Abstract:

The work describes the generation of nanoscale double shelled hollow particles generated through a rapid aerosol based process. The inner shell is a thin carbon layer, while the outer shell is made with silica. The double shelled morphology evolves by exploiting concepts of salt bridging to lock in a templating surfactant and prevent the formation of mesoporous materials. The hollow particles can be used as vehicles to encapsulate surfactants and thus generate a new class of dispersants. This dataset contains SEM and TEM images, surface area measurements, x-ray diffraction measurements, and energy-dispersive X-ray spectroscopy measurements for nanoscale particles. Dataset supporting the publication Synthesis of submicrometer hollow particles with a nanoscale double-layer shell structure., Langmuir, 2012 Oct 20; 28 (39): 13783-7. DOI: 10.1021/la302841c.

Suggested Citation:

Wang, Yingqing, Bhanukiran Sunkara, Jingjing Zhan, Jibao He, Ludi Miao, Gary McPherson, Leonard Spinu, Vijay John. 2016. Dataset for: Synthesis of submicrometer hollow particles with a nanoscale double-layer shell structure. Distributed by: GRIIDC, Harte Research Institute, Texas A&M University–Corpus Christi. doi:10.7266/N71G0J8R

Publications:

Wang, Y., Sunkara, B., Zhan, J., He, J., Miao, L., McPherson, G. L., … Spinu, L. (2012). Synthesis of Submicrometer Hollow Particles with a Nanoscale Double-Layer Shell Structure. Langmuir, 28(39), 13783–13787. doi:10.1021/la302841c

Purpose:

We describe a scalable, rapid aerosol-based process for fabricating hollow submicrometer particles with novel morphology, one where the shell is made up of two thin layers: an outer layer of silica and an inner layer of carbon. The purpose is the development of nanoscale carriers for dispersant components.

Data Parameters and Units:

jpg images - image1.jpg - TEM of as-synthesized submicrometer hollow particle with double silica/carbon layer shell; image2.jpg, image3.jpg, image4.jpg- TEM of pyrolyzed submicrometer hollow particle with double silica/carbon layer shell; image5.jpg - cross sectional TEM of pyrolyzed submicrometer hollow particle with a detached carbon layer; image6.jpg - SEM of pyrolyzed submicrometer hollow particle; image7.jpg and image8.jpg - cross sectional SEM of pyrolyzed submicrometer hollow particle; image9.jpg, image10.jpg, image11.jpg - TEM of calcined particle; image12.jpg - cross sectional TEM of calcined particle; image13.jpg - SEM of calcined particle; image14.jpg - cross sectional SEM of calcined particle; image15.jpg, image16.jpg, image17.jpg - TEM of etched particle; image18.jpg - cross sectional TEM of etched particle; image19.jpg - SEM of etched particle; image20.jpg -cross sectional SEM of etched particle. xy data.xlsx: BET and XRD data: Brunauer–Emmett–Teller (BET) surface area measurements [Relative Pressure (P/P0); Volume Adsorbed (cm^3/g)] for each particle type; X-ray diffraction (XRD) [2 Theta (degrees); Intensity (a.u.)] for each particle type EDS data: Energy-dispersive X-ray spectroscopy (EDS) [analysis of double layer particles, characterization of single silica layer particles, analysis of single carbon layer particles] [inner layer, outer layer], Element [C, O, Si, Fe], Weight (%), Atomic (%)

Methods:

Particle creation: Dissolved FeCl3.6H2O in 15 mL ethanol, added 1.1 g cetyl trimethylammonium bromide (CTAB) and 4.5 mL tetraethyl orthosilicate (TEOS). The solution sat for 0.5 hrs, aerosol droplets were formed atomized Model 3076, TSI Inc. atomizer. Droplets went through a quartz tube in a furnace at 400 degrees C which took approx. 15 seconds. Particles were filtered and pyrolized at 500 degrees C for 3 hrs under N2 gas. Particles were calcined at 500 degrees C for 3 hrs then at 1000 degrees C for 2 hrs in air. Particles were reduced at 400 degrees C for 2 hrs under H2N2. For silica layer removal, 10% HF solution was added to the particles which then sat for 2 days. Morphology of particles was characterized by field emission scanning electron microscopy (SEM, Hitachi S-4700 operated at 20 kV) and transmission electron microscopy (TEM, JEOL 2010 operated at 200 kV). Cross section samples for TEM and SEM were prepared by embedding particles within a resin (Embed 812) at 70 degrees Celsius for 48 hours and cut by a Leica ultracuts Microtome.

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