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Iridium complex and its synthesis method

A technology for iridium complexes and synthesis methods, which is applied in chemical instruments and methods, compounds containing elements of Group 8/9/10/18 of the periodic table, organic chemistry, etc. Sex, enhanced shading, the effect of increasing the volume of space

Inactive Publication Date: 2008-10-15
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to overcome the low volatility of the prior art, the invention provides a synthetic method for iridium complexes

Method used

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  • Iridium complex and its synthesis method
  • Iridium complex and its synthesis method
  • Iridium complex and its synthesis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Example 1: Weigh 1 mmol of iridium trichloride and add it to a three-necked flask containing 50 ml of carbon tetrachloride solvent, and heat until the iridium trichloride dissolves completely. 6mmol of hexafluoroacetylacetone was carefully added dropwise, and the mixture was heated at 60°C for 45 hours. The reaction formula is as follows:

[0017]

[0018] The hot mixture was suction filtered to remove a small amount of white solid, then the solution was evaporated to dryness, the resulting solid was dissolved in 30 ml of carbon tetrachloride solution at 20°C, the solution was filtered, and the filtrate was placed in The temperature was 5°C and kept in a refrigerator for 24 hours. During this time, yellow crystals of hexafluoroacetylacetone of iridium appeared. Filter, wash and dry in vacuo. product is obtained.

Embodiment 2

[0019] Example 2: Weigh 1 mmol of iridium trichloride and add it to a three-necked flask containing 50 ml of cyclohexane solvent, and heat until the iridium trichloride is completely dissolved. 7mmol of hexafluoroacetylacetone was carefully added dropwise, then the mixture was heated at 50°C for 60 hours, the reaction formula was the same as in Example 1; the hot mixture was suction filtered to remove a small amount of white solid, and then the solution was evaporated to dryness, The obtained solid was dissolved in 30 ml of a cyclohexane solution at a temperature of 20°C, the solution was filtered, and the filtrate was kept in a refrigerator at a temperature of 5°C for 24 hours. During this time, yellow crystals of hexafluoroacetylacetone of iridium appeared. Filter, wash and dry in vacuo. product is obtained.

Embodiment 3

[0020] Example 3: Weigh 1 mmol of iridium trichloride and add it to a three-necked flask containing 50 ml of hexane solvent, and heat until the iridium trichloride is completely dissolved. 8mmol of hexafluoroacetylacetone was carefully added dropwise, and then the mixture was heated at 60°C for 48 hours, the reaction formula was the same as in Example 1; the hot mixture was suction filtered to remove a small amount of white solid, and then the solution was evaporated to dryness, The obtained solid was dissolved in 30 ml of hexane at a temperature of 20°C, the solution was filtered, and the filtrate was kept in a refrigerator at a temperature of 5°C for 24 hours. During this time, yellow crystals of hexafluoroacetylacetone of iridium appeared. Filter, wash and dry in vacuo. product is obtained.

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Abstract

The disclosed synthesis method for Ir complex comprises: loading inert solvent with half volume of the three-necked flask, adding 1mmol IrCl3, and heating to full dissolution; dripping carefully 6-10mmol hexafluoroacetylacetone into the mixed liquid to react for 40-60h at 50-70Deg; filtering the white solid deposit to evaporate and dry; dissolving the obtained solid into 30ml inert solvent at 20Deg; filtering, putting the filtrate into icebox of 5Deg for 24h; finally, filtering, and vacuum drying. This invention solves the low-volatility problem of acetylacetone complex in prior art.

Description

technical field [0001] The present invention relates to a kind of synthetic method of iridium complex. Background technique [0002] The metal organic chemical vapor deposition method is widely used in the preparation of various thin films. In the metal organic chemical vapor deposition process, the properties of the precursor play a very important role in the deposition. The iridium precursor commonly used in metal iridium films at present is the acetylacetone complex of iridium, and its structural formula is: [0003] [0004] The acetylacetonate complex of iridium has low volatility, and requires a higher volatilization temperature in actual use, which imposes higher requirements on the entire deposition equipment and limits its application range. SUMMARY OF THE INVENTION [0005] In order to overcome the deficiency of low volatility in the prior art, the present invention provides a method for synthesizing iridium complexes. [0006] The technical scheme adopted ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F15/00
Inventor 张秋禹阎鑫张和鹏张军平
Owner NORTHWESTERN POLYTECHNICAL UNIV
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