Rapid formation of phase-clean 110 K (Bi-2223) powders derived via freeze-drying process

Balachandran, Uthamalingam

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Title: Rapid formation of phase-clean 110 K (Bi-2223) powders derived via freeze-drying process

Abstract

A process for the preparation of amorphous precursor powders for Pb-doped Bi.sub.2 Sr.sub.2 Ca.sub.2 Cu.sub.3 O.sub.x (2223) includes a freeze-drying process incorporating a splat-freezing step. The process generally includes splat freezing a nitrate solution of Bi, Pb, Sr, Ca, and Cu to form flakes of the solution without any phase separation; grinding the frozen flakes to form a powder; freeze-drying the frozen powder; heating the dried powder to form a dry green precursor powders; denitrating the green-powders; heating the denitrated powders to form phase-clean Bi-2223 powders. The grain boundaries of the 2223 grains appear to be clean, leading to good intergrain contact between 2223 grains.

Inventors:

Balachandran, Uthamalingam ^[1]

Hinsdale, IL

Issue Date:: 1996-01-01

Research Org.:: Argonne National Laboratory (ANL), Argonne, IL (United States)

OSTI Identifier:: 870443

Patent Number(s):: 5523285

Assignee:: United States of America as represented by United States (Washington, DC)

Patent Classifications (CPCs):: C - CHEMISTRY C01 - INORGANIC CHEMISTRY C01G - COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F

C - CHEMISTRY C01 - INORGANIC CHEMISTRY C01P - INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

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C - CHEMISTRY C01 - INORGANIC CHEMISTRY C01G - COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
C01G29/006 - {Compounds containing, besides bismuth, two or more other elements, with the exception of oxygen or hydrogen}

C - CHEMISTRY C01 - INORGANIC CHEMISTRY C01P - INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
C01P2002/02 - Amorphous compounds
C01P2002/54 - one element only
C01P2002/72 - by d-values or two theta-values, e.g. as X-ray diagram
C01P2002/88 - by thermal analysis data, e.g. TGA, DTA, DSC
C01P2004/03 - obtained by SEM
C01P2004/04 - obtained by TEM, STEM, STM or AFM

Y - NEW / CROSS SECTIONAL TECHNOLOGIES Y10 - TECHNICAL SUBJECTS COVERED BY FORMER USPC Y10S - TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
Y10S505/733 - Rapid solidification, e.g. quenching, gas-atomizing, melt-spinning, roller-quenching
Y10S505/737 - From inorganic salt precursors, e.g. nitrates
Y10S505/782 - Bismuth-, e.g. BiCaSrCuO

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DOE Contract Number:: W-31109-ENG-38

Resource Type:: Patent

Country of Publication:: United States

Language:: English

Subject:: rapid; formation; phase-clean; 110; bi-2223; powders; derived; via; freeze-drying; process; preparation; amorphous; precursor; pb-doped; sr; cu; 2223; incorporating; splat-freezing; step; splat; freezing; nitrate; solution; pb; form; flakes; phase; separation; grinding; frozen; powder; heating; dried; dry; green; denitrating; green-powders; denitrated; grain; boundaries; grains; appear; clean; leading; intergrain; contact; nitrate solution; phase separation; grain boundaries; precursor powder; precursor powders; drying process; dried powder; freeze-drying process; /505/252/

Citation Formats


                    Balachandran, Uthamalingam. Rapid formation of phase-clean 110 K (Bi-2223) powders derived via freeze-drying process.  United States: N. p., 1996. 
        Web.

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                    Balachandran, Uthamalingam. Rapid formation of phase-clean 110 K (Bi-2223) powders derived via freeze-drying process.  United States.

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                    Balachandran, Uthamalingam. Mon .  
        "Rapid formation of phase-clean 110 K (Bi-2223) powders derived via freeze-drying process".  United States.  https://www.osti.gov/servlets/purl/870443.

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@article{osti_870443,

  title        = {Rapid formation of phase-clean 110 K (Bi-2223) powders derived via freeze-drying process},

  author       = {Balachandran, Uthamalingam},

  abstractNote = {A process for the preparation of amorphous precursor powders for Pb-doped Bi.sub.2 Sr.sub.2 Ca.sub.2 Cu.sub.3 O.sub.x (2223) includes a freeze-drying process incorporating a splat-freezing step. The process generally includes splat freezing a nitrate solution of Bi, Pb, Sr, Ca, and Cu to form flakes of the solution without any phase separation; grinding the frozen flakes to form a powder; freeze-drying the frozen powder; heating the dried powder to form a dry green precursor powders; denitrating the green-powders; heating the denitrated powders to form phase-clean Bi-2223 powders. The grain boundaries of the 2223 grains appear to be clean, leading to good intergrain contact between 2223 grains.},

  doi          = {},

  journal      = {},
number       = ,

  volume       = ,

  place        = {United States},

  year         = {1996},

  month        = {1}

}

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Works referenced in this record:

Synthesis and microstructure of Bi1.8Pb0.4Sr2Ca2.2Cu3Ox obtained from freeze-dried precursors
journal, October 1993

Krishnaraj, P.; Lelovic, M.; Eror, N. G.
Physica C: Superconductivity, Vol. 215, Issue 3-4
https://doi.org/10.1016/0921-4534(93)90230-N

Glass Formation of High- T _c Compound BiCaSrCu ₂ O _x by Rapid Quenching
journal, May 1988

Minami, Tsutomu; Akamatsu, Yoshinori; Tatsumisago, Masahiro
Japanese Journal of Applied Physics, Vol. 27, Issue Part 2, No. 5
https://doi.org/10.1143/JJAP.27.L777

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Title: Rapid formation of phase-clean 110 K (Bi-2223) powders derived via freeze-drying process

Abstract

Citation Formats

Synthesis and microstructure of Bi1.8Pb0.4Sr2Ca2.2Cu3Ox obtained from freeze-dried precursors journal, October 1993

Glass Formation of High- T c Compound BiCaSrCu 2 O x by Rapid Quenching journal, May 1988

Synthesis and microstructure of Bi1.8Pb0.4Sr2Ca2.2Cu3Ox obtained from freeze-dried precursors
journal, October 1993

Glass Formation of High- T _c Compound BiCaSrCu ₂ O _x by Rapid Quenching
journal, May 1988