y 1À x SiN 1À x O x (x > 0). [5][6][7][8][9][10] For NaSi 2 N 3 , CaGaSiN 3 and Ca 1 + x Y 1À x SiN 1À x O x , the synthesis was only possible using the ammonothermal route. In these syntheses, the elemental silicon was activated in situ by the use of alkali-metalcontaining mineralizers.…”

Section: Introductionmentioning

confidence: 99%

Ammonothermal Synthesis and Solid‐State NMR Study of the Imidonitridosilicate Rb₃Si₆N₅(NH)₆

Engelsberger,

Chau,

Bräuniger

et al. 2024

Chemistry A European J

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The imidonitridosilicate Rb3Si6N5(NH)6, being only the second representative of this compound class, was synthesized ammonothermally at 870 K and 230 MPa. Its crystal structure was solved from single‐crystal X‐ray diffraction data. The imidonitridosilicate crystallizes isotypically with the respective potassium compound in space group P4132 with the lattice parameter a = 10.9422(4) Å forming a three‐dimensional imidonitridosilicate tetrahedra network with voids for the rubidium ions. The structure model and the presence of the imide groups were verified by Fourier‐Transform infrared (FTIR) and magic‐angle spinning (MAS) NMR spectroscopy, using cross polarization 15N{1H} and 29Si{1H} MAS NMR experiments. Rb3Si6N5(NH)6 represents a possible intermediate during the ammonothermal synthesis of nitridosilicates. The characterization of these intermediates improves the understanding of the reaction pathway from ammonothermal solutions to nitrides. Thus, the ammonothermal synthesis is an alternative approach to the well‐established high‐temperature synthesis leading to the compound class of nitridosilicates.

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Nitride Zeolites from Ammonothermal Synthesis

Engelsberger,

Schnick

2024

Chemistry A European J

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Oxide zeolites are synthesized from aqueous solutions in an established way employing hydrothermal synthesis. Transferring this approach to nitride zeolites requires a solvent providing nitrogen for which ammonia has proven to be particularly suitable. We present the successful ammonothermal synthesis of the (oxo)nitridosilicate compounds Ce3[Si6N11], Li2RE4[Si4N8]O3 (RE = La, Ce) and K1.25Ce7.75[Si11N21O2]O0.75. Within this procedure, the usage of supercritical ammonia as a solvent as well as the utilization of the mineralizers NaN3, Li3N and KN3, respectively, allowed the targeted synthesis of large single crystals. Formation of these (oxo)nitridosilicates depend mainly on the employed mineralizer despite their similar degree of condensation. The three compounds were structurally characterized using X‐ray diffraction and their crystal structures contain a wide range of different ring sizes within their tetrahedra networks. The zeolite(‐like) crystal structures are elucidated and compared to known nitridosilicate representatives of the respective structure types. Their elemental composition was investigated using energy‐dispersive X‐ray (EDX) spectroscopy and incorporation of the O rather than N−H functionality was confirmed by Fourier‐Transform infrared (FTIR) spectroscopy as well as by charge distribution (CHARDI) and bond valence sum (BVS) calculations. The presented examples demonstrate that ammonothermal synthesis provides a one‐step access from elemental starting materials towards nitride zeolites.

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Ammonothermal Synthesis and Crystal Growth of the Chain‐type Oxonitridosilicate Ca_1+xY_1–xSiN_3–xO_x (x > 0)

Cited by 3 publications

References 41 publications

Ammonothermal Crystal Growth of Functional Nitrides for Semiconductor Devices: Status and Potential

Ammonothermal Crystal Growth of Functional Nitrides for Semiconductor Devices: Status and Potential

Ammonothermal Synthesis and Solid‐State NMR Study of the Imidonitridosilicate Rb₃Si₆N₅(NH)₆

Nitride Zeolites from Ammonothermal Synthesis

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Ammonothermal Synthesis and Crystal Growth of the Chain‐type Oxonitridosilicate Ca1+xY1–xSiN3–xOx (x > 0)

Cited by 3 publications

References 41 publications

Ammonothermal Crystal Growth of Functional Nitrides for Semiconductor Devices: Status and Potential

Ammonothermal Crystal Growth of Functional Nitrides for Semiconductor Devices: Status and Potential

Ammonothermal Synthesis and Solid‐State NMR Study of the Imidonitridosilicate Rb3Si6N5(NH)6

Nitride Zeolites from Ammonothermal Synthesis

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Ammonothermal Synthesis and Crystal Growth of the Chain‐type Oxonitridosilicate Ca_1+xY_1–xSiN_3–xO_x (x > 0)

Ammonothermal Synthesis and Solid‐State NMR Study of the Imidonitridosilicate Rb₃Si₆N₅(NH)₆