Thermally assisted electron beam induced deposition can result in an improvement of the purity of nano-scale depositions. Six commonly used organic precursors were examined: W(CO)(6), TEOS (tetraethylorthosilicate), MeCpPtMe(3), Co(CO)(3)NO, Co(2)(CO)(8), and Me(2)Auacac. The last two precursors were also tested on two different instruments to confirm reproducibility of the results. The influence of the substrate temperature on the composition of the deposition has been quantified systematically in the temperature range 25-360 °C. It has been shown that most purities improve when applying an elevated temperature, while the shape of the deposition remains intact. The purity improvement is achieved at the cost of a lower deposition yield. The amount of improvement is different for each precursor. Within the maximum temperature range of 360 °C, the best improvement was found for W(CO)(6): from 36.7 at.% at 25 °C to 59.2 at.% at 280 °C. For both cobalt precursors an additional transition region between patterned electron beam induced deposition (EBID) and thermal thin film growth has been identified. In this region seeded growth occurs with strongly increased growth rates.
The use of lignin from forests as a renewable resource is a greener alternative to the petrochemical industry and accelerates the progress towards the development of more environmentally friendly industrial...
A new method of direct, rapid nano- to micro-scale patterning of high purity cobalt is presented. The method utilizes a combination of electron beam induced deposition (EBID) and seeded growth at elevated temperatures below the temperature of spontaneous thermal decomposition. Dicobalt octacarbonyl Co₂(CO)₈ is used as the precursor and carbon as a seed layer. Seeded deposition is carried out in the substrate temperature range from 55 to 75 °C. Deposition yield is significantly higher than conventional EBID and magnetotransport measurements indicate that resistivity, 22 µΩ cm, and saturation magnetization, 1.55 T, are much closer to the corresponding values for bulk Co than those for standard EBID.
Cellulose nanocrystals (CNCs) possess the ability to form helical periodic structures that generate structural colors. Due to the helicity, such self‐assembled cellulose structures preferentially reflect left‐handed circularly polarized light of certain colors, while they remain transparent to right‐handed circularly polarized light. This study shows that combination with a liquid crystal enables modulation of the optical response to obtain light reflection of both handedness but with reversed spectral profiles. As a result, the nanophotonic systems provide vibrant structural colors that are tunable via the incident light polarization. The results are attributed to the liquid crystal aligning on the CNC/glucose film, to form a birefringent layer that twists the incident light polarization before interaction with the chiral cellulose nanocomposite. Using a photoresponsive liquid crystal, this effect can further be turned off by exposure to UV light, which switches the nematic liquid crystal into a nonbirefringent isotropic phase. The study highlights the potential of hybrid cellulose systems to create self‐assembled yet advanced photoresponsive and polarization‐tunable nanophotonics.
The development of advanced hybrid materials based on polymers from biorenewable sources and mineral nanoparticles is currently of high importance. In this paper, we applied softwood kraft lignins for the synthesis of lignin/SiO2 nanostructured composites. We described the peculiarities of composites formation in the sol-gel process through the incorporation of the lignin into a silica network during the hydrolysis of tetraethoxysilane (TEOS). The initial activation of lignins was achieved by means of a Mannich reaction with 3-aminopropyltriethoxysilane (APTES). In the study, we present a detailed investigation of the physicochemical characteristics of initial kraft lignins and modified lignins on each step of the synthesis. Thus, 2D-NMR, 31P-NMR, size-exclusion chromatography (SEC) and dynamic light scattering (DLS) were applied to analyze the characteristics of pristine lignins and lignins in dioxan:water solutions. X-Ray photoelectron spectroscopy (XPS) and Fourier transform infrared (FTIR) were used to confirm the formation of the lignin–silica network and characterize the surface and bulk structures of the obtained hybrids. Termogravimetric analysis (TGA) in nitrogen and air atmosphere were applied to a detailed investigation of the thermal properties of pristine lignins and lignins on each step of modification. SEM confirmed the nanostructure of the obtained composites. As was demonstrated, the activation of lignin is crucial for the sol-gel formation of a silica network in order to create novel hybrid materials from lignins and alkoxysilanes (e.g., TEOS). It was concluded that the structure of the lignin had an impact on its reactivity during the activation reaction, and consequently affected the properties of the final hybrid materials.
Nanoporous microspheres with divinylbenzene (DVB), styrene (St), and lignin were synthesized by an emulsion-suspension polymerization method. Several types of lignins were used: (1) kraft lignin before (L-unmod) and after modification with methacryloyl chloride (L-Met) and (2) low-molecularweight kraft lignin unmodified (LWL-unmod) and modified with methacrylic anhydride (LWL-Met). LWL was prepared by ultrafiltration of industrial black liquor using a ceramic membrane with a molecular weight (Mw) cut-off of 5 kDa. The synthesis was optimized by addition of different amounts of lignins. The microsphere texture was characterized using low-temperature nitrogen adsorption and small angle X-ray scattering analyses. The microspheres were nano-and mesoporous with a specific surface area in the range of 0.1-409 m 2 /g. The morphology of the copolymers was studied using field emission scanning electron microscopy and atomic force microscopy. The thermal properties were studied using differential scanning calorimetry and thermogravimetric analysis methods. A significant difference in the microsphere roughness is affected by lignins due to the presence of lignin nanoparticles at the surface of the microspheres. Molecular modeling was used to predict the sorption properties of the copolymers affected by various fields around the particles. The particle size, polydispersity and zeta potential of the St ? DVB, L-Met ? St ? DVB and L-unmod ? St ? DVB samples were measured by dynamic light scattering. Additionally, the point of zero charge of the samples was determined using potentiometric titration. The materials studied have a great potential for sorption processes due to their developed porosity and the presence of a number of active surface functionalities.
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