CN100425615C - Iridium complex and its synthesis method - Google Patents
Iridium complex and its synthesis method Download PDFInfo
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- CN100425615C CN100425615C CNB2006100416084A CN200610041608A CN100425615C CN 100425615 C CN100425615 C CN 100425615C CN B2006100416084 A CNB2006100416084 A CN B2006100416084A CN 200610041608 A CN200610041608 A CN 200610041608A CN 100425615 C CN100425615 C CN 100425615C
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- iridium
- hexafluoroacetylacetone
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Abstract
The present invention discloses an iridium complex and a synthesis method thereof, which has the purpose of solving the problem the acetylacetone complex of iridium has low volatility in the prior art. The synthesis method of the iridium complex comprises the following steps: half the volume of a three-neck flask is filled with solution of inert solvent, and 1 mmol of iridium trichloride is added into the three-neck flask which is heated until the iridium trichloride completely dissolves; after that 6 to 10 mmol hexafluoroacetylacetone is carefully dripped into the mixed solution, and reacts under the condition of the temperature from 50 DEG C to 70 DEG C for 40 to 60 hours, and the hexafluoroacetylacetone is sucked and filtered so as to remove a white solid deposit, and is evaporated and dried into solid. The obtained solid is dissolved in the solution of inert solvent of which the volume is 30 ml and the temperature is 20 DEG C, and is filtered; the filtrate is placed in a refrigerator of which the temperature is 5 DEG C for 24 hours so as to keep the temperature of the filtrate, and then is filtered, washed and dried in the vacuum so as to obtain the hexafluoroacetylacetone complex of the iridium. Because the fluoric hexafluoroacetylacetone is used in the place of acetylacetone, the spatial volume of the hexafluoroacetylacetone complex of the iridium is increased so as to reduce the capability of forming a polynuclear polymer and increase volatility.
Description
Technical field
The present invention relates to a kind of synthetic method of complex of iridium.
Background technology
Mocvd method is widely used in the preparation of various films.In metal organic chemical vapor deposition technology, the character of presoma plays crucial effect for deposition.Iridium presoma commonly used is the acetyl acetone complex of iridium in the metal iridium film at present, and its structural formula is:
The volatility of the acetyl acetone complex of iridium is lower, when reality is used, needs higher volatilization temperature, and whole depositing device has been proposed higher requirement, has limited to its range of application.
Summary of the invention
In order to overcome the low deficiency of prior art volatility, the invention provides a kind of synthetic method of complex of iridium.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of synthetic method of the complex of iridium that is shown below,
Its characteristics are to comprise the steps:
1) pack in three-necked flask inert solvent carbon trichloride, hexane or the cyclohexane solution of flask volume half add the iridous chloride of 1mmol in the three-necked flask, and heating is dissolved fully until iridous chloride;
2) carefully splash into the hexafluoroacetylacetone of 6～10mmol in the prepared mixed solution of step 1), and reacted 40～60 hours under 50 ℃～70 ℃ conditions, suction filtration is removed white solid precipitates, and evaporation drying becomes solid;
3) with step 2) to be dissolved in 30ml, temperature be in 20 ℃ the inert solvent solution to resulting solid and filter;
4) step 3) gained filtrate being placed on temperature is 24 hours after-filtration of insulation in 5 ℃ of refrigerators, washing, and vacuum-drying obtains the hexafluoroacetylacetone title complex of iridium.
The invention has the beneficial effects as follows: owing to adopt the fluoric hexafluoroacetylacetone to replace methyl ethyl diketone, from molecular structure, because the volume of fluorine atom is greater than the volume of hydrogen atom, make the spatial volume of hexafluoroacetylacetone title complex of iridium increase, thereby strengthen covering to the center iridium ion, weaken intermolecular interaction, reduce forming the polymeric ability of multinuclear, improved the volatility of title complex.
The present invention is further described below in conjunction with embodiment.
Embodiment
Embodiment 1: the iridous chloride that takes by weighing 1mmol joins in the three-necked flask that the 50ml carbon tetrachloride solvent is housed, and heating until the iridous chloride dissolving fully.Carefully splash into the hexafluoroacetylacetone of 6mmol, then mixture was heated 45 hours under 60 ℃ of temperature, reaction formula is as follows:
The mixture suction filtration that this is hot to be to remove a spot of white solid, then with solution evaporation to doing, it is in 20 ℃ the carbon tetrachloride solution that the solid that obtains is dissolved in 30ml, temperature, solution is filtered, and filtrate is placed on temperature is insulation 24 hours in 5 ℃ of refrigerators.During this period, the hexafluoroacetylacetone yellow crystals that iridium occurred.Filter washing, vacuum-drying.Obtain product.
Embodiment 2: the iridous chloride that takes by weighing 1mmol joins in the three-necked flask that the 50ml cyclohexane solvent is housed, and heating until the iridous chloride dissolving fully.Carefully splash into the hexafluoroacetylacetone of 7mmol, then mixture was heated 60 hours under 50 ℃ of temperature, reaction formula is with embodiment 1; The mixture suction filtration that this is hot to be to remove a spot of white solid, then with solution evaporation to doing, it is in 20 ℃ the cyclohexane solution that the solid that obtains is dissolved in 30ml, temperature, solution is filtered, and filtrate is placed on temperature is insulation 24 hours in 5 ℃ of refrigerators.During this period, the hexafluoroacetylacetone yellow crystals that iridium occurred.Filter washing, vacuum-drying.Obtain product.
Embodiment 3: the iridous chloride that takes by weighing 1mmol joins in the three-necked flask that the 50ml hexane solvent is housed, and heating until the iridous chloride dissolving fully.Carefully splash into the hexafluoroacetylacetone of 8mmol, then mixture was heated 48 hours under 60 ℃ of temperature, reaction formula is with embodiment 1; The mixture suction filtration that this is hot to be to remove a spot of white solid, then with solution evaporation to doing, it is in 20 ℃ the hexane that the solid that obtains is dissolved in 30ml, temperature, solution is filtered, and filtrate is placed on temperature is insulation 24 hours in 5 ℃ of refrigerators.During this period, the hexafluoroacetylacetone yellow crystals that iridium occurred.Filter washing, vacuum-drying.Obtain product.
Embodiment 4: the iridous chloride that takes by weighing 1mmol joins in the three-necked flask that 50ml carbon trichloride solvent is housed, and heating until the iridous chloride dissolving fully.Carefully splash into the hexafluoroacetylacetone of 10mmol, then mixture was heated 40 hours under 70 ℃ of temperature, reaction formula is with embodiment 1; The mixture suction filtration that this is hot to be to remove a spot of white solid, then with solution evaporation to doing, it is in 20 ℃ the carbon trichloride that the solid that obtains is dissolved in 30ml, temperature, solution is filtered, and filtrate is placed on temperature is insulation 24 hours in 5 ℃ of refrigerators.During this period, the hexafluoroacetylacetone yellow crystals that iridium occurred.Filter washing, vacuum-drying.Obtain product.
Claims (1)
1, a kind of synthetic method of the complex of iridium that is shown below,
It is characterized in that comprising the steps:
1) pack in three-necked flask inert solvent carbon trichloride, hexane or the cyclohexane solution of flask volume half add the iridous chloride of 1mmol in the three-necked flask, and heating is dissolved fully until iridous chloride;
2) carefully splash into the hexafluoroacetylacetone of 6～10mmol in the prepared mixed solution of step 1), and reacted 40～60 hours under 50 ℃～70 ℃ conditions, suction filtration is removed white solid precipitates, and evaporation drying becomes solid;
3) with step 2) to be dissolved in 30ml, temperature be in 20 ℃ the inert solvent solution to resulting solid and filter;
4) step 3) gained filtrate being placed on temperature is 24 hours after-filtration of insulation in 5 ℃ of refrigerators, washing, and vacuum-drying obtains product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100416084A CN100425615C (en) | 2006-01-06 | 2006-01-06 | Iridium complex and its synthesis method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100416084A CN100425615C (en) | 2006-01-06 | 2006-01-06 | Iridium complex and its synthesis method |
Publications (2)
| Publication Number | Publication Date |
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| CN1803814A CN1803814A (en) | 2006-07-19 |
| CN100425615C true CN100425615C (en) | 2008-10-15 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB2006100416084A Expired - Fee Related CN100425615C (en) | 2006-01-06 | 2006-01-06 | Iridium complex and its synthesis method |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP6423007B2 (en) * | 2015-01-07 | 2018-11-14 | 国立研究開発法人産業技術総合研究所 | Method for producing cyclometalated iridium complex |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2105008C1 (en) * | 1996-08-14 | 1998-02-20 | Институт неорганической химии СО РАН | Method of preparing rhodium (iii) and iridium (iii) beta- diketonates |
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2006
- 2006-01-06 CN CNB2006100416084A patent/CN100425615C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2105008C1 (en) * | 1996-08-14 | 1998-02-20 | Институт неорганической химии СО РАН | Method of preparing rhodium (iii) and iridium (iii) beta- diketonates |
Non-Patent Citations (4)
| Title |
|---|
| 三乙酰丙酮铱的合成及性质研究. 阎鑫等.中国稀土学报，第20卷第增刊期. 2002 |
| 三乙酰丙酮铱的合成及性质研究. 阎鑫等.中国稀土学报，第20卷第增刊期. 2002 * |
| 金属b-二酮化合物用于MOCVD法生长铁电氧化物薄膜. 许效红等.化学进展，第14卷第1期. 2002 |
| 金属b-二酮化合物用于MOCVD法生长铁电氧化物薄膜. 许效红等.化学进展，第14卷第1期. 2002 * |
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| CN1803814A (en) | 2006-07-19 |
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