Low-temperature synthesis of superconducting iron selenide using a triphenylphosphine flux†,Dalton Transactions

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Low-temperature synthesis of superconducting iron selenide using a triphenylphosphine flux†
Dalton Transactions ( IF 3.5 ) Pub Date : 2019-10-08 , DOI: 10.1039/c9dt03723c
M. Jewels Fallon _{1,

2,

3,

4} , Andrew J. Martinolich _{1,

2,

3,

4} , Annalise E. Maughan _{1,

2,

3,

4} , Leighanne C. Gallington _{4,

5,

6,

7} , James R. Neilson _{1,

2,

3,

4}

Affiliation

Many functional materials have relatively low decomposition temperatures (T ≤ 400 °C), which makes their synthesis challenging using conventional high-temperature solid-state chemistry. Therefore, non-conventional techniques such as metathesis, hydrothermal, and solution chemistry are often employed to access low-temperature phases; the discovery of new chemistries is needed to expand access to these phases. This contribution discusses the use of triphenylphosphine (PPh₃) as a molten flux to synthesize superconducting iron selenide (Fe_1+δSe) at low temperature (T = 325 °C). Powder X-ray diffraction and magnetism measurements confirm the successful formation of superconducting iron selenide while nuclear magnetic resonance spectroscopy and in situ X-ray diffraction show that the formation of superconducting FeSe at low temperatures is enabled by an adduct between the triphenylphosphine and selenium. Exploration of the Fe–Se–PPh₃ phase space indicates that the PPh₃–Se adduct effectively reduces the chemical potential of the selenium at high concentrations of triphenylphosphine. This contribution demonstrates that the use of a poorly-solvating yet reactive flux has the potential to enable the synthesis of new low-temperature phases of solid materials.

中文翻译：

三苯基膦助熔剂的低温合成超导硒化铁†

许多功能材料具有相对低的分解温度（Ť ≤400℃），这使得它们的合成利用常规的高温固态化学挑战。因此，通常采用复分解，水热和溶液化学等非常规技术来进入低温相。需要发现新的化学物质以扩大进入这些阶段的机会。这种贡献讨论了使用三苯基膦（PPH ₃），其为熔化的助熔剂，以合成超导硒化铁（铁_{1+ δ}低温硒）（Ť= 325°C）。粉末X射线衍射和磁性测量结果证实了超导硒化铁的成功形成，而核磁共振波谱和原位X射线衍射表明，三苯基膦与硒之间的加合物能够在低温下形成超导FeSe。Fe-Se-PPh ₃相空间的探索表明，PPh ₃ -Se加合物有效降低了高浓度三苯膦中硒的化学势。这一贡献表明，使用不良溶剂化但反应性较弱的助焊剂具有潜力，可以合成固体材料的新的低温相。

更新日期：2019-11-06

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