Monophyletic mixture of metal oxygen silicide
A technology of silicide and mixture, which is applied in the direction of silicon organic compounds, compounds of group 4/14 elements of the periodic table, metal material coating technology, etc.
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Embodiment 1
[0039] With empirical composition Hf(NEt 2 ) 3.15 (OEiEt 3 ) 0.85 synthesis of the parent
[0040] With empirical composition Hf(NEt 2 ) 3.15 (OSiEt 3 ) 0.85 The synthesis of the precursor was carried out by the following method. All manipulations were performed under nitrogen and argon in the absence of moisture and air using standard Schlenk and glove box techniques. In the glove box, weigh Hf(NEt 2 ) 4 (75.71 g, 162.3 mmol) was placed in a 500 ml Schlenk flask equipped with a stir bar. Hexane (-200ml) was added to the flask. will be fitted with HOSiEt 3 An isobaric addition funnel of (21.3 g, 161 mmol) and hexane (-50 ml) was secured to the flask and capped with a glass stopper. The reaction apparatus was removed from the glove box and secured to a Schlenk line.
[0041] Place the reaction flask in a dry ice / isopropanol bath before adding the reactants. The silanol solution was added dropwise to the reaction mixture over 30-45 min. Stirring was continued ove...
Embodiment 2
[0044] With empirical composition Hf(NEt 2 ) 1.66 (OSiEt 3 ) 2.34 synthesis of the parent
[0045] With empirical composition Hf(NEt 2 ) 1.66 (OSiEt 3 ) 2.34 The synthesis of the precursor was carried out by the following method. All manipulations were performed under nitrogen and argon in the absence of moisture and air using standard Schlenk and glove box techniques. In the glove box, weigh Hf(NEt 2 ) 4 (74.96g, 160.7mmol) was placed in a 500ml Schlenk flask equipped with a stir bar. Hexane (-100ml) was added to the flask. will be fitted with HOSiEt 3 (47.5 g, 359 mmol) and hexane (-50 ml) with an isobaric addition funnel secured to the flask and capped with a glass stopper. The reaction apparatus was removed from the glove box and secured to a Schlenk line.
[0046] While cooling the reaction flask in a dry ice / isopropanol bath, the silanol solution was added dropwise to the reaction mixture over about 15 min. Stirring was continued overnight while the flask ...
Embodiment 3
[0048] With empirical composition Hf(OtBu) 3.30 (OSiEt 3 ) 0.70 synthesis of the parent
[0049] With empirical composition Hf(OtBu) 3.30 (OSiEt 3 ) 0.70 The synthesis of the precursor (Hf / Si ratio ~4.7) was carried out by the following method. All manipulations were performed under nitrogen and argon in the absence of moisture and air using standard Schlenk and glove box techniques. In the glove box, weigh Hf(OtBu) 4 (81.80 g, 173.7 mmol) was placed in a 500 ml Schlenk flask equipped with a stir bar. Hexane (-200ml) was added to the flask. will be fitted with HOSiEt 3 (23.01 g, 173.9 mmol) and hexane (-10 mL) an isobaric addition funnel was secured to the flask and capped with a glass stopper. The reaction apparatus was removed from the glove box and secured to a Schlenk line.
[0050] While cooling the reaction flask in a dry ice / isopropanol bath, the silanol solution was added dropwise to the reaction mixture over about 50 min. Stirring was continued overnight w...
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