Development and Application of On-Wafer Small Angle X-Rayscattering for the Quantification of Pore Morphology in Low Kporous Silk Semiconductor Dielectrics

Landes, Brian; Kern, Brandon; Stokich, T. M.; Niu, Jilei; Yontz, Dorie J.; Radler-Carol, Mike; Ouellette, M.; Lucero, S.; Hahnfeld, Jerry L.; King, D. F.; Quintana, J. P.; Weigand, Steve

doi:10.1557/proc-766-e9.10

Cited by 4 publications

(4 citation statements)

References 8 publications

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“…The porous organic low- k material especially prepared for this research was based on a developmental version (V7) of Dow Chemical's SiLK 47 polyphenylene precursor. Such materials have been described in detail elsewhere. − The samples in question contained a deuterated porogen that degrades completely at 430 °C. All the samples discussed here (150A, 400A and 43040A) underwent a bake at 150 °C for 24 h. Sample 150A did not undergo further processing.…”

Section: Methodsmentioning

confidence: 99%

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SANS and XRR Porosimetry of a Polyphenylene Low-k Dielectric

et al. 2006

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Nanometer scale porosity is introduced into low-dielectric constant ("low-k") materials to achieve permittivities less than 2.0. X-ray reflectivity (XRR) and small-angle neutron scattering (SANS) are complementary methods for characterizing pore size distributions (PSD). In this paper, the PSD in a polyphenylene low-k material is characterized via solvent vapor porosimetry experiments using both SANS and XRR to probe solvent permeation, and the significant differences in these techniques are described and discussed. Previous work assumed a singlemode PSD, but the solvent porosimetry measurements indicate the presence of a bimodal PSD. A PSD maximum is observed at about 5 Å via XRR porosimetry while SANS seems less sensitive to structure at high q (relatively small size scales). A sorption/desorption hysteresis suggests the presence of "ink-bottle" pores in which solventfilled small pores block the desorption from large pores. A combination of these techniques is also able to describe the structure in a film with partially developed porosity that contains matrix, pores, and porogen.

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Section: Methodsmentioning

confidence: 99%

“…Such materials have been described in detail elsewhere. [31][32][33][34][35] The samples in question contained a deuterated porogen that degrades completely at 430 °C. All the samples discussed here (150A, 400A and 43040A) underwent a bake at 150 °C for 24 h. Sample 150A did not undergo further processing.…”

Section: Introductionmentioning

confidence: 99%

SANS and XRR Porosimetry of a Polyphenylene Low-k Dielectric

et al. 2006

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“…Additionally, a large number of standard environments are available on-site for regular use. The first sample environment along the path of the beam is a large 12 inch, 6-way cross vacuum chamber (Landes et al, 2003;Quintana, 2003). The chamber is equipped with a perforated wheel mounted normal to the beam, which can be loaded with static samples for small or wide angle data collection.…”

Section: Id-d Beamline Descriptionmentioning

confidence: 99%

D-49 Invited—Flexibility and High Throughput: Supporting SAXS users at a Joint Industrial Academic Beamline

Weigand¹,

Stillwell²,

Keane³

et al. 2008

Powder Diffr.

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From its inception, the DuPont-Northwestern-Dow Collaborative Access Team (DND-CAT) at the Advanced Photon Source has had to adapt to the changing needs of industry as well as a diverse academic user base. This has resulted in a sector with support for a broad range of techniques and sample environments. Among the techniques supported at DND-CAT are small and wide angle scattering, reflectivity, spectroscopy, tomography, and powder diffraction. The D station on the insertion device line at DND-CAT (5ID-D) is a general purpose hutch that is primarily used for small angle X-ray scattering (SAXS). Approximately 10 12 photons/sec can be delivered to a .04mm 2 spot using multiple sets of slits with pinhole camera geometry. Scattering can be measured down to 2θ = 0.014° on a 10m long camera with 1.5Å to 0.7Å radiation. Many 5ID-D users are polymer scientists, thus standard techniques supported include SAXS and WAXS image collection simultaneous with thermal, extension/compression, shear, or calorimetric data. Often, an individual user will come with arrays of several sample types requiring different environments and/or camera configurations to fully analyze. This paper describes how the joint goals of flexibility and high throughput are balanced at 5ID-D for small and wide angle X-ray scattering. A unique simultaneous SAXS/WAXS detector system for collecting anisotropic X-ray scattering is described. Also a method for calibrating sample to detector distance for long tanks using a silicon diffraction grating is presented.

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“…This work investigates pore formation in a polyphenylene low- k dielectric based on pyrolysis of a porogen in a polyphenylene oligomer matrix . Several techniques, such as ellipsometry and small-angle X-ray scattering, have been used to characterize such materials. , One unique aspect of this research is the description of the nanoscale structure at various stages of pore formation through the use of a deuterated porogen. The use of a deuterated porogen provides exceptional neutron scattering contrast in the porogen−oligomer system.…”

Section: Introductionmentioning

confidence: 99%

Nanopore Formation in a Polyphenylene Low-kDielectric

Silverstein¹,

Shach-Caplan²,

Bauer³

et al. 2005

Macromolecules

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Nanometer-scale porosity is being introduced into low-k dielectrics in an attempt to achieve inter-level metal insulators with permittivities less than 2.0. It has proven extremely difficult to describe pore formation and to characterize the porous structure. This work investigates pore formation in a polyphenylene low-k dielectric based on pyrolysis of a porogen (27 vol %) in a polyphenylene matrix. One unique aspect presented here is the characterization of the nanoscale structure at various stages of pore formation through the use of a deuterated porogen. The combination of X-ray reflectivity (XRR) and smallangle neutron scattering (SANS) is found to be a powerful technique for describing porogen degradation and pore formation in nanoporous materials. The average radius of the porogen domains was approximately 60 Å with a relatively broad size distribution. During degradation the smaller porogen domains collapse, while the larger domains yield stable pores. This collapse of the relatively large number of smaller domains results in a significant reduction in film thickness, a porosity that is significantly smaller than the porogen content, a pore size distribution that is narrower than the porogen domain size distribution, and an average pore size of approximately 80 Å.

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Development and Application of On-Wafer Small Angle X-Rayscattering for the Quantification of Pore Morphology in Low Kporous Silk Semiconductor Dielectrics

Cited by 4 publications

References 8 publications

SANS and XRR Porosimetry of a Polyphenylene Low-k Dielectric

SANS and XRR Porosimetry of a Polyphenylene Low-k Dielectric

D-49 Invited—Flexibility and High Throughput: Supporting SAXS users at a Joint Industrial Academic Beamline

Nanopore Formation in a Polyphenylene Low-kDielectric

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