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Direct-Write Fabrication of Pb(Nb,Zr,Ti)O3 Devices: Influence of Paste Rheology on Print Morphology and Component Properties

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Direct-Write Fabrication of Pb(Nb,Zr,Ti)O3 Devices: Influence of Paste Rheology on Print Morphology and Component Properties journal J. Am. Ceram. Soc., 84 [11] 2462–68 (2001) Direct-Write Fabrication of Pb(Nb,Zr,Ti)O3 Devices: Influence of Paste Rheology on Print Morphology and Component Properties Sherry L. Morissette*,† and Jennifer A. Lewis* Department of Materials Science and Engineering, University of Illinois, Urbana, Illinois 61801 Paul G. Clem,* Joseph Cesarano III,* and Duane B. Dimos* Sandia National Laboratories, Albuquerque, New Mexico 87185 Lead niobium zirconate titanate (PNZT) pastes with tailored required before deposition of additional layers, this direct-write rheological properties have been developed for direct-write approach yields significant advantages over the conventional fabrication of thick-film capacitor elements in highly inte- method for producing multilayer devices, such as those based on grated, multifunctional electroceramic devices. Such pastes lamination of tape-cast layers with screen-printed elements, in- exhibited pseudoplastic behavior with a low shear apparent cluding the ability to modify patterned designs on-line during .viscosity of roughly 1 ؋ 106 cP. On aging, the degree of shear printing and to incorporate multiple materials in individual layers thinning and the low shear apparent viscosity decreased. The rheological requirements of thick film pastes for micropen Pastes prepared from as-received powders attained printable, printing and screen printing are nearly identical.7–9,11–17 Hence, -steady-state viscosities of ϳ2 ؋ 105 cP after 50 days of aging. commercially available screen printing pastes (e.g., silver–palla In contrast, pastes prepared from dispersant-coated powders dium conductor, ruthenium oxide resistor, and dielectric pastes) showed no measurable rheological changes after 1 day of can be readily utilized in this direct-write approach. There is, aging. Square elements were patterned on dense alumina however, a need to develop rheologically tailored, cofireable thick substrates or Teflon sheets. Leveling behavior as a function of film pastes of functional ceramic materials (e.g., lead niobium time for single line prints, and the resulting surface topogra- zirconate titanate (PNZT), zinc oxide (ZnO), etc.).18–20 Such phies of dried PNZT films were measured by laser profilom- pastes offer one the ability to fabricate fully integrated devices etry. PNZT layers sintered at varying temperatures between containing high-performance PNZT capacitor and/or ZnO varistor 950° and 1050°C for5hineither air or a lead-rich atmosphere elements. yielded porous microstructures as revealed by scanning elec- The influence of paste rheology on line resolution and surface tron microscopy (SEM). Such layers exhibited dielectric con- topography of as-deposited elements has been investigated previ- stants (K) of 1400–1570 at 1 kHz with dissipation factors (D)of ously for micropen printing9,11 and related screen printing sys- less than 4.1%. tems.14,16,17,21,22 Dimos et al.9,11 studied the relation between the rheological behavior and print properties of a series of commer- cially available thick film pastes patterned using a micropen I. Introduction apparatus. These studies showed that the commercially available thick film pastes exhibited shear thinning behavior with apparent ABRICATION of advanced electrical ceramic devices is com- ϳ ϫ 5 ␥ ϭ Ϫ1 Fmonly achieved via a multilayer build sequence that utilizes viscosities of 1 10 cP in the printing range (˙ 20–85s ); thick film process technologies such as tape casting and screen- however, significant differences in their rheological behavior were ␥ Ͻ Ϫ1 printing.1–8 As device complexity increases, the need for alternate observed in the low-shear (˙ 1s ) or settling regime. Such fabrication methods which offer a simple and rapid means of differences resulted in markedly different line resolution and integrating multiple materials in three-dimensional architectures is surface topographies. For example, conductor pastes which exhib- required. Currently, solid free-form fabrication (SFF) techniques ited high viscosity at low shear yielded high definition patterns, whereas the lower-viscosity resistor pastes produced low- are receiving considerable attention. Direct-write fabrication, an 9,11 emerging SFF method, utilizes a micropen technique to produce definition traces with smooth surface topographies. Clearly, the integrated multifunctional, multimaterial electroceramic devices in low shear rheological behavior of thick film pastes dictates the a rapid, simplistic way.9,10 In this method, a thin cylindrical settling behavior and, hence, the resulting line resolution and extrudate (minimum diameter Ϸ25 ␮m) is deposited in a precise surface topographies of printed features. pattern onto a substrate via computer-aided design (CAD) instruc- We have developed PNZT thick film pastes with tailored tion. Complex, three-dimensional architectures can be constructed rheological properties for micropen fabrication of capacitor ele- in a layer-by-layer build sequence from individual layers contain- ments. In this paper, we describe the protocol utilized to produce ing multiple materials. Although drying of as-printed layers is these PNZT pastes, and the resulting properties of printed capac- itor devices. ZnO pastes prepared via this protocol and the properties of ZnO printed components will be presented in a companion paper.23 In this study, we first examined the influence S. E. Trolier-McKinstry—contributing editor of dispersant and vehicle composition on the respective rheologi- cal behavior of PNZT suspensions and ethyl cellulose solutions. These results served as a benchmark for the design of subsequent paste formulations. Smooth surface topographies which are nec- Manuscript No. 188921. Received November 29, 1999; approved May 7, 2001. essary to achieve uniform dielectric thickness in printed capacitor This research was supported by the National Science Foundation under Grant No. devices were achieved by optimization of paste rheology via DMR94-53446 and by the U.S. Department of Energy under Contract DE-AC04- 94AL8500. Sandia is a multiprogram laboratory operated by Sandia Corp., a compositional tailoring; i.e., the rheological behavior of PNZT Lockheed Martin Co., for the U.S. Department of Energy. pastes mimicked that of the commercial resistor paste described *Member, American Ceramic Society. † above. Stress viscometry measurements of representative PNZT Now at the Materials Processing Center, Massachusetts Institute of Technology, ␾ ϭ Cambridge, Massachusetts 02139. pastes (volume fraction PNZT ( PNZT) 0.35) prepared from 2462 November 2001 Direct-Write Fabrication of Pb(Nb,Zr,Ti)O3 Devices 2463 as-received and dispersant-coated powders revealed that aging (10 ␮m gap, 4 passes) (Charles Ross and Son Co., Hauppauge, phenomena in such systems are related to dispersant adsorption NY). A fineness-of-grind (FOG) gauge (BKY-Gardner U.S.A., kinetics. Laser profilometry, which was used to assess the surface Columbia, MD) was used to determine the average agglomerate topography of as-deposited layers, showed that printed layers had size in the as-milled pastes. smooth surface topography and thus uniform thickness. Finally, the microstructure and electrical properties of sintered capacitor (3) Rheological Measurements devices were evaluated. Ethyl cellulose/terpineol vehicles and PNZT suspensions and pastes were characterized using a controlled stress rheometer II. Experimental Procedure (Carri-med 50, Carri-med Corp. (now TA Instruments), New Castle, DE) in stress viscometry mode. The rheometer was fitted (1) Materials System with either a double concentric cylinder (DG) or cone and plate Lead zirconate niobium titanate (PNZT: Pb(Zr0.52Ti0.48)x- geometry. The rheological behaviors of PNZT suspensions and 24 Nb1ϪxO3) powder, derived via a coprecipitation method, served ethyl cellulose/terpineol solutions were measured using a DG cell, as the ceramic phase in this study. The powder contained 6% which yielded a stress range of 1 ϫ 10Ϫ4–1 ϫ 101 Pa. The 9,25,26 excess lead to lower the required sintering temperature and, higher-viscosity PNZT pastes were characterized using a cone and hence, improve the cofireability of multilayer electroded packages. plate geometry (cone diameter ϭ 2.0 cm, cone angle ϭ 0.5°), The as-received PNZT powders exhibited a trimodal size distribu- which yielded a stress range of 5 ϫ 10Ϫ2–5 ϫ 103 Pa. The tion with characteristic sizes of roughly 2–5, 20, and 45–50 ␮m, as rheological behavior of as-milled pastes was characterized first, determined by particle size analysis (Coulter LS Particle Size followed by a series of measurements as a function of aging time. Analyzer, Fullerton, CA). This powder had a specific surface area After a representative aliquot of paste was tested initially, the 2 of 2.63 Ϯ 0.02 m /g, and an apparent density of 7.740 Ϯ 0.001 remaining paste was allowed to age undisturbed under ambient 3 g/cm , as measured using nitrogen gas adsorption (BET) (ASAP conditions. Subsequent aliquots were then removed and character- 2010 Chemisorption Analyzer, Micromeritics Corp., Norcross, ized at various time intervals. The apparent viscosity of each GA) and helium pycnometry (Ultrapycnometer 1000, Quanta- sample was measured as a function of shear stress in ascending chrome Corp., Boynton Beach, FL), respectively. On attrition order. All rheological measurements were conducted at 22°C. milling, the specific surface area of the powder increased to 3.04 Ϯ Given the low volatility of the solvent, no special precautions 2 0.04 m /g and a bimodal
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