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1.  Formation of precise 2D Au particle arrays via thermally induced dewetting on pre-patterned substrates 
Summary
The fabrication of precise 2D Au nanoparticle arrays over a large area is presented. The technique was based on pre-patterning of the substrate before the deposition of a thin Au film, and the creation of periodic particle arrays by subsequent dewetting induced by annealing. Two types of pre-patterned substrates were used: The first comprised an array of pyramidal pits and the second an array of circular holes. For the dewetting of Au films on the pyramidal pit substrate, the structural curvature-driven diffusion cooperates with capillarity-driven diffusion, resulting in the formation of precise 2D particle arrays for films within a structure dependent thickness-window. For the dewetting of Au films on the circular hole substrate, the periodic discontinuities in the films, induced by the deposition, can limit the diffusion paths and lead to the formation of one particle per individual separated region (holes or mesas between holes), and thus, result in the evolution of precise 2D particle arrays. The influence of the pre-patterned structures and the film thickness is analyzed and discussed. For both types of pre-patterned substrate, the Au film thickness had to be adjusted in a certain thickness-window in order to achieve the precise 2D particle arrays.
doi:10.3762/bjnano.2.37
PMCID: PMC3148046  PMID: 21977445
Au particles; dewetting; nanoimprint lithography; nanoparticle array
2.  General preparation for Pt-based alloy nanoporous nanoparticles as potential nanocatalysts 
Scientific Reports  2011;1:37.
Although Raney nickel made by dealloying has been used as a heterogeneous catalyst in a variety of organic syntheses for more than 80 years, only recently scientists have begun to realize that dealloying can generate nanoporous alloys with extraordinary structural characteristics. Herein, we achieved successful synthesis of a variety of monodisperse alloy nanoporous nanoparticles via a facile chemical dealloying process using nanocrystalline alloys as precursors. The as-prepared alloy nanoporous nanoparticles with large surface area and small pores show superior catalytic properties compared with alloyed nanoparticles. It is believed that these novel alloy nanoporous nanoparticles would open up new opportunities for catalytic applications.
doi:10.1038/srep00037
PMCID: PMC3216524  PMID: 22355556
3.  Electrochemical and Structural Study of a Chemically Dealloyed PtCu Oxygen Reduction Catalyst 
A carbon-supported, dealloyed platinum-copper (Pt-Cu) oxygen reduction catalyst was prepared using a multi-step synthetic procedure. Material produced at each step was characterized using high angle annular dark field scanning transmission electron microscopy (HAADF-STEM), electron energy loss spectroscopy (EELS) mapping, x-ray absorption spectroscopy (XAS), x-ray diffraction (XRD), and cyclic voltammetry (CV), and its oxygen reduction reaction (ORR) activity was measured by a thin-film rotating disk electrode (TF-RDE) technique. The initial synthetic step, a co-reduction of metal salts, produced a range of poorly crystalline Pt, Cu, and Pt-Cu alloy nanoparticles that nevertheless exhibited good ORR activity. Annealing this material alloyed the metals and increased particle size and crystallinity. TEM shows the annealed catalyst to include particles of various sizes, large (>25 nm), medium (12–25 nm), and small (<12 nm). Most of the small and medium-sized particles exhibited a partial or complete coreshell (Cu-rich core and Pt shell) structure with the smaller particles typically having more complete shells. The appearance of Pt shells after annealing indicates that they are formed by a thermal diffusion mechanism. Although the specific activity of the catalyst material was more than doubled by annealing, the concomitant decrease in Pt surface area resulted in a drop in its mass activity. Subsequent dealloying of the catalyst by acid treatment to partially remove the copper increased the Pt surface area by changing the morphology of the large and some medium particles to a “Swiss cheese” type structure having many voids. The smaller particles retained their core-shell structure. The specific activity of the catalyst material was little reduced by dealloying, but its mass activity was more than doubled due to the increase in surface area. The possible origins of these results are discussed in this report.
doi:10.1021/jp106042z
PMCID: PMC3691677  PMID: 23807900
Dealloyed catalyst; fuel cell; PtCu catalyst; HAADF STEM; EELS; TEM
4.  Mechanically Modulated Dewetting by Atomic Force Microscope for Micro- and Nano- Droplet Array Fabrication 
Scientific Reports  2014;4:6524.
Organizing a material into well-defined patterns during the dewetting process provides an attractive micro-/nano-fabrication method without using a conventional lithographic process, and hence, offers potential applications in organic electronics, optics systems, and memory devices. We report here how the mechanical modification of polymer surface by an Atomic Force Microscope (AFM) can be used to guide thin film dewetting evolution and break the intrinsic spatial correlation of spontaneous instability. An AFM is used to implement the mechanical modification of progressively narrow grids to investigate the influence of pattern size on the modulation of ultrathin polystyrene films dewetting evolution. For films with different initial thicknesses, when grid size is close to or below the characteristic wavelength of instability, the spinodal dewetting is suppressed, and film rupture is restricted to the cutting trench. We will show in this paper it is possible to generate only one droplet per gridded area on a thin film subsequent to nucleation dominated dewetting on a non-patterned substrate. Furthermore, when the grid periodicity exceeds the spinodal length, the number of droplets in predefined areas gradually approaches that associated with unconfined dewetting.
doi:10.1038/srep06524
PMCID: PMC4185381  PMID: 25283744
5.  Catalytic activity of nanostructured Au: Scale effects versus bimetallic/bifunctional effects in low-temperature CO oxidation on nanoporous Au 
Summary
The catalytic properties of nanostructured Au and their physical origin were investigated by using the low-temperature CO oxidation as a test reaction. In order to distinguish between structural effects (structure–activity correlations) and bimetallic/bifunctional effects, unsupported nanoporous gold (NPG) samples prepared from different Au alloys (AuAg, AuCu) by selective leaching of a less noble metal (Ag, Cu) were employed, whose structure (surface area, ligament size) as well as their residual amount of the second metal were systematically varied by applying different potentials for dealloying. The structural and chemical properties before and after 1000 min reaction were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). The catalytic behavior was evaluated by kinetic measurements in a conventional microreactor and by dynamic measurements in a temporal analysis of products (TAP) reactor. The data reveal a clear influence of the surface contents of residual Ag and Cu species on both O2 activation and catalytic activity, while correlations between activity and structural parameters such as surface area or ligament/crystallite size are less evident. Consequences for the mechanistic understanding and the role of the nanostructure in these NPG catalysts are discussed.
doi:10.3762/bjnano.4.13
PMCID: PMC3596058  PMID: 23503603
AuAg alloy; AuCu alloy; CO oxidation; dynamic studies; kinetics; nanoporous Au (NPG) catalyst; oxygen storage capacity (OSC); temporal analysis of products (TAP)
6.  Supported Membranes Embedded with Fixed Arrays of Gold Nanoparticles 
Nano Letters  2011;11(11):4912-4918.
We present a supported membrane platform consisting of a fluid lipid bilayer membrane embedded with a fixed array of gold nanoparticles. The system is realized by preforming a hexagonal array of gold nanoparticles (∼5–7 nm) with controlled spacing (∼50–150 nm) fixed to a silica or glass substrate by block copolymer lithography. Subsequently, a supported membrane is assembled over the intervening bare substrate. Proteins or other ligands can be associated with the fluid lipid component, the fixed nanoparticle component, or both, providing a hybrid interface consisting of mobile and immobile components with controlled geometry. We test different biochemical coupling strategies to bind individual proteins to the particles surrounded by a fluid lipid membrane. The coupling efficiency to nanoparticles and the influence of nanoparticle arrays on the surrounding membrane integrity are characterized by fluorescence imaging, correlation spectroscopy, and super-resolution fluorescence microscopy. Finally, the functionality of this system for live cell experiments is tested using the ephrin-A1–EphA2 juxtacrine signaling interaction in human breast epithelial cells.
doi:10.1021/nl202847t
PMCID: PMC3212849  PMID: 21967595
Nanoparticles; supported lipid bilayers; nanoparticle labeling; FCS; PALM
7.  RNA Nanotechnology: Engineering, Assembly and Applications in Detection, Gene Delivery and Therapy 
Biological macromolecules including DNA, RNA, and proteins, have intrinsic features that make them potential building blocks for the bottom-up fabrication of nanodevices. RNA is unique in nanoscale fabrication due to its amazing diversity of function and structure. RNA molecules can be designed and manipulated with a level of simplicity characteristic of DNA while possessing versatility in structure and function similar to that of proteins. RNA molecules typically contain a large variety of single stranded loops suitable for inter- and intra-molecular interaction. These loops can serve as mounting dovetails obviating the need for external linking dowels in fabrication and assembly.
The self-assembly of nanoparticles from RNA involves cooperative interaction of individual RNA molecules that spontaneously assemble in a predefined manner to form a larger two- or three-dimensional structure. Within the realm of self-assembly there are two main categories, namely template and non-template. Template assembly involves interaction of RNA molecules under the influence of specific external sequence, forces, or spatial constraints such as RNA transcription, hybridization, replication, annealing, molding, or replicas. In contrast, non-template assembly involves formation of a larger structure by individual components without the influence of external forces. Examples of non-template assembly are ligation, chemical conjugation, covalent linkage, and loop/loop interaction of RNA, especially the formation of RNA multimeric complexes. The best characterized RNA multiplier and the first to be described in RNA nanotechnological application is the motor pRNA of bacteriophage phi29 which form dimers, trimers, and hexamers, via hand-in-hand interaction. phi29 pRNA can be redesigned to form a variety of structures and shapes including twins, tetramers, rods, triangles, and 3D arrays several microns in size via interaction of programmed helical regions and loops. 3D RNA array formation requires a defined nucleotide number for twisting and a palindromic sequence. Such arrays are unusually stable and resistant to a wide range of temperatures, salt concentrations, and pH. Both the therapeutic siRNA or ribozyme and a receptor-binding RNA aptamer or other ligands have been engineered into individual pRNAs. Individual chimeric RNA building blocks harboring siRNA or other therapeutic molecules have been fabricated subsequently into a trimer through hand-in-hand interaction of the engineered right and left interlocking RNA loops. The incubation of these particles containing the receptor-binding aptamer or other ligands results in the binding and co-entry of trivalent therapeutic particles into cells. Such particles were subsequently shown to modulate the apoptosis of cancer cells in both cell cultures and animal trials. The use of such antigen-free 20–40 nm particles holds promise for the repeated long-term treatment of chronic diseases. Other potentially useful RNA molecules that form multimers include HIV RNA that contain kissing loop to form dimers, tecto-RNA that forms a “jigsaw puzzle,” and the Drosophila bicoid mRNA that forms multimers via “hand-by-arm” interactions.
Applications of RNA molecules involving replication, molding, embossing, and other related techniques, have recently been described that allow the utilization of a variety of materials to enhance diversity and resolution of nanomaterials. It should eventually be possible to adapt RNA to facilitate construction of ordered, patterned, or pre-programmed arrays or superstructures. Given the potential for 3D fabrication, the chance to produce reversible self-assembly, and the ability of self-repair, editing and replication, RNA self-assembly will play an increasingly significant role in integrated biological nanofabrication. A random 100-nucleotide RNA library may exist in 1.6 × 1060 varieties with multifarious structure to serve as a vital system for efficient fabrication, with a complexity and diversity far exceeding that of any current nanoscale system.
This review covers the basic concepts of RNA structure and function, certain methods for the study of RNA structure, the approaches for engineering or fabricating RNA into nanoparticles or arrays, and special features of RNA molecules that form multimers. The most recent development in exploration of RNA nanoparticles for pathogen detection, drug/gene delivery, and therapeutic application is also introduced in this review.
PMCID: PMC2842999  PMID: 16430131
RNA; Nanotechnology; Self-Assembly; RNA Application; phi29 pRNA
8.  Characterization of protein immobilization on nanoporous gold using atomic force microscopy and scanning electron microscopy† 
Nanoscale  2011;3(8):3395-3407.
Nanoporous gold (NPG), made by dealloying low carat gold alloys, is a relatively new nanomaterial finding application in catalysis, sensing, and as a support for biomolecules. NPG has attracted considerable interest due to its open bicontinuous structure, high surface-to-volume ratio, tunable porosity, chemical stability and biocompatibility. NPG also has the attractive feature of being able to be modified by self-assembled monolayers. Here we use scanning electron microscopy (SEM) and atomic force microscopy (AFM) to characterize a highly efficient approach for protein immobilization on NPG using N-hydroxysuccinimide (NHS) ester functionalized self-assembled monolayers on NPG with pore sizes in the range of tens of nanometres. Comparison of coupling under static versus flow conditions suggests that BSA (Bovine Serum Albumin) and IgG (Immunoglobulin G) can only be immobilized onto the interior surfaces of free standing NPG monoliths with good coverage under flow conditions. AFM is used to examine protein coverage on both the exterior and interior of protein modified NPG. Access to the interior surface of NPG for AFM imaging is achieved using a special procedure for cleaving NPG. AFM is also used to examine BSA immobilized on rough gold surfaces as a comparative study. In principle, the general approach described should be applicable to many enzymes, proteins and protein complexes since both pore sizes and functional groups present on the NPG surfaces are controllable.
doi:10.1039/c1nr10427f
PMCID: PMC3168530  PMID: 21750834
9.  Fabrication of Nickel Nanostructure Arrays Via a Modified Nanosphere Lithography 
In this paper, we present a modified nanosphere lithographic scheme that is based on the self-assembly and electroforming techniques. The scheme was demonstrated to fabricate a nickel template of ordered nanobowl arrays together with a nickel nanostructure array-patterned glass substrate. The hemispherical nanobowls exhibit uniform sizes and smooth interior surfaces, and the shallow nanobowls with a flat bottom on the glass substrate are interconnected as a net structure with uniform thickness. A multiphysics model based on the level set method (LSM) was built up to understand this fabricating process by tracking the interface between the growing nickel and the electrolyte. The fabricated nickel nanobowl template can be used as a mold of long lifetime in soft lithography due to the high strength of nickel. The nanostructure–patterned glass substrate can be used in optical and magnetic devices due to their shape effects. This fabrication scheme can also be extended to a wide range of metals and alloys.
doi:10.1007/s11671-010-9770-3
PMCID: PMC3211311
Electroforming; Level set method; Nanostructure arrays; Nanosphere lithography
10.  Emerging use of nanostructure films containing capped gold nanoparticles in biosensors 
The localized surface plasmon resonance (LSPR) property of gold nanoparticles (GNP) has been exploited in a variety of optical sensor configurations including solution-based bioassays, paper-based colorimetric detection, surface-confined nanoparticle film/array-based sensing, etc. Amongst these, gold nanostructured films are of great interest because of their high stability, good reproducibility, robustness, and cost-effectiveness. The inherent optical characteristics of GNP, are attributed to parameters like size and shape (eg, nanospheres, nanorods, nanostars), eg, LSPR spectral location sensitivity to the local environment, composition (eg, gold–silver or silica–gold nanoshells), sensing volume, mesospacing, and multiplexing. These properties allow sensor tunability, enabling enhanced sensitivity and better performance of these biosensors. Ultrasensitive biosensor designs were realized using gold nanostructured films fabricated by bottom-up as well as top-down approaches. In this review, we describe the past, present, and future trends in the development of GNP-LSPR-based sensors, concentrating on both design (fabrication) and application. In the process, we have discussed various combinations of GNP size and shape, substrate, and application domains.
doi:10.2147/NSA.S8981
PMCID: PMC3781700  PMID: 24198481
localized surface plasmon resonance; gold nanoparticles; label-free optical biosensor
11.  Preparation and characterization of supported magnetic nanoparticles prepared by reverse micelles 
Summary
Monatomic (Fe, Co) and bimetallic (FePt and CoPt) nanoparticles were prepared by exploiting the self-organization of precursor loaded reverse micelles. Achievements and limitations of the preparation approach are critically discussed. We show that self-assembled metallic nanoparticles can be prepared with diameters d = 2–12 nm and interparticle distances D = 20–140 nm on various substrates. Structural, electronic and magnetic properties of the particle arrays were characterized by several techniques to give a comprehensive view of the high quality of the method. For Co nanoparticles, it is demonstrated that magnetostatic interactions can be neglected for distances which are at least 6 times larger than the particle diameter. Focus is placed on FePt alloy nanoparticles which show a huge magnetic anisotropy in the L10 phase, however, this is still less by a factor of 3–4 when compared to the anisotropy of the bulk counterpart. A similar observation was also found for CoPt nanoparticles (NPs). These results are related to imperfect crystal structures as revealed by HRTEM as well as to compositional distributions of the prepared particles. Interestingly, the results demonstrate that the averaged effective magnetic anisotropy of FePt nanoparticles does not strongly depend on size. Consequently, magnetization stability should scale linearly with the volume of the NPs and give rise to a critical value for stability at ambient temperature. Indeed, for diameters above 6 nm such stability is observed for the current FePt and CoPt NPs. Finally, the long-term conservation of nanoparticles by Au photoseeding is presented.
doi:10.3762/bjnano.1.5
PMCID: PMC3045932  PMID: 21977392
Co; CoPt; core–shell particles; FePt; magnetic anisotropy; magnetic particles; plasma etching; reverse micelles; self-assembly
12.  Towards Optical DNA Sequencing Using Nanopore Arrays 
Next generation DNA sequencing methods that utilize nanometersize pores have been subject of numerous studies in past years. One of the compelling features of the nanopore technique lies in its ability to electrophoretically focus long DNA strands towards the pore area and thread the molecules inside the pore in a highly efficient manner. Thus extremely small copy numbers of the target DNA are required for analyses†, circumventing the need for costly and time-consuming target amplification. One of the major bottlenecks for the realization of a viable nanopore-based DNA sequencing has been the ability to simultaneously read the electrical signals from hundreds to thousands of nanopores densely fabricated on sub-millimeter size silicon chip. To address this issue we develop an extremely high throughput single molecule DNA sequencing technique, which employs optical, widefield readout from DNA molecules electrically mobilized through the nanopores. Our method consists of two steps: First, target DNA molecules are converted according to pre-determined code, which is recognized by molecular beacons with four types of fluorophores (each uniquely corresponding to one of the four DNA bases). Solid-state nanopores are then used to sequentially strip off the beacons, leading to a series of photon bursts that can be detected with a custom made microscope. Notably the method circumvents the use of enzymes in the readout stage, and is thus not affected by their limited processivity and lifetime. Here we demonstrate the feasibility of this method using a two color model system, and show for the first time, individual nucleotide recognition from multiple nanopores simultaneously‡, allowing straightforward parallelization of our system to nanopore arrays. †. Wanunu, M., W. Morrison, Y. Rabin, A. Y. Grosberg, and A. Meller. 2010. Electrostatic Focusing of Unlabeled DNA into Nanoscale Pores using a Salt Gradient. Nature Nanotechnology 5:160–165. ‡. McNally, B., A. Singer, Z. Yu, Y. Sun, Z. Weng, and A. Meller. 2010. Optical Recognition of Converted DNA Nucleotides for Single-Molecule DNA Sequencing Using Nanopore Arrays. Nano Letters 10:2237–2244.
PMCID: PMC3186509
13.  Ordered arrays of nanoporous silicon nanopillars and silicon nanopillars with nanoporous shells 
The fabrication of ordered arrays of nanoporous Si nanopillars with and without nanoporous base and ordered arrays of Si nanopillars with nanoporous shells are presented. The fabrication route is using a combination of substrate conformal imprint lithography and metal-assisted chemical etching. The metal-assisted chemical etching is performed in solutions with different [HF]/[H2O2 + HF] ratios. Both pore formation and polishing (marked by the vertical etching of the nanopillars) are observed in highly doped and lightly doped Si during metal-assisted chemical etching. Pore formation is more active in the highly doped Si, while the transition from polishing to pore formation is more obvious in the lightly doped Si. The etching rate is clearly higher in the highly doped Si. Oxidation occurs on the sidewalls of the pillars by etching in solutions with small [HF]/[H2O2 + HF] ratios, leading to thinning, bending, and bonding of pillars.
doi:10.1186/1556-276X-8-42
PMCID: PMC3570473  PMID: 23336430
Nanoporous Si; Pillars; Nanowires; Metal-assisted chemical etching; Nanoimprint lithography
14.  Lithography-Free Fabrication of Large Area Subwavelength Antireflection Structures Using Thermally Dewetted Pt/Pd Alloy Etch Mask 
Nanoscale Research Letters  2009;4(4):364-370.
We have demonstrated lithography-free, simple, and large area fabrication method for subwavelength antireflection structures (SAS) to achieve low reflectance of silicon (Si) surface. Thin film of Pt/Pd alloy on a Si substrate is melted and agglomerated into hemispheric nanodots by thermal dewetting process, and the array of the nanodots is used as etch mask for reactive ion etching (RIE) to form SAS on the Si surface. Two critical parameters, the temperature of thermal dewetting processes and the duration of RIE, have been experimentally studied to achieve very low reflectance from SAS. All the SAS have well-tapered shapes that the refractive index may be changed continuously and monotonously in the direction of incident light. In the wavelength range from 350 to 1800 nm, the measured reflectance of the fabricated SAS averages out to 5%. Especially in the wavelength range from 550 to 650 nm, which falls within visible light, the measured reflectance is under 0.01%.
doi:10.1007/s11671-009-9255-4
PMCID: PMC2893707  PMID: 20596495
Subwavelength antireflection structure; Nanostructure; Thermal dewetting; Self-agglomeration
15.  Lithography-Free Fabrication of Large Area Subwavelength Antireflection Structures Using Thermally Dewetted Pt/Pd Alloy Etch Mask 
Nanoscale Research Letters  2009;4(4):364-370.
We have demonstrated lithography-free, simple, and large area fabrication method for subwavelength antireflection structures (SAS) to achieve low reflectance of silicon (Si) surface. Thin film of Pt/Pd alloy on a Si substrate is melted and agglomerated into hemispheric nanodots by thermal dewetting process, and the array of the nanodots is used as etch mask for reactive ion etching (RIE) to form SAS on the Si surface. Two critical parameters, the temperature of thermal dewetting processes and the duration of RIE, have been experimentally studied to achieve very low reflectance from SAS. All the SAS have well-tapered shapes that the refractive index may be changed continuously and monotonously in the direction of incident light. In the wavelength range from 350 to 1800 nm, the measured reflectance of the fabricated SAS averages out to 5%. Especially in the wavelength range from 550 to 650 nm, which falls within visible light, the measured reflectance is under 0.01%.
doi:10.1007/s11671-009-9255-4
PMCID: PMC2893707  PMID: 20596495
Subwavelength antireflection structure; Nanostructure; Thermal dewetting; Self-agglomeration
16.  Fabrication of Highly Ordered Polymeric Nanodot and Nanowire Arrays Templated by Supramolecular Assembly Block Copolymer Nanoporous Thin Films 
Nanoscale Research Letters  2009;4(5):459-464.
Realizing the vast technological potential of patternable block copolymers requires both the precise controlling of the orientation and long-range ordering, which is still a challenging topic so far. Recently, we have demonstrated that ordered nanoporous thin film can be fabricated from a simple supramolecular assembly approach. Here we will extend this approach and provide a general route to fabricate large areas of highly ordered polymeric nanodot and nanowire arrays. We revealed that under a mixture solvent annealing atmosphere, a near-defect-free nanoporous thin film over large areas can be achieved. Under the direction of interpolymer hydrogen bonding and capillary action of nanopores, this ordered porous nanotemplate can be properly filled with phenolic resin precursor, followed by curation and pyrolysis at middle temperature to remove the nanotemplate, a perfect ordered polymer nanodot arrays replication was obtained. The orientation of the supramolecular assembly thin films can be readily re-aligned parallel to the substrate upon exposure to chloroform vapor, so this facile nanotemplate replica method can be further extend to generate large areas of polymeric nanowire arrays. Thus, we achieved a successful sub-30 nm patterns nanotemplates transfer methodology for fabricating polymeric nanopattern arrays with highly ordered structure and tunable morphologies.
doi:10.1007/s11671-009-9263-4
PMCID: PMC2893920  PMID: 20596454
Supramolecular assembly; Nanoporous template; Hydrogen bonding; Polymeric nanodot arrays
17.  Fabrication of Highly Ordered Polymeric Nanodot and Nanowire Arrays Templated by Supramolecular Assembly Block Copolymer Nanoporous Thin Films 
Nanoscale Research Letters  2009;4(5):459-464.
Realizing the vast technological potential of patternable block copolymers requires both the precise controlling of the orientation and long-range ordering, which is still a challenging topic so far. Recently, we have demonstrated that ordered nanoporous thin film can be fabricated from a simple supramolecular assembly approach. Here we will extend this approach and provide a general route to fabricate large areas of highly ordered polymeric nanodot and nanowire arrays. We revealed that under a mixture solvent annealing atmosphere, a near-defect-free nanoporous thin film over large areas can be achieved. Under the direction of interpolymer hydrogen bonding and capillary action of nanopores, this ordered porous nanotemplate can be properly filled with phenolic resin precursor, followed by curation and pyrolysis at middle temperature to remove the nanotemplate, a perfect ordered polymer nanodot arrays replication was obtained. The orientation of the supramolecular assembly thin films can be readily re-aligned parallel to the substrate upon exposure to chloroform vapor, so this facile nanotemplate replica method can be further extend to generate large areas of polymeric nanowire arrays. Thus, we achieved a successful sub-30 nm patterns nanotemplates transfer methodology for fabricating polymeric nanopattern arrays with highly ordered structure and tunable morphologies.
doi:10.1007/s11671-009-9263-4
PMCID: PMC2893920  PMID: 20596454
Supramolecular assembly; Nanoporous template; Hydrogen bonding; Polymeric nanodot arrays
18.  Fabrication of Porous Anodic Alumina with Ultrasmall Nanopores 
Nanoscale Research Letters  2010;5(8):1257-1263.
Anodization of Al foil under low voltages of 1–10 V was conducted to obtain porous anodic aluminas (PAAs) with ultrasmall nanopores. Regular nanopore arrays with pore diameter 6–10 nm were realized in four different electrolytes under 0–30°C according to the AFM, FESEM, TEM images and current evolution curves. It is found that the pore diameter and interpore distance, as well as the barrier layer thickness, are not sensitive to the applied potentials and electrolytes, which is totally different from the rules of general PAA fabrication. The brand-new formation mechanism has been revealed by the AFM study on the samples anodized for very short durations of 2–60 s. It is discovered for the first time that the regular nanoparticles come into being under 1–10 V at the beginning of the anodization and then serve as a template layer dominating the formation of ultrasmall nanopores. Under higher potentials from 10 to 40 V, the surface nanoparticles will be less and less and nanopores transform into general PAAs.
doi:10.1007/s11671-010-9634-x
PMCID: PMC2897034  PMID: 20676199
Anodic alumina; Nanofabrication; Nanopore; Ultrasmall; Nanoparticle
19.  Fabrication of Porous Anodic Alumina with Ultrasmall Nanopores 
Nanoscale Research Letters  2010;5(8):1257-1263.
Anodization of Al foil under low voltages of 1–10 V was conducted to obtain porous anodic aluminas (PAAs) with ultrasmall nanopores. Regular nanopore arrays with pore diameter 6–10 nm were realized in four different electrolytes under 0–30°C according to the AFM, FESEM, TEM images and current evolution curves. It is found that the pore diameter and interpore distance, as well as the barrier layer thickness, are not sensitive to the applied potentials and electrolytes, which is totally different from the rules of general PAA fabrication. The brand-new formation mechanism has been revealed by the AFM study on the samples anodized for very short durations of 2–60 s. It is discovered for the first time that the regular nanoparticles come into being under 1–10 V at the beginning of the anodization and then serve as a template layer dominating the formation of ultrasmall nanopores. Under higher potentials from 10 to 40 V, the surface nanoparticles will be less and less and nanopores transform into general PAAs.
doi:10.1007/s11671-010-9634-x
PMCID: PMC2897034  PMID: 20676199
Anodic alumina; Nanofabrication; Nanopore; Ultrasmall; Nanoparticle
20.  High-Throughput Top-Down Fabrication of Uniform Magnetic Particles 
PLoS ONE  2012;7(5):e37440.
Ion Beam Aperture Array Lithography was applied to top-down fabrication of large dense (108–109 particles/cm2) arrays of uniform micron-scale particles at rates hundreds of times faster than electron beam lithography. In this process, a large array of helium ion beamlets is formed when a stencil mask containing an array of circular openings is illuminated by a broad beam of energetic (5–8 keV) ions, and is used to write arrays of specific repetitive patterns. A commercial 5-micrometer metal mesh was used as a stencil mask; the mesh size was adjusted by shrinking the stencil openings using conformal sputter-deposition of copper. Thermal evaporation from multiple sources was utilized to form magnetic particles of varied size and thickness, including alternating layers of gold and permalloy. Evaporation of permalloy layers in the presence of a magnetic field allowed creation of particles with uniform magnetic properties and pre-determined magnetization direction. The magnetic properties of the resulting particles were characterized by Vibrating Sample Magnetometry. Since the orientation of the particles on the substrate before release into suspension is known, the orientation-dependent magnetic properties of the particles could be determined.
doi:10.1371/journal.pone.0037440
PMCID: PMC3365077  PMID: 22693574
21.  Nanofabricated particles for engineered drug therapies: A preliminary biodistribution study of PRINT™ nanoparticles 
A novel method for the fabrication of polymeric particles on the order of tens of nanometers to several microns is described. This imprint lithographic technique called PRINT™ (Particle Replication In Non-wetting Templates), takes advantage of the unique properties of elastomeric molds comprised of a low surface energy perfluoropolyether network, allowing the production of monodisperse, shape-specific nanoparticles from an extensive array of organic precursors. This engineered nature of particle production has a number of advantages over the construction of traditional nanoparticles such as liposomes, dendrimers, and colloidal precipitates. The gentle “top down” approach of PRINT enables the simultaneous and independent control over particle size and shape, composition, and surface functionality, and permits the loading of delicate cargos such as small organic therapeutics and biological macromolecules. Thus, this single tool serves as a comprehensive platform for the rational design and investigation of new nanocarriers in medicine, having applications ranging from therapeutics to advanced diagnostics. Preliminary in vitro and in vivo studies were conducted, demonstrating the future utility of PRINT particles as delivery vectors in nanomedicine. Monodisperse 200 nm poly(ethylene glycol)-based (PEG) particles were fabricated using PRINT methodology and characterized via scanning electron microscopy and dynamic light scattering. Incubation with HeLa cells showed very little cytotoxicity, even at high concentrations. The biodistribution and pharmacokinetics of [125I]-labeled particles were studied in healthy mice following bolus tail vein administration. The particles were distributed mainly to the liver and the spleen with an apparent distribution t1/2 of approximately 17 min followed by slow redistribution with a t1/2 of 3.3 h. The volume of distribution for the central and peripheral compartments was found to be approximately 3 mL and 5 mL, respectively.
doi:10.1016/j.jconrel.2007.05.027
PMCID: PMC1994820  PMID: 17643544
PRINT; biodistribution; nanoparticles; pharmacokinetics; nanomedicine
22.  The Pursuit of a Scalable Nanofabrication Platform for Use in Material and Life Science Applications 
Accounts of chemical research  2008;41(12):1685-1695.
CONSPECTUS
In this Account, we describe the use of perfluoropolyether (PFPE)-based materials that are able to accurately mold and replicate micro- and nanosized features using traditional techniques such as embossing as well as new techniques that we developed to exploit the exceptional surface characteristics of fluorinated substrates. Because of the unique partial wetting and nonwetting characteristics of PFPEs, we were able to go beyond the usual molding and imprint lithography approaches and have created a technique called PRINT (Particle [or Pattern] Replication In Nonwetting Templates).
PRINT is a distinctive “top-down” fabrication technique capable of generating isolated particles, arrays of particles, and arrays of patterned features for a plethora of applications in both nanomedicine and materials science. A particular strength of the PRINT technology is the high-resolution molding of well-defined particles with precise control over size, shape, deformability, and surface chemistry. The level of replication obtained showcases some of the unique characteristics of PFPE molding materials. In particular, these materials arise from very low surface energy precursors with positive spreading coefficients, can be photocured at ambient temperature, and are minimally adhesive, nonswelling, and conformable. These distinctive features enable the molding of materials with unique attributes and nanometer resolution that have unprecedented scientific and technological value. For example, in nanomedicine, the use of PFPE materials with the PRINT technique allows us to design particles in which we can tailor key therapeutic parameters such as bioavailability, biodistribution, target-specific cell penetration, and controlled cargo release. Similarly, in materials science, we can fabricate optical films and lens arrays, replicate complex, naturally occurring objects such as adenovirus particles, and create 2D patterned arrays of inorganic oxides.
doi:10.1021/ar8000348
PMCID: PMC2645958  PMID: 18720952
23.  Platinum nanoparticles from size adjusted functional colloidal particles generated by a seeded emulsion polymerization process 
Summary
The benefits of miniemulsion and emulsion polymerization are combined in a seeded emulsion polymerization process with functional seed particles synthesized by miniemulsion polymerization. A systematic study on the influence of different reaction parameters on the reaction pathway is conducted, including variations of the amount of monomer fed, the ratio of initiator to monomer and the choice of surfactant and composition of the continuous phase. Critical parameters affecting the control of the reaction are determined. If carefully controlled, the seeded emulsion polymerization with functional seed particles yields monodisperse particles with adjustable size and functionalities. Size-adjusted platinum-acetylacetonate containing latex particles with identical seed particles and varied shell thicknesses are used to produce arrays of highly ordered platinum nanoparticles with different interparticle distances but identical particle sizes. For that, a self-assembled monolayer of functional colloids is prepared on a solid substrate and subsequently treated by oxygen plasma processing in order to remove the organic constituents. This step, however, leads to a saturated state of a residual mix of materials. In order to determine parameters influencing this saturation state, the type of surfactant, the amount of precursor loading and the size of the colloids are varied. By short annealing at high temperatures platinum nanoparticles are generated from the saturated state particles. Typically, the present fabrication method delivers a maximum interparticle distance of about 260 nm for well-defined crystalline platinum nanoparticles limited by deformation processes due to softening of the organic material during the plasma applications.
doi:10.3762/bjnano.2.50
PMCID: PMC3190616  PMID: 22003452
colloid lithography; functional colloids; miniemulsion polymerization; nanoparticles; seeded emulsion polymerization
24.  Highly organised and dense vertical silicon nanowire arrays grown in porous alumina template on <100> silicon wafers 
Nanoscale Research Letters  2013;8(1):287.
In this work, nanoimprint lithography combined with standard anodization etching is used to make perfectly organised triangular arrays of vertical cylindrical alumina nanopores onto standard <100>−oriented silicon wafers. Both the pore diameter and the period of alumina porous array are well controlled and can be tuned: the periods vary from 80 to 460 nm, and the diameters vary from 15 nm to any required diameter. These porous thin layers are then successfully used as templates for the guided epitaxial growth of organised mono-crystalline silicon nanowire arrays in a chemical vapour deposition chamber. We report the densities of silicon nanowires up to 9 × 109 cm−2 organised in highly regular arrays with excellent diameter distribution. All process steps are demonstrated on surfaces up to 2 × 2 cm2. Specific emphasis was made to select techniques compatible with microelectronic fabrication standards, adaptable to large surface samples and with a reasonable cost. Achievements made in the quality of the porous alumina array, therefore on the silicon nanowire array, widen the number of potential applications for this technology, such as optical detectors or biological sensors.
doi:10.1186/1556-276X-8-287
PMCID: PMC3686656  PMID: 23773702
Anodic alumina oxide; Nanoimprint lithography; Templates; Chemical vapour deposition; Nanowires; Silicon; Hexagonal array; Defect-free
25.  Single Molecule Tracking on Supported Membranes with Arrays of Optical Nanoantennas 
Nano Letters  2012;12(3):1717-1721.
Coupling of the localized surface plasmons between two closely apposed gold nanoparticles (nanoantenna) can cause strong enhancements of fluorescence or Raman signal intensity from molecules in the plasmonic “hot-spot”. Harnessing these properties for practical applications is challenging due to the need to fabricate gold particle arrays with well-defined nanometer spacing and a means of delivering functional molecules to the hot-spot. We report fabrication of billions of plasmon-coupled nanostructures on a single substrate by a combination of colloid lithography and plasma processing. Controlled spacing of the nanoantenna gaps is achieved by taking advantage of the fact that polystyrene particles melt together at their contact point during plasma processing. The resulting polymer thread shadows a gap of well-defined spacing between each pair of gold triangles in the final array. Confocal surface-enhanced Raman spectroscopy imaging confirms the array is functionally uniform. Furthermore, a fully intact supported membrane can be formed on the intervening substrate by vesicle fusion. Trajectories of freely diffusing individual proteins are traced as they sequentially pass through, and are enhanced by, multiple gaps. The nanoantenna array thus enables enhanced observation of a fluid membrane system without static entrapment of the molecules.
doi:10.1021/nl300294b
PMCID: PMC3626319  PMID: 22352856
Lipid membranes; nanoantennas; fluorescence enhancement; Raman spectroscopy

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