Novel thin film deposition aluminum precursor and preparation method thereof
A thin film deposition and precursor technology, applied in chemical instruments and methods, semiconductor/solid-state device manufacturing, electrical solid-state devices, etc., can solve unfavorable storage, transportation and subsequent use, poor thermal stability of precursors, and limit the advantages of ALD and other problems, to achieve the effect of reduced volatility, improved stability, and simple and clean synthesis process
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[0041] The preparation of the precursor compound of structural formula (I) comprises the following steps: (1) the second reactant comprising alane is placed in the reaction vessel, the solvent is added and stirred evenly, and the first reactant comprising aminopyridine or its derivative is placed in Add it into a reaction vessel under low temperature conditions, stir at room temperature or heat and stir to react overnight; (2) filter the mixture in step (1), concentrate under low pressure to obtain a small amount of solid-liquid mixture, add a solvent, and stand overnight to obtain The color block crystal is the precursor (I).
[0042] Wherein, the temperature of the cryogenic conditions and / or cryogenic storage is -78°C to 0°C, using any cooling means selected from liquid nitrogen, dry ice, liquid ammonia, cryogenic circulating pumps and combinations thereof; the stirring at room temperature or The time of heating and stirring is 1 to 10 hours; the temperature of stirring at ...
Embodiment 1
[0046] Put 10.0mmol of trimethylamine alane in the reaction vessel, add n-hexane and stir evenly, then slowly add 10.0mmol of 2-n-butylaminopyridine dissolved in toluene into the system at a low temperature of -78°C, during the dropwise addition process The medium system becomes turquoise translucent with bubbles coming out. After stirring at room temperature for 1 hour, heat to 25°C and reflux overnight; filter the obtained mixture, and concentrate at a temperature of 25°C under a low pressure of 0.05 MPa to obtain a very small amount of solid-liquid mixture. Leave it overnight to obtain a colorless block crystal, which is the compound [Al 2 h 2 {N(2-C 5 h 4 N)n-Bu} 2 ], productive rate 87%, coded as 1#.
Embodiment 2
[0048] Put 15.0mmol of trimethylamine alane in the reaction vessel, add n-hexane and stir evenly, then slowly add 10.0mmol of 2-n-butylaminopyridine dissolved in toluene into the system at a low temperature of -56°C, during the dropwise addition process The medium system becomes turquoise translucent with bubbles coming out. After stirring at room temperature for 3 hours, heat to 75°C and reflux overnight; filter the obtained mixture, and concentrate at a temperature of 45°C under a low pressure of 0.1MPa to obtain a small amount of solid-liquid mixture. Leave it overnight to obtain a colorless block crystal, which is the compound [Al 2 h 2 {N(2-C 5 h 4 N)n-Bu} 2 ], productive rate 88%, coded as 2#.
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