Solid Freeform Fabrication from Gas Precursors Using Laser Processing
Table of Contents:
- Principal Investigator.
- Productivity Measures.
- Summary of Objectives and Approach.
- Detailed Summary of Technical Progress.
- Transitions and DOD Interactions.
- Software and Hardware Prototypes.
- List of Publications.
- Invited and Contributed Presentations.
- Honors, Prizes or Awards Received.
- Project Personnel Promotions.
- Project Staff.
- Multimedia URL.
- Keywords.
- Business Office.
- Expenditures.
- Students.
- Book Plans.
- Sabbatical Plans.
- Related Research.
- History.
Harris Marcus
- PI Name: Harris L. Marcus
- PI Institution: University of Connecticut at Storrs
- Phone Number: (860)486-4623
- Fax Number: (860)486-4745
- Street Address: Institute of Materials Science 69 N. Eagleville Rd.
- City, State, Zip: Storrs, CT 06269-3136
- PI E-mail address: hmarcus@mail.ims.uconn.edu
- PI URL Home Page: http://www.ims.uconn.edu/metal/faculty/marcus.htm
- Grant/Contract Title: Solid Freeform Fabrication from Gas Precursors Using Laser Processing
- ONR Grant/Contract Number: N00014-95-1-0978
- Mipr Number:
- R&T Number:
- Period of Performance7/1/95 to 6/30/98
- Today's Date: 11/10/97
Productivity Measures.
- Number of unrefereed reports and articles: 6
- Number of book or parts thereof published: 2
- Number of graduate students supported: 5
Summary of Objectives and Approach.
- Understanding of the fundamental processes in SALD and SALDVI deposition
- SALDVI
- A silicon carbide structure, formed by SALDVI from tetramethylsilane gas precursor and silicon carbide powder. Properties evaluated:
- Single layer density-investigated by changing deposition temperature distribution, TMS gas pressure, powder size, scan speed, and scan spacing
- Interlayer bonding-investigated by changing deposition temperature distribution, TMS gas pressure, powder size, scan speed, scan spacing, and scan geometry
- Powder bubbling effect-the bubbling of powder particles around the edges of the SALDVI shape, creating bonding difficulties. This effect was first seen in the SALDVI process in this project because of the video monitoring capabilities of the UCONN SFF systems
- The effects of powder size, powder density, powder shape, precursor gas pressure and composition, scan spacing, preheat temperature, and deposition temperature were all examined for their role in the powder bubbling
- SALD:
- Multiple composition deposition, focusing on silicon nitride thin layers from TMS and ammonia gas precursors, silicon carbide and carbon lines from TMS and acetylene respectively. Properties evaluated
- Chemical composition, examined with changes in gas pressure, deposition temperature field, and laser beam size
- Silicon nitride insulative quality
- Deposited line electrical resistance, investigated with variations in the deposition temperature field, gas pressure, laser beam size, line width, and scan speed
- EMF response of the silicon carbide and carbon lines to temperature
- Technical application of SALD/SALDVI research: Functional thermocouples have been fabricated and demonstrated for a DARPA sponsored project using the SALDVI and SALD materials systems discussed above
- SALD Joining of ceramics, an extension of SALD to a participating substrate deposition situation
- The goal of this research effort is to join together ceramic parts by using filler material from the SALD gas-phase reaction. This method of fabrication is a patented process, a unique SALD deposition process with substrate interaction.
- Research approaches:
- Design and fabrication of a rotating joining device to handle tubes. This device serves to 'scan' the seam relative to the laser beam, and the speed of rotation can be varied
- Improving weld filler material continuity from one tube to the other by rastering of the laser beam across the joint seam, by changing deposition temperature, gas pressure, and rotational speed
- Analysis of the adhesion of the SALD material to the tubes themselves using an Environmental SEM(ESEM)
- Progress to date: Several silicon carbide tubes have been joined using silicon carbide filler material from the tetramethylsilane gas-phase reaction.
- Selection and use of materials for deposition
- Thermodynamic calculations from a modified CET89 free energy minimization computer program have been utilized to select gas precursors for specific gas-phase reactions. These thermodynamic determinations present the equilibrium reaction products and phases for ranges of gas pressures, gas mixtures, and temperatures.
Detailed Summary of Technical Progress
The assembly and construction of the Solid Freeform Fabrication(SFF) laboratory, begun in late 1995, is essentially completed. Three operational SFF systems are in place with the appropriate ancillary equipment. The lab contains two SAL/SALDVI machines, one with a 4 inch by 4 1/2 inch working area powder delivery system(PDS) and the other with a 1 inch round diameter working area PDS, and a SALD joining machine, incorporating a rotational device designed to work with tube structures. Five lasers are available, including a brand new, power stability optimized 50 watt continuous wave Nd:YAG laser. Two new in-situ chemical analysis tools will be implemented on the SFF systems. The first is a residual gas analyzer, and the second is a four point sampling emission spectrometer.
The specific research programs at the UCONN SFF lab focus on ceramic fabrication from the gas-phase reactions. Fundamental understanding of the SALD and SALDVI processes are essential to applying the technology to real world applications. The SALDVI work focused on three main properties in the silicon carbide material system. The deposited shapes were composed of silicon carbide from tetramethylsilane(TMS) gas precursor infiltrating into silicon carbide powder. The intralayer density and interlayer bonding were the important structure properties to control, in addition to an interesting bubbling phenomenon was observed during the SALDVI process. The individual layer densities were improved to approximately 85% by tweaking such properties as powder size, scan speed, and the temperature field induced by the laser. Similarly, the bonding between successive layers was enhanced with this optimization approach, including the scan path of the laser beam in forming the shape. The bubbling phenomenon had not been noted before and was detected because of the video capabilities of the SFF systems. This effect is a bubbling of the powder particles at the edge of the deposited shape. It is believed to arise from the thermal expansion of the gas in the powder bed porosity. A new bed preheating approach is expected to diminish the bubbling effect. SALD research looked at multiple material deposition. Specifically, silicon nitride, from TMS and ammonia, and silicon carbide and carbon, from TMS and acetylene respectively, were examined. The silicon nitride was deposited as a thin film, and analyzed with respect to its insulative quality. The deposition was performed at low ammonia pressures, approximately 10 to 20 torr, using a carbon dioxide laser. The successful formation of the nitride layer countered previous notions of not being able to use ammonia gas precursors with a CO2 laser. Silicon carbide and carbon were deposited in line formations, with the resulting electrical properties coming under scrutiny. The line resistances and emf response to temperature changes were tested with respect to varied line widths(a function of scan speed and laser beam size) and deposition temperature field. These SALD/SALDVI investigations were applied to an embedded sensor project sponsored by DARPA. The DARPA program studied the feasibility to fabricate a ceramic matrix with an operational, in-situ thermocouple formed inside the matrix structure in one continuous process. An example of a SALD/SALDVI silicon carbide/carbon thermocouple in a silicon carbide matrix, along with its temperature and emf response, can be found at the UCONN website .
The second area of investigation in the SFF laboratory is ceramic joining by SALD, a patented process for substrate-involved SALD deposition. The joining of ceramic parts is accomplished by using a filler material deposited from the gas-phase reaction in SALD. In this manner, the ceramic joint can be tailored to match the material composition of the constituent ceramic part to be joined. The initial efforts focused on joining clay-bonded silicon carbide(approximate 75 to 80% density) tubes with silicon carbide deposited from TMS precursor. The adhesion of the SALD material to the tube is excellent. In fact, the interface between the SALD material and the tube is inconspicuous. The success of joints in this initial phase has been inconsistent. While the adhesion is outstanding, successful connective bonding of the SALD material across the joint has been challenging. An example of two clay-bonded silicon carbide tubes connected by the SALD joining method can be found at the UCONN website .
Transitions and DOD Interactions.
- Presentation on "Solid Freeform Fabrication at the University of Connecticut" at the ONR annual review meeting in Woods Hole, MA, June 16th , 1997
- Presentation of research programs and tour of the SFF laboratory for Dr. William Coblenz of DARPA, August 8th, 1997
- Dr. Marcus took a 4 day trip on the USS Tunney submarine from San Diego, CA to Seattle, WA, September, 1997
Software and Hardware Prototypes.
Thermocouple and Joining Samples
List of Publications.
- "Current and Future Trends in Solid Freeform Fabrication", by D.L. Bourell, J.J. Beaman, J.W. Barlow, R.H. Crawford, H.L. Marcus, and L.E. Weiss, SPIE Proceedings Volumer 2910, Rapid Product Development Technologies, Boston, MA, November, 1996.
- "Selective Area Laser Deposition of Titanium Oxide" by K.J. Jakubenas, Y.L. Lee, M.S. Shaarawi, H.L. Marcus, and J.M. Sanchez, Rapid Prototyping Journal, Vol. 3, No. 2, 1997, p. 66-70.
- "Recent Advances in SALD and SALDVI", by K. Jakubenas, B.R. Birmingham, S. Harrison, J.E. Crocker, J. Sanchez, and H.L. Marcus, Proceedings of the Seventh International Conference on Rapid Prototyping 1997, edited by R.P. Chartoff, A.J. Lightman, M.K. Agarwala, and F. Prinz, University of Dayton, p. 60-69.
- The following four papers are found in the Proceedings from the 1997 Solid Freeform Fabrication Symposium, edited by D.L. Bourell, J.J. Beaman, H.L. Marcus, R.H. Crawford, and J.W. Barlow, August, 1997, Austin, TX, to be published
- 1. "The Use of VRML to Integrate Design and Solid Freeform Fabrication", by Y. Wang, J. Dong, and H.L. Marcus
- 2. "Fabrication of In-Situ SiC/C Thermocouples by Selective Area Laser Deposition", by L. Sun, K.J. Jakubenas, J.E. Crocker, S. Harrison, L.L. Shaw, and H.L. Marcus
- 3. "Gas Phase SFF Control System for Silicon Nitride Deposition by SALD/SALDVI", by S. Harrison, C.F. Costa, K.J. Jakubenas, J.E. Crocker, and H.L. Marcus
- 4. "Net Shape Functional Parts Using Diode Laser", by T. Manzur, C. Roychoudhuri, P. Dua, F. Hossain, and H.L. Marcus
- "Rapid Prototyping and Solid Free Form Fabrication", by J.G. Conley and H.L. Marcus, to be published in the Journal of Manufacturing Science and Engineering, November, 1997
- "Multiple Material Solid Free-Form Fabrication by Selective Area Laser Deposition" by K. J. Jakubenas, J.M. Sanchez, and H.L. Marcus, Materials & Design. Paper accepted and to be published.
- US Patent granted for "Joining Ceramics and Attaching Fasteners to Ceramics by Gas Phase Selective Beam Deposition, March 18, 1997, Patent #5,611,883
Invited and Contributed Presentations.
- "Recent Advances in SALD and SALDVI," Seventh International Conference on Rapid Prototyping 1997, San Francisco, March 31-April 3, 1997
- "Gas Phase Solid Freeform Fabrication at the University of Connecticut," MRS Annual Meeting, Solid Freeform Fabrication Session, San Francisco, March 31 - April 4, 1997
- "Selective Area Laser Deposition (SALD) of Titanium Oxide," 6th European Conference on Rapid Prototyping and Manufacturing 1997, Nottingham, UK, July 1-3, 1997
- Solid Freeform Fabrication Symposium 1997, Austin, TX , August 11-13, 1997, 4 presentations on the following topics: a) The Use of VRML to Integrate Design and Solid Freeform Fabrication, b) Gas Phase SFF Control System for Silicon Nitride Deposition by SALD/SALDVI, c) Fabrication of In-Situ SiC/C Thermocouples by Selective Area Laser Deposition, d) Net Shape Functional Parts Using Diode Laser
- "Selective Area Laser Deposition Joining of Silicon Carbide," American Ceramic Society 1997 Fall Meeting, San Francisco, October 12-15, 1997
Honors, Prizes or Awards Received.
Dr. Harris Marcus was elected to the Connecticut Academy of Science and Engineering(CASE) in 1997. The total membership is limited, by state statute, to 200.
Project Personnel Promotions.
Project Staff.
- Dr. Kevin Jakubenas, post-doctoral fellow from November, 1996 to November, 1997. Dr. Jakubenas' doctoral research focused on SALD of titanium dioxide and silicon dioxide along with selection methods for SALD gas precursors.
Multimedia URL.
- EOYL FY96
- QUAD FY96
Keywords.
- Gas-Phase Solid Freeform Fabrication
- Selective Area Laser Deposition (SALD)
- Selective Area Laser Deposition Vapor Infiltration (SALDVI)
- Embedded Thermocouple Fabricated by SALD/SALDVI
- Ceramic Joining by SALD
- Laser-induced Gas Reactions
Business Office
- Business Office Phone Number: (860)486-1729
- Business Office Fax Number: (860)486-1727
- Business Office Email: grtadm18@uconnvm.uconn.edu
Expenditures
- Est. FY98: 100%
- FY97: 100%
- FY96: 100%
- FY95: 100%
- FY94: 100%
Current and Former Students
- Name: Mr. Shay Harrison
- Position: Graduate Research Assistant
- Nationality: United States
- Task: Ceramic joining project, including design of the joining system and performing deposition experiments
- Thesis: Joining of structural ceramics using SALD deposition
- Graduated: PhD, estimated winter, 1998
- Name: Mr. James E. Crocker
- Position: Graduate Research Assistant
- Nationality: United States
- Task: Embedded sensor project, focusing on the SALDVI deposition of the silicon carbide matrix
- Thesis: Silicon carbide shapes with embedded devices by SALD/SALDVI (expected)
- Graduated: Masters, November, 1997
- : Name: Mr. Lianchao Sun
- Position: Graduate Research Assistant
- Nationality: China
- Task: Embedded sensor project, focusing on the SALD deposition of the thermocouple lines and insulating layers
- Thesis:
- : Name: Mr. Erik Geiss
- Position: Graduate Research Assistant
- Nationality: United States
- Task: Design and implementation of a photolytic deposition system
- Thesis:
- : Name: Mr. Yanshuo Wang
- Position: Graduate Research Assistant
- Nationality: China
- Task: Computer programming involving the use of VRML language for 3-D modeling and sectioning routines
- Thesis: Implementation of VRML in Design with Solid Freeform Fabrication, granted Masters degree in August, 1997
Book Plans
- Title: Proceeding of the Solid Freeform Fabrication Symposium 1997 edited by D.L. Bourell, J.J. Beaman, H.L. Marcus, R.H. Crawford, and J.W. Barlow
- Publisher: University of Texas at Austin
- Publication Year: 1997
- Type of Publication: SFF conference proceeding
- Additional Support: No
- Title: Solid Freeform Fabrication: A New Direction in Manufacturing by J.J. Beaman, J.W. Barlow , D.L. Bourell, R.H. Crawford, H.L. Marcus, and K.P. McAlea
- Publisher: Kluwer Academic Publishers
- Publication Year: 1997
- Type of Publication: Textbook
- Additional Support: No
Sabbatical Plans
Related Research
- The Concurrent Design and Manufacturing Simulation Laboratory (CDMS Lab), Dept. of Mechanical Engineering, University of Connecticut
- University of Texas at Austin
- Massachusettes Institute of Technology (MIT)
- Rutgers University
- Stanford University
History
- Dr. Marcus has been involved in the solid freeform fabrication research field for over 10 years, beginning with his involvement is selective laser sintering(SLS) investigations at the University of Texas at Austin. Gas-phase SFF is a tangent from the SLS work, using gas precursors as the source of material to form a desired object. The initial gas-phase work dealt with the deposition of carbon and silicon carbide by straight SALD. Iterations of the SALD approach lead to SALDVI, the vapor infiltration of the solid reaction product into consecutive layers of powder, and SALD joining, the use of the reaction product to 'weld' together parts. Dr. Marcus left the University of Texas at Austin in the summer of 1995 to become the director of the Institute of Materials Science(IMS) at the University of Connecticut. At IMS, Dr. Marcus began a new gas-phase program, building up a fully equipped laboratory and launching the SALD/SALDVI thermocouple program and the SALD ceramic joining effort. Future investigations will focus on inhomogenous chemical deposition to form chemically varied, gradient structures.