Preparation And Characterization Of Micron-nano-sized Organic Inorganic Hybrid Fibers

Two micron-nano-sized organic inorganic hybrid fibers were prepared：viscose-based zirconia fiber cloth was prepared by precursor process that cellulose textilesimpregnated with zirconium salt solution， nano-modified bamboo charcoalPolypropylene (BC/PP) fiber was prepared by blend granulation-melt spinning method.The main contents of this article contains three aspects as following：Part Ⅰ：Yttrium doped nano-ZrO2was prepared by sol-gel method with inexpensiveinorganic zirconium salt as starting material，water and ethanol as solvent，NH3·H2O asprecipitant，Yttrium nitrate as stabilizer. The influence factors on properties of productswhich contained the titration order of precipitant, the concentration of zirconiumoxychloride, solvents, drying method and calcining heat were systematically discussed.The precursor dried gel powders and resultant products were characterized by FT-IR,TG/DSC, XRD and SEM. The formation mechanism of nano-ZrO2prepared by sol-gelmethod was discussed，and the appropriate process parameters of the preparation wereobtained from the experimental data. It was shown that a single component of tetragonalzirconia powders with average particle size of39nm can be synthesized through thefollowing conditions: using water as solvent, chose the positive titration order, theconcentration of zirconium oxychloride was0.5mol/L, the gel was dried in vacuum ovenand the dried gel was calcined at550℃for2h.Part Ⅱ：Zirconia cloth was prepared by precursor process that cellulose textilesimpregnated with zirconium salt solution with commercial viscose fibers woven asprecursor. The thermal properties of the impregnated and unimpregnated cloth were studied by TG/DSC. The structure of the cloth before and after heat treatment wasexamined by FT-IR, SEM and XRD，and the influence of different heat treatmentprocesses on the organizational structure of cloth was discussesed. The results showedthat the start creating temperature of zirconia cloth was400℃. The zirconia cloth beforeheat treatment was made of cellulose fiber and zirconium salts but after heat treatmentthe sample was made of single component of ZrO2. The zirconia cloth had the samephysical morphology with the precursor cloth and any individual fiber had full core withthe diameter of about5μm. The cloth was mainly consisted of t-ZrO2, and c-ZrO2wasappeared with the increase of heat treatment temperature.Part Ⅲ：Polypropylene (PP) had been compounded with bamboo charcoal (BC)modified by nano-TiO2for preparing3%、5%、7%(wt) BC/PP masterbatch using atwin-screw extruder, the BC/PP fibers and hot pressing non-woven were prepared usinghigh-speed melt-spinning device. The particle size distribution and structure of BCpowders before and after modification were characterized by Mastersizer2000laserparticle size analyzer，SEM，TEM，FT-IR and XRD. The physical properties ofmasterbatch and fibers were examined using SEM, and TG/DSC. These techniquesindicated that the BC particle size was found to be less than5.8μm and the particleswere dispersed uniformly in PP matrix. The diameter of the BC/PP fibers prepared was25～80μm，the surface was not smooth as the BC particles were distributed on thesurface of the fibers. TG/DSC results showed that the melting point of PP increased andthe degradation of PP accelerated as the addition of BC powders. Qualitative analysis ofantibacterial effects of masterbatch and non-woven was researched by inhibition zonemethod，the results showed that the antibacterial effects of non-woven was better；Quantitative analysis of antibacterial effects of BC/PP fiber was implemented by shakeflask test，the results showed that inhibition rates of3%，5%，7%(wt) BC/PP fiber againstE.coli were77.32%，80.62%，92.95%. It was shown that the three BC/PP fiber had anexcellent antibacterial performance against E.coli.