Cellular Ceramics / p2
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2.2 Honeycombs 77
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Fig. 11 Viscosity curves from the literature: Top to bottom:
GE fused silica (low-hydroxyl) [116], Corning 7940 (HPFS glass, ca. 0.16 wt % OH) [117], 7971 (ULE glass, ca. 0.16 wt % OH) [117], Pyrex 7761 (potassium borosilicate) glass [118].
glass honeycomb was then heated at the middle of its length and then drawn down to make a honeycomb funnel. A balance of temperature gradients and channel pressure [21, 22, 52] and axial tension controlled the draw geometry. The funnel was cut from the draw; it is the root and not the gob. The resulting honeycomb funnel was ground and polished to have a macro base with about 90 channels per square centimeter, a micro top with about 2000, and web thicknesses of about 200 and 20 mm, respectively (see Fig. 10).
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Fig. 12 Two powders: Pyrex 7761 glass particles with a 12 mm mean diameter and spherical ULE soot with a 0.2 mm mean diameter.
78 Part 2 Manufacturing
This honeycomb funnel is used as an ink reservoir for applications in combinatorial chemistry and biology [119]. The inks are loaded into the macro-array of openings from where they are conveyed through the channels by capillary action resulting from the axial diameter gradient of the funnel. The net force from surface tension is greater than that of gravity on the slugs of ink, so the inks move from the macro to the micro end of the funnel to form a micro array of ink menisci. A matching pin array dips into this menisci array, picks up and transfers a drop array, and prints it on a slide.
This same Pyrex preform can be drawn down further to make a honeycomb fiber (see Fig. 9). However, the extent to which this Pyrex preform can be hot-drawn is limited by the stone, grinding, and metal wear debris from all the previous Pyrex processing steps.
An example at the other end of the glass spectrum is the production of high-purity fused silica honeycomb by paste-extrusion of high-purity fused silica (HPFS ) soot powder [120–125]. This work was an interdepartmental effort at Corning Inc. to merge existing technologies of soot generation, honeycomb extrusion, beneficiation, and sintering for a cost-effective manufacture of clear honeycomb structures [126, 127].
The strategy was to use existing materials (standard HPFS soot and binder, about 10 % Methocel solution [120–125]) and processes (mixing and extrusion equipment) to create clear honeycombs without making any significant changes to the current processes, and so this approach differed substantially from the literature on silica paste extrusion. Current approaches in the literature use the least amount of polymer [127–130] to make a simple final shape: a rod or a tube. These objects have much thicker diffusion distances (ca. 1 mm) than the honeycomb web (ca. 0.1 mm) described here, and so the literature objects are more difficult to dry, debind, and clean. This honeycomb experiment was to determine whether the easy-cleaning thinness of the honeycomb webs was sufficient to compensate for the rest of the process, so as to allow the production of clear honeycombs from the existing infrastructure.
Silica soot is made by flame combustion of silica precursors. It is an aerosol process that grows a particle up to the desired diameter. Unlike the above Pyrex glass powder, it is a clean process. The precursors are made by digesting silica particles to synthesize silicon tetrafluoride [131], silicon tetrachloride [132], and now environmentally friendly organosilicon precursor molecules. These are purified and flame hydrolyzed to make pyrogenic silica soot particles [133]. Other compositions can be made, too (e.g., ULE 7–8 % titania glass [134]). The flame combustion process controls the nucleation and growth (coalescence of molten particles), and can generate small soot particles with a desired shape (fractal to spheroid) and size (0.1–1.0 mm diameter) without grinding. The soot powder production process differs from the commercial process for making HPFS and ULE glass, which is a glassmaking process in which the molten/viscous soot particles are directly deposited and sintered, layer by layer, to make boules for making fibers [135] and blanks for making lenses and mirrors [133, 134]. In soot powder production, the soot particles are quenched to prevent consolidation and collected in a bag house. The bagged soot particles are free of hard agglomerates. Silica soots are also commercially available from Cabot (Cabosil powder) and Degussa (Aerosil powder); alumina and carbon soots are also available.
2.2 Honeycombs 79
The soot particles used in this honeycomb experiment were beautiful spheres (Fig. 12). These soot particles were easily made into an extrudable paste and were plastically extruded into the shape of a honeycomb [123–126]. The honeycomb was dried, debinded, and purified by a beneficiation with hot chlorine gas, so that only silica remained [91, 92, 115].
The goal was to purify the honeycomb with the aid of all of its accessible surface area. The thin porous webs of the honeycomb geometry were perfect for chlorine beneficiation for the removal of iron and sodium resulting from the extrusion process: wear debris from the mixing equipment and ash from the binder, respectively. The honeycomb geometry is optimal for this beneficiation process because the diffusion length is half a web thickness, which is very small compared to the radius of the honeycomb substrate or boule. The honeycomb channels are like “superhighways” to the torturosity of the porosity of the webs. The hot chlorine gas reacts/scavenges for rogue cations to form volatile substances such as iron chloride, sodium chloride, and so on. It is important to minimize the trace sodium content to prevent devitrification of the silica during sintering [115, 136].
The debinding process window was a bit larger for HPFS soot powder than it was for the above Pyrex example. Here, binder removal (< 600 C) occurred at a much lower temperature than surface area removal (sintering, > 1200 C), and so there was sufficient temperature difference to carry out the purification step between these two processes: between the opening/growing of porosity by drying and debinding and the closing/shrinking of porosity by viscous sintering in fast diffusing helium [113, 114]. These processes were very dependent on permeablility.
Once the honeycomb was sufficiently purified, the temperature was ramped up to sinter the silica particles to full density and make a clear honeycomb. The sinter process was fast to avoid devitrification [137, 138] and gravitational slump. Fast is not a problem for silica glass, because of its extremely low CTE (0.5 ppm K–1), and it is extremely resistant to thermal shock.
Large HPFS and ULE honeycombs (120 0 120mm 0 25mm) have been sintered. They were made by this paste extrusion process (see Figs. 4 and 13) as an alternative to the present production method of water-jet cutting of a honeycomb from a solid blank of glass in order to make lightweight cores for telescope mirrors [14, 121]. These honeycombs were made from a soot with a particle size distribution which is favorable to both crack-free drying (a problem if the particles are too small) and slump-free firing (a problem if the particles are too large). The same particle surface curvature that drives sintering also drives cracking during drying.
Smaller particles sinter faster to full density at a lower temperature than do larger particles, because the energy released from the reduction of surface area and curvature drives the sintering process [115]. In the final stage of sintering to full density, the closed pore size distribution should scale to the original particle size distribution, to the original interstitial size distribution. Sintering time tsint is a function of particle size d, particle packing, surface energy c, and viscosity g (see Fig. 11). The sintering model is rate-controlled by the energy released by the reduction of surface area (shrinkage) and consumed by viscous dissipation [93, 115, 139, 140]:
tsint = . dg/c. |
(1) |
80 Part 2 Manufacturing
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Fig. 13 High purity fused silica honeycombs.
The other viscous processes which occur simultaneously are loss of channel area (open frontal area, OFA) and gravitational slump. Roughly, the time dependence for slump is a function of gravity g, density , viscosity g, and height h of the honeycomb (Fig. 14). The slump time tslump is the time required to thicken the web at the base of the honeycomb by 5 % (e = 0.05) [141]:
tslump= (4 eg)/( gh). |
(2) |
The other time-dependent process is devitrification: nucleation and growth [117, 137, 138]. The goal is to sinter the honeycomb before the nucleation and growth of crystobalite can occur. This requires low-temperature sintering with small particles to avoid both slump and/or devitrification [115].
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Fig. 14 Slump as a function of height for HPFS glass consolidated in helium. As expected, shorter honeycombs have less gravitational pressure and less slump flow.
Figure 15 shows sinter time (Eq. 1), induction time [117] and slump time (Eq. 2) as a function of temperature. It defines a region of process space in which it is pos-
2.2 Honeycombs 81
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Fig. 15 Sintering, induction, and slump times as a function of temperature for HPFS glass as extrapolated from Mazurin’s data on Corning 7940 glass (ca. 0.16 wt % OH) [117]. Two sintering curves are shown: 0.1 and 0.5 mm particle size d (Eq. 1). Two slump curves are
shown: 10 and 50 mm honeycomb height h (Eq. 2). The slump time was calculated for a 5 % thickening at the base (e = 0.05). The sintering, slump, and devitrification times would be longer for drier glass and for more viscous glass, such as the GE fused silica in Fig. 11.
sible to sinter silica soot honeycombs clear without bubbles, crystals, and slump. Decreasing the particle size, temperature, and height/ thickness of the honeycomb puts the process in a more optimal space. But this is only true if there are no unintended pore formers that result in pores and consequential bubbles which are much larger than the soot particles. To remove these bubbles requires a higher temperature and longer time than is predicted from the size of the soot particles, and this higher temperature and longer time result in some slumping of the honeycomb during sintering. Get rid of the unintended pore formers during batching and mixing [65, 66, 69], and bubble-free sintering will occur at a lower temperature and in a shorter time with less slump and less devitrification (crystallites).
Clear honeycombs have been made by this paste extrusion process (see Figs. 13 and 14), and these have demonstrated the robustness of the honeycomb geometry (thin porous webs and fast channels) for the removal of water, polymer, sodium, iron, and finally the surface area of porosity.
Currently, efforts in soot extrusion are directed at making a bubble-free honeycomb which is free of microstructure but not free of channels. This honeycomb is the preform from which a honeycomb fiber can be hot drawn. In the previous exam-
82 Part 2 Manufacturing
ple we were trying to minimize slump from bulk viscous flow due to gravity. In this example we want slump – in particular, hot viscous draw – in order to make a honeycomb fiber. The fiber drawing process (> 1900 C) requires more thermal processing time than does simple sintering, so it has a greater probability of devitrification, which causes the honeycomb to fail to draw. Devitrification can be prevented by melting all of the crystobalite nuclei in the preform, and this is done by ramping its temperature to above the melting point of crystobalite (ca. 1725 C).
Currently, silica photonic crystal fibers are routinely hot drawn from preforms made by tube bundling and fusing. The resulting honeycomb fibers have channel diameters on the order of a micrometer with web thicknesses of less than 200 nm (see Fig. 2). These are some of the finest and highest aspect ratio objects ever made. However, the same will be possible for preforms made by paste extrusion, too [98]. This is our current focus. After all, no one wants to bundle tubes if they do not have to, and it would be satisfying to demonstrate:
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The surface area lost in sintering is regained in hot draw. |
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A submicrometer web thickness that can be made from submicron soot par- |
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ticles in the roundabout way of paste extrusion. |
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A preform made by paste extrusion with no irreductible microstructure, a |
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preform which has only the reducible synthetic meso fi micro fi nanostruc- |
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ture of channels. |
2.2.6
Summary
Our quest for honeycombs with higher cell densities began with the porous cordierite honeycomb with a few hundred channels per square centimeter and ended with a fused silica photonic crystal fiber with almost a billion channels per square centimeter. Along the way, the following observations were made:
. Ceramic and glass honeycombs can be made by paste extrusion, which is an effective way to mechanically create porosity: geometric porosity and geometric surface area. The porous honeycomb geometry is beneficial to its own fabrication (drying, debinding, beneficiation, and firing).
. The paste-extruded honeycomb is a convenient way to arrange particles for easy access for fast chemical and thermal diffusion. Large honeycomb objects can be made with very short effective diffusion distances.
. Nonporous honeycombs start off as being porous when made by paste extrusion. The process of sintering to full density follows the path of open porosity to closed porosity to no porosity. The initial porosity gives access to the surface area of the particles for beneficiation and gas exchange before the porosity closes, after which corrections cannot be easily made.
. Creating a porous honeycomb preform with a microstructure much finer than its web thickness is a prerequisite for reduction extrusion and hot draw.
2.2 Honeycombs 83
Sintering a glass honeycomb to have no microstructure is prerequisite for the hot drawing of a honeycomb fiber.
. A glass honeycomb can be hot drawn down to make a honeycomb funnel and a honeycomb fiber, the limiting case being a photonic crystal fiber.
This chapter described the manufacturing of honeycombs by paste extrusion, but in so doing, it necessarily described the manufacturing of porous ceramic and glass microstructures, because to make a good ceramic or glass honeycomb by paste extrusion, one must have a composition and process to make a good porous microstructure, which is a prerequisite to obtaining the final web microstructure of the honeycomb.
An excellent set of tables describing ceramic honeycombs can be found on the web at www.dieselnet.com/tech/dpf_wall-flow.html’intro [96] and http://customer2.corning.com/environmental/ [11].
Acknowledgements
The work presented in this chapter was carried out at Corning Incorporated with a wide cross section of expertise: P. Bardhan, D. Beall, N. Borrelli, C. Booker, A. Buchtel, P. Cimo, T. Dannoux, G. Dillon, J. Fajardo, C. Fekety, M. Fischer, E. Funk, D. Gokey, E. Hale, L. Holleran, J. Humphrey, C. He, K. Hrdina, T. Johnson, K. Koch, R. Layton, R. McCarthy, G. Merkel, A. Olszewski, P. Oram, S. Rajamma, A. Roselstad, D. St. Julien, E. Sanford, N. Venkataraman, J. Wang, M. Wasilewski, J. M. Whalen, D. Witte, J. Wight, S. Wu, R. Wusirika, K. Zaun.
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