This paper describes a new method for forming micron-and submicron-scale patterns of copper on surfaces. This method uses microcontact printing (µCP) to deposit colloids that serve as catalysts for the selective electroless deposition of copper. A patterned elastomeric stamp fabricated from poly-(dimethylsiloxane) was used to deliver the catalystspalladium colloids stabilized with tetraalkylammonium bromidessto the substrate surface. The electroless deposition of the copper on the sample occurred only where palladium colloid was transferred to the substrate. Electroless deposition catalyzed by the colloids resulted in the formation of metal structures with features having submicron dimensions, with an edge resolution in the range of 100 nm. This technique of activating substrates for electroless metalization was successfully used to pattern glass, (Si/SiO 2), and polymers; both flat and curved substrates were used. Microcontact printing of colloids was also used to fabricate metal structures whose thicknesses were varied in different regions of the sample (multilevel metal structures). Free-standing metal structures were produced by dissolving the substrate after the metal film had reached the desired thickness.
Scanning tunneling microscopy (STM) and high-resolution transmission electron microscopy (TEM) have been used to determine the dimensions of a series of palladium clusters stabilized by tetraalkylammonium salts. Electrochemically prepared colloids were used in which the average diameter of the inner metal core was varied between 2 and 4 nanometers, and the size of the ammonium ions was adjusted in the series (+)N(n-C(4)H(9))(4) < (+)N(n-C(8)H(17))(4) < (+)N(n-C(18)H(37))(4). The difference between the mean diameter determined by STM and that measured by TEM allows the determination of the thickness of the protective surfactant layer. On the basis of these studies, a model of the geometric properties of ammonium-stabilized palladium clusters has been proposed. Suggestions for the mechanism of the STM imaging process are also made.
This paper describes a new method of reducing the size of the metal features made by electroless deposition and fabricating complex-shaped, patterned surfaces. Microcontact printing (µCP) was used to pattern oriented glassy polymers with palladium colloids, stabilized with tetraoctadecylammonium bromide. These colloids are catalysts for the selective electroless deposition of copper. Annealing of the activated polymer at a temperature slightly above its glass transition temperature led to a shrinkage of the substrate. Immersion of the shrunken substrate in the plating bath yielded the metal features. The maximum shrinkage of the feature size achieved was on the order of a factor of ∼4 in one direction of the oriented polymer and of ∼7 in the perpendicular direction. Control of the extent and direction of shrinkage allowed the fabrication of metal features with sizes and shapes different from those on the polydimethylsiloxane stamp used for the patterning of the substrate and from the draw ratios. Free-standing metal structures were produced by dissolving the substrate after the metal film had reached the desired thickness. Complexshaped, patterned surfaces could be fabricated by wrapping the activated polymer film around a scaffolding or template; during the annealing, the polymer adapted the shape of the underlying scaffolding. Metalization of the activated, shaped substrate resulted in patterned three-dimensional structures.
The magnetization of stabilized cobalt colloids in tetrahydrofuran has been studied by a superconducting quantum interference device (SQUID) and magnetic balance measurements in dependence of applied magnetic field and temperature. The colloids are generated by a newly developed electrochemical method which allows one to generate clusters containing about 1000 atoms with a narrow size distribution. The final size distribution of the clusters is examined by high resolution transmission electron microscopy and small angle x-ray scattering. The magnetization curves have been determined with special emphasis on changes at the freezing point of the solution. The curves of the liquid phase can be reasonably described by the Langevin function and the magnetic moments of isolated cobalt clusters that have been recently measured by Stern–Gerlach experiments. Deviations that appear at the freezing point can be understood in terms of magnetic anisotropy effects. It is shown that the cluster sizes and the susceptibilities of the dispersions are related. Therefore the growth of the clusters during the electrolysis can be directly observed by measuring the susceptibility in dependence of the charge transport in the cell.
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