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IEEE TRANSACTIONS ON ELECTRONICS PACKAGING MANUFACTURING, VOL. 31, NO. 2, APRIL 2008 97

Laser Micromachining of Barium Titanate(BaTiO3)-Epoxy Nanocomposite-Based

Flexible/Rollable Capacitors: New Approachfor Making Library of Capacitors

Rabindra Nath Das, Frank D. Egitto, John M. Lauffer, and Voya R. Markovich, Member, IEEE

Abstract—This paper discusses laser micromachining of bariumtitanate (BaTiO3)-polymer nanocomposite thin films. In par-ticular, recent developments on high-capacitance, large-area,thin, flexible, embedded capacitors are highlighted. A variety ofbarium titanate (BaTiO3)-epoxy polymer nanocomposite-basedflexible/rollable thin films ranging from 2 to 25 m thick were pro-cessed on large-area substrates (330 mm 470 mm, or 495 mm607 mm) by liquid coating processes. The electrical performance ofcomposites was characterized by dielectric constant (Dk), capaci-tance, and dissipation factor (loss) measurements. Nanocompositesprovided high capacitance density (10–100 nF in2) and low loss(0.02–0.04) at 1 MHz. Scanning electron microscopy (SEM) mi-crographs showed uniform particle distribution in the coatings.Uniform mixing of nanoparticles in the epoxy matrix results inhigh dielectric ( 3 107 V m) and mechanical strengths( 3700 PSI). Reliability of the capacitor was ascertained bythermal cycling. Capacitance change was less than 5% afterbaking at 140 C for 4 h, and 1100 cycles from 55 C to 125 C(deep thermal cycle). A frequency-tripled Nd:YAG laser operatingat a wavelength of 355 nm was used for the micromachiningstudy. The micromachining was used to generate arrays of vari-able-thickness capacitors from the nanocomposites. The resultantthickness of the capacitors depends on the number of laser pulsesapplied.

Index Terms—Barium titanate, capacitor, dielectric constant,flexible, laser micromachining, polymer nanocomposite.

I. INTRODUCTION

ORGANIC/polymer/nanocomposite materials have at-tracted much attention for building large-area, mechani-

cally flexible electronic devices [1]–[6]. Organic light-emittingdiodes for flat-panel displays appear ready for mass production[7], [8], and significant progress has also been made in organicthin-film transistors [9], and solar cells [10], [11]. There isalso a strong desire to develop new large-scale advanced ma-terials that can meet the growing demand for miniaturization,high-speed performance, and flexibility for microelectronicproducts. An effort in this direction is presented in this paper.

Manuscript received September 5, 2007; revised January 3, 2008. This workwas recommended for publication by Associate Editor A. Shapiro upon evalu-ation of the reviewers comments.

The authors are with the Endicott Interconnect Technologies, Inc., Endicott,NY 13760 USA (e-mail: [email protected]).

Color versions of one or more of the figures in this paper are available onlineat http://ieeexplore.ieee.org.

Digital Object Identifier 10.1109/TEPM.2008.919337

Passives account for a very large part of today’s electronicassemblies. This is particularly true for digital products suchas cellular phones, camcorders, and computers. Market pres-sures for new products with more features, smaller size, andlower cost virtually demand smaller, compact, complex circuitboards. An obvious strategy is to reduce the number of surfacemounted passives by embedding them in the substrate or printedwiring boards. In addition, current interconnect technology toaccommodate surface-mounted passives imposes certain limitson board design, limiting the overall circuit speed. Embeddingpassives is one way to save substrate real estate, reduce parasiticeffects, and improve performance [12].

Among the various passives, embedded capacitors deservespecial attention as they provide the greatest potential benefitfor high-density, high-speed, and low-voltage IC packaging.Capacitors can be embedded into the interconnect substrates(printed wiring board, flex, MCM-L, interposer) to providedecoupling, bypass, termination, and frequency-determiningfunctions [13], [14]. Available commercial polymer com-posite technology is not adequate for high capacitance density,thin-film, embedded passives. Several polymer nanocompositestudies have been focused on processing of high capacitancedensity thin films within small substrates and wafers [15]–[19].One of the important processing issues in thin-film polymernanocomposite-based capacitors is to achieve high capacitancedensity on large coatings. This high capacitance and dielectricconstant on large coatings is also important to commercializelow operating voltage organic transistors for RFID and displayapplications [20]–[22]. Recent interest in the development offlexible electronics such as roll-up displays, e-papers, and key-boards has peaked interest in flexible embedded componentssuch as embedded capacitors.

Barium titanates, BaTiO , have become increasingly impor-tant in the electronics industry, because of their ferroelectric,piezoelectric, and thermoelectric properties. Recent advancesin nanotechnology, understanding and utilizing the exoticelectronic properties of nanomaterials, and organization ofnanostructures into predefined superstructures, promises toplay an increasingly important role in many key technologies[23]–[29]. In this paper, we report novel barium titanate-epoxy-based polymer nanocomposites that have the potential tosurpass conventional composites to produce high capacitancedensity, low loss, flexible, large-area, thin-film capacitors.

1521-334X/$25.00 © 2008 IEEE

98 IEEE TRANSACTIONS ON ELECTRONICS PACKAGING MANUFACTURING, VOL. 31, NO. 2, APRIL 2008

Fig. 1. Schematic representations of (A) the capacitance layer, and (B) lasermicromachining, top view showing a library (arrays) of discrete and variable-thickness capacitors (prior to deposition of metal for upper electrode).

Laser micromachining is becoming increasingly popular forfabrication of advanced electronic packaging substrates, for ex-ample, for drilling of small-diameter vias for electrical intercon-nection between layers. The present study is focused on lasermicromachining of the nanocomposites to produce novel mi-cromachined 3-D capacitors. Micromachining technologies canproduce variable-thickness capacitors by selectively thinningthe capacitor material in desired areas. Discrete capacitors canbe formed by complete removal of capacitor material, forming achannel that isolates individual capacitors from the remainder ofthe capacitance layer. Both types of capacitors (variable-thick-ness and discrete) can be integrated in the same layer. Fig. 1shows a schematic representation of laser micromachining. Ascan be seen in Fig. 1, part of a capacitance layer deposited ona substrate can be converted to arrays of variable-thickness anddiscrete capacitors by laser micromachining.

In the present composite, BaTiO nanoparticles increasethe overall dielectric constant, whereas the polymer matrixprovides better processability and mechanical robustness. Theeffects of particle size, thickness, and loading parameters on theobserved electrical performance of the embedded capacitorsare presented. Uniform mixing of nanoparticles in the epoxymatrix results in highly flexible and rollable thin (2–25 m)film capacitors.

II. EXPERIMENTAL PROCEDURE

A variety of BaTiO epoxy-based nanocomposites were pre-pared by mixing appropriate amounts of BaTiO powder andepoxy resin in solvent. The materials that were required for thepreparation of nanocomposite thin films were epoxy novolacresin sold under the product name “LZ 8213” (Huntsman, SaltLake City, UT), phenoxy resin sold under the product name“PKHC” (Phenoxy Associates, Rock Hill, SC), barium titanatepowder (BaTiO with mean particle size m, surfacearea m g, Cabot Corporation, Boyertown, PA), propy-lene glycol methyl ether acetate (PGMEA) and methyl ethyl

TABLE ILASER PARAMETERS USED FOR MICROMACHINING OF CAPACITOR

MATERIALS HAVING TWO DIFFERENT THICKNESSES

ketone (MEK). In a typical procedure, 38.5 g of an epoxy no-volac resin containing about 35 wt% methyl ethyl ketone and6.5 g of a phenoxy resin containing 50 wt% methyl ethyl ketonewere mixed together with 100 g of barium titanate powder, 13 gpropylene glycol methyl ether acetate, and 12 g methyl ethylketone, and ball milled for three days. A thin film of this mixedcomposite was then deposited on a copper substrate and dried atapproximately 140 C for 3 min in an oven to remove residualorganic solvents. This was followed by curing in an oven at190 C for 2 h. A second electrode of BaTiO -epoxy/Cuwas fabricated by sputtering 0.5–1.0- m-thick Cu film througha shadow mask onto the composite films.

Laser micromachining was performed on an ESI (Electro Sci-entific Industries, Inc., Portland, OR) 5210 Laser Microvia DrillSystem. A frequency-tripled Nd:YAG laser operating at a wave-length of 355 nm was used. The pulse width of the laser was onthe order of 50 ns. The beam was positioned relative to the sur-face of the work piece by coordinated motion of the stage onwhich the sample is mounted ( axis), the optics ( axis), andgalvo mirrors ( and axes). The position of the sample withrespect to the focal plane of the imaged laser beam (along the

axis) can also be adjusted. The spatial distribution of energyin the circular laser spot is homogenized by use of ESI-suppliedoptics. In this instance, beam diameter at the surface of the work-piece was varied by adjusting the relative position of the imagedbeam with respect to the surface of the film. Other salient pa-rameters are listed in the table below. Parameters are defined asfollows.

Rep Rate is the number of laser pulses delivered to theworkpiece per unit time.Power is the average power of the laser.Z-Offset is the relative position of the imaged beam withrespect to surface of the substrate; a negative number indi-cates that the beam is imaged below the surface.Velocity is the speed at which the beam is traced along theprogrammed beam path.Repetitions is the number of times the system traces theprogrammed beam path.Bite Size is the distance the system moves the beamrelative to the workpiece between pulses, along the pro-grammed beam path.

Laser ablation of nanocrystalline BaTiO -filled epoxy was per-formed using the parameters given in Table I. The BaTiO -filledepoxy nanocomposite film was micromachined using a varietyof conditions to form various surface morphologies and capac-itors arrays .

DAS et al.: LASER MICROMACHINING OF BARIUM TITANATE 99

Fig. 2. Larger area SEM images of composite specimens. (A) 120-nm particles.(B) 500-nm particles. (C) 120-nm and 10-nm particles.

Electrical properties (capacitance, Dk, loss) of the nanocom-posite thin films were measured at room temperature usingan impedance/gain-phase analyzer (Model 4194A, Hewlett-Packard). Surface morphology and particle distributions ofnanocomposite films were characterized by a LEO 1550 scan-ning electron microscope (SEM). Micromachining depths offilms were determined by optical microscope and SEM.

III. RESULTS AND DISCUSSION

A real challenge in the development of large-area, thin-filmnanocomposites is the incompatibility that exists between thetypically hydrophilic nanoparticles and hydrophobic polymermatrix, which leads to nanoparticle agglomeration. As a result,inferior coatings with poor performance are obtained. We haveidentified proper surface treatment that results in excellentdispersability [5], [25] of the nanoparticles and good quality,monolithic coatings. Appropriate surface treatment of ceramicsdepends on the specific processing routes. For example, Rameshet al. [19] reported silane treatment of hydro-thermally preparedBaTiO nanoparticles. The finer details of the particles andtheir surface morphologies were investigated using SEM. Fig. 2

Fig. 3. Photographs of (BaTiO )-epoxy polymer nanocomposite films. Thesize of each panel is on the order of 300 mm � 400 mm. (A) 2–25 �m films,where the white film is 25�m thick, and the rest are 2–3�m thick. (B) 8–10-�mfilm. (C) Flexed capacitance layer (inset is at lower magnification). (D) Rolledcapacitance layer (rolled area at top of photo shows backside copper).

shows scanning electron micrographs of nanocomposite thinfilms. Nanoparticles formed uniform dispersion in the epoxymatrix. The particles in the epoxy matrix are so intimately com-pacted that analysis of individual particles is difficult. However,closer observation of the micrographs clearly reveals a uni-form distribution of closely packed, well connected particles.Fig. 2(a) and (b) shows surface morphologies of nanocompositesconsisting of 120- and 500-nm particles. Fig. 2(c) shows surfacemorphology of a nanocomposite prepared from 10- and 120-nmparticles. Here, small particles are well distributed throughoutthe thin film. Use of 10-nm particles produces transparent films.Introduction of small particles improves overall transparencyfor use in photo-definable thin films for discrete capacitors.

Fig. 3 shows a series of large-area thin films. The color ofthe underlying copper substrate is more apparent for the thinnernanocomposite films, as can be seen in Fig. 3(a) and (b). Filmsthat are 2–3 m thick are nearly transparent, and the color ofthe copper substrate is clearly visible. Film transparency reduceswith increasing thickness, and films eventually become the colorof the BaTiO nanocomposite. Fig. 3(c) and (d) shows large-area, thin, flexible capacitors. Capacitors can be bent [Fig. 3(c)]or rolled [Fig. 3(d)] without damaging the structure. For con-ventional composites, rolling or bending will cause structuraldamage such as cracking. The remarkably increased flexibilityof the nanocomposite is due to uniform mixing of nanoparticlesin the polymer matrix, resulting in an improved polymer–ce-ramic interface. Integration of this flexible capacitance layerinto a flexible structure could be useful for developing high-per-formance, multilayer, flexible electronics, such as roll-up dis-plays, e-papers, and keyboards.

Fig. 4 shows cross sections of thin films sandwiched betweentwo metal electrodes. It is possible to make a wide variety offilms with different thickness. Desired thickness of the film canbe achieved by controlling the viscosity of the coatings, com-position, and the number of layers deposited. In the presentprocess, we can easily deposit thin films from about 2 m toabout 25 m. Fig. 4 shows a variety of thin films with average


Fig. 4. Cross sections of thin films. (A) 2 �m. (B) 3 �m. (C) 8.5 �m.

Fig. 5. Dielectric constant (Dk) and dielectric loss versus loading.

thicknesses of 2, 3, and 8.5 m, as typical representative ex-amples. Film thickness uniformity achieved using this coatingprocess is typically on the order of , and depends pri-marily on the planarity of the bottom electrode. The SEM imageof a 2- m film, shown in cross section [Fig. 4(a)], shows welldefined nanoparticles that help maintain such a thin structure.

The electrical properties of 2-100 mm capacitors fabri-cated from nanocomposite thin films showed high capacitancedensity ranging from 10 nF in to 100 nF in , depending oncomposition, particle size, and thickness of the coatings. Fig. 5shows the variation of dielectric constant (Dk) and dissipa-tion factor for nanocomposites with varying filler content. Dkas well as loss increases with increasing filler content. Min-imum Dk (3.7) and loss (0.017) was observed for pure epoxy.Thin-film capacitors fabricated from 40%–60% v/v BaTiOepoxy nanocomposites showed a capacitance density in therange of 40–80 nF in that was stable over a frequency range

Fig. 6. Capacitance density and loss as a function of frequency and thickness.D-8 and L-8 represent capacitance density and loss of 8.5-�m thin film. Sim-ilarly, D-2 and L-2 represent capacitance density and loss of 2-�m thin film.Each data point represents the average of five measurements. Standard devia-tion for these measurements was within 5%.

Fig. 7. Capacitance change with particle size.

of 1–10 MHz. Electrical properties of capacitors fabricatedfrom 70 v/v nanocomposite showed capacitance density ofabout 100 nF in . For a given composition, capacitance densityand dielectric loss increase with decreasing thickness. Fig. 6shows the room-temperature capacitance profile measured at1.0–10 MHz for a BaTiO -epoxy nanocomposite thin film as atypical representative example. It was found that with increasingfrequency (1–10 MHz), the capacitance density decreased.Change in capacitance with frequency was less pronounced inthe case of thicker films. Most of the nanocomposites tested,2.0 m through 25 m thick, for which the BaTiO -based ce-ramic filler concentration was less than 60 vol%, passed 100–Vtest. The outcome of high-voltage testing depends upon themicrostructure and thickness of the film. Nanocomposite film2 to 3 m thick and consisting of 120-nm particles [Fig. 2(a)]passed 100 V, whereas 15- and 25- m-thick films passed 500-Vand 1000-V tests, respectively. Nanocomposites films 2 to 3 mthick and consisting of 120- and 10-nm particles [Fig. 2(c)] easilypassed 150-V test. This is high enough for the nanocompositeto serve as an insulating material for embedded capacitors. Sim-ilarly, tensile strength with 1 oz copper for all nanocompositesbelow 60 vol% was found to be higher than 3700 PSI. Rameshet al. [19] reported over 200 nF in capacitance density from asubmicrometer surface-modified nanocomposite film obtained


Fig. 8. Change in capacitance after baking at 140 C for 4 h, and thermal shockup to 1100 cycles (�55 C to 125 C)1 for 1-cm diameter capacitors.

Fig. 9. Micromachined nanocomposite-based capacitor array. (A) Optical pho-tograph. (B) SEM micrograph of array machined with 20 pulses. (C) Micrographof array machined with 50 pulses. (D) Micrograph of array machined with 200pulses.

from a spin coating process. The material set used in the presentinvestigation can also produce high capacitance from a submi-crometer thick spin-coated film deposited on a small copper

Fig. 10. (A) Schematic representations, cross sectional views, showing arraysof discrete and variable-thickness capacitors. (B) Variation of depth with thenumber of laser pulses for a BaTiO nanocomposite (Dk = 30). Theoreticalcalculation of capacitance with number of laser pulses for nanocomposite thinfilm (Dk = 30, thickness = 15 �m).

substrate. However, film quality degrades when deposited on alarge substrate.

A variety of BaTiO nanoparticles were used to preparenanocomposites. For example, we have used hydrothermallyprocessed 65-nm and 120-nm particles, as well as sol-gel pro-cessed 500-nm BaTiO particles. All nanocomposite capacitorsfabricated from BaTiO with average particle size below 700nm show stable high capacitance. It is difficult to establish adirect correlation between particle size and capacitance densityin this work because the different sized BaTiO nanoparticleswere derived through different ceramic processing routes,resulting in different dielectric properties and capacitance [30].However, we could establish that at low filler content, finer par-ticle composites show significantly higher capacitance density.Fig. 7 represents electrical properties of capacitors fabricatedfrom different sized nanoparticle composites containing around40% v/v BaTiO . Finer particles with higher surface area mayhave better particle to particle contact for improving the overallproperties of the nanocomposites.

Embedded passives exhibit improved reliability by virtue ofsolder joint elimination. However, they also introduce other po-tential defects such as cracks, material mismatch, and delami-nation. Embedded capacitors are of little value unless they cansurvive the same rigors of testing that modules or boards wouldreceive. Reliability of the composites in the present study wasascertained by thermal cycling. Capacitors, in some cases, ex-hibited large changes (up to 10 ) after 1000 cycles of DTCtesting ( 55 C to 125 C, 10-min soak). This large capacitancechange could be due to the lack of copper annealing of unassem-bled boards. This was overcome by baking prior to thermal cy-cling. Fig. 8 shows capacitance change after baking at 140 C


Fig. 11. Laser micromachining produces a discrete capacitor from a capacitance layer. (A) Optical photograph. (B) Optical 3-D photograph of another sample.

for 4 h, and thermal shock up to 1100 cycles ( 55 C to 125 C)for 1.0-cm diameter capacitors. The reduced change in capaci-tance with baking indicates that copper annealing could possiblystabilize capacitors prior to thermal cycling.

Fig. 9(a) shows an optical photograph, top view, of lasermicromachined capacitor arrays. The basic structure consistsof two layers: the micromachined capacitor and the sub-strate. Using this method, fully micromachined capacitors canbe consistently generated. SEM micrographs are shown inFig. 9(b)–(d) for a series of arrays machined using varyingnumbers of laser pulses. The depth of microfabricated capac-itors varies from 4 to 70 m, depending on the number oflaser pulses. The surface smoothness of the ablated areas thatdefine the laser micromachined capacitors depends upon theuniformity of the spatial energy distribution of the laser beam.Although the smoothness of the ablated regions shown in Fig. 9are not optimum, adjustment of the optics used in the presentstudy could produce a more homogeneous energy profile forthe beam. Alternatively, excimer laser micromachining sys-tems have been shown to produce very uniform ablation overreasonably large areas.

Fig. 10(a) and (b) shows variation of the depth of the mi-cromachined areas with the number of laser pulses. Fig. 10(b)also shows possible capacitance density nF in for a 15- mcapacitor film assuming a dielectric constant of 30. The thick-ness of the capacitors decreases with an increasing numberof laser pulses. It is clear from Fig. 10(a) and (b) that as thedepth of the micromachined area is increased (thickness ofthe remaining dielectric reduced), the corresponding capaci-tance increases. In other words, micromachining can generatecapacitor libraries (arrays) with variable capacitance density.Epoxy BaTiO nanocomposite layers with dielectric constantaround 30 have been fabricated. The micromachined depthfrom the top nanocomposite surface has been measured. Theaverage depth for 20 laser pulses is 5 m, and for 50 pulsesthe average depth is 12 m. A theoretical capacitance densitycalculation was made considering a total nanocomposite layerthickness of 15 m [Fig. 10(b)]. Actual measurement of capac-itance values for these variable-thickness capacitor structuresusing top and bottom electrodes has not been performed.Increasing the number of pulses eventually results in completeremoval of the dielectric. This would be useful for makingdiscrete capacitors from a capacitance layer. Fig. 11 shows arepresentative example of discrete capacitors formed from alarger capacitance layer. Fig. 11(b) represents a 3-D opticalmicrograph where the capacitor dielectric was removed to thepoint where the bottom electrode was exposed.

IV. CONCLUSION

A thin-film technology based on BaTiO -epoxy polymernanocomposites was developed to manufacture reliable,high-performance, large-area, flexible/rollable, thin-film capac-itors. It was possible to produce very thin nanocomposite films,in the range of 2 m. The remarkable flexibility and thicknessof the nanocomposite is due to uniform mixing of nanoparticlesin the polymer matrix, resulting in improved polymer-ceramicinterfaces. Size and loading level of nanoparticles were foundto have significant influences on the dielectric and mechanicalproperties of the nanocomposite system. Capacitors experi-enced less than 5% loss over a frequency range 1–10 MHz. Afrequency-tripled Nd:YAG laser operating at a wavelength of355 nm was used for the micromachining study. This microma-chining technique can be used to prepare capacitors of variousthickness from the same capacitance layer, and ultimately canproduce variable capacitance density, or a library of capacitors.The process is also capable of making discrete capacitors froma single layer of capacitance material.

ACKNOWLEDGMENT

The authors would like to thank S. Hurban, M. Shay,G. Kohut, and D. Thorne for their contributions.

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Rabindra Nath Das received the M.S. and Ph.D. de-grees in chemistry from the Indian Institute of Tech-nology, Kharagpur.

He is a Senior Advisory Technologist at EndicottInterconnect Technologies, Inc., Endicott, NY. Priorto this, he was a Visiting Scientist in the MaterialsScience and Engineering Department, Cornell Uni-versity, Ithaca, NY. His research work focuses in thearea of nanotechnology where he has over ten yearsof experience . He has developed a number of ad-vanced nanomaterials for applications ranging from

interconnect to lasers to passives to magnetics. He has written one book chapter,over 40 nano-based technical papers, and several issued/pending U.S. patents.

Frank D. Egitto received the B.A. and M.A.degrees in physics from Binghamton University,Binghamton, NY.

He is a Senior Advisory Technologist at EndicottInterconnect Technologies, Inc, Endicott, NY. Hehas 30 years of experience working in the electronicsindustry. Previously, he was a Senior Engineerfor IBM Corporation in the design, process, mate-rials, and assembly development group for organiclaminate products. Earlier positions included de-velopment of plasma equipment and processes at

Texas Instruments, Inc., Dallas, TX, and Applied Materials, Inc., Santa Clara,CA. He is a coauthor of six book chapters and over 50 technical papers, andholds 60 U.S. patents. His areas of expertise include plasma interactions withmaterials, laser ablation, modification of polymers with ultraviolet radiation,and advanced packaging.

John M. Lauffer received the B.S. degree in photo science and instrumentationfrom the Rochester Institute of Technology, Rochester, NY.

He is a Senior Advisory Technologist at Endicott Interconnect Technologies,Inc, Endicott, NY. He has 25 years of experience working in the electronicsindustry which include four years at IBM Corporation, East Fishkill, NY, insemiconductor manufacturing. He worked for IBM Endicott for 20 years and hasover 25 years experience in electronic packaging development including PWBand semiconductor packaging process and product development. His areas ofexpertise include embedded passives and actives, power packaging, fine-pitchC4 packages, and new technologies. He serves on the Technical Advisory Boardof the Georgia Institute of Technology Packaging Research Center, Atlanta. Heholds 93 issued U.S. patents and has published numerous technical papers.

Voya R. Markovich (M’04) received the M.S. de-gree in chemistry from The Polytechnic Institute ofNew York in 1980.

He is Senior Vice President and Chief TechnologyOfficer at Endicott Interconnect Technologies, Inc.,Endicott, NY. He was previously a Senior TechnicalStaff Member with IBM Corporation and SeniorManager of the WW materials, processes, andassembly development group for organic laminateproducts. He was elected to the IBM Academy ofTechnology in 1997, and holds 185 U.S. patents.

His areas of current active interests are in development of new processes andmaterials for integrated actives, passives, optical, and RF for advanced systemsintegrated electronic packaging.

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