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Organic phosphine-stabilized alkyl silver disulfonate complex, and synthetic method and application thereof

A technology of silver alkyl disulfonate and organic phosphine, which is applied in the direction of silver organic compounds, phosphorus organic compounds, compounds of group 5/15 elements of the periodic table, etc., to achieve high yield, good stability, and simple synthesis method Effect

Inactive Publication Date: 2011-06-15
NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] For application: the synthesized alkyl disulfonate silver complex is a new complex, so there is no report on growing metal thin film materials using it as a precursor

Method used

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  • Organic phosphine-stabilized alkyl silver disulfonate complex, and synthetic method and application thereof
  • Organic phosphine-stabilized alkyl silver disulfonate complex, and synthetic method and application thereof
  • Organic phosphine-stabilized alkyl silver disulfonate complex, and synthetic method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] [CH 2 (SO 3 ) 2 Ag 2 ][PPh 3 ] 2 Synthesis

[0029]

[0030] in N 2 Under atmosphere, 0.2623 g (1 mmol) triphenylphosphine colorless clear solution dissolved in 20 mL dichloromethane was added dropwise to 0.1949 g (0.5 mmol) silver methanedisulfonate dissolved in 10 mL dichloromethane In the suspension, keep at -10°C to -20°C for 30 minutes overnight to obtain a colorless clear liquid, filter under nitrogen protection, and remove the solvent with an oil pump to obtain a white solid, namely the complex. Yield: 92%. M.p.: 189 ℃ dec. Anal. Calc. for C 37 h 32 o 6 Ag 2 P 2 S 2 : C, 48.60; H, 3.53. Found: C, 48.53; H, 3.44%. 1 H NMR (CDCl 3 ): d 4.2 (s, 2H, CH 2 –H), 7.2–7.4 (m, 30H, Ph–H). 13 C{H} NMR (CDCl 3 ): d 68.9 (CH 2 ), 134.0 (J PC = 16.4 Hz, C 6 h 5 ), 131.2 (J PC = 32.7 Hz, C6 h 5 ), 130.5 (C 6 h 5 ), 129.0 (J PC = 10.00 Hz, C 6 h 5 ). IR (KBr) data (cm -1 ): 3052 (m), 1479 (m), 1434 (vs), 1243 (s), 1202 (s), 1157 (m), 1095 (m...

Embodiment 2

[0032] [CH 2 (SO 3 ) 2 Ag 2 ][PPh 3 ] 3 Synthesis

[0033]

[0034] in N 2 Under atmosphere, 0.3935 g (1.5 mmol) triphenylphosphine colorless clear solution dissolved in 20 mL dichloromethane was added dropwise to 0.1949 g (0.5 mmol) silver methanedisulfonate dissolved in 10 mL dichloromethane The suspension was stirred at 0°C to -10°C for 1 hour to obtain a colorless clear liquid, which was filtered under nitrogen protection, and the solvent was removed by an oil pump to obtain a white solid, namely the complex. Yield: 92%. M.p.: 194 ℃ dec. Anal. Calc. for C 55 h 47 o 6 Ag 2 P 2 S 2 : C, 56.14; H, 4.03. Found: C, 56.03; H, 4.01%. IR (KBr) data (cm -1 ): 3051 (m), 1477 (m), 1434 (vs), 1242 (s), 1202 (s), 1158 (m), 1094 (m), 1008 (m), 792 (m), 743 (s ), 692 (vs), 576 (m), 515 (s).

Embodiment 3

[0036] [CH 2 (SO 3 ) 2 Ag 2 ][PPh 3 ] 4 Synthesis

[0037]

[0038] in N 2 Under the atmosphere, 0.7239 g (2.76 mmol) of triphenylphosphine, a colorless clear liquid dissolved in 20 mL of dichloromethane, was added dropwise to 0.2690 g (0.69 mmol) of methanedisulfonic acid dissolved in 10 mL of dichloromethane In the silver suspension, stir at 10°C to 0°C for 2 hours to obtain a colorless clear liquid, filter under nitrogen protection, and remove the solvent with an oil pump to obtain a white solid, namely the complex. Yield: 94%. Mp.: 202 o C dec.. Anal. Calc. for C 73 h 62 o 6 Ag 2 P 4 S 2 : C, 60.93; H, 4.34. Found: C, 60.87; H, 4.56. 1 H NMR (CDCl 3 ): d 3.9 (s, 2H, CH 2 ), 7.2–7.4 (m, 60H, Ph). 13 C{H} NMR (CDCl 3 ): d 68.6 (CH 2 ), 134.1 (J PC = 16.4 Hz, C 6 h 5 ), 132.1 (J PC = 26.5 Hz, C 6 h 5 ), 130.0 (C 6 h 5 ), 128.8 (J PC = 9.43 Hz, C 6 h 5 ). IR (KBr) data (cm -1 ): 3052 (m), 1480 (m), 1435 (vs), 1251 (s), 1204 (s), 1096 (m)...

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Abstract

The invention relates to an organic phosphine-stabilized alkyl silver disulfonate complex, and a synthetic method and application thereof. The synthetic method comprises the following steps of: under inert atmosphere and a dark condition, placing a mixture of alkyl silver disulfonate and an organic phosphine complex into an anhydrous organic solvent to stir; reacting at the temperature of between20 and -20 DEG C for 30 minutes to 4 hours under stirring; after the reaction is finished, filtering to obtain colorless clear solution; and pumping the solvent completely by using an oil pump to obtain the complex. The organic phosphine-stabilized alkyl silver disulfonate complex has typical beta-diketone rings, wherein a methyl silver disulfonate complex has two typical beta-diketone rings, so that the complex has high stability and low decomposition temperature; decomposition products are in gas state; small environmental pollution occurs in a substrate; and the organic phosphine-stabilized alkyl silver disulfonate complex can serve as a precursor for growing a silver film material by a chemical vapor deposition method and the like.

Description

[0001] technical field [0002] The invention relates to a metal organic complex and its synthesis method and application, in particular to an organophosphine-stabilized alkyl disulfonic acid silver complex, its synthesis method and its application in the preparation of silver film materials. [0003] Background technique [0004] For the product: there is no report in the literature, and what is synthesized is a new organophosphine-stabilized alkyl disulfonic acid silver complex. [0005] As for the method: the synthesis of these complexes is generally carried out under anhydrous and oxygen-free conditions. [0006] For the application: the synthesized silver alkyl disulfonate complex is a new complex, so there is no report on using it as a precursor to grow metal thin films. [0007] On the basis of the maturity of copper interconnection technology, a new generation of metal interconnection technology has become the focus of attention in the scientific and technological ...

Claims

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Application Information

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IPC IPC(8): C07F9/06C23C16/06C07F1/10C07F9/50C07F19/00
Inventor 沈应中陶弦沈克成冯猛汤清云王玉龙
Owner NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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