Graduate Thesis Or Dissertation
 

Intercalation, exfoliation, and nanocomposites of layered inorganic compounds

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  • The melt intercalation of poly(ethylene oxide) (PEO) between layers of MoO₃ and MPS3 (M=Mn,Cd) is obtained by heating the ground mixture and LiₓMoO₃, KₓMn₁-ₓ/₂PS₃, or KCd₁-ₓ/₂PS₃. The products are characterized by powder X-ray diffraction (XRD). Below the melting temperature of PEO (66 °C), intercalation rates and yields are low. By heating at 125 °C for 5-30 hours, high intercalation yields are achieved. Layered titanate compounds are not amenable for melt intercalation. The exfoliationladsorption method is studied in this thesis. Titanate layers are swollen or exfoliated in aqueous solution by using ultrasound and a swelling agent, tetrabutylammonium hydroxide (TBAOH). The exfoliation/swelling behavior is investigated by particle size distribution analysis and UV-Vis spectrometry. HₓTi₂-ₓ/₄☐ₓ/₄O₄.yH₂O (H-Ti) is exfoliated in TBAOH aqueous solution with the ratio of TBA ions per protons in titanate (TBA/H) ≥ 0.5 by ultrasonication at 120 W for 30 minutes. H₂Ti₄O₉.xH₂O (H-Ti4) is not exfoliated, but significantly swollen when it is treated by ultrasonication at 180 W for 1 hour in the presence of TBA/H = 5. The exfoliated H-Ti and swelled H-Ti4 are used as precursors to polymercontaining nanocomposites. Water-soluble polymer, such as PEO, polyvinylpyrrolidone (PVP), and polyethylenimine (PEI) are added to these exfoliation/swelling precursors, and subsequently acidified to pH ~ 1-3. The gels of nanocomposites are obtained immediately. The nanocomposites are characterized by XRD, thermal analyses, elemental analyses, SEM, and FTIR. The data indicate polymer intercalation along with a decreased water content and decreased water interaction with titanate sheet surfaces. Ultrasound is also studied for the intercalation of long-chain alkylammonium (CₙH₂ₙ₊₁NH₃, n = 6-18) into H-Ti4. H-Ti4 is ultrasonicated at 180 W for 15 minutes in an aqueous or ethanoic solution of alkylamines. XRD indicates smaller increases of repeating layer distances, as compared to previous reports. This may result from the presence of kinked conformations in the alkylammonium chains.
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