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In-situ Preparation And Characterization Of Nickel Picrate Energetic Thin Film

Posted on:2014-02-14Degree:MasterType:Thesis
Country:ChinaCandidate:B XuFull Text:PDF
GTID:2231330395483060Subject:Chemical Engineering
Abstract/Summary:PDF Full Text Request
In order to meet the requirements of energy and function diversity, micro-energetic device by integrating the energetic materials into micro-electro-mechanical systems (MEMS) has attracted interests from scientific communities. Energetic materials are classified as those that convert chemical enthalpy to thermal enthalpy rapidly, due to the great energy storage rate, integrate energetic materials with micro-electromechanical systems as energy source is helpful to reduce the volume of the system. Take the compatibility of energetic materials and MEMS into account, in this study we prepared porous structure of the silicon which is the basis materials of the semiconductor industry by photoelectrochemical (PEC) process, this porous structure increase the specific surface area of the plate so that the attachment point of the unit volume embodied energy increased. The detail process was as follows:Firstly,3D ordered silicon micro-channel plate (MCP) with high depth-to-width ratio was prepared by PEC process, and then a thin film of nickel (Ni) were synthesized by electroless plating of nickel on the sidewalls of the Si-MCP. The thin film of nickel picrate were successfully produced with an in-situ chemical reaction method by introducing picric acid into the channels. Field emission scanning electron microscope (SEM), Fourier transform infrared (FT-1R) spectroscopy and nuclear magnetic resonance (NMR) were used to study the morphological and structural properties of the thin film. The results were obtained as follows:1) The depth-to-width ratio of silicon micro-channel plates prepared by PEC process can reach50and the channel uniform distribution. From the SEM picture, it can be observed that the silicon MCP is well aligned with little impurities and the pore diameter is about5μm with Si walls on the lateral surface,the silicon MCP has a vertical sidewall. EDS was performed on the sidewalls to determine the components of the sidewalls of MCP, it shows the Ni is well distributed on the sidewalls after electroless plating.2) We can get yelloegreen thin film by introduce picric acid into the micro-channel, Both1H-NMR and FT-IR results indicated that the substance produced by the complete reaction of picric acid with nickel possessed symmetrical structure which is Ni(pic)2consistent with that of nickel picrate powder, and there is no picric acid remain on the film. From the SEM we can see that there are amount of nickel picrate stay on the surface of the plate.3) TG-DSC was used to study the decomposition of the film, the results suggests that the decomposition of nickel picrate thin film takes place with formation of one endotherm and one exotherm. The exothermic reaction in DSC curve reveals the heat producing from the decomposition of energetic film equal to650.27J/g, which is less than the values of4150-4760J/g reported by Matsukawa et al. Low heat of the reaction is mainly caused by that the inert material (Si+Ni) with significant proportion of the plate, it has no contribution to heat. The other factor is that the measurement condition during the DSC experiment is. different from that of conference. Meanwhile, the thermal decompositioin reaction started from260℃lower than that of reaction onset temperature of Al/metal or Al/metal oxide.
Keywords/Search Tags:Energetic materials, nickel picrate, in-situ reaction, electroless plating, siliconmicro-channel plates
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