Organoaminodisilazanes for high temperature atomic layer deposition of silicon oxide thin films
A technology of organoaminodisilazane and pentamethyldisilazane, which is applied in the field of a method for depositing silicon oxide, and can solve problems such as harmful semiconductor applications
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Embodiment 1
[0116] Example 1: Preparation of 1-dimethylamino-1,1,2,3,3,3-hexamethyldisilazane.
[0117] Dimethyldichlorosilane (1.13 mol, 146 g) was added to heptamethyldisilazane (1.13 mol, 198 g) in a 1 L flask via an addition funnel. The mixture was stirred and heated to about 60°C. Upon completion of the reaction as determined by GC analysis, the reaction mixture was distilled. 157 g of 1-chloro-1,1,2,3,3,3-hexamethyldisilazane were obtained under reduced pressure (68° C. / 25 torr) with a yield of 71%.
[0118] Dimethylamine solution (2M) in THF (1.0mol, 500mL) was slowly added to 1-chloro-1,1,2,3,3,3-hexamethyldisilazane (0.67mol, 131g ), triethylamine (0.80mol, 81g) and hexane in a mixture. Once the addition was complete, the resulting slurry was stirred and then heated at about 50°C for 2 hours. The mixture was filtered, and the solvent was removed under reduced pressure, and the crude product was purified by distillation to give 93.0 g (b.p. 185° C.) of 1-dimethylamino-1,1,2,3,...
Embodiment 3
[0127] Example 3. Precursor thermal stability of 1-dimethylamino-1,1,2,3,3,3-hexamethyldisilazane vs DMATMS
[0128] 1-Dimethylamino-1,1,2,3,3,3-hexamethyldisilazane and DMATMS were introduced into the ALD chamber as silicon precursors in the following steps: (a) introduction of silicon precursor 12 seconds; (b) purged with nitrogen. Repeat steps (a) and (b) for 300 cycles. Film thickness and refractive index (RI) were measured using a FilmTek 2000SE ellipsometer by fitting reflection data from the film to a preset physical model (eg, a Lorentz oscillator model). Table 4 summarizes the films formed by thermal deposition of silazane precursors at substrate temperatures of 600 °C and 650 °C, respectively, showing that 1-dimethylamino-1,1,2,3,3,3-hexamethyl Disilazane decomposes slightly less than DMATMS, and therefore it is a better precursor for high temperature ALD applications.
[0129] Table 4 Thermal decomposition of silazane precursors vs DMATMS
[0130]
Embodiment 4
[0131] Example 4. Atomic layer deposition of silicon oxide films using 1-dimethylamino-1,1,2,3,3,3-hexamethyldisilazane
[0132] Atomic layer deposition of silicon oxide films was performed using the following silicon precursor: 1-dimethylamino-1,1,2,3,3,3-hexamethyldisilazane. Deposition was performed on a laboratory-scale ALD processing facility. The silicon precursor is delivered into the chamber by vapor pumping. The deposition process and parameters are provided in Table 2. Repeat steps 2 to 6 for 500 cycles until the desired thickness is achieved. Table 5 provides the deposition process parameters, deposition rate, refractive index, and WER using a 1% solution of 49% hydrofluoric (HF) acid in deionized water.
[0133] Table 5. Summary of process parameters and results for 1-dimethylamino-1,1,2,3,3,3-hexamethyldisilazane
[0134]
[0135] It can be seen that the silicon precursor 1-dimethylamino-1,1,2,3,3,3-hexamethyldisilazane provides a slightly higher deposition...
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