Gravimetric measurements of steady-state moisture uptake in spin-coated polyimide films

ABSTRACTMoisture absorption and its effect on electrical properties were measured for several polyimides. A Quartz Crystal Microbalance (QCM) was used to investigate the moisture absorption in BPDA/PPD, PMDA/ODA, and BTDA//ODA/MPD polyimides. The steady-state moisture uptake in polyimides as a function of relative humidity (RH) was determined by exposing film samples to successively higher RH values ranging from 10 to 85% at 25°C. The isothermal moisture absorption as a function of percent RH was found to be nearly linear for all of the polyimides studied. The effect of moisture on the electrical properties of a BPDA/PPD polyimide was also investigated. The relative dielectric constant at 25 °C was found to be a linear function of the moisture absorbed.

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Gravimetric Measurements of Moisture Uptake in Polyimide Films Used in Integrated Circuit Packaging

MRS Proceedings ◽

10.1557/proc-154-97 ◽

1989 ◽

Vol 154 ◽

Cited By ~ 8

Author(s):

Denice D. Denton ◽

Hartono Pranjoto

Keyword(s):

Steady State ◽

High Temperature ◽

Integrated Circuit ◽

Dielectric Material ◽

Measurement Techniques ◽

Moisture Uptake ◽

Electrical Measurements ◽

Polyimide Films ◽

Cure Temperature ◽

Hygroscopic Behavior

AbstractPolyimide is used extensively in a variety of integrated circuit packaging applications. It is a good dielectric material with excellent planarizing capabilities, but like most polymers, it absorbs moisture. This hygroscopic behavior can lead to reliability problems in integrated circuit packages. The effects of variations in process history on moisture uptake are examined using gravimetric measurement techniques. In particular, the effects of cure schedule and exposure to high temperature/high humidity environments on steady state moisture uptake are reported. Steady state moisture uptake is shown to be a decreasing function of cure temperature. Moreover, the steady state moisture uptake in polyimide is greater after the samples have been “aged” in a high temperature and humidity ambient. Electrical measurements are used to examine the effects of cure temperature on diffusion kinetics of moisture in polyimide. The diffusion coefficient decreases with increasing cure temperature.

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Waxd Study of Low TCE Polyimide Films Formed from Polyamic Acid Blends and Copolymers.

MRS Proceedings ◽

10.1557/proc-264-213 ◽

1992 ◽

Vol 264 ◽

Author(s):

Thomas L. Nunes ◽

Krishna G. Sachdev

Keyword(s):

Molecular Structure ◽

Tensile Strength ◽

Crystallinity Index ◽

Moisture Uptake ◽

Chain Segment ◽

Polyimide Films ◽

Flexible Chain ◽

Polyamic Acid ◽

Out Of Plane ◽

Molecular Anisotropy

AbstractLow TCE polyimides, typically BPDA-PDA and related materials are well known for their special properties which include low in-plane TCE, up to 3X higher elastic modulus and ultimate tensile strength, and lower moisture uptake relative to the commonly known flexible chain polyimides [1]. These differences are due to the rod-like orientation and highly organized molecular structure of the polyimides that are derived from linear-planar precursors resulting in more anisotropic properties such as the X-Y vs Z-direction TCE [2], and optical as well as dielectric properties.In the present study, we have measured the WAXD patterns of polyimide films formed from BPDA-PDA and BTDA-PDA polyamic acid mixtures and BPDA-BTDA-PDA random copolyamic acids. In order to examine the effect of a highly flexible chain segment on the molecular anisotropy of rod-like polyimides, preliminary WAXD patterns were recorded for films of BPDA-BDAF and a BPDA-PDA-BDAF copolyimide.An in-plane and an out-of-plane crystallinity index, measures of molecular order within the polyimide films studied were estimated from the WAXD patterns. The data are correlated with the various blends and copolymer compositions and discussed in terms of structural implications.

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Effects of process history and aging on the properties of polyimide films

Journal of Materials Research ◽

10.1557/jmr.1991.2747 ◽

1991 ◽

Vol 6 (12) ◽

pp. 2747-2754 ◽

Cited By ~ 14

Author(s):

Denice D. Denton ◽

Milan C. Buncick ◽

Hartono Pranjoto

Keyword(s):

Steady State ◽

High Temperature ◽

Chemical Composition ◽

Integrated Circuit ◽

Dielectric Material ◽

Measurement Techniques ◽

Moisture Uptake ◽

Bulk Chemical ◽

Cure Temperature ◽

Hygroscopic Behavior

Polyimide is used extensively in a variety of integrated circuit packaging applications. It is a good dielectric material with excellent planarizing capabilities, but like most polymers, it absorbs moisture. This hygroscopic behavior can lead to reliability problems in integrated circuit packages. The effects of variations in process history on moisture uptake are examined using gravimetric measurement techniques. In particular, the effects of cure schedule and exposure to high temperature/high humidity environments (85 °C/85% RH) on steady state moisture uptake are reported. Steady state moisture uptake is shown to be a decreasing function of cure temperature. Samples cured at 250 °C absorb 25% more moisture by weight than do samples cured at 400 °C. Moreover, the steady state moisture uptake in polyimide is greater after the samples have been “aged” in a high temperature and humidity ambient. The bulk and surface chemical composition are also monitored as a function of aging using Fourier transform infrared spectroscopy (FTIR) and electron spectroscopy for chemical analysis (ESCA), respectively. The PI surface chemistry degrades after 700 h in an 85 °C/85% RH environment. The bulk chemical composition appears to be unaffected.

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Kinetics of metal interlayer growth in polyimide films and metal distributions in the non-steady-state regime and with constraints of patterned boundaries

The Journal of Physical Chemistry ◽

10.1021/j100311a029 ◽

1987 ◽

Vol 91 (27) ◽

pp. 6699-6705 ◽

Cited By ~ 6

Author(s):

Gregory T. Dee ◽

Lewis E. Manring ◽

Stephen. Mazur

Keyword(s):

Steady State ◽

Steady State Regime ◽

Polyimide Films ◽

State Regime ◽

Kinetics Of

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Electron microscopy and diffraction studies of polyimides

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100074069 ◽

1983 ◽

Vol 41 ◽

pp. 28-29

Author(s):

O.C. de Hodgins ◽

K. R. Lawless ◽

R. Anderson

Keyword(s):

Electron Microscopy ◽

Electron Microscope ◽

Structural Features ◽

Inert Atmosphere ◽

Polyimide Films ◽

Resolution Electron ◽

The Matrix ◽

High Resolution Electron Microscope ◽

Diffraction Patterns ◽

Polymeric Samples

Commercial polyimide films have shown to be homogeneous on a scale of 5 to 200 nm. The observation of Skybond (SKB) 705 and PI5878 was carried out by using a Philips 400, 120 KeV STEM. The objective was to elucidate the structural features of the polymeric samples. The specimens were spun and cured at stepped temperatures in an inert atmosphere and cooled slowly for eight hours. TEM micrographs showed heterogeneities (or nodular structures) generally on a scale of 100 nm for PI5878 and approximately 40 nm for SKB 705, present in large volume fractions of both specimens. See Figures 1 and 2. It is possible that the nodulus observed may be associated with surface effects and the structure of the polymers be regarded as random amorphous arrays. Diffraction patterns of the matrix and the nodular areas showed different amorphous ring patterns in both materials. The specimens were viewed in both bright and dark fields using a high resolution electron microscope which provided magnifications of 100,000X or more on the photographic plates if desired.

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Studies on Water in the Hydration Chamber of a Modified Electron Microscope

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100069715 ◽

1970 ◽

Vol 28 ◽

pp. 544-545

Author(s):

R. C. Moretz ◽

G. G. Hausner ◽

D. F. Parsons

Keyword(s):

Thin Film ◽

Thin Films ◽

Electron Microscope ◽

Steady State ◽

Room Temperature ◽

Small Mass ◽

Equilibrium Pressure ◽

Biological Objects ◽

Mechanical Pump ◽

Differential Pumping

Use of the electron microscope to examine wet objects is possible due to the small mass thickness of the equilibrium pressure of water vapor at room temperature. Previous attempts to examine hydrated biological objects and water itself used a chamber consisting of two small apertures sealed by two thin films. Extensive work in our laboratory showed that such films have an 80% failure rate when wet. Using the principle of differential pumping of the microscope column, we can use open apertures in place of thin film windows.Fig. 1 shows the modified Siemens la specimen chamber with the connections to the water supply and the auxiliary pumping station. A mechanical pump is connected to the vapor supply via a 100μ aperture to maintain steady-state conditions.

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Continuous hydrogenolysis of acetal-stabilized lignin in flow

Green Chemistry ◽

10.1039/d0gc02928a ◽

2021 ◽

Author(s):

Wu Lan ◽

Yuan Peng Du ◽

Songlan Sun ◽

Jean Behaghel de Bueren ◽

Florent Héroguel ◽

...

Keyword(s):

Steady State ◽

Challenges And Opportunities

We performed a steady state high-yielding depolymerization of soluble acetal-stabilized lignin in flow, which offered a window into challenges and opportunities that will be faced when continuously processing this feedstock.

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