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A kind of preparation method and application of highly volatile composite ligand barium precursor salt

A technology with high volatility and ligands, which is applied in the usage of superconductor elements, chemical instruments and methods, cable/conductor manufacturing, etc., can solve the problems of volatility and poor thermal stability of metal barium precursor salts, and achieve excellent superconductivity , The effect of simplifying the preparation process

Inactive Publication Date: 2019-11-05
BEIJING JIAOTONG UNIV +1
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to overcome the disadvantages of poor volatility and thermal stability of the metal barium precursor salt prepared by the prior art, and propose a method for preparing a complex ligand barium precursor salt

Method used

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  • A kind of preparation method and application of highly volatile composite ligand barium precursor salt
  • A kind of preparation method and application of highly volatile composite ligand barium precursor salt
  • A kind of preparation method and application of highly volatile composite ligand barium precursor salt

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preparation example Construction

[0033] A preparation method of a high volatility composite ligand barium precursor salt, comprising the following steps:

[0034] A, first join metal barium and dry organic solvent in the glass there-necked flask, then feed nitrogen, and the glass there-necked flask is provided with a condenser tube, a drying tube and a nitrogen gas inlet conduit;

[0035] B. Mix 2,2,6,6-tetramethyl-3,5-heptanedione and an organic solvent evenly to form a mixed solution;

[0036] C, first slowly drop the mixed solution described in the step B into the there-necked flask described in the step A, then react under the airtight conditions of anhydrous and oxygen-free, until the metallic barium disappears completely;

[0037] D, fluorinated bis-trifluoromethanesulfonimide auxiliary ligand L is dissolved in dry organic solvent two, forming mixed solution two;

[0038] E, first slowly drop the mixed solution two described in the step D into the glass there-necked bottle described in the step C, then...

specific Embodiment

[0052] In a 2000 ml three-necked flask equipped with a condenser tube, a drying tube and a nitrogen gas inlet conduit, 6.85 g of metal barium particles and 700 ml of dry n-pentane were sequentially added, and 18.4 g of 2,2,6,6 - Tetramethyl-3,5-heptanedione (β-diketone, tmhd) and 184 ml of n-pentane were mixed uniformly to form a mixed solution.

[0053] The above mixed solution was slowly added dropwise into the three-necked flask through a normal pressure dropping funnel, and under anhydrous and oxygen-free airtight conditions, the reaction was vigorously stirred at 30°C until the metal barium particles completely disappeared; then, 140 ml containing 14.1 g The chloroform solution of fluorinated bistrifluoromethanesulfonimide was slowly added dropwise into a glass three-necked flask, under anhydrous and oxygen-free airtight conditions, mixed and stirred at 60°C for 12 hours, and then the solvent was distilled off under reduced pressure through a rotary evaporator. , vacuum d...

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Abstract

The invention belongs to the field of preparation of high-temperature superconducting materials and particularly relates to a preparation method and application of high-volatility complex ligand barium precursor salt. After anhydrous beta-barium diketone precursor salt (Ba(tmhd)2) is prepared by being reacted with 2,2,6,6-tetramethyl-3,5-heptadione and taking barium as a raw material, a barium salt reaction system is directly added with fluorinated difluoromethane sulfonylimide as an auxiliary ligand L to obtain the colorless and transparent complex ligand barium precursor salt Ba(tmhd)2(L). With the technology, aggregation of the Ba(tmhd)2 precursor salt in the post-treatment process to form Ba4(tmhd)8 low-ploidy which is not easy to evaporate is inhibited, preparation of the complex ligand barium precursor salt is greatly simplified, and YBCO (yttrium barium copper oxide) superconducting films with excellent superconductivity are prepared by the aid of the complex ligand barium precursor salt.

Description

technical field [0001] The invention belongs to the field of high-temperature superconducting material preparation, in particular to a preparation method and application of a high-volatile composite ligand barium precursor salt. Background technique [0002] The preparation of yttrium barium copper oxide (YBCO) high temperature superconducting long ribbons by metal organic salt chemical vapor deposition (MOCVD) is considered to be an effective way to produce second-generation high temperature superconducting long ribbons on a large scale. In the MOCVD process, the purity, volatility, stability and other factors of the metal-organic precursor salt will directly determine the superconducting properties of the final deposited YBCO thin film. At present, the preparation of YBCO superconducting thin films at home and abroad is mainly based on highly volatile yttrium, copper, Barium metal organic salt (such as Y(tmhd) 3 , Cu(tmhd) 2 , Ba(tmhd) 2 ·xH 2 O). However, unlike the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F3/00H01B13/00H01B12/06
CPCC07F3/003H01B12/06H01B13/00Y02E40/60
Inventor 张腾戴少涛莫思铭蔡渊马韬袁文胡磊王邦柱陈慧娟熊旭明
Owner BEIJING JIAOTONG UNIV
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