The self-assembly of block copolymers to generate nanopatterns is of great interest as an inexpensive approach to sub-20 nm lithography. Compared to thermal annealing, solvent vapor annealing has several intriguing advantages with respect to the annealing of thin films of block copolymers, particularly for polymers with high interaction parameters, χ, and high molecular weights. In this methods paper, we describe a controlled solvent vapor flow annealing system with integrated in situ microscopy and laser reflectometry, as well as a feedback loop that automatically controls the solvent vapor flow rate, based upon real-time calculations of the difference between thickness set point and the observed film thickness. The feedback loop enables precise control of swelling and deswelling of the polymer thin film, the degree of swelling at the dwell period, and preprogrammed complex multistep annealing profiles. The in situ microscope provides critical insight into the morphological evolution of the block copolymer thin films over a broad area of the sample, revealing information about terraced phases, on the scale of tens and hundreds of micrometers, during the annealing process. This device could be a powerful tool for understanding and optimizing solvent annealing by providing multiple sources of in situ information, at both the micro- and nanoscales.
The self-assembly of block copolymer (BCP) thin films is a versatile method for producing periodic nanoscale patterns with a variety of shapes. The key to attaining a desired pattern or structure is the annealing step undertaken to facilitate the reorganization of nanoscale phase-segregated domains of the BCP on a surface. Annealing BCPs on silicon substrates using a microwave oven has been shown to be very fast (seconds to minutes), both with and without contributions from solvent vapor. The mechanism of the microwave annealing process remains, however, unclear. This work endeavors to uncover the key steps that take place during microwave annealing, which enable the self-assembly process to proceed. Through the use of in situ temperature monitoring with a fiber optic temperature probe in direct contact with the sample, we have demonstrated that the silicon substrate on which the BCP film is cast is the dominant source of heating if the doping of the silicon wafer is sufficiently low. Surface temperatures as high as 240 °C are reached in under 1 min for lightly doped, high resistivity silicon wafers (n- or p-type). The influence of doping, sample size, and BCP composition was analyzed to rule out other possible mechanisms. In situ temperature monitoring of various polymer samples (PS, P2VP, PMMA, and the BCPs used here) showed that the polymers do not heat to any significant extent on their own with microwave irradiation of this frequency (2.45 GHz) and power (∼600 W). It was demonstrated that BCP annealing can be effectively carried out in 60 s on non-microwave-responsive substrates, such as highly doped silicon, indium tin oxide (ITO)-coated glass, glass, and Kapton, by placing a piece of high resistivity silicon wafer in contact with the sample-in this configuration, the silicon wafer is termed the heating element. Annealing and self-assembly of polystyrene-block-poly(2-vinylpyridine) (PS-b-P2VP) and polystyrene-block-poly(methyl methacrylate) (PS-b-PMMA) BCPs into horizontal cylinder structures were shown to take place in under 1 min, using a silicon wafer heating element, in a household microwave oven. Defect densities were calculated and were shown to decrease with higher maximum obtained temperatures. Conflicting results in the literature regarding BCP annealing with microwave are explained in light of the results obtained in this study.
Vous avez des questions? Nous pouvons vous aider. Pour communiquer directement avec un auteur, consultez la première page de la revue dans laquelle son article a été publié afin de trouver ses coordonnées. Si vous n'arrivez pas à les repérer, communiquez avec nous à PublicationsArchive-ArchivesPublications@nrc-cnrc.gc.ca. Questions? Contact the NRC Publications Archive team atPublicationsArchive-ArchivesPublications@nrc-cnrc.gc.ca. If you wish to email the authors directly, please see the first page of the publication for their contact information. NRC Publications Archive Archives des publications du CNRCThis publication could be one of several versions: author's original, accepted manuscript or the publisher's version. / La version de cette publication peut être l'une des suivantes : la version prépublication de l'auteur, la version acceptée du manuscrit ou la version de l'éditeur. For the publisher's version, please access the DOI link below./ Pour consulter la version de l'éditeur, utilisez le lien DOI ci-dessous.http://doi.org/10.1021/acs.langmuir.6b01365Access and use of this website and the material on it are subject to the Terms and Conditions set forth at Sequential nanopatterned block copolymer self-assembly on surfaces Jin, Cong; Olsen, Brian C.; Wu, Nathanael L. Y.; Luber, Erik J.; Buriak, Jillian M.http://nparc.cisti-icist.nrc-cnrc.gc.ca/fra/droits L'accès à ce site Web et l'utilisation de son contenu sont assujettis aux conditions présentées dans le site LISEZ CES CONDITIONS ATTENTIVEMENT AVANT D'UTILISER CE SITE WEB. NRC Publications Record / Notice d'Archives des publications de CNRC:http://nparc.cisti-icist.nrc-cnrc.gc.ca/eng/view/object/?id=ae78d03e-4423-4de5-89fb-823bb3c0676b http://nparc.cisti-icist.nrc-cnrc.gc.ca/fra/voir/objet/?id=ae78d03e-4423-4de5-89fb-823bb3c0676bSequential Nanopatterned Block Copolymer Self-Assembly on Surfaces ABSTRACT: Bottom-up self-assembly of high-density blockcopolymer nanopatterns is of significant interest for a range of technologies, including memory storage and low-cost lithography for on-chip applications. The intrinsic or native spacing of a given block copolymer is dependent upon its size (N, degree of polymerization), composition, and the conditions of selfassembly. Polystyrene-block-polydimethylsiloxane (PS-b-PDMS) block copolymers, which are well-established for the production of strongly segregated single-layer hexagonal nanopatterns of silica dots, can be layered sequentially to produce density-doubled and -tripled nanopatterns. The center-tocenter spacing and diameter of the resulting silica dots are critical with respect to the resulting double-and triple-layer assemblies because dot overlap reduces the quality of the resulting pattern. The addition of polystyrene (PS) homopolymer to PS-b-PDMS reduces the size of the resulting silica dots but leads to increased disorder at higher concentrations. The quality of these density-multiplied patterns can be calculated and predicted using parameters easily derived from SEM micrographs of corresponding single...
Block copolymer (BCP) self-assembly is of great interest as a cost-effective method for large-scale, high-resolution nanopattern fabrication. Directed self-assembly can induce long-range order and registration, reduce defect density, and enable access to patterns of higher complexity. Here we demonstrate preferential orientation of two incommensurate BCP dot arrays. A bottom layer of hexagonal silica dots is prepared via typical self-assembly from a PS-b-PDMS block copolymer. Self-assembly of a second, or top, layer of a different PS-b-PDMS block copolymer that forms a hexagonal dot pattern with different periodicity results in a predictable moiré superstructure. Four distinct moiré superstructures were demonstrated through a combination of different BCPs and different order of annealing. The registration force of the bottom layer of hexagonal dots is sufficient to direct the self-assembly of the top layer to adopt a preferred relative angle of rotation. Large-area helium ion microscopy imaging enabled quantification of the distributions of relative rotations between the two lattices in the moiré superstructures, yielding statistically meaningful results for each combination. It was also found that if the bottom layer dots were too large, the resulting moiré pattern was lost. A small reduction in the bottom layer dot size, however, resulted in large-area moiré superstructures, suggesting a specific size regime where interlayer registration forces can induce long-range preferential alignment of incommensurate BCP dot arrays.
Interfaces comprising incommensurate or twisted hexagonal lattices are ubiquitous and of great interest, from adsorbed organic/inorganic interfaces in electronic devices, to superlubricants, and more recently to van der Waals bilayer heterostructures (vdWHs) of graphene and other 2D materials that demonstrate a range of properties such as superconductivity and ferromagnetism. Here we show how growth of 2D crystalline domains of soft block copolymers (BCPs) on patterned hard hexagonal lattices provide fundamental insights into van der Waals heteroepitaxy. At moderate registration forces, it is experimentally found that these BCP-hard lattice vdWHs do not adopt a simple moiré superstructure, but instead adopt local structural relaxations known as mass density waves (MDWs). Simulations reveal that MDWs are a primary mechanism of energy minimization and are the origin of the observed preferential twist angle between the lattices.
β-sialon bonded corundum-based sliding gate plate was developed from raw materials of Al, metallic silicon and alumina through nitriding-reaction process. It was found that the effects of β-sialon content on the physical properties are significant and the mechanical properties of developed sliding gate plate are strongly related to the Z-value. The materials with Z value of 2 and 20wt% β-sialon, exhibit the highest hot modulus of rupture and cold crushing strength. It was also found that sialon bonded corundum-based material has good oxidation resistance because a protective layer is formed during oxidation process.
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