Iridium complex and its synthesis method

A technology for iridium complexes and synthesis methods, applied in chemical instruments and methods, compounds containing elements of Group 8/9/10/18 of the periodic table, organic chemistry, etc., can solve the problems of low volatility, low synthesis yield, etc. problem, to achieve the effect of increasing volatility, weakening interaction, and strengthening shading

Inactive Publication Date: 2008-09-24
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to overcome the shortcomings of low volatility and low synthetic yield in the prior art, the present 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] Embodiment 1: take by weighing the chloroiridic acid solution of 1mmol, add 2mmol ascorbic acid, obtain the solution of trivalent iridium, reaction formula is as follows:

[0017]

[0018] Transfer to a 100ml three-necked flask; weigh 6mmol of the ligand 2,2,6,6-tetramethyl-3,5-heptanedione, dissolve it in absolute ethanol, then add 3ml of 2M ammonia solution, The reaction formula is as follows:

[0019]

[0020] The resulting solution was transferred to a separatory funnel, slowly added to a three-necked flask under stirring, stirred and heated at 85°C for 8 hours, and the reaction formula was as follows:

[0021]

[0022] After the reaction, place in a filter bottle to filter and wash until the solution is neutral. After vacuum drying, a yellow crude product was obtained; the yellow crude product to be obtained after recrystallization from benzene-hexane was dissolved in a benzene solvent and heated slightly to obtain a yellow translucent solution. Speed ​​...

Embodiment 2

[0023] Embodiment 2: take by weighing the chloroiridic acid solution of 1mmol, add 2mmol sodium nitrite, obtain the solution of trivalent iridium,

[0024] Ir 4+ +NO 2 - →Ir 3+ +NO 3 - (4)

[0025] Transfer to a 100ml three-necked flask; weigh 7mmol of the ligand 2,2,6,6-tetramethyl-3,5-heptanedione, dissolve it in absolute ethanol, and then add 2M sodium bicarbonate solution 3.5ml, the reaction formula is as follows:

[0026]

[0027] The resulting solution was transferred to a separatory funnel, slowly added to a three-necked flask under stirring, stirred and heated at 80°C for 10 hours, and the reaction formula was the same as in Example 1 (3); The solution is neutral. After vacuum drying, a yellow crude product was obtained; the 2,2,6,6-tetramethyl-3,5-heptanedione complex of iridium obtained after recrystallization from benzene-hexane was 0.1630 grams, and the 2 , 2,6,6-tetramethyl-3,5-heptanedione complex theoretical mass value is 0.7410 grams, the ratio of t...

Embodiment 3

[0028] Embodiment 3: take by weighing the chloroiridic acid solution of 1mmol, add 2mmol hydrazine hydrate, obtain the solution of trivalent iridium, reaction formula is as follows:

[0029] Ir 4+ +H 2 NNH 2 →Ir 3+ +N 2 ↑(6)

[0030] Transfer to a 100ml three-necked flask; weigh 8mmol of the ligand 2,2,6,6-tetramethyl-3,5-heptanedione, dissolve it in absolute ethanol, and then add 2M sodium bicarbonate solution 4ml, the resulting solution was transferred to a separatory funnel, and the reaction formula was the same as in Example 2 (5); under stirring, it was slowly added to a three-necked flask, stirred and heated at 95°C for 6 hours, and the reaction formula was shown in Example 1 (3). After the reaction, place it in a filter bottle to filter and wash until the solution is neutral. After vacuum drying, a yellow crude product was obtained; after recrystallization from benzene-hexane, 2,2,6,6-tetramethyl-3,5-heptanedione complex of iridium was obtained. The quality was 0....

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Abstract

The disclosed synthesis method for Ir complex comprises: weighing 1mmol iridichloride to load into the reactor, and adding NaNO2 or hydrazine hydrate or ascorbic acid to obtain the solution of Ir3+; dissolving complex of 2, 2, 6, 6-tetramethyl -3, 5-hptyldiketone instead of acetylacetone and NaHCO3 or ammonia solution both of 6-10mmold into the anhydrous alcohol to obtain opposite salt solution; finally, stirring slowly and loading into the reactor to heat to 80-100Deg and react for 6-10h. This invention solves the low-volatility problem of acetylacetone complex in prior art and improves the yield from 10% to 22-25%.

Description

technical field [0001] The invention relates to a synthesis method of an iridium complex. Background technique [0002] Metal-organic chemical vapor deposition methods are 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. At present, the iridium precursor commonly used in metal iridium thin films is the acetylacetonate complex of iridium, and its structural formula is: [0003] [0004] The document "F.P.Dwyer, A.M.Sargeson, The preparation of tris-acetylacetone-Rhodium (III) and tris-acetylacetone-Iridium (III), J.Am.Chem.Soc, 1953, 75:984-985." discloses a The synthesis method of the acetylacetone complex of iridium, the method starts from the simple iridium, dissolves and reduces the iridium, and then reacts with the ligand acetylacetone. [0005] Due to the low volatility of the acetylacetone complex of iridium, a higher volatili...

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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