Lewis-base copper(I) formates: Synthesis, reaction chemistry, structural characterization and their use as spin-coating precursors for copper deposition

Tuchscherer, André; Shen, Yingzhong; Jakob, Alexander; Mothes, Robert; Al-Anber, Mohammed A.; Walfort, Bernhard; Rüffer, Tobias; Frühauf, S.; Ecke, Ramona; Schulz, Stephan E.; Geßner, Thomas; Lang, Heinrich

doi:10.1016/j.ica.2010.05.048

Cited by 17 publications

(12 citation statements)

References 65 publications

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“…The films contain traces of solvent, which was also observed previously in the case of Schiff base layers and [(nBu 3 P) 2 CuO 2 CH•HO 2 CH]. 28,59 This induces non-completed solidification of the complex solution during the spin coating process. The EDS results indicated the decrease of copper contents in the layers obtained at higher rotation speed, which is favorable for a thinner layer of the complex upon rotation speed increase.…”

Section: Thin Layer Studiessupporting

confidence: 64%

New nickel(ii) and copper(ii) complexes with unsymmetrical Schiff bases derived from (1R,2R)(−)cyclohexanediamine and the application of Cu(ii) complexes for hybrid thin layers deposition

et al. 2013

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New unsymmetrical Schiff bases obtained by condensation of (1R,2R)(-)cyclohexanediamine with 2-hydroxy-3,5-di-tert-butylbenzaldehyde (3,5-(t)bba) and 2-hydroxy-3-methoxybenzaldehyde (3-metoxba) or 2-hydroxy-5-nitrobenzaldehyde (5-nba) and 2-hydroxyacetophenone (hacphen) were used for the synthesis of Cu(ii) and Ni(ii) complexes. The ligands and complexes were characterized by circular dichroism (CD), UV-vis, IR, (1)H (NOE diff) (ligand) and (13)C NMR (ligand) spectra. The X-ray crystal structures solved for Ni(II)(1R,2R)(-)chxn(3,5-(t)bba)(hacphen) exhibit distortion of the coordination sphere towards tetrahedral in the solid phase. The complex crystallized in the orthorhombic non-centrosymmetric P2(1)2(1)2(1) space group. Thin layers of copper(II) complexes were deposited on Si(111) by a spin coating technique and characterized by scanning electron microscopy (SEM/EDS), atomic force microscopy (AFM) and fluorescence spectroscopy. Layer deposition conditions were studied and optimal parameters were found (1500 rpm, time 30 s). For copper(ii) layers the most intensive fluorescence band from intraligand transition at 514 nm was observed. CD spectra of complexes in MeCN suggest the tetrahedral distortion from the square planar geometry of the central ion of the coordination sphere in solution. The (1)H NMR NOE diff. spectra of ligands were measured and the positions of the nearest hydrogen atoms in the cyclohexane and aromatic rings were discussed.

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Section: Thin Layer Studiessupporting

confidence: 64%

New nickel(ii) and copper(ii) complexes with unsymmetrical Schiff bases derived from (1R,2R)(−)cyclohexanediamine and the application of Cu(ii) complexes for hybrid thin layers deposition

et al. 2013

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“…The enhancement of the roughness is a consequence of the solvent lose and decomposition of the copper complex. Other authors observed the same effect in the case of silver and copper complexes [ 13 , 14 , 45 ]. After heating, the layers’ shape, structure, and composition were changed significantly.…”

Section: Resultssupporting

confidence: 65%

“…Due to a good solubility of the compounds, we have tested the applicability of these metal-organic compounds application in ‘wet’ coating methods. The literature data indicate that using spin- or dip- coating techniques and then heating the deposited precursors, metal or metal oxide layers at a thickness from a few tens up to several hundred nanometers can be obtained [ 13 , 14 ] in a low-cost process because they do not require complicated technical and hence, expensive equipment.…”

Section: Introductionmentioning

confidence: 99%

Copper(II) Perfluorinated Carboxylate Complexes with Small Aliphatic Amines as Universal Precursors for Nanomaterial Fabrication

et al. 2021

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Copper(II) carboxylate compounds with ethylamine and isopropylamine of the general formula [Cu2(RNH2)2(µ-O2CRf)4], where R = Et, iPr, and Rf = CnF2n+1, n = 1–6, were characterised in the condensed and gas phases by electron impact mass spectrometry (EI MS), IR spectroscopy, and thermal analysis. A mass spectra analysis confirmed the presence of metallated species in the gas phase. Among the observed fragments, the pseudomolecular ions [Cu2(RNH2)2(µ-O2CRf)3]+ were found, which suggests the dimeric structure of the studied complexes with axially N-coordinated ethyl- or isopropylamine molecules and bridging perfluorinated carboxylates. TGA studies demonstrated that copper transfer to the gas phase occurs even under atmospheric pressure. The temperature range of the [Cu2(RNH2)2(µ-O2CRf)4] and other copper carriers detection, observed in variable temperature infrared spectra, depends on the type of amine. The possible mechanisms of the decomposition of the tested compounds are proposed. The copper films were produced without additional reducing agents despite using Cu(II) CVD precursors in the chemical vapor deposition experiments. The layers of the gel-like complexes were fabricated in both spin- and dip-coating experiments, resulting in copper or copper oxide materials when heated. Dinuclear copper(II) carboxylate complexes with ethyl- and isopropylamine [Cu2(RNH2)2(µ-O2CRf)4] can be applied for the formation of metal or metal oxide materials, also in the nanoscale, by vapour and ‘wet’ deposition methods.

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“…For the formation of copper and copper oxides several methods have been applied including electrochemical deposition,, thermal oxidation of copper, magnetron sputtering, spin‐coating, chemical beam epitaxy (CBE), atomic layer deposition (ALD), and chemical vapor deposition (CVD) , , …”

Section: Introductionmentioning

confidence: 99%

“…media, [15] solar cells, [16] sensors, [17] batteries, [18,19] and catalysis. [20][21][22] For the formation of copper and copper oxides several methods have been applied including electrochemical deposition, [23,24] thermal oxidation of copper, [25] magnetron sputtering, [26] spin-coating, [27][28][29][30][31] chemical beam epitaxy (CBE), [32] atomic layer deposition (ALD) [6,[33][34][35][36][37] and chemical vapor deposition (CVD). [8,10,[38][39][40] For the vacuum-based deposition of copper or copper oxide films the precursors can be classified in two groups: Copper(I) and copper(II) compounds, respectively.…”

Section: Introductionmentioning

confidence: 99%

Synthesis of β‐Ketoiminato Copper(II) Complexes and Their Use in Copper Deposition

Preuß

Korb

Rüffer

et al. 2020

Zeitschrift anorg allge chemie

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The template synthesis of ethylenediamine (1) with 2‐acetylcyclopentanone (2) and [Cu(OAc)2·H2O] (5) produced [Cu(1‐(2‐cC5H6(O))C(Me)NCH2)2)] (6) in 82 % yield. Reaction of 5 with bis(benzoylacetone)diethylenetriamine (7, = LH)[1] gave [Cu(μ‐OAc)(L)(H2O)]2 (8). The solid‐state structures of 6 and 8 were determined confirming that 8 possesses intra‐ and intermolecular hydrogen bonds resulting in a dimer formation. The thermal behavior of 6–8 was studied by TG and TG‐MS. Under oxygen CuO was formed, whereas under Ar Cu/Cu2O (6) or Cu (8) was obtained. Complex 6 was used as CVD precursor for Cu and Cu‐oxide deposition (substrate temp., 400–500 °C, N2, 60 mL·min–1; O2, 60 mL·min–1; pressure, 0.87–1.5 mbar). The as‐obtained deposits show separated particles of different appearance at the substrate surface as evidenced by SEM. Non‐volatile 8 was applied as spin‐coating precursor for Cu and CuO formation [conc. 0.25 mol·L–1; volume 0.2 mL; 3000 rpm; depos. time 2 min; heating rate 50 K·min–1; holding time 60 min (Ar), 120 min (air) at 800 °C]. The samples on silicon consist of granulated particles (Ar) or are non‐dense with a grainy topography (air). EDX and XPS measurements confirmed the formation of Cu (Ar) or CuO (O2) with up to 13 mol‐% C impurity.

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Lewis-base copper(I) formates: Synthesis, reaction chemistry, structural characterization and their use as spin-coating precursors for copper deposition

Cited by 17 publications

References 65 publications

New nickel(ii) and copper(ii) complexes with unsymmetrical Schiff bases derived from (1R,2R)(−)cyclohexanediamine and the application of Cu(ii) complexes for hybrid thin layers deposition

New nickel(ii) and copper(ii) complexes with unsymmetrical Schiff bases derived from (1R,2R)(−)cyclohexanediamine and the application of Cu(ii) complexes for hybrid thin layers deposition

Copper(II) Perfluorinated Carboxylate Complexes with Small Aliphatic Amines as Universal Precursors for Nanomaterial Fabrication

Synthesis of β‐Ketoiminato Copper(II) Complexes and Their Use in Copper Deposition

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