Example 1
InCl (1 eq.) was added to a Schlenk flask charged with LiCp(CH2)3NMe2 (11 mmol) in Et2O (50 mL). The reaction mixture was stirred overnight at room temperature. After filtration of the reaction mixture, the solvent was evaporated under reduced pressure to obtain a red oil. After distillation a yellow liquid final product was collected (mp˜5° C.). Various measurements were done to the final product. 1H NMR (C6D6, 400 MHz): δ 5.94 (t, 2H, Cp-H), 5.82 (t, 2H, Cp-H), 2.52 (t, 2H, N—CH2—), 2.21 (t, 2H, Cp-CH2—), 2.09 (s, 6H, N(CH3)2, 1.68 (q, 2H, C—CH2—C). Thermogravimetric (TG) measurement was carried out under the following measurement conditions: sample weight: 22.35 mg, atmosphere: N2 at 1 atm, and rate of temperature increase: 10.0° C./min. 97.2% of the compound mass had evaporated up to 250° C. (Residue <2.8%). T (50%)=208° C. Vacuum TG measurement was carried out under delivery conditions, under the following measurement conditions: sample weight: 5.46 mg, atmosphere: N2 at 20 mbar, and rate of temperature increase: 10.0° C./min. TG measurement was carried out under delivery conditions into the reactor (about 20 mbar). 50% of the sample mass is evaporated at 111° C.
Using In(Cp(CH2)3NMe2) synthesized in Example 1 as an indium precursor and H2O and O3 as reaction gases, indium oxide film may be formed on a substrate by ALD method under the following deposition conditions. First step, a cylinder filled with In(Cp(CH2)3NMe2) is heated to 90° C., bubbled with 100 sccm of N2 gas and the In(Cp(CH2)3NMe2) is introduced into a reaction chamber (pulse A). Next step, O3 generated by an ozone generator is supplied with 50 sccm of N2 gas and introduced into the reaction chamber (pulse B). Following each step, a 4 second purge step using 200 sccm of N2 as a purge gas was performed to the reaction chamber. 200 cycles were performed on a Si substrate having a substrate temperature of 150° C. in the reaction chamber at a pressure of about 1 torr. As a result, an indium oxide film will be obtained at approximately 150° C.
Example 2
Same procedure as Example 1 started from Li(CpPiPr2) was performed to synthesize In(CpPiPr2). An orange liquid was obtained. 1H NMR (C6D6, 400 MHz): δ 6.17 (t, 2H, Cp-H), 5.99 (t, 2H, Cp-H), 1.91 (sept, 2H, P—CH—), 1.20-1.00 (m, 12H, C—CH3).
Using In(CpPiPr2) synthesized in Example 2 as the indium precursor and H2O and O3 as the reaction gases, indium oxide film may be formed on a substrate by the ALD method under the following deposition conditions. First step, a cylinder filled with In(CpPiPr2) is heated to 90° C., bubbled with 100 sccm of N2 gas and the In(CpPiPr2) is introduced into a reaction chamber (pulse A). Next step, O3 generated by an ozone generator is supplied with 50 sccm of N2 gas and introduced into the reaction chamber (pulse B). Following each step, a 4 second purge step using 200 sccm of N2 as a purge gas was performed to the reaction chamber. 200 cycles were performed on the Si substrate having a substrate temperature of 150° C. in an ALD chamber at a pressure of about 1 torr. As a result, an indium oxide was obtained at 150° C.