Dense periodic arrays of holes and dots have been fabricated in a silicon nitride–coated silicon wafer. The holes are 20 nanometers across, 40 nanometers apart, and hexagonally ordered with a polygrain structure that has an average grain size of 10 by 10. Spin-coated diblock copolymer thin films with well-ordered spherical or cylindrical microdomains were used as the templates. The microdomain patterns were transferred directly to the underlying silicon nitride layer by two complementary techniques that resulted in opposite tones of the patterns. This process opens a route for nanometer-scale surface patterning by means of spontaneous self-assembly in synthetic materials on length scales that are difficult to obtain by standard semiconductor lithography techniques.
As technology continues towards smaller, thinner and lighter devices, more stringent demands are placed on thin polymer films as diffusion barriers, dielectric coatings, electronic packaging and so on. Therefore, there is a growing need for testing platforms to rapidly determine the mechanical properties of thin polymer films and coatings. We introduce here an elegant, efficient measurement method that yields the elastic moduli of nanoscale polymer films in a rapid and quantitative manner without the need for expensive equipment or material-specific modelling. The technique exploits a buckling instability that occurs in bilayers consisting of a stiff, thin film coated onto a relatively soft, thick substrate. Using the spacing of these highly periodic wrinkles, we calculate the film's elastic modulus by applying well-established buckling mechanics. We successfully apply this new measurement platform to several systems displaying a wide range of thicknessess (nanometre to micrometre) and moduli (MPa to GPa).
The elastic moduli of ultrathin poly(styrene) (PS) and poly(methylmethacrylate) (PMMA) films of thickness ranging from 200 nm to 5 nm were investigated using a buckling-based metrology. Below 40 nm, the apparent modulus of the PS and PMMA films decreases dramatically, with an order of magnitude decrease compared to bulk values for the thinnest films measured. We can account for the observed decrease in apparent modulus by applying a composite model based on the film having a surface layer with a reduced modulus and of finite thickness. The observed decrease in the apparent modulus highlights issues in mechanical stability and robustness of sub-40 nm polymer films and features.
We have studied the ordering dynamics of the striped patterns of a single layer of cylindrical block copolymer microdomains in a thin film. By tracking disclinations during annealing with time-lapse atomic force microscopy, we observe a dominant mechanism of disclination annihilation involving three or four disclinations (quadrupoles). Pairwise disclination annihilation events are suppressed as a result of the topological constraints in this system. The kinetic scaling laws with exponents observed here are consistent with topologically allowed annihilation events involving multiple disclinations. The results provide insight into two-dimensional pattern formation and may lead to the successful application of block copolymer lithography.
The structure of thin films of a symmetric diblock copolymer, P(dS-b-MMA) (dS ) perdeuterated styrene, MMA ) methyl methacrylate), was investigated near preferential and nonpreferential (neutral) surfaces. Neutral surfaces were achieved at the substrate and air interfaces by localizing random copolymer, P(S-r-MMA), having a styrene fraction of 0.60, to each of these interfaces. This was performed by chemically grafting the random copolymer to the substrate and anchoring a surface active random copolymer having a perfluorinated end group to the air interface, respectively. Neutron reflectivity and small-angle neutron scattering were used to determine the orientation of the lamellar microdomains for films having various boundary conditions. Successive steps of CF 4 reactive ion etching followed by field emission scanning electron microscopy were used to ascertain the orientation of the microdomains as a function of film depth. For films confined between two continuous neutral surfaces, the orientation of the lamellar microdomains is observed to be perpendicular to the film surfaces throughout the entire film thickness.
We have followed the coarsening dynamics of a single layer of cylindrical block copolymer microdomains in a thin film. This system has the symmetry of a two-dimensional smectic. The orientational correlation length of the microdomains was measured by scanning electron microscopy and found to grow with the average spacing between +/-1/2 disclinations, following a power law xi2(t) approximately t(1/4). By tracking disclinations during annealing with time-lapse atomic force microscopy, we observe dominant mechanisms of disclination annihilation involving tripoles and quadrupoles (three and four disclinations, respectively). We describe how annihilation events involving multiple disclinations result in similarly reduced kinetic exponents as observed here. These results map onto a wide variety of physical systems that exhibit similarly striped patterns.
Frontal photopolymerization (FPP) offers numerous advantages for the rapid prototyping of microfluidic devices. Quantitative utilization of this method, however, requires a control of the vertical dimensions of the patterned resist material. To address this fundamental problem, we study the ultraviolet (UV) photopolymerization of a series of multifunctional thiolene resists through a combination of experiments and analytical modeling of the polymerization fronts. We describe this nonlinear spatio-temporal growth process in terms of a "minimal" model involving an order parameter phi(x, t) characterizing the extent of monomer-to-polymer conversion, the optical attenuation T(x, t), and the solid front position h(t). The latter exhibits an induction time (or equivalent critical UV dose) characterizing the onset of frontal propagation. We also observe a novel transition between two logarithmic rates of growth, determined by the Beer-Lambert attenuation constants mu(0) and mu(infinity) of the monomer and fully polymerized material, respectively. The measured frontal kinetics and optical transmission of the thiolene resist materials are consistent with our photopolymerization model, exhibiting both "photodarkening" and "photoinvariant" polymerization. This is apparently the first observation of photodarkening reported in FPP. On the basis of these results, multilevel fluidic devices with controlled height are readily fabricated with modulated illumination. A representative two-level microfluidic device, incorporating a chaotic mixer, a T junction, and a series of controlled flow constrictions, illustrates the practical versatility of this fabrication method.
We investigate a buckling instability by both small angle light scattering and atomic force microscopy, demonstrating that a tunable phase grating can be created with a mechanical instability. The instability is realized in a prestressed silicone sheet coated with a glassy polymer film. Compression of the sample results in a sinusoidally wrinkled surface where the amplitude is controlled by the degree of compression and the wavelength by film thickness. We model the system with Fourier optics, explaining the positions and relative intensities of the diffraction orders.
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