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RAPID COMMUNICATIONS Resonant Infrared Pulsed-Laser Deposition Of RAPID COMMUNICATIONS This section is reserved for short submissions which contain important new results and are intended for accelerated publication. Resonant infrared pulsed-laser deposition of polymer films using a free-electron laser Daniel M. Bubb,a) J. S. Horwitz, J. H. Callahan, R. A. McGill, E. J. Houser, and D. B. Chrisey Naval Research Laboratory, Washington, DC 20375 M. R. Papantonakis and R. F. Haglund, Jr. Department of Physics and Astronomy and W. M. Keck Foundation Free-Electron Laser Center, Vanderbilt University, Nashville, Tennessee 37235 M. C. Galicia and A. Vertes Department of Chemistry, George Washington University, Washington, DC 20001 ͑Received 12 March 2001; accepted 29 May 2001͒ Thin films of polyethylene glycol ͑MW 1500͒ have been prepared by pulsed-laser deposition ͑PLD͒ using both a tunable infrared ͑␭ϭ2.9 ␮m, 3.4 ␮m͒ and an ultraviolet laser ͑␭ϭ193 nm͒.A comparison of the physicochemical properties of the films by means of Fourier transform infrared spectroscopy, electrospray ionization mass spectrometry, and matrix-assisted laser desorption and ionization shows that when the IR laser is tuned to a resonant absorption in the polymer, the IR PLD thin films are identical to the starting material, whereas the UV PLD show significant structural modification. These results are important for several biomedical applications of organic and polymeric thin films. © 2001 American Vacuum Society. ͓DOI: 10.1116/1.1387052͔ I. INTRODUCTION physical characteristics of the bulk PEG material, whereas Polyethylene glycol ͑PEG͒ is a technologically important the UV PLD deposited PEG materials do not. In addition, the polymer with many biomedical applications.1 Examples in- results also show clearly that the mechanism of IR PLD is clude tissue engineering,2 spatial patterning of cells,3,4 drug fundamentally different than UV PLD. These results are very delivery coatings,5,6 and antifouling coatings.7 In these appli- important in the context of such biomedical technologies as cations, a need exists for a technique capable of depositing drug-delivery coatings and in vivo applications where it is thin, uniform, and adherent coatings of PEG. Whereas in crucial to effect transfer of polymeric coatings without sig- some cases it is acceptable to deposit chemically modified nificant chemical or physical modification to the polymer. PEG polymeric material,7,8 in drug delivery and in vivo ap- plications it is important that there is no difference in the II. BACKGROUND chemical and structural properties of PEG films compared Pulsed-laser deposition has been an extremely successful with the bulk polymer. technique for depositing thin films of a large variety of inor- In this article, we report the first successful pulsed-laser ganic materials.9 PLD has also been applied to the growth of deposition ͑PLD͒ of thin polyethylene glycol ͑PEG͒ films thin polymeric and organic films, albeit with varying degrees using a tunable IR source in the midinfrared. A direct com- of success. For example, when PLD is used to fabricate parison is made between PEG films grown with an UV laser chemical sensors from polymer–carbon nanocomposites, ͑193 nm͒ and a tunable infrared laser. The IR laser is tuned both the molecular weight distribution and the chemical to be resonant with the O–H ͑2.9 ␮m͒ or C–H ͑3.4 ␮m͒ structure of the polymeric material are substantially altered, stretch mode in PEG. The films were characterized by means but the required functional groups for the sensor remain of Fourier transform infrared spectroscopy ͑FTIR͒, electro- intact.10 In other cases, the damage caused during UV abla- spray ionization mass spectrometry ͑ESI͒, and matrix- tion is limited to a reduction in the molecular weight with the assisted laser desorption and ionization time-of-flight mass chemical structure remaining intact.11 It has been shown that spectrometry ͑MALDI͒. The comparisons show that when certain polymers such as poly-methyl methacrylate the IR laser is tuned to a resonant feature in the organic ͑PMMA͒, poly-tetraflouroethylene ͑PTFE͒, and poly-␣- material, the IR PLD films retain the optical, structural, and methyl styrene ͑PAMS͒, undergo rapid depolymerization a͒ during UV laser ablation, with the monomer of each strongly Author to whom correspondence should be addressed; ASEE/NRL Post- 12–14 doctoral Fellow; present address: Seton Hall University, Department of present in the ablation plume. For these polymers, the Physics, 400 South Orange Ave., South Orange, NJ 07079; electronic mail: molecular weight distribution of the deposited thin-film ma- [email protected] Õ Õ Õ Õ Õ Õ 2698 J. Vac. Sci. Technol. A 19„5…, Sep Oct 2001 0734-2101 2001 19„5… 2698 5 $18.00 ©2001 American Vacuum Society 2698 2699 Bubb et al.: Resonant IR pulsed-laser deposition 2699 terial can be increased by simply raising the substrate such an approach has been successfully applied to the temperature.15 Therefore, even in the most successful cases matrix-assisted laser desorption and ionization mass spectro- of UV PLD of polymers there is an intense interaction be- scopic technique.31 tween the target material and laser resulting in chemical modification of the polymer during ablation. If repolymeriza- IV. EXPERIMENT tion is incomplete at the substrate, this can lead to both a reduction of molecular weight and a change in chemical The light source of the IR PLD films was the W. M. Keck structure. Foundation Free-Electron Laser ͑FEL͒ at Vanderbilt Univer- The mechanism for UV ablation of organic materials has sity. The Vanderbilt FEL produces a 4 ␮s macropulse at a been debated for some time. In the photochemical model of repetition rate of 30 Hz; the macropulse in turn comprises ablation,16,17 absorption of an UV photon leads to direct some 11 400 1 ps micropulses separated by 350 ps. The en- bond dissociation and fragmentation of the organic molecule. ergy in each micropulse is of order 10 ␮J, so that the peak In the photothermal model,18,19 the energy absorbed by the unfocused power in each micropulse is very high ͑ϳ107 W͒. UV photon is rapidly converted to heat and the polymer The average power of the FEL is of order 2–3 W and it is undergoes pyrolysis. Rapid pyrolysis results in depolymer- continuously tunable over the range 2–10 ␮m. ization of target material in the plume; repolymerization oc- The characteristics of the laser are discussed in greater curs on the substrate, possibly initiated by the pressure of detail elsewhere.31,32 For the IR PLD films the macropulse free radicals.12–15,19 fluence was between 2 and 9 J/cm2, the target substrate dis- Ablation may also proceed through the absorption by tance was 3 cm, and the spot size was 0.0022 cm2. The extrinsic20 or laser-generated impurities such as color background pressure in the chamber during deposition was Ϫ Ϫ centers.21 Extrinsic impurities may absorb the light directly between 10 5 and 10 6 Torr. A typical deposition rate for resulting in local heating by electron–phonon coupling, or these conditions ͑␭ϭ3.4 ␮m, fluence ϭ 6.8 J/cm2, spot size the interaction length may be increased through scattering, ϭ 0.0022 cm2͒ was 140 ng/cm2 macropulse. Amorphous resulting in absorption by the polymer. Thin films or poly- PEG is a soft material, thus making contact profilometry styrene doped with anthracene,22 and polyethylene oxide problematic. For a film deposited using 10 000 macropulses, with a ZrO additive23 have been successfully ablated in this this corresponds to a film thickness of approximately 10 ␮m way. using the bulk density of amorphous PEG ͑Ref. 33͒ and the In general, the interaction between organic molecules and areal density measured after deposition. UV light is very complicated, occurring as it does with ex- Films were also deposited using nonresonant radiation Ϫ treme rapidity24 and through many different excitation- from the FEL. The laser was tuned to 3.3 ␮m ͑3030 cm 1), relaxation pathways.25 This certainty seems to present a at which PEG is nonabsorbing. The fluence was 6.1 J/cm2 number of challenges to polymer film growth using UV la- and all other experimental parameters were the same as in sers. the resonant ͑3.4 ␮m, 2.9 ␮m͒ cases. The deposition rate was 68 ng/cm2 macropulse. We observe that there are significant differences in the infrared absorbance spectrum, yet the ESI mass spectrum is nearly identical to the resonant IR case. It III. MOTIVATION FOR THIS EXPERIMENT „ … is possible that the material is modified in such a way as to For organics, an alternative approach to PLD with UV be difficult, if not impossible, to detect by ESI or MALDI. It lasers is matrix-assisted pulsed-laser evaporation ͑MAPLE͒, is also possible that the ablation proceeds due to a multiple in which roughly 0.1% to 1% of a material to be deposited is photon process, which is certainly possible at the high flu- dissolved in an appropriate solvent and frozen to form an ences at which the FEL operates. Further study is needed in ablation target.26–28 The UV laser light interacts mostly with order to clarify these points and the results will be discussed the solvent and the guest material is thus ablated much more elsewhere. gently than in conventional PLD. While this can result in For purposes of comparison, an ArF excimer laser smooth uniform films suitable for a variety of applications, it ͑Lambda Physik 305; ␭ϭ193 nm; FWHMϭ30 ns͒ was used nevertheless requires that the polymer of interest be soluble for UV PLD. The experimental setup has been described in in a noninteracting solvent. The one serious disadvantage to detail previously.26 The laser was operated at a repetition rate MAPLE is that the deposition rate is about an order of mag- of 10 Hz with the fluence varied between 150 and 300 nitude lower than in conventional PLD.26,27 mJ/cm2.
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