Optimization of the crystal growth of the superconductor CaKFe4As4 from solution in the FeAs-CaFe2As2-KFe2As2 system

Meier, W. R.; Kong, T.; Bud'ko, S. L.; Canfield, P. C.

doi:10.1103/PhysRevMaterials.1.013401

Title: Optimization of the crystal growth of the superconductor ${CaKFe}_{4} {As}_{4}$ from solution in the $FeAs - {CaFe}_{2} {As}_{2} - {KFe}_{2} {As}_{2}$ system

Journal Article · Mon Jun 19 00:00:00 EDT 2017 · Physical Review Materials

DOI:https://doi.org/10.1103/PhysRevMaterials.1.013401· OSTI ID:1417372

Meier, W. R. ^[1]; Kong, T. ^[2]; Bud'ko, S. L. ^[1]; Canfield, P. C. ^[1]

Ames Lab. and Iowa State Univ., Ames, IA (United States)
Ames Lab. and Iowa State Univ., Ames, IA (United States); Princeton Univ., Princeton, NJ (United States)

Measurements of the anisotropic properties of single crystals play a crucial role in probing the physics of new materials. Determining a growth protocol that yields suitable high-quality single crystals can be particularly challenging for multicomponent compounds. Here we present a case study of how we refined a procedure to grow single crystals of CaKFe₄As₄ from a high temperature, quaternary liquid solution rich in iron and arsenic (“FeAs self-flux”). Temperature dependent resistance and magnetization measurements are emphasized, in addition to the x-ray diffraction, to detect intergrown CaKFe₄As₄, CaFe₂As₂, and KFe₂As₂ within what appear to be single crystals. Guided by the rules of phase equilibria and these data, we adjusted growth parameters to suppress formation of the impurity phases. The resulting optimized procedure yielded phase-pure single crystals of CaKFe₄As₄. In conclusion, this optimization process offers insight into the growth of quaternary compounds and a glimpse of the four-component phase diagram in the pseudoternary FeAs–CaFe₂As₂–KFe₂As₂ system.

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Research Organization:: Ames Lab., Ames, IA (United States)

Sponsoring Organization:: USDOE

Grant/Contract Number:: AC02-07CH11358; GBMF4411

OSTI ID:: 1417372

Alternate ID(s):: OSTI ID: 1364212

Report Number(s):: IS-J-9525; PRMHAR; TRN: US1801051

Journal Information:: Physical Review Materials, Vol. 1, Issue 1; ISSN 2475-9953

Publisher:: American Physical Society (APS)Copyright Statement

Country of Publication:: United States

Language:: English

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Cited by: 59 works

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References (33)

Anisotropic thermodynamic and transport properties of single-crystalline ${CaKFe}_{4} {As}_{4}$ Meier, W. R.; Kong, T.; Kaluarachchi, U. S. Physical Review B, Vol. 94, Issue 6 https://doi.org/10.1103/PhysRevB.94.064501	journal	August 2016
First-order structural phase transition in ${CaFe}_{2} {As}_{2}$ Ni, N.; Nandi, S.; Kreyssig, A. Physical Review B, Vol. 78, Issue 1 https://doi.org/10.1103/PhysRevB.78.014523	journal	July 2008
Use of frit-disc crucibles for routine and exploratory solution growth of single crystalline samples Canfield, Paul C.; Kong, Tai; Kaluarachchi, Udhara S. Philosophical Magazine, Vol. 96, Issue 1 https://doi.org/10.1080/14786435.2015.1122248	journal	December 2015
Anisotropic thermodynamic and transport properties of single-crystalline ${Ba}_{1 - x} K_{x} {Fe}_{2} {As}_{2}$ ( $x = 0$ and 0.45) Ni, N.; Bud’ko, S. L.; Kreyssig, A. Physical Review B, Vol. 78, Issue 1 https://doi.org/10.1103/PhysRevB.78.014507	journal	July 2008
A rigorous proof of the Alkemade theorem Malakhov, Dmitri V. Calphad, Vol. 28, Issue 2 https://doi.org/10.1016/j.calphad.2004.08.002	journal	June 2004
Superconductivity in Hole-Doped (Sr _1−x K _x )Fe ₂ As ₂ Gen-Fu, Chen; Zheng, Li; Gang, Li Chinese Physics Letters, Vol. 25, Issue 9 https://doi.org/10.1088/0256-307X/25/9/083	journal	September 2008
Synthesis and Thermal Stability Studies of CaFe4As3 Yi, Tanghong; Dioguardi, Adam P.; Klavins, Peter European Journal of Inorganic Chemistry, Vol. 2011, Issue 26 https://doi.org/10.1002/ejic.201100349	journal	August 2011
Single Crystal Growth and Characterization of the Iron-Based Superconductor KFe ₂ As ₂ Synthesized by KAs Flux Method Kihou, Kunihiro; Saito, Taku; Ishida, Shigeyuki Journal of the Physical Society of Japan, Vol. 79, Issue 12 https://doi.org/10.1143/JPSJ.79.124713	journal	December 2010
Jump in specific heat at the superconducting transition temperature in $Ba {({Fe}_{1 - x} {Co}_{x})}_{2} {As}_{2}$ and $Ba {({Fe}_{1 - x} {Ni}_{x})}_{2} {As}_{2}$ single crystals Bud’ko, Sergey L.; Ni, Ni; Canfield, Paul C. Physical Review B, Vol. 79, Issue 22 https://doi.org/10.1103/PhysRevB.79.220516	journal	June 2009
High-temperature solution growth of intermetallic single crystals and quasicrystals Canfield, Paul C.; Fisher, Ian R. Journal of Crystal Growth, Vol. 225, Issue 2-4 https://doi.org/10.1016/S0022-0248(01)00827-2	journal	May 2001
New-Structure-Type Fe-Based Superconductors: Ca A Fe ₄ As ₄ ( A = K, Rb, Cs) and Sr A Fe ₄ As ₄ ( A = Rb, Cs) Iyo, Akira; Kawashima, Kenji; Kinjo, Tatsuya Journal of the American Chemical Society, Vol. 138, Issue 10 https://doi.org/10.1021/jacs.5b12571	journal	March 2016
Anisotropic $H_{c 2}$ , thermodynamic and transport measurements, and pressure dependence of $T_{c}$ in $K_{2} {Cr}_{3} {As}_{3}$ single crystals Kong, Tai; Bud'ko, Sergey L.; Canfield, Paul C. Physical Review B, Vol. 91, Issue 2 https://doi.org/10.1103/PhysRevB.91.020507	journal	January 2015
Resistivity and Upper Critical Field in KFe ₂ As ₂ Single Crystals Terashima, Taichi; Kimata, Motoi; Satsukawa, Hidetaka Journal of the Physical Society of Japan, Vol. 78, Issue 6 https://doi.org/10.1143/JPSJ.78.063702	journal	June 2009
Superconducting Fe-Based Compounds $(A_{1 - x} {Sr}_{x}) {Fe}_{2} {As}_{2}$ with $A = K$ and Cs with Transition Temperatures up to 37 K Sasmal, Kalyan; Lv, Bing; Lorenz, Bernd Physical Review Letters, Vol. 101, Issue 10 https://doi.org/10.1103/PhysRevLett.101.107007	journal	September 2008
A magnetic structure investigation of tetragonal (Fe1 − xCox)2 As Önnerud, Per; Andersson, Yvonne; Tellgren, Roland Journal of Magnetism and Magnetic Materials, Vol. 147, Issue 3 https://doi.org/10.1016/0304-8853(95)00018-6	journal	June 1995
Growth of single crystals from metallic fluxes Canfield, P. C.; Fisk, Z. Philosophical Magazine B, Vol. 65, Issue 6 https://doi.org/10.1080/13642819208215073	journal	June 1992
Intrinsic Properties of A Fe ₂ As ₂ ( A = Ba, Sr) Single Crystal under Highly Hydrostatic Pressure Conditions Matsubayashi, Kazuyuki; Katayama, Naoyuki; Ohgushi, Kenya Journal of the Physical Society of Japan, Vol. 78, Issue 7 https://doi.org/10.1143/JPSJ.78.073706	journal	July 2009
X-Ray diffraction on large single crystals using a powder diffractometer Jesche, A.; Fix, M.; Kreyssig, A. Philosophical Magazine, Vol. 96, Issue 20 https://doi.org/10.1080/14786435.2016.1192725	journal	June 2016
Superconductivity and Crystal Structures of (Ba _{1− x} K _x )Fe ₂ As ₂ ( x =0-1) Rotter, Marianne; Pangerl, Michael; Tegel, Marcus Angewandte Chemie International Edition, Vol. 47, Issue 41 https://doi.org/10.1002/anie.200803641	journal	September 2008
Graphische Behandlung einiger thermodynamischen Probleme über Gleichgewichtszustände von Salzlösungen mit festen Phasen Rijn van Alkemade, A. C. van Zeitschrift für Physikalische Chemie, Vol. 11U, Issue 1 https://doi.org/10.1515/zpch-1893-1121	journal	January 1893
High-temperature superconductivity in iron-based materials Paglione, Johnpierre; Greene, Richard L. Nature Physics, Vol. 6, Issue 9 https://doi.org/10.1038/nphys1759	journal	August 2010
Control of magnetic, nonmagnetic, and superconducting states in annealed Ca(Fe $_{1 - x}$ Co $_{x}$ ) $_{2}$ As $_{2}$ Ran, S.; Bud'ko, S. L.; Straszheim, W. E. Physical Review B, Vol. 85, Issue 22 https://doi.org/10.1103/PhysRevB.85.224528	journal	June 2012
Pauli-Limited Multiband Superconductivity in ${KFe}_{2} {As}_{2}$ Zocco, D. A.; Grube, K.; Eilers, F. Physical Review Letters, Vol. 111, Issue 5 https://doi.org/10.1103/PhysRevLett.111.057007	journal	August 2013
Superconductivity at 26 K in (Ca _{1- x} Na _x )Fe ₂ As ₂ Shirage, Parasharam Maruti; Miyazawa, Kiichi; Kito, Hijiri Applied Physics Express, Vol. 1 https://doi.org/10.1143/APEX.1.081702	journal	August 2008
Upper critical field, anisotropy, and superconducting properties of ${Ba}_{1 - x} K_{x} {Fe}_{2} {As}_{2}$ single crystals Wang, Zhao-Sheng; Luo, Hui-Qian; Ren, Cong Physical Review B, Vol. 78, Issue 14 https://doi.org/10.1103/PhysRevB.78.140501	journal	October 2008
Superconductivity at 23 K and low anisotropy in Rb-substituted ${BaFe}_{2} {As}_{2}$ single crystals Bukowski, Z.; Weyeneth, S.; Puzniak, R. Physical Review B, Vol. 79, Issue 10 https://doi.org/10.1103/PhysRevB.79.104521	journal	March 2009
Comprehensive scenario for single-crystal growth and doping dependence of resistivity and anisotropic upper critical fields in (Ba $_{1 - x}$ K $_{x}$ )Fe $_{2}$ As $_{2}$ ( $0.22 \leq x \leq 1$ ) Liu, Y.; Tanatar, M. A.; Straszheim, W. E. Physical Review B, Vol. 89, Issue 13 https://doi.org/10.1103/PhysRevB.89.134504	journal	April 2014
Synthesis and Thermal Stability Studies of CaFe4As3 Yi, Tanghong; Dioguardi, Adam P.; Klavins, Peter European Journal of Inorganic Chemistry, Vol. 2011, Issue 32 https://doi.org/10.1002/ejic.201101030	journal	October 2011
Superconductivity at 23 K and low anisotropy in Rb-substituted BaFe2As2 single crystals Bukowski, Z.; Weyeneth, S.; Punziak, R. American Physical Society https://doi.org/10.5167/uzh-18268	text	January 2009
Superconductivity and Crystal Structures of (Ba1-xKx)Fe2As2 (x = 0 - 1) Rotter, Marianne; Pangerl, Michael; Tegel, Marcus arXiv https://doi.org/10.48550/arxiv.0807.4096	text	January 2008
High-temperature superconductivity in iron-based materials Paglione, Johnpierre; Greene, Richard L. arXiv https://doi.org/10.48550/arxiv.1006.4618	text	January 2010
Use of frit-disc crucibles for routine and exploratory solution growth of single crystalline samples Canfield, Paul C.; Kong, Tai; Kaluarachchi, Udhara S. arXiv https://doi.org/10.48550/arxiv.1509.08131	text	January 2015
X-Ray diffraction on large single crystals using a powder diffractometer Jesche, A.; Fix, M.; Kreyssig, A. arXiv https://doi.org/10.48550/arxiv.1605.02549	text	January 2016

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Unique defect structure and advantageous vortex pinning properties in superconducting CaKFe4As4 Ishida, Shigeyuki; Iyo, Akira; Ogino, Hiraku npj Quantum Materials, Vol. 4, Issue 1 https://doi.org/10.1038/s41535-019-0165-0	journal	June 2019
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Optimization of superconducting properties of the stoichiometric CaKFe ₄ As ₄ Singh, Shiv J.; Cassidy, Simon J.; Bristow, Matthew Superconductor Science and Technology, Vol. 33, Issue 2 https://doi.org/10.1088/1361-6668/ab58be	journal	December 2019
Enhancement of critical current density in CaKFe ₄ As ₄ single crystals through 3 MeV proton irradiation Haberkorn, N.; Xu, M.; Meier, W. R. Superconductor Science and Technology, Vol. 33, Issue 2 https://doi.org/10.1088/1361-6668/ab5f4b	journal	January 2020
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Odd and Even Modes of Neutron Spin Resonance in the Bilayer Iron-Based Superconductor ${CaKFe}_{4} {As}_{4}$ Xie, Tao; Wei, Yuan; Gong, Dongliang Physical Review Letters, Vol. 120, Issue 26 https://doi.org/10.1103/physrevlett.120.267003	journal	June 2018
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Ultrahigh Elastically Compressible and Strain-Engineerable Intermetallic Compounds Under Uniaxial Mechanical Loading Song, Gyuho; Borisov, Vladislav; Meier, William R. arXiv https://doi.org/10.48550/arxiv.1904.02256	preprint	January 2019
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Title: Optimization of the crystal growth of the superconductor ${CaKFe}_{4} {As}_{4}$ from solution in the $FeAs - {CaFe}_{2} {As}_{2} - {KFe}_{2} {As}_{2}$ system