Preparation of titanium (III) acetylacetonate [Tris (2,4-pentanediono) titanium (III)]

Chakravarti, B. N.

doi:10.1007/bf00622874

Cited by 19 publications

(5 citation statements)

References 3 publications

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“…The production of Ti(acac) 3 from TiN when using Sn(acac) 2 should be feasible based on earlier studies that have prepared Ti(acac) 3 . 40 In contrast, the production of Ti(CH 3 ) 3 from TiF 3 when using TMA as the metal precursor is not expected because there are no previous reports for Ti(CH 3 ) 3 in the literature. Likewise, the production of TiCl 3 from TiF 3 when using DMAC or SiCl 4 as the metal precursor may not be viable because TiCl 3 has low volatility with a boiling point of 960 °C.…”

Section: Resultsmentioning

confidence: 99%

“…The ligand-exchange reaction between TiF 3 and Sn(acac) 2 may also be possible. The production of Ti(acac) 3 from TiN when using Sn(acac) 2 should be feasible based on earlier studies that have prepared Ti(acac) 3 . In contrast, the production of Ti(CH 3 ) 3 from TiF 3 when using TMA as the metal precursor is not expected because there are no previous reports for Ti(CH 3 ) 3 in the literature.…”

Section: Resultsmentioning

confidence: 99%

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Selectivity in Thermal Atomic Layer Etching Using Sequential, Self-Limiting Fluorination and Ligand-Exchange Reactions

2016

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Atomic layer etching (ALE) can result from sequential, selflimiting thermal reactions. The reactions during thermal ALE are defined by fluorination followed by ligand exchange using metal precursors. The metal precursors introduce various ligands that may transfer during ligand exchange. If the transferred ligands produce stable and volatile metal products, then the metal products may leave the surface and produce etching. In this work, selectivity in thermal ALE was examined by exploring tin(II) acetylacetonate (Sn(acac) 2 ), trimethylaluminum (TMA), dimethylaluminum chloride (DMAC), and SiCl 4 as the metal precursors. These metal precursors provide acac, methyl, and chloride ligands for ligand exchange. HF-pyridine was employed as the fluorination reagent. Spectroscopic ellipsometry was used to measure the etch rates of Al 2 O 3 , HfO 2 , ZrO 2 , SiO 2 , Si 3 N 4 , and TiN thin films on silicon wafers. The spectroscopic ellipsometry measurements revealed that HfO 2 was etched by all of the metal precursors. Al 2 O 3 was etched by all of the metal precursors except SiCl 4 . ZrO 2 was etched by all of the metal precursors except TMA. In contrast, SiO 2 , Si 3 N 4 , and TiN were not etched by any of the metal precursors. These results can be explained by the stability and volatility of the possible reaction products. Temperature can also be used to obtain selective thermal ALE. The temperature dependence of ZrO 2 , HfO 2 , and Al 2 O 3 ALE was examined using SiCl 4 as the metal precursor. Higher temperatures can discriminate between the etching of ZrO 2 , HfO 2 , and Al 2 O 3 . The temperature dependence of Al 2 O 3 ALE was also examined using Sn(acac) 2 , TMA, and DMAC as the metal precursors. Sn(acac) 2 etched Al 2 O 3 at temperatures ≥150 °C. DMAC etched Al 2 O 3 at higher temperatures ≥225 °C. TMA etched Al 2 O 3 at even higher temperatures ≥250 °C. The combination of different metal precursors with various ligands and different temperatures can provide multiple pathways for selective thermal ALE.

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Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Selectivity in Thermal Atomic Layer Etching Using Sequential, Self-Limiting Fluorination and Ligand-Exchange Reactions

2016

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“…β-Diketonate ligands hold an important place in the history of coordination chemistry and continue to be among the most ubiquitous ligands for use as catalysts, precatalyts, NMR shift reagents, biochemically active agents, and volatile reagents for metal vapor deposition. − Perhaps the most unique feature distinguishing them from many other organic ligands is their ability to coordinate the majority of all known elements. One challenge with β-diketonate chemistry, particularly in the area of catalysis, is their tendency to form substitutionally inert complexes of the type M(acac) 3 or M(acac) 4 (acac = acetylacetonate) for most transition and main-group metals. − Alternately, metals complexed with two β-diketonates tend to form oligomeric species that can have unfavorable solubility characteristics or lead to bimolecular decomposition pathways during catalysis. − …”

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confidence: 99%

Bulky β-Diketones Enabling New Lewis Acidic Ligand Platforms

et al. 2017

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The synthesis of a sterically encumbered β-diketone ligand (acac) substituted with 2,6-(2,4,6-MeCH)CH is described. Coordination complexes of the type M(acac)Cl(solv) (M = Ti, V, Cr; solv = THF, CHCN) were prepared by the reaction of acac with MCl (M = V, Cr) or with TiCl to generate Ti(acac)Cl, followed by reduction. These complexes show a trend of alternating the cis/trans geometric preference with increasing d electron count (n = 0, 1, 2, 3), which is rationalized in part by the unusual ability of β-diketonates to behave as either a weak π donor or a π acceptor in the cis and trans geometries, respectively. In this way, the bis-β-diketonate platform can accommodate the varying electronic demands of the coordinated metal ion. These results demonstrate the ability to limit the coordination of β-diketonates on metal complexes for the first time, providing a chemically robust and coordinatively versatile platform for mechanistic investigations, metal functionalization, and improved catalyst design.

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“…(2)). The formation of similar tris-complex of titanium with acetylacetone and other related β-diketones was already reported [29][30][31][32]. In addition, the Ti-acac complexes formed by using acetylacetone with Hacac/Ti = 1.0 and 2.0 in the molar ratio were found to be relatively less stable in an aqueous medium as compared to that prepared by using Hacac/Ti molar ratio = 3.0.…”

Section: Synthesis Of Crystalline Batiomentioning

confidence: 69%

Wet-chemical synthesis of crystalline BaTiO3 from stable chelated titanium complex: Formation mechanism and dispersibility in organic solvents

Pramanik

Seok

Ahn

2006

Journal of Colloid and Interface Science

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Preparation of titanium (III) acetylacetonate [Tris (2,4-pentanediono) titanium (III)]

Cited by 19 publications

References 3 publications

Selectivity in Thermal Atomic Layer Etching Using Sequential, Self-Limiting Fluorination and Ligand-Exchange Reactions

Selectivity in Thermal Atomic Layer Etching Using Sequential, Self-Limiting Fluorination and Ligand-Exchange Reactions

Bulky β-Diketones Enabling New Lewis Acidic Ligand Platforms

Wet-chemical synthesis of crystalline BaTiO3 from stable chelated titanium complex: Formation mechanism and dispersibility in organic solvents

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