smart materials systems through mesoscale patterning

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Final Report for the period 06/19/1995-05/31/2001

TITLE AND SUBTITLE Smart Materials Systems through Mesoscale Patterning

5. FUNDING NUMBERS DAAH04-95-1-0102

AUTHOR(S) llhan A. Aksay, W.-H. Shih, P. C. Y. Lee, R. K. Prud'homme, G. M. Whitesides, and S. M. Grüner

7. PERFORMING ORGANIZATION NAME(S) AND ADDRESS(ES) Princeton University, Princeton, NJ; Harvard University, Cambridge, MA; Cornell University, Ithaca, NY; Drexel University, Philadelphia, PA

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13. ABSTRACT (Maximum 200 words)

This project emphasized the production of smart material systems using advanced 3-dimensional processing techniques. The specific aim was the fabrication and characterization of smart organic/inorganic composites at the mesoscale (~1nm -1 mm length scale) to achieve improved performance. Two approaches were used: (i) the synthesis and processing of organic/inorganic composites and (ii) developing two novel materials systems. Synthesis and processing studies involve the use of three methods: (i) laser stereolithography, (ii) self-assembled monolayers, and (iii) 3-dimensional co-assembly. The two novel systems developed for use in sensor and actuator technologies were piezoelectric shell transducers and 1-3 piezocomposite hydrophones.

This is the final technical report for the project, covering period 06/19/1995 - 05/31/2001. Proof of concept and feasibility studies have successfully demonstrated (i) the utility of rapid prototyping in the fabrication of ceramic structures for use in sensor and actuator applications; (ii) the formation of mesostructured ceramics via templation of liquid crystal structures in solution; (iii) guided growth and orientation in microcontact printing microinfiltration; and (iv) optimization of piezo-composite properties through analytical modeling.

14. SUBJECT TERMS 3-dimensional processing, smart materials, organic/inorganic composites, stereolithography, microcontact printing, co-assembly, self-assembled monolayers, piezocomposites, shell transducers

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Smart Materials Systems through Mesoscale Patterning

Ilhan A. Aksay,§ Sol M. Gruner,f Peter C. Y. Lee,{ Robert K. Prud'homme,§ Wei-H. Shih,* and George M. Whitesides

Departments of §Chemical Engineering, ^Chemistry, and Princeton Materials Institute, Princeton University

^Department of Physics, Cornell University

*Materials Engineering Department, Drexel University

department of Chemistry, Harvard University

Scientific Progress and Accomplishments

The accomplishments for the project are detailed in the following sections. Active projects during the period of performance include the following task areas:

1. Piezoelectric Cantilevers as Sensors Wan Y. Shih, James S. Vartuli, David L. Milius, Huiming Gu, Xiaoping Li, Wei-Heng Shih, and Ilhan A. Aksay

2. Dynamics of Piezoelectric Cantilevers-Size Sensors Peter C. Y. Lee, Rui Huang, Ninghui Liu, and Arthur Ballato

3. Synthesis and Characterization of PMN-PT Piezoelectrics Huiming Gu, Wan Y. Shih, and Wei-Heng Shih

4. Stereolithography of Organic/Inorganic Composites Robert K. Prud'homme, Ilhan A. Aksay, DavidL. Milius, James S. Vartuli, Rajeev Garg, Aaron J. Dulgar, Peter J. Photos, Jim H. Lee, and James Liang

5. Mesoscopic Composites as Small Materials Systems George M. Whitesides, et al.

6. Micropatterning through Field-Assisted Flow Ilhan A. Aksay, George M. Whitesides, SolM. Grüner, Robert K. Prud'homme, Dudley A. Saville, James S. Vartuli, Daniel M. Dabbs, Matt Trau, Srinivas Manne, Linbo Zhou, Anthony Ku, Hak Fei Poon, and Macit Ozenbas

7. The Sponge Phase: Synthesis and Characterization Sol M. Grüner, Karen J. Edler, Daniel M. Dabbs, Nan Yao, Aaron Rabinovitch, Akin Akinc, Robert K. Prud 'homme, and Ilhan A. Aksay

8. L3 "Sponge" Phase: Applications Daniel M. Dabbs, Sol M. Grüner, Karen J. Edler, Nan Yao, Aaron Rabinovitch, Akin Akinc, Robert K. Prud'homme, and Ilhan A. Aksay

Publications

1996 1. "Design of Materials with Extreme Thermal Expansion using a Three-Phase Topology Optimization

Method," O. Sigmund and S. Torquato, Danish Center for Applied Mathematics and Mechanics, Report No. 525 (Technical University of Denmark, Lyngby, Denmark, 1996).

2. "Patterning with Magnetic Materials at the Micron Scale," S. Palacin, P. C. Hidber, J.-P. Bourgoin, C. Miramond, C. Fermon, and G. M. Whitesides, Chem. Mat. 8 [6] 1316-25 (1996).

1

3. "Microcontact Printing of Palladium Colloids: Micron-Scale Patterning by Electroless Deposition of Copper," P. C. Hidber, W. Helbig, E. Kim, and G. M. Whitesides, Langmuir 12 [5] 1375-80 (1996).

4. "Micromolding in Capillaries: Applications in Materials Science," E. Kim, Y. Xia, and G. M. Whitesides, J. Am. Chem. Soc. 118 [24] 5722-31 (1996).

5. "Composites with Extremal Thermal Expansion Coefficients," O. Sigmund and S. Torquato, Appl. Phys. Lett. 69 [21] 1-3 (1996).

6. "Biomimetic Pathways for Assembling Inorganic Thin Films," I. A. Aksay, M. Trau, S. Manne, I. Honma, N. Yao, L. Zhou, P. Fenter, P. M. Eisenberger, S. M. Grüner, Science 273 892-8 (1996).

7. "Governing Equations of Piezoelectric Plates with Graded Properties across the Thickness," P. C. Y. Lee and J. D. Yu, 1996 IEEE Int. Frequency Control Symp., 623-31 (1996).

8. "Nanostructured Materials Through Self-Assembly," I. A. Aksay, in Frontier Nanostructured Ceramics, (Tohwa University Press, Fukuoka, Japan, 1996) pp. 35-41.

9. "Meso-Scale Smart Materials Fabrication Technologies of the Future," R. K. Prud'homme, I. A. Aksay and G. M. Whitesides, in Proc. 1996 Int'I Congress on Transportation Electronics (SAE, Warrendale, PA, 1996) pp. 497-501.

10. "Smart Materials Systems Through Mesoscale Patterning," I. A. Aksay, J. T. Groves, S. M. Grüner, P. C. Y. Lee, R. K. Prud'homme, W.-H. Shih, S. Torquato, and G. M. Whitesides, Smart Materials Technologies and Biomimetics, SPIEProc. 2716, 280-91 (1996).

11. "A New Strategy for Controlling the Size and Shape of Metallic Features Formed by Electroless Deposition of Copper: Microcontact Printing of Catalysts on Oriented Polymers, Followed by Thermal Shrinkage", P. C. Hidber, P. F. Nealey, W. Helbig, and G. M. Whitesides, Langmuir [12] 5209-15 (1996).

12. "Mechanisms of BaTiC<3 Formation by Hydrothermal Reactions," I. A. Aksay, C. M. Chun, and T. Lee, Proc. 2nd Int. Conf. Solvothermal Reactions (1996).

13. "A New 2-D Theory for Vibrations of Piezoelectric Crystal Plates with Electroded Faces," P. C. Y. Lee, J. D. Yu, and W. S. Lin, Proc. 1996 IEEE Int. Ultrason. Symp., pp. 1591-4 (1996).

1997 14. "Size Effects in BaTi03 Particles and Clusters," X. Li and W.-H. Shih, J. Am. Ceram. Soc. 80 [11], 2844-

52, (1997).

15. "Nanostructured Ceramics through Self-Assembly," I. A. Aksay, in Proc. 9th International Metallurgy and Materials Congress, Istanbul (Chamber of Metallurgical Engrs, Turkey, Publ. 33, 1997) pp. 575-82.

16. "Imaging of Organic/Inorganic Interfaces," I. A. Aksay, S. Manne, and N. Yao, in Proc.13th National Electron Microscopy Congress, Ankara (Middle East Technical University, Ankara, Turkey, 1997).

17. "Thin Films and Nanolaminates Incorporating Organic-Inorganic Interfaces," S. Manne and I. A. Aksay, Current Opinion in Solid State & Materials Science 2 [3] 358-64 (1997).

18. "The Formation of a Silicate L3 Phase with Continuously Adjustable Pore Sizes," K. McGrath, D. M. Dabbs, N. Yao, I. A. Aksay, and S. M. Grüner, Science 277 [5325] 552-56 (1997).


19. "Self-Assembly Structures of Nonionic Surfactants at Graphite/Solution Interfaces," H. N. Patrick, G. G. Warr, S. Manne, and I. A. Aksay, Langmuir 13 [16] 4349-56 (1997).

20. "Scaling Analysis for the Axial Displacement and Pressure of Flextensional Transducers," W. Y. Shih, W.- H. Shih, and I. A. Aksay, J. Am. Ceram. Soc. 80 [5] 1073-78 (1997).

21. "Multilayer Electromechanical Composites with Controlled Piezoelectric Coefficient Distribution," J. S. Vartuli, D. L. Milius, X. Li, W. Y. Shih, W.-H. Shih, R. K. Prud'homme, and I. A. Aksay, Smart Materials Technologies and Biomimetics, SPIEProc. 3040, 93-98 (1997).

22. "Thermal Expansion of Isotropie Multiphase Composites and Polycrystals," L. V. Gibiansky, and S. R. Torquato, J. Mech. Phys. Solids 45 [7] 1223-52 (1997).

23. "Mesoscopic Silica Thin Films via Template-Assisted Self-Assembly," N. Yao, M. Trau, S. Manne, N. Nakagawa, T. Lee, I. Honma, and I. A. Aksay, in Proc. Microscopy and Microanalysis 1997, eds.: G. W. Bailey, R. V. W. Dimlich, K. B. Alexander, J. J. McCarthy, T. P. Pretlow (Springer-Verlag, New York, NY, 1997) pp. 395-96.

24. "On the Use of Homogenization Theory to Design Optimal Piezocomposites for Hydrophone Applications," L. V. Gibiansky and S. Torquato, J. Mech. Phys. Solids 45 [5] 689-708 (1997).

25. "Design of Materials with Extreme Thermal Expansion Using a Three-Phase Topology Optimization Method," O. Sigmund and S. Torquato, J. Mech. Phys. Solids 45 [6] 1037-67 (1997).

26. "Optimal design of 1-3 composite piezoelectrics," L. V. Gibiansky and S. Torquato, Structural Optimization 13 23-8 (1997).

27. "Imbibition and Flow of Wetting Liquids in Noncircular Capillaries", Kim, E. and Whitesides, G. M., J. Phys. Chem. 101 855-863 (1997).

28. "Solvent-Assisted Microcontact Molding: A Convenient Method for Fabricating Three-Dimensional Structures on Surfaces of Polymers", E. Kim, Y. Xia, X.-M. Zhao, and G. M. Whitesides, Adv. Mater. 9 651-654(1997).

29. "On the Design of Hydrophones Made as 1-3 Piezoelectrics," O. Sigmund, S. Torquato, L. V. Gibiansky, and I. A. Aksay, in Proc. IUTAM Symp. on Transformation Problems in Composite and Active Materials, eds.: Y. A. Bahei-El Din, G. J. Dvorak (Kluwer Acad. Publ., 1997).

30. "Microscopic Patterning of Oriented Mesoscopic Silica through Guided Growth," M. Trau, N. Yao, Y. Xia, G. M. Whitesides, and I. A. Aksay, Nature 390 [6661] 674-76 (1997).

31. "Effects of Copper Coating on the Crystalline Structure of Fine BaTi03 Particles," X. Liu, W. Y. Shih, and W.-H. Shih, J. Am. Ceram. Soc. 80 [11], 2781-88 (1997).

32. "Gemini Surfactants at Solid-Liquid Interfaces: Control of Interfacial Aggregate Geometry," S. Manne, T. E. Schäffer, Q. Huo, P. K. Hansma, D. E. Morse, G. D. Stucky, and I. A. Aksay, Langmuir 13 [24] 6382- 87(1997).

33. "Titanium Dioxide-Surfactant Mesophases and Ti-TMSl," R. L. Putnam, N. Nakagawa, K. M. McGrath, N. Yao, I. A. Aksay, S. M. Grüner, and A. Navrotsky, Chem. Mater. 9 [12] 2690-93 (1997).

34. "Assembly of Colloidal Crystals at Electrode Interfaces," M. Trau, D. A. Saville, and I. A. Aksay, Langmuir 13 [24] 6375-81 (1997).


35. "Force Microscopy: Measurement of Local Interfacial Forces and Surface Stresses," S. Manne and H. E. Gaub, Current Opinion in Colloid and Interface Science 2 [2] 145-152 (1997).

36. "Surfactant Aggregates at a Metal Surface," M. Jaschke, H.-J. Butt, H. E. Gaub, and S. Manne, Langmuir 13 1381-4(1997).

37. "Piezoelectric Ceramic Disks with Thickness-Graded Properties," P. C. Y. Lee, J. D. Yu, X. Li, and W.-H. Shih, Proc. 1997 IEEE International Frequency Control Symposium, 769-777, (1997)

38. "Depolarization Effect on the Crystalline Structure Fine BaTi03 Particles," X.Liu, W.Y. Shih, W.-H. Shih Am. Ceram. Soc. Proc. Advances in Dielectric Ceramic Materials 225-236 (1997).

1998 39. "Fabrication of Microstructures Using Shrinkable Polystyrene Films", X.-M. Zhao, Y.N. Xia,

O.J.A. Schueller, D. Qin, G.M. Whitesides, Sensors and Actuators A: Physical 65 [2-3] 209-17 (1998).

40. "Optical Transmission in Highly-Concentrated Dispersions," R. Garg, R. K. Prud'homme, I. A. Aksay, F. Liu, and R. Alfano, J. Opt. Soc. Am. 15 [4] 932-35 (1998).

41. "Soft Lithography", Y. Xia and G. M. Whitesides, Annu. Rev. Mater. Sei., 28 153-184 (1998).

42. "On the Design of 1-3 Piezocomposites Using Topology Optimization," O. Sigmund, S. Torquato, I. A. Aksay, J. Mater. Res. 13 [4] 1038-48 (1998).

43. "The Use of Soft Lithography to Fabricate Arrays of Schottky Diodes," J. Hu, R.G. Beck, R.M. Westervelt, G.M. Whitesides, Adv. Mater. 10 574-577 (1998).

44. "Governing Equations for a Piezoelectric Plate with Graded Properties Across the Thickness," P. C. Y. Lee, J. D. Yu, IEEE Transactions on Ultrasonics, Ferroelectrics, and Frequency Control, 45 [1], 236-250 (1998).

45. "A New Dimensional Theory for Vibrations of Piezoelectric Crystal Plates with Electroded Faces," P.C.Y. Lee, J.D. Yu, W.S. Lin, J. Appl. Phys. 83 [3] 1213-1223 (1998).

46. "Effect of Thickness Ratio on Vibrations of an Asymmetric Bimorph Plate of Piezoelectric Ceramics," P.C.Y. Lee, N.H. Liu, IEEE 1998 Inter. Frequency Control Symp. (1998).

47. "Vibrations and Static Responses of Asymmetric Bimorph Disks of Piezoelectric Ceramics," P.C.Y. Lee, R. Huang, X. Li, W.-H. Shih, IEEE 1998 Inter. Frequency Control Symp. (1998).

48. "Solvent-Assisted Microcontact Molding: A Convenient Method for Fabricating Three-Dimensional Structures on Surfaces of Polymers," E. Kim, Y. Xia, X-M. Zhao, G.M. Whitesides, Adv. Mater. 9 651-654 (1998).

49. "Absorption Length for Photon Propogation in Highly Dense Colloidal Dispersions," R. Garg, R. K. Prud'homme, I. A. Aksay, F. Liu, and R. Alfano, J. Mater. Res. 13 3463-3467 (1998).

50. "Nanostructured Ceramics through Self-Assembly," I. A. Aksay, in R&D Status and Trends in Nanoparticles, Nanostructured Materials, and Nanodevices in the United States, eds. R. W. Siegel, E. H. Hu, M. C. Roco (International Technology Research Institute, WTEC, Baltimore, MD, 1998) pp. 79- 82.


51. "Biomaterials: Is This Really a Field of Research?" I. A. Aksay and S. Weiner, Current Opinion in Solid State & Materials Science 3 [3] 219-20 (1998).

52. "Rapid Prototyping Techniques for Bone Implant," R. Garg, R. K. Prud'homme, I. A. Aksay, in Proc. Fifth International Conference on Composites Engineering (ICCE/5), ed. David Hui (International Community for Composites Engineering, University of New Orleans, LA, 1998) pp. 739-40.

53. "Self-Assembled and Micro-patterned Mesoscopic Thin Films," N. Yao, M. Tau, N. Nakagawa, and I. A. Aksay, in Proc. Microscopy and Microanalysis 1998 eds:. G. W. Bailey, K. B. Alexander, W. B. Jerome, M. G. Bond, J. J. McCarthy, (Springer-Verlag, New York, NY, 1998) pp. 730-31.

54. "Fabrication of Silicon MOSFETs Using Soft Lithography", N.L. Jeon, J.M. Hu, G.M. Whitesides, M.K. Erhardt, R.G. mzzo, Adv. Mater. 10 [17] 1466-69 (1998).

55. "Hierarchically Ordered Oxides," P. Yang, T. Deng, D. Zhao, B.F. Chmelka, G.M. Whitesides, G.D. Stucky, Science 282 [5397] 2244-46 (1998).

56. "Maskless Photolithography: Embossed Photoresist as its Own Optical Element," K.E. Paul, T.L. Breen, J. Aizenberg, G.M. Whitesides^/?/. Phys. Lett. 73 [20] 2893-95 (1998).

57. "The use of soft lithography to fabricate arrays of Schottky diodes," J.M Hu, R.G. Beck, R.M. Westervelt, G.M. Whitesides Adv. Mater. 10 [8] 574-78 (1998).

1999 58. "The Elastic and Yield Behavior of Flocculated Colloids," W. Y. Shih, W.-H. Shih, and I. A. Aksay, J. Am.

Cer. Soc. 82 [3]: 616-24 (1999).

59. "Mesoscale Self-Assembly of Hexagonal Plates Using Lateral Capillary Forces: Synthesis Using the "Capillary Bond," N. Bowden, I.S. Choi, B. Grzybowski, G.M. Whitesides J. Am. Chem. Soc. 121 [23] 5373-91 (1998).

60. "Conversion of Fly Ash into Mesoporous Aluminosilicate," H-L. Chang, C-M. Chun, I.A. Aksay, W-H. Shih, Ind. & Eng. Chem. Res. 38 973-977 (1999).

61. "Matrix laminate composites: Realizable approximations for the effective moduli of piezoelectric composites," L. V. Gibiansky and S. Torquato, J. Mat. Res. 14 [1] 49-63 (1999).

62. "Surface Micellization Patterns of Quaternary Ammonium Surfactants on Mica," H.N. Patrick, G.G. Warr, S. Manne, I.A. Aksay, Langmuir 15 [5] 1685-92 (1999).

63. "Piezoelectric ceramic disks with thickness-graded material properties," P.C.Y. Lee, J. D. Yu, X. Li, and W.-H. Shih IEEE Intern. Frequency Control Symp. Proc. 46 [1] (1999).

64. "Electromechanical behavior of PZT-brass unimorphs," X.P. Li, W.Y. Shih, I.A. Aksay, W.H. Shih J. Am. Ceram. Soc. 82 [7] 1733-40 (1999).

65. "Making Negative Poisson's Ratio Microstructures by Soft Lithography," B. Xu, F. Arias, S.T. Brittain, X- M. Zhao, B. Grzybowski, S. Torquato, G.M. Whitesides, Adv. Mater. 11 [17] 1433-37 (1999).

66. "The interaction of proteins and cells with self-assembled monolayers of alkanethiolates on gold and silver," E. Ostuni, L. Yan, G.M. Whitesides Coll. Surf B-Biointerf 15 [1] 3-30 (1999).


67. "Control of crystal nucleation by patterned self-assembled monolayers," J. Aizenberg, A.J. Black, G.M. Whitesides Mtfw«? 398 [6727] 495-8 (1999).

68. "Complexity in Chemistry," G.M. Whitesides, R.F. Ismagilov, Science 284 [5411] 89-92 (1999).

2000 69. "Silica Gels with Tunable Nanopores through Templating of the L3 Phase," K.M. McGrath, D.M. Dabbs,

N. Yao, K.J. Edler, I.A. Aksay, S.M. Grüner Langmuir 16 [2] 398-406 (2000).

70. "Synthesis of Mesostructured NiO with Silica," X. Liu, C.-M. Chun, I.A. Aksay, W.-H. Shih, Ind. Eng. Chem. Res. 39 [3] 684-92 (2000).

71. "Patterning mammalian cells using elastomeric membranes," E. Ostuni, R. Kane, C.S. Chen, D.E. Ingber, G.M. Whitesides Langmuir 16 [20] 7811-19 (2000).

72. "Colloidal Crystals with Tunable Micropatterns: Current Density Modulation with UV-light During Electrophoretic Deposition," R.C. Hayward, D.A. Saville, I.A. Aksay, Nature 404 [6773] 56-9 (2000).

2001 73. "Electromechanical properties of a ceramic d(31)-gradient flextensional actuator," X.P. Li, J.S. Vartuli,

D.L. Milius, I.A. Aksay, W.Y. Shih, W.H. Shih J Am. Ceram. Soc. 84 [5] 996-1003 (2001).

74. "Fabrication and characterization of microscale sandwich beams," F. Arias, P.J.A. Kenis, B. Xu, T. Deng, O.J.A. Schueller, G.M. Whitesides, Y. Sugimura, A.G. Evans J. Mater. Res. 16 [2] 597-605 (2001).

75. "Cure depth in photopolymerization: Experiments and theory" J.H. Lee, R.K. Prud'homme, I.A. Aksay, J. Mater. Res. 16 [12] 3536-44 (2001).

76. "Simultaneous Liquid Viscosity and Density Determination with Piezoelectric Unimorph Cantilevers," W.Y. Shih, X. Li, H. Gu, W.-H. Shih, I.A. Aksay, J. Appl. Phys. 89 [2] 1497-1505 (2001).

77. "Hierarchical Structure-Ferroelectricity Relationships of Barium Titanate Particles" T. Lee, I.A. Aksay, Crys. Growth Des. 1 [5] 401-19 (2001).

78. "Barium Titanate Nanoparticles in Block Copolymer" T. Lee, N. Yao, H. Imai, I.A. Aksay, Langmuir 17 [24] 7656-63 (2001).

79. "Deformation Mechanisms in Nacre," R. Z. Wang, Z. Suo, A.G. Evans, N. Yao, I. A. Aksay, J. Mater. Res. 16 [9] 2485-93 (2001).

80. "Model for the Robust Mechanical Behavior of Nacre" A.G. Evans, Z. Suo, R. Z. Wang, I. A. Aksay, M. Y. He, J. W. Hutchinson, J. Mater. Res. 16 [9] 2475-84 (2001).

Manuscripts 81. "Segment Density Profiles at the A/B Interface of Microphase Separated AB Di-Block Copolymers," W. Y.

Shih and I. A. Aksay, Macromolecules (submitted, 1998).

82. "Colloidal Crystal Assembly on Electrode Surfaces," Y. Xiao, H.F. Poon, M. Trau, S. Torquato, D.A. Saville, I.A. Aksay, Langmuir (submitted February 1999).

83. "Electrical Field-Induced Processing of Ceramic-Metal Composite Coatings," J. S. Lettow, M. Trau, D. A. Saville, and I. A. Aksay, J. Am. Ceram. Soc. (submitted, Jan. 22, 1999).


84. "Processing of a High Displacement Ceramic-Ceramic Flextensional Actuator (PrinDrex)," J. S. Vartuli, D. L. Milius, X. Li, W. Y. Shih, and W.-H. Shih, R. K. Prud'homme, and I. A. Aksay, J. Am. Ceram. Soc. (submitted, 1999).

Patent Activity

Patents Awarded 85. M. Trau, I.A. Aksay, D.A. Saville, "Method and Apparatus for Electrohydrodynamically Assembling

Colloidal Structures," U.S. Patent # 5,855,753, January 05, 1999.

86. I. A. Aksay et al., "Biomimetic Pathways for Assembling Inorganic Thin Films and Oriented Mesoscopic Silicate Patterns through Guided Growth," U.S. Patent Application Serial No. 08/964 876; Docket No. 97- 1376-1 (allowed). Licensed to American Biomimetic Corp.

Patent Applications 87. K. M. McGrath, D. M. Dabbs, I. A. Aksay, S. M. Grüner, "Formation of a Silicate Sponge (L3) Phase,"

U.S. Provisional Patent Application Serial No. 60/047,463; Docket No. 97-1407-1.

88. W. Happer, G. Cates, M.-F. Hsu, and I. A. Aksay, "Sol-Gel Coated Polarization Vessels," U.S. Provisional Patent Application Serial No. PCT/US98/16834; Docket No 98-1443-1.

89. R. K. Prud'homme, I. A. Aksay, and R. Garg, "Method for the Preparation of Ceramic Articles," U.S. Patent Application Serial No. 846,764; Docket No. 98-1470-1. (Co-owned by Dow Chemical Co.).

90. I.A. Aksay, R. Garg, R.K. Prud'homme, "Controlled Microarchitecture Ceramic by Stereolithography," U.S. Patent Application Serial No. 09/191,606, Docket No. 98-1500-1.

Invention Disclosures 91. J. S. Vartuli,, R. K. Prud'homme, W.-H. Shih, D. L. Milius, W. Y. Shih, X. Li and I. A. Aksay, "Multi-

Layer Piezoelectric Laminate," Docket No. 98-1512-1.


Scientific Personnel

Principal Investigators Ilhan A. Aksay, Chemical Engineering, Princeton University Peter C. Y. Lee, Civil and Environmental Engineering, Princeton University Robert K. Prud'homme, Chemical Engineering, Princeton University Jean-H. Prevost, Civil and Environmental Engineering, Princeton University Sol M. Grüner, Physics, Cornell University George M. Whitesides, Chemistry, Harvard University Wei-Heng Shih, Materials Engineering, Drexel University

Collaborating Faculty Dudley A. Saville, Chemical Engineering, Princeton University Macit Ozenba§, Middle East Technical University, Turkey

Research Staff D. M. Dabbs L. V. Gibiansky D. L. Milius W. Y. Shih 0. Sigmund N.Yao

Postdoctoral Researchers C.-M. Chun D. Cule K. J. Edler P. Fenter E.Kim S. Manne K. M. McGrath M. Trau R. Wang Y.Xia

Graduate Students S. Brittain R. Garg H. Gu R. Huang E. Hutchins H.-L. Ker A. Y. Ku J. H. Lee T. Lee X. Li J. Liang N.Liu H.-F. Poon J. S. Vartuli L. Zhou

Undergraduate Students A. Akinc C. Brown A. J. Dulgar R. Hayward M.Hsu K. LaMarche S.Lu K. Mattern J. McDonald C. Monroe J. Mysen M. Pagnotto P. J. Photos A. Rabinovitch S. Rea D. Volk


Technology Transfer

Collaborations and Interactions Army Research Office

ARO, U.S. Army Research Laboratory, Arthur Ballato, Fort Monmouth, New Jersey

Industrial

PrinDrex technology licensed to Leading Edge Ceramics

Sponge phase technology licensed to American Biomimetics

Ceramic stereolithography licensed to Johnson and Johnson

L3 phase technology transfer agreement with Lucent Technologies

Other Industral Connections

Company/Corporation Contact Company/Corporation Contact

3D Systems Valencia, California

Dr. Paul F. Jacobs Johnson & Johnson Somerville, New Jersey

Dr. Mark Roller

Dow Chemical Co. Midland, Michigan

Dr. Alan M. Hart Dr. Alek J. Pyzik

Rohm and Haas Specialty Materials Spring House, PA

Dr. Edward Greer

EDO Corporation Salt Lake City, Utah

Mr. Donald Bascow TPL, Inc. Albuquerque, New Mexico

Mr. Hap Stoller

Lord Corporation Cary, North Carolina

Dr. Gerald Estes Lucent Technologies Murray Hill, New Jersey

Dr. Cherry Murray Dr. Howard Katz

Allied Signal Dr. Clifford Ballard ILC Cherry Hill, New Jersey

Mr. Howard Stein

Leading Edge Ceramics Seattle, Washington

Mr. Clare Nordquist Praxair Specialty Ceramics Seattle, Washington

Mr. Randy Kurosky

Nanodyne Piscataway, New Jersey

Mr. Frank Shinnemon AMT Venture Partners Dallas, Texas

Mr. Tom Delimitros

SMART MATERIALS SYSTEMS THROUGH MESOSCALE PATTERNING

ILHAN A. AKSAY§, SOL M. GRUNER+ PETER C. Y. LEE*,, ROBERT K. PRUD'HOMME5, WEI-H. SHIH*, WAN Y. SHIH**

DANIEL M. DABBS§, GEORGE M. WHITESIDES*

DEPARTMENTS OF §CHEMICAL ENGINEERING, * CIVIL ENGINEERING AND

OPERATIONS RESEARCH, AND PRINCETON MATERIALS INSTITUTE

PRINCETON UNIVERSITY, PRINCETON, NEW JERSEY 08544

DEPARTMENT OF CHEMISTRY, HARVARD UNIVERSITY

CAMBRIDGE, MASSACHUSETTS 02138

DEPARTMENT OF PHYSICS, CORNELL UNIVERSITY

ITHACA, NEW YORK 14853

*MATERIALS ENGINEERING DEPARTMENT, DREXEL UNIVERSITY

PHILADELPHIA, PENNSYLVANIA 19104

FIFTH ARO/MURI PROGRAM REVIEW HARVARD UNIVERSITY

CAMBRIDGE, MASSACHUSETTS

SEPTEMBER 28-29,1999

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WAN Y. SHIH§#, JAMES S. VARTULI§#, DAVID L. MILIUS5'*, HUIMING GU*, XIAOPING LI*, WEI-HENG SHIH*,

AND ILHAN A. AKSAY5'*

*DEPARTMENT OF CIVIL ENGINEERING AND OPERATIONS RESEARCH DEPARTMENT OF CHEMICAL ENGINEERING, AND

*PRINCETON MATERIALS INSTITUTE PRINCETON UNIVERSITY, PRINCETON, NEW JERSEY 08544

^DEPARTMENT OF MATERIALS ENGINEERING DREXEL UNIVERSITY, PHILADELPHIA, PENNSYLVANIA 19104



SEPTEMBER 28 -29,1999

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"DEPARTMENT OF CIVIL ENGINEERING AND OPERATIONS RESEARCH, AND PRINCETON MATERIALS INSTITUTE


DEPARTMENT OF MATERIALS ENGINEERING DREXEL UNIVERSITY, PHILADELPHIA, PENNSYLVANIA 19104



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Synthesis and Characterization of PMN-PT Piezoelectrics

HUIMING GU*. WAN Y. SHIH§, WEI-HENG SHIH*,

*DEPARTMENT OF MATERIALS ENGINEERING DREXEL UNIVERSITY, PHILADELPHIA, PENNSYLVANIA 19104

DEPARTMENT OF CHEMICAL ENGINEERING, AND PRINCETON MATERIALS INSTITUTE



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ROBERT K.PRUD'HOMME*'5, ILHAN A. AKSAY* §, DAVID L. MILIUS*'5, JAMES S. VARTULI*5, RAJEEV GARG*'§ AARON J. DULGAR*§,

PETER J. PHOTOS*'8, JAMES LEE**§, JAMES LIANG*8

DEPARTMENTS OF *CHEMICAL ENGINEERING, #PHYSICS, AND §PRINCETON MATERIALS INSTITUTE


DEPARTMENT OF CHEMISTRY, HARVARD UNIVERSITY CAMBRIDGE, MASSACHUSETTS 02138

DEPARTMENT OF PHYSICS, CORNELL UNIVERSITY ITHACA, NEW YORK 14853


CAMBRIDG, MASSACHUSETTS

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Mesoscopic Composites as Small Materials Systems

GEORGE M. WHITESIDES





SEPTEMBER 28 - 29,1999

MURI Program Review Harvard University September 28,1999

Agenda for Whitesides Group Presentation

Introduction Soft Lithography Rapid Prototyping using Soft Lithography

Methods for the fabrication of small, functional structures Metals:

Microorigami Trusses Slot Filters Heat Exchangers Composites Self-Assembly of 3D Circuits Microcontact Printing on Curved Surfaces Microfabrication of Complex Geometries FLO for Fabrication of Microelectrode Systems

Ceramics, etc.: C/Si Si/B/C/N

General Methods Metals:

Microelectrochemistry: Applications for non-planar surfaces

Rapid Prototyping Using Silver Halide Film 3D Microfabrication in Microfluidic Systems Self-Assembly of Microstructures

Polymers: Dali Crosses

Future Directions

George Wh Kateri Paul Tao Deng

Scott Brittai Scott Brittai Kateri Paul Francisco A Francisco A David Graci Hongkai Wi Hongkai Wi Paul Kenis

Scott Brittai Hong Yang

Scott Brittai Tao Deng Janelle And Tom Clark

Hong Yang

Kateri Paul

Techniques of Soft Lithography Master: prepared by photolithography, micromolding, or other techniques

Pour prepolymer and cure

Remove stamp

Microcontact printing Micromolding in capillaries

^>

PDMS

iiicLdi ictyci i Si 1

alkanethiol _ ""si™ "l

PDMS

precursor

substrate l

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prepolymer ̂Q^b^^]

PDMS substrate

cured polymer F—i r~~i i—i substrate

solvent

polymer

embossed polymer

Replica molding Near field lithography

P"DMS

PDMS J—L-r-L

ST

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Fabrication of Microtruss

Fabricate planar Ag grid using |xCP and electroplating.

Fold 70 deg along axes using tweezers and brass die.

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Fabrication of Heat Exchangers

Photoresist

Silicon wafer

500 um

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polymer structure

PDMS membrane

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Ni or Cu

ative replica sist structure

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PU or epoxy membrane

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Electroplated membrane

Remove polymer: Dissolve PDMS in TBAF/THF or Burn PU and epoxy at 400°C

Metallic heat exchanger

200 urn thick walls

Characterization of Heat Exchangers 400 |im unfilled cylinders 150 |im posts

1 cm 1 cm

Performance of nickel specimen with 400 fim unfilled cylinders

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Fabrication of Microgrids

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Microorigami, composites and trusses (ullAVs, read arms) • tensegrity structures—incorporation of polymeric elements

into metallic, 3D structures • maximize the stiffness-to-weight ratio of the panels • use diffusion bonding of nickel instead of tin/lead soldering to

assemble sandwich panels

Slot filters (thermophotovoltaics) • smaller critical dimensions (~100 nm line width) • fabrication on curved surfaces

Heat exchangers (high power microelectronics) • modules with high surface area and low thermal resistance • non-planar heat exchangers

Microcontact printing on curved/spherical surfaces (curved focal plane IR detector) • solve the distortion problem for printing on spherical surfaces • additive methods • functional components

FLO for fabrication of microelectrode systems (BWD) • integrated micro-analysis systems • use for logic/problem solving

Dali crosses (photonic bandgap materials) • increase yield and quality of the crosses • modify faces of the crosses and self-assemble into ordered

3D structures

Future Directions: Far Term or Technology Base

Rapid prototyping using Soft Lithography • generate structures at 1-um scale

Microelectrochemistry on Saran Wrap (curved surface fabrication) • quantify and minimize distortion during stretching • reduce feature size to 1 urn

Self-assembly (3D electronic circuits) • controlling assembly size and shape through templating • add transistors to the faces • Self-assembly of photonic bandgap crystals

Rapid prototyping using silver halide film • smaller structures; more functional applications, color films

Ceramics (rapid microfabrication of complex ceramic microstructures) • C/Si: new start to convert Si layer on glassy C to SiC • Si/B/C/N: improve fidelity; fabricate useful structures such

as membranes and microcomponents

3D microfabrication in microfluidic systems (BWD) • apply methods to systems that require compactness or have

topological constraints • generate complex fluidic components


Micropatterning through Field-Assisted Flow

ILHAN A. AKSAY* 5, GEORGE M. WHITESIDESf, SOL M. GRÜNER*, ROBERT K. PRUD'HOMME*5,DUDLEY A. SAVILLE*'5,

JAMES S. VARTULI*'5, DANIEL M. DABBS*'5,MATT TRAU5, SRINIVAS MANNE5, LINBO ZHOU*, ANTHONY KU*'5,

HAK FEI POON* 5, MACIT ÖZENBAS5

DEPARTMENTS OF *CHEMICAL ENGINEERING, *PHYSICS, AND 5PRINCETON MATERIALS INSTITUTE




*DEPARTMENT OF PHYSICS, CORNELL UNIVERSITY

ITHACA, NEW YORK 14853




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The Sponge Phase: Synthesis and Characterization

SOL M. GRÜNER*, KAREN J. EDLER*, DANIEL M. DABBS§#, NAN YAO#, AARON RABINOVITCH*, AKIN AKINC*,

ROBERT K. PRUD'HOMME5'*, AND ILHAN A. AKSAY§#

DEPARTMENTS OF *PHYSICS AND §CHEMICAL ENGINEERING, AND

*PRINCETON MATERIALS INSTITUTE



ITHACA, NEW YORK

FIFTH ARO/MURI PROGRAM REVIEW

HARVARD UNIVERSITY CAMBRIDGE, MASSACHUSETTS

SEPTEMBER 28-29, 1999

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DANIEL M. DABBS§#, SOL M. GRÜNER*, KAREN J. EDLER*, NAN YAO#, AARON RABINOVITCH*, AKIN AKINC*,

ROBERT K. PRUD'HOMME§#, AND ILHAN A. AKSAY5*

DEPARTMENTS OF *PHYSICS AND §CHEMICAL ENGINEERING, AND

*PRINCETON MATERIALS INSTITUTE



ITHACA, NEW YORK



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