Design, fabrication and testing of a high temperature ceramic microreactor for synthesizing silicon nitride nanoparticles Public Deposited

http://ir.library.oregonstate.edu/concern/graduate_thesis_or_dissertations/wh246x46x

Descriptions

Attribute NameValues
Creator
Abstract or Summary
  • An alumina microreactor was designed and fabricated to study the synthesis of nanosized silicon nitride powder via the ammonolysis of SiO vapor at temperatures ranging from 1300°C to 1400°C. It is the first high temperature ceramic microreactor capable of operating at temperatures upto 1600°C. The microreactor was designed using 3D CAD software SolidWorks and AutoCAD. This entirely new design of the microreactor simplifies the lamination and bonding techniques by using just 3 plates instead of stacking a number of plates together. This design simplification was made feasible by using a combination of advanced processing techniques such as laser machining, extrusion, and tape casting. A CO₂ laser was used for fabricating the top and bottom plates, while the extruded body of the microreactor was fabricated using highly porous alumina (50-60% porosity). These porous microchannel walls simplify the use of multiple flows in the microreactor, because it facilitates the reactant gas stream to enter into the microreactor through the pores. The microreactor was finally tested in a horizontal tube heating furnace to synthesize silicon nitride nanoparticles by performing gas-phase reactions between SiO and ammonia. The SiO vapor generation was controlled by the flow of argon gas. The ammonia dissociation at high temperatures was taken into account by maintaining flow rate of ammonia atleast 5 times higher than the flow rate of SiO. Due to its portability, and hence reduced reaction volume this microreactor provides a better control over the residence time and diffusion length of the reactants in the hot reaction zone, resulting in a better control over the particle morphology and size distribution. The reaction between SiO and ammonia was carried out by varying the flow rates of ammonia ranging between 1000-4000 cc/min, while the flow rate of argon was kept constant at 240 cc/min. The reaction was carried out at a constant temperature of 1350°C for a cycle time of 1hr. The reaction yielded silicon nitride nanoparticles were then collected on different filter papers at the exit of the microreactor. Different powder characterization techniques such as transmission electron microscopy (TEM) and x-ray diffraction (XRD) were used to determine the particle size, particle size distribution, and chemical composition of the nano-sized particles. XRD analysis indicated peaks of silicon oxy-nitride (Si₂N₂O) in all the samples except the sample obtained after the first run. This is because Si₃N₄ nanoparticles on exposure to atmosphere were oxidized to form Si₂N₂O. Toxicology tests were also conducted in order to determine the toxicity effects of Si₃N₄ nanoparticles on different body parts of zebra fish. The data obtained was then further used to discuss the advantages of the microreactor in synthesis of Si₃N₄ nanoparticles and its integration to a post processing system such as compaction press, injection molding, and extrusion.
Resource Type
Date Available
Date Copyright
Date Issued
Degree Level
Degree Name
Degree Field
Degree Grantor
Commencement Year
Advisor
Committee Member
Academic Affiliation
Non-Academic Affiliation
Keyword
Subject
Rights Statement
Language
File Format
File Extent
  • 9329973 bytes
Replaces
Additional Information
  • description.provenance : Submitted by Kartavya Jain (jaink@onid.orst.edu) on 2007-06-23T04:02:44Z No. of bitstreams: 10 Appendices.pdf: 38705 bytes, checksum: 7085e6eb0849addbbdb7c857520db892 (MD5) Bibliography_final version.pdf: 37530 bytes, checksum: f21961c1fe9dc6819a9f769ac4d8c6e9 (MD5) Chapter 7-Conclusion_final version.pdf: 19932 bytes, checksum: e850c1250420b7b7cddaa3aa607c88c8 (MD5) Chapter 6- Results_final version.pdf: 2398190 bytes, checksum: b7fdc50e843f3a62702fa3117ca6c867 (MD5) Chapter 5- Experimental Analysis_final version.pdf: 531400 bytes, checksum: 96e30bfc8911adbdad40bbea9f3e6a47 (MD5) Chapter 4- Fabrication_final version.pdf: 2468268 bytes, checksum: b329649d3f56eb57b29df766478b1f2f (MD5) Chapter 3- Design_final version.pdf: 1423308 bytes, checksum: 0d030f77a9bca76bf0aa52649dad7f79 (MD5) Chapter 2-Literature review_final version.pdf: 2603952 bytes, checksum: 6d808c2a84f5810bd4aa29fed26affe4 (MD5) Chapter 1-Introduction_final version.pdf: 185098 bytes, checksum: 30b33f586bace660c8c6e21d15ad799b (MD5) Pretext pages_final version.pdf: 51828 bytes, checksum: fc0e76a24fd7f2cbcae7fa5c5a7e30d2 (MD5)
  • description.provenance : Rejected by Julie Kurtz(julie.kurtz@oregonstate.edu), reason: Rejecting second submission. ~Julie on 2007-06-29T16:21:44Z (GMT)
  • description.provenance : Made available in DSpace on 2007-07-03T20:56:16Z (GMT). No. of bitstreams: 1 MS thesis- Kartavya Jain 2007.pdf: 9329973 bytes, checksum: 32cc92d73c058f31e2b476fca06df291 (MD5)
  • description.provenance : Approved for entry into archive by Julie Kurtz(julie.kurtz@oregonstate.edu) on 2007-07-03T17:59:20Z (GMT) No. of bitstreams: 1 MS thesis- Kartavya Jain 2007.pdf: 9329973 bytes, checksum: 32cc92d73c058f31e2b476fca06df291 (MD5)
  • description.provenance : Submitted by Kartavya Jain (jaink@onid.orst.edu) on 2007-06-29T21:43:35Z No. of bitstreams: 1 MS thesis- Kartavya Jain 2007.pdf: 9329973 bytes, checksum: 32cc92d73c058f31e2b476fca06df291 (MD5)
  • description.provenance : Rejected by Julie Kurtz(julie.kurtz@oregonstate.edu), reason: Rejecting to convert all word documents to one PDF. When done - 1)open the item that was rejected 2)replace files with one PDF 3)resubmit the item. Thanks, Julie on 2007-06-28T17:31:22Z (GMT)
  • description.provenance : Submitted by Kartavya Jain (jaink@onid.orst.edu) on 2007-06-28T19:26:02Z No. of bitstreams: 1 MS thesis- Kartavya_Jain_Thesis.pdf: 9327550 bytes, checksum: 032bfa68bf1cc84e6b916dab7c66fa84 (MD5)

Relationships

Parents:

This work has no parents.

Last modified

Downloadable Content

Download PDF

Items