Synthesis of 1,1,1-trichlorodisilane
A method of making a trihalodisilane, the method comprising: combining a reductive effective amount of an alkylaluminum hydride, a halodisilane comprising at least 4 halogen atoms, and a solvent at a temperature <80° C. and reducing the halodisilane to form a reaction product mixture comprising a trihalodisilane and an alkylaluminum halide.
1. A method of making a trihalodisilane, the method comprising:
combining a reductive effective amount of an alkylaluminum hydride, a halodisilane comprising at least 4 halogen atoms, and a solvent at a temperature <150° C. and reducing the halodisilane to form a reaction product mixture comprising a trihalodisilane, an alkylaluminum halide, and the solvent.
2. The method according to claim 1 , wherein the solvent has a boiling point>the boiling point of the trihalodisilane, and the combining is at a temperature of <25° C.
3. The method according to claim 1 , wherein the alkylaluminum hydride is diisobutylaluminum hydride and the halodisilane is hexachlorodisilane.
4. The method according to claim 1 , wherein the molar ratio of the alkylaluminum hydride to halodisilane is from 3:1 to 3.5:1.
5. The method according to claim 1 , further comprising: combining the solvent and the halodisilane to form a halodisilane-solvent mixture and combining the halodisilane-solvent mixture formed with the alkylaluminum hydride.
6. The method according to claim 5 , further comprising: combining the alkylaluminum hydride with a second solvent to form an alkylaluminum hydride-solvent mixture, and combining the halodisilane-solvent mixture with the alkylaluminum hydride by adding the alkylaluminum hydride-solvent mixture to the halodisilane-solvent mixture.
7. The method according to claim 1 , further comprising recovering the trihalodisilane.
8. The method according to claim 7 , wherein the trihalodisilane is recovered by distillation.
9. The method according to claim 1 , wherein the trihalodisilane is 1,1,1-trichlorodisilane and the alkylaluminum halide is diisobutylaluminum chloride.
10. A trihalodisilane composition, comprising: <2% (w/w) of an alkylsilane and >98% (w/w) of a trihalodisilane, wherein the composition further comprises an alkylaluminum halide.
11. A method of depositing a silicon-containing film on a substrate, the method comprising, introducing a trihalodisilane composition into a reactor with a substrate and, optionally, additional reactants under deposition sufficient conditions to form a silicon-containing film on the substrate, wherein the trihalodisilane composition comprises <2% (w/w) of an alkylsilane, >98% (w/w) of a trihalodisilane, and an alkylaluminum halide.
12. The method according to claim 11 , wherein the additional reactant is oxygen or nitrogen.
13. The method according to claim 11 , wherein the silicon-containing film is deposited by ALD, PEALD, cyclic CVD, CVD or PECVD.