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{1250}
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ref: -0 tags: polyimide electrodes thermosonic bonding Stieglitz adhesion delamination date: 03-06-2017 21:58 gmt revision:7 [6] [5] [4] [3] [2] [1] [head]

IEEE-6347149 (pdf) Improved polyimide thin-film electrodes for neural implants 2012

  • Tested adhesion to Pt / SiC using accelerated aging in saline solution.
  • Targeted at retinal prostheses.
  • Layer stack:
    • 50nm SiC deposited through PECVD @ 100C using SPS, with low frequency RF modulation.
    • 100nm Pt
    • 100nm Au
    • 100nm Pt
      • These layers will alloy during cure, and hence reduce stress.
    • 30nm SiC
    • 10nm DLC (not needed, imho; PI sticks exceptionally well to clean SiC)
  • Recent studies have concluded that adhesion to PI is through carbon bindings and not through oxide formation.
    • Adhesion of polyimide to amorphous diamond-like carbon and SiC deteriorates at a minimal rate.
  • Delamination is caused by residual stress, which is not only inevetable but a major driving force for cracking in thin films.
    • Different CTE in layer stack -> different contraction when cooling from process temperature.
  • Platinum, which evaporates at 1770C, and is deposited ~100C (photoresists only withstand ~115C) results in a high-stress interface.
    • Pt - Carbon bonds only occur above 1000C
  • After 9 and 13 days of incubation the probes with 400 nm and 300nm of SiC, respectively, which were not tempered, showed complete delamination of the Pt from the SiC.
    • 60C, 0.9 M NaCl, 1 year.
    • The SiC remained attached to the PI.
      • Tempering: repeated treatment at 450C for 15 min in a N2 atmosphere.
    • All other probes remained stable.
  • Notably, used thermosonic bonding to the PI films, using sputtered (seed layer) then 12um electroplated Au.
  • Also: fully cured the base layer PI film.
  • Used oxygen plasma de-scum after patterning with resists to get better SiC adhesion to PI.
    • And better inter-layer adhesion (fully cured the first polyimide layer @ 450C).
  • Conclusion: "The fact that none of the tempered samples delaminated even after ~5 years of lifetime (extrapolated for 37 C) shows a tremendous increase in adhesion.

{1377}
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ref: -0 tags: nanopore membrane nanostraws melosh surface adhesion intracellular date: 02-06-2017 23:34 gmt revision:0 [head]

PMID-22166016 Nanostraws for Direct Fluidic Intracellular Access

  1. Used track-etched polycarbonate membranes, which have controlled pore density & ID.
  2. Deposited alumina on the pores & external surfaces using ALD
  3. Then etched away the top alumina
  4. and finally used O2 RIE to etch away the polycarbonate.
  • Show that these nanopores have cytosolic access (via Fluor 488 - hydrazide membrane impermeant dye
  • Also used nanostraws to deliver Co+2 to quench GFP fluorescence.

PMID-24710350, Quantification of nanowire penetration into living cells.

  • We discover that penetration is a rare event: 7.1±2.7% of the nanostraws penetrate the cell to provide cytosolic access for an extended period for an average of 10.7±5.8 penetrations per cell.
  • Using time-resolved delivery, the kinetics of the first penetration event are shown to be adhesion dependent and coincident with recruitment of focal adhesion-associated proteins.
    • Hours for unmodified, 5 minutes for adhesion-promoting surface.
  • Chinese hamster oviary cells expressing GFP, Co+2 quenching, EDTA chelation.
  • To modulate cell adhesion, nanostraw substrates were incubated in 10 μg ml−1 fibronectin, a well-characterized cell adhesion molecule, in addition to the standard polyornithine coating.

{1360}
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ref: -0 tags: L1 cell adhesion neural implants microglia DRG spinal cord dorsal root inflammation date: 11-19-2016 22:55 gmt revision:1 [0] [head]

PMID-22750248 In vivo effects of L1 coating on inflammation and neuronal health at the electrode-tissue interface in rat spinal cord and dorsal root ganglion.

  • Kolarcik CL1, Bourbeau D, Azemi E, Rost E, Zhang L, Lagenaur CF, Weber DJ, Cui XT.
  • Quote: With L1, neurofilament staining was significantly increased while neuronal cell death decreased.
  • These results indicate that L1-modified electrodes may result in an improved chronic neural interface and will be evaluated in recording and stimulation studies.
  • Ok, so this CAM seems to mitigate against microglia / inflammation, but how was it selected vs any of the other CAMs and surface proteins? (This domain is almost completely unknown by me..)
  • Ultimate strategy likely to be a broad combination of mechanical (size, flexibility), biochemical (inflammation, cell migration), electrochamical (surface coatings) and vasculature-avoiding approaches.

{1266}
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ref: -0 tags: polyimide adhesion delamination Stieglitz date: 08-18-2015 22:19 gmt revision:1 [0] [head]

Thin films and microelectrode arrays for neuroprosthetics

  • Juan Ordonez, Martin Schuettler, Christian Boehler, Tim Boretius and Thomas Stieglitz
  • Discussion of adhesion & ideas of using siliconcarbides as opposed to adhesion promoters (Silane A-174) to maintain good metal-polymer adhesion even with an equilibrium water vapor pressure.
  • Transition metals form carbide bonds with polyimide, but noble metals do not.
  • A one-metal (preferably noble) system is advantageous, as two metals will form a galvanic cell and eventually corrode.
  • Therefore it's best to develop non-metallic non-toxic adhesion promotion technologies.

{1322}
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ref: -0 tags: polyimide silicon carbide adhesion DBS syle electrodes date: 07-22-2015 18:01 gmt revision:0 [head]

PMID-25571176 Fabrication and characterization of a high-resolution neural probe for stereoelectroencephalography and single neuron recording.

  • Layer stack:
    • 5um PI (UBE U-varnish S)
    • 50nm SiC
      • Deposited at 100C.
    • 300nm Pt
    • 30nm SiC
    • 10nm DLC
    • 5um PI
      • Cured at 450C
    • 100nm Al hard mask (removed)
    • Cytop dry adhesion layer
      • softbake to remove solvent,
      • then hardbake at 290C for 4 hours to anneal the PI and adhere the Cytop to it.

{1319}
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ref: -0 tags: polyimide epoxy potassium hydroxide etch adhesion date: 06-25-2015 00:28 gmt revision:0 [head]

Improvement in the adhesion of polyimide/epoxy joints using various curing agents

  • Used 1M KOH, ~2min, followed by 0.2M HCl for 6 min to ring-open the imide.
  • PMDA/ODA polyimide (Pyromellitic Dianhydride, single aromatic ring + 4,4 diamino diphenyl ether )
  • Epoxy of the DGEBA + linear amide or aromatic (3,3 methylenedianiline)
  • Best result was with a polyamide curing agent, and high-temp curing profile. Unlikely that this will work for us, parylene will decompose..

{1317}
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ref: -0 tags: tantalum chromium polyimide adhesion date: 06-24-2015 23:20 gmt revision:1 [0] [head]

Tantalum and chromium adhesion to polyimide. Part 2. Peel and locus of failure analyses

  • CF4 etch followed by Ar sputter yielded the strongest bond to the PI.
  • Suggest that failure may be within the PI (cohesive), not between the PI and metal (adhesive).

Tantalum, tantalum nitride, and chromium adhesion to polyimide: effect of annealing ambient on adhesion

  • The peel adhesion at T-0 (initial) shows the following order: TaNx∼ TaN < Ta∼ Cr, with all samples failing in apparently virgin PI.
  • After ten thermal cycles to 400°C
    • in forming gas the peel adhesion showed the following trend: TaNx < TaN∼ Ta ∼ Cr,
    • whereas if the annealing was done in N2 the order changed to TaNx∼ TaN « Ta < Cr.
  • The peel locus of failure was
    • always in the apparently virgin PI in the Cr/PI samples,
    • while the Ta/PI samples failed in the modified PI,
    • and the TaN/PI and TaNx/PI samples failed between the Ta-nitride and the Cu peel backing film after thermal cycling.

{1316}
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ref: -0 tags: polyimide adhesion chromium copper tie layer upilex date: 06-24-2015 23:14 gmt revision:3 [2] [1] [0] [head]

Adhesion Evaluation of Adhesiveless Metal/Polyimide Substrate for MCM and high density packaging

  • Adhesion degradation after thermal and humidity stresses can occur for a number of reasons.
    • Copper diffusion can promote adhesion loss at elevated temperatures and can be inhibited by coating a barrier layer of metal – tie layer2.
    • Oxygen diffusion through polyimide film to the metal/polyimide interface plays a critical role in promoting degradation too3. Adhesion of Cr/polyimide interface is degraded significantly upon exposure to high temperature and humidity environment due to the hydrolysis of polyimide4,5 .
    • Catastrophic adhesion loss has been linked to moisture induced oxidation of chromium interfaces based on studies using radioactively tagged water4, 5.
  • That said, most of these vendors use Cr (20nm) as and adhesion layer, and Cu (200nm) as the conductor.
  • Upilex A faired very well after the pressure cooker test -- > 60% retention after 192 hours.
  • Seemingly Ta and Cr both adhere similarly to PI -- {1317}
    • Though Ta is much more ductile, and forms a stronger carbide, Cr is preferred... cheaper?

{1306}
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ref: -2008 tags: tantalum chromium polyimide tungsten flexible neural implants adhesion layer date: 06-24-2015 22:53 gmt revision:2 [1] [0] [head]

PMID-18640155 Characterization of flexible ECoG electrode arrays for chronic recording in awake rats.

  • Yeager JD1, Phillips DJ, Rector DM, Bahr DF.
  • We tested several different adhesion techniques including the following: gold alone without an adhesion layer, titanium-tungsten, tantalum and chromium.
  • All films were DC magnetron sputtered, without breaking vacuum between the adhesion layer (5nm) and gold counductor layer (300nm).
  • We found titanium-tungsten to be a suitable adhesion layer considering the biocompatibility requirements as well as stability and delamination resistance.
  • While chromium and tantalum produced stronger gold adhesion, concerns over biocompatibility of these materials require further testing.
    • Thought: use tantalum directly, no Ti needed.
    • Much better than Cr -- much more ductile and biocompatible.
    • Caveat: studies showing reduction to stociometric Ta results in delamination.
  • Ta conductivity: 1.35e-7 Ohms * m; Ti 4.2e-7; 3x better (film can be 3x thinner..)

{1315}
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ref: -0 tags: adhesion polymer metal FTIR epoxy eponol paint date: 05-01-2015 19:20 gmt revision:0 [head]

Degradation of polymer/substrate interfaces – an attenuated total reflection Fourier transform infrared spectroscopy approach

  • Suggests why eponol is used as an additive to paint.
  • In this thesis, attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy has been used to detect changes at the interfaces between poly (vinyl butyral-co-vinyl alcohol-co-vinyl acetate) (PVB) and ZnSe upon exposure to ozone, humidity and UV-B light.
  • Also, the response of PVB-aluminum interfaces to liquid water has been studied and compared with the same for eponol (epoxy resin, diglycidyl ether of bisphenol A)-aluminum interfaces.
  • In the presence of ozone, humidity and UV-B radiation, an increase in carbonyl group intensity was observed at the PVB-ZnSe interface indicating structural degradation of the polymer near the interface. However, such changes were not observed when PVB coated ZnSe samples were exposed to moisture and UV-B light in the absence of ozone showing that ozone is responsible for the observed structural deterioration. Liquid water uptake kinetics for the degraded PVB monitored using ATR-FTIR indicated a degradation of the physical structural organization of the polymer film.
  • Exposure of PVB coated aluminum thin film to de-ionized water showed water incorporation at the interface. There were evidences for polymer swelling, delamination and corrosion of the aluminum film under the polymer layer.
    • On the contrary, delamination/swelling of the polymer was not observed at the eponol-aluminum interface, although water was still found to be incorporated at the interface. Al-O species were also observed to form beneath the polymer layer.
    • A decrease of the C-H intensities was detected at the PVB-aluminum interface during the water uptake of the polymer, whereas an increase of the C-H intensities was observed for the eponol polymer under these conditions.
    • This is assigned to rearrangement of the macromolecular polymer chains upon interaction with water.

{1265}
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ref: -0 tags: nickel chrome polyimide adhesion date: 10-11-2014 00:13 gmt revision:7 [6] [5] [4] [3] [2] [1] [head]

Adhesiveless copper on polyimide substrate with nickel-chromium tiecoat

  • Chrome works the best, with Nichrome lagging slightly behind. Thicker tie layers (20nm) work slightly better.
  • 17 nm Cr and 5nm NiCr both work well after gold plating
    • in aggressive cyanide solution -- without tie layer, the copper was released.
    • note how thin the layers are!
  • Surface benefits from oxygen plasma pre-treatment. (de-scum?)
  • Still not sure how to get second layer of polyimide to adhere to top layer of Cr.

Adhesion Between Polymers and Other Substances - A Review of Bonding Mechanisms, Systems and Testing

  • The adhesion between the polyimide, PMDA-ODA and metals such as copper or chromium has received considerable attention due to its importance in the microelectronics industries.
  • As mentioned, the PMDA-ODA is normally deposited from solution as the polyamic acid and cured in-situ to the imide form.
  • Adhesion of the polyimide deposited on a metal is therefore a different problem than adhesion of a metal deposited on the cured polyimide.
  • The former situation (polyimide on metal) tends to give stronger adhesion than the latter (metal on polyimide) but there can be problems of metal, particularly copper, dissolution.
  • Great! (is this a reliable source?)
  • The interaction between the metals and the polyimide has been studied in great detail using x-ray photoelectron spectroscopy (XPS) and other surface analysis techniques but there is not complete agreement on the form of the interaction.
    • It is clear that strong interaction and electron transfer occurs when the metal is deposited from vapour onto the polyimide.
    • When the polyamic acid is deposited on the metal and cured then reaction occurs between the acid and the metal.
  • The strong interface formed between chromium and the polyimide is clearly a result of the strong chemical interaction but there is still considerable interest in making it more resistant to water and oxidation.

High-Performance Polymers (book) Guy Rabilloud (via google books.)

  • Order of metals by increasing adhesion:
    • Cu, Pd, Ni, V, Cr, Nb, Ti [140]
  • The adhesion between chromium and polyimide is degraded sharply as the interface is exposed to temperature-humidity stressing (85C, 81% RH [612]
  • Polyimide-polyimide self-adhesion strongly benefits from partial cure of the first layer (which is not possible with lithographic processes, TMAH etches uncured film). Plasma and adhesion treatments would likely help, due to molecular tangling (?). Presumably VM-651 helps. We'll cross that bridge when we get to it.
  • PMDA-PPD or PMDA-PDA is perhaps the most rigid of all the polyimides, but due to the extremely hydrophillic nature of PMDA & associated electron affinity of the dianhydride ( E a ), and the fact that it tends to crystalize & not be tough/plastic, it's infrequently used.

{1276}
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ref: -0 tags: polyimide silicon oxide aluminum adhesion pressure cooker date: 06-16-2014 21:28 gmt revision:2 [1] [0] [head]

Interfacial adhesion of polymeric coatings for microelectronic encapsulation

  • Find that, after a pressure-cooker test, adhesion of polyimide PI-2610 (what we use) to SiO2 was weaker than to Al, SiN, and copper.
  • Aluminum adhesion is quite good, at least to (only) 15 days @ 85C / 85% RH. Reference studies that find the adhesion to be 'acceptable' for the microelectronics industry.
    • Should we use an aluminum adhesion layer? Less biocompatible metal than Ti, and more likely to degrade in saline.
  • Found that copper adhesion actually went up with water exposure!
  • Polyimide adheres more strongly to glass than epoxy following accelerated aging.

{1282}
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ref: -0 tags: polyimide adhesion aluminum integrated circuit date: 05-07-2014 19:29 gmt revision:0 [head]

Polyimide insulators for multilevel interconnections Arthur M. Wilson

  • Old article (1981), but has useful historical information on the development of various PI insulators and their adhesion to aluminum, SiOx, etc.
  • Suggests that a higher-temperature cure (400C) is needed to fully drive water from the PI & cause a glass-transition. Might want to do this for the second PI layer.

{1275}
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ref: -0 tags: polyimide adhesion oxygen nitrogen plasma surface energy date: 03-10-2014 22:33 gmt revision:0 [head]

Adhesion Properties of Electroless-Plated Cu Layers on Polyimide Treated by Inductively Coupled Plasmas

  • O2 then N2/H2 ICP treatment of polyimide surfaces dramatically lowers the surface energy (as measured by contact angle), and increases the adhesion of palladium-catalyzed electroless copper.
  • Particularly, C-N bonds are increased as revealed by XPS.
  • No peel-strength measurements given.

{1258}
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ref: -0 tags: polyimide platinum electrodes Spain longitudinal intrafasicular adhesion delamination date: 10-05-2013 22:24 gmt revision:4 [3] [2] [1] [0] [head]

PMID-17278585 Assessment of biocompatibility of chronically implanted polyimide and platinum intrafascicular electrodes. 2007

  • Designed platinum/polyimide longitudinal intrafasicular electrodes (LIFEs)
    • 25um PT/Ir, insulated to 60-75um diameter. PT/IR has a young's modulus of 202 Gpa.
      • Plated with platinum black under sonication, as this forms a tougher surface than without sonication.
      • See also: PMID-20485478 Improving impedance of implantable microwire multi-electrode arrays by ultrasonic electroplating of durable platinum black. Desai SA, Rolston JD, Guo L, Potter SM. 2010
    • Polyimide PI2611, 10um thick, 50mm long, 220um wide in the electrode segment.
  • Implanted into rat sciatic nerve for 3 months.
  • These electrodes have been tested in people for two days:
    • Electrical stimulation through the implanted electrodes elicited graded sensations of touch, joint movement, and position, referring to the missing limb. This suggested that peripheral nerve interfaces could be used to provide amputees with prosthetic limbs with sensory feedback and volitional control that is more natural than what is possible with current myoelectric and body-powered prostheses.
  • CMAPs = compound muscle action potentials.
  • CNAPs = compound nerve action potentials.
  • Platinum wire LIFE performed very similarly to the thin-film polyimide LIFE in most all tests, with slightly higher potentials recorded by the larger polyimide probe.
  • 'Higher encapsulation with the polyimide probes! Geometry?
  • However, the polyimide LIFEs induced less functional decline than the wire LIFEs.
  • Other polyimide studies [14] [16] [24] -- one of which they observed a 70% reduction of tensile strength after 11 months of implantation.
    • [14] F. J. Rodríguez, D. Ceballos, M. Schüttler, E. Valderrama, T. Stieglitz, and X. Navarro, “Polyimide cuff electrodes for peripheral nerve stimulation,” J. Neurosci. Meth., vol. 98, pp. 105–118, 2000.
    • [16] N. Lago, D. Ceballos, F. J. Rodríguez, T. Stieglitz, and X. Navarro, “Long term assessment of axonal regeneration through polyimide regenerative electrodes to interface the peripheral nerve,” Biomaterials, vol. 26, pp. 2021–2031, 2005.
    • [24] M. Schuettler, K. P. Koch, and T. Stieglitz, “Investigations on explanted micromachined nerve electrodes,” in Proc. 8th Annu. Int. Conf. Int. Functional Electrical Stimulation Soc., Maroochydore, Australia, 2003, pp. 306–310.
      • The technology of sandwiching a metallization layer between two layers of polyimide seems to be suitable, because no delamination of the polyimide layers was observed even after 11 months. The right choice of metals for building the electrical conductive elements of the microelectrodes is crucial. Ti/Au/Ti/Pt layers tend to flake off from polyimide while delamination of Ti/Pt layers was not observed. However, adhesion of Ti/Pt layers was investigated after 2.5 months of implantation while Ti/Au/Ti/Pt layers were exposed after 11 months to the biological system. In previous research projects, surgeons also reported on delamination of Ti/Au layers from polyimide substrate after three months. Unfortunately, we had no possibility of inspecting these microelectrodes in our laboratory.
      • See also {1250}

{1248}
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ref: -0 tags: polyimide adhesion silver surface treatment adhesion delamination date: 10-04-2013 01:30 gmt revision:8 [7] [6] [5] [4] [3] [2] [head]

Improved polyimide/metal adhesion by chemical modification approaches

  • Suggest fuming sulfuric acid (H2S04) + Ag2SO4 for 30s as the most effective treatment.
  • 1 minute in 1M KOH also effective.
  • Silver was magnetron-sputtered on; peel test performed with tape.

IEEE-4936772 (pdf) Studies of adhesion of metal films to polyimide

  • Suggest Ar / O2 plasma treatment of surface to increase Cr/Cu adhesion (mechanical effect?)
  • Used two different polyimides: one derived from (BPDA‐PDA) polyamic acid, and pyromellitic dianhydride‐4,4’‐oxydianiline (PMDA‐ODA).

IEEE-670747 (pdf) Adhesion evaluation of adhesiveless metal/polyimide substrate for MCM and high density packaging

  • Adhesion of Cr / polyimide interface is degraded significantly upon exposure to high temperature and humidity environment due to the hydrolysis of polyimide.
  • There is also some worry of Cu diffusion into the polyimide.
  • All used a Cr tie layer, 200A thick (20nm).
  • Deposited photoresist, electroplated copper, then etched to define pattern.
  • Testing performed at 121C 100% RH, +15psi. (tough!)

On polyimide-polyimide interlayer adhesion: Diffusion and self-adhesion of the polyimide PMDA-ODA (1987)

  • Diffusion occurred during the curing process of the second layer and was controlled by the cure schedule.
  • It was found that a large diffusion distance, at least 200 nm, was required to obtain a bond whose strength was equal to that of bulk material.
  • Good protocol:
    • Dry first layer at 80C for 30 minutes.
    • 150C (or lower?) bake of first layer. "as the polyamic acid imidizes (and the solvent is lost) its diffusive mobility decreases rapidly; very little diffusion occurs after the first few minutes of the second bake.
    • Spin coat second layer.
    • 400C second bake.
  • Ductility is increased for polyimide that has experienced a series of increasing cure temperatures.
  • In this context it is worth noting that the contour length of a PMDA-ODA of 30,000 molecular weight is about 130nm, a value very similar to the diffusion distances measured when T1 (first layer bake) was 150C.

{1252}
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ref: -0 tags: parylene metal adhesion Stieglitz date: 08-15-2013 17:22 gmt revision:0 [head]

PMID-20119944 Characterization of parylene C as an encapsulation material for implanted neural prostheses.

  • On Si3N4, platinum, and a first film of parylene-C, satisfactory adhesion was achieved with silane A-174, even after steam sterilization. (>1 N/cm)
  • higher adhesion for the parylene that was deposited at lower pressures.
  • but: higher deposition pressures results in lower crystalinity.
  • [33] parylene can be used to build freestanding nanowires.
  • Parylene does not stick to polyimide.
  • Parylene sticks to parylene well if left untreated.
  • Annealing parylene dramatically increased crystalinity / decreases elongation to break.
  • The deposited parylene C layers on untreated and with oxygen plasma-treated samples delaminated immediately after contact with saline. The behavior was also observed at two out of three samples of the A-174 treated wafers, but not in this magnitude.
    • A potential reason for these results could be contamination of the samples during assembly or excessive treatment with the adhesion promoter.

{1245}
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ref: -0 tags: polyimide aging deadhesion humidity water absorption date: 06-28-2013 02:07 gmt revision:1 [0] [head]

Environmental Aging and Deadhesion of Polyimide Dielectric films

  • At 35C, 85% RH (not immersion!) there was little degradation in the polyimide to 2000 hours.
  • Suggest chromium or titanium as an adhesion promoter & to prevent copper from diffusing into the polyimide.
  • Plasma treatment of polyimide is commonly used prior to metal deposition in order to improve adhesion of polyimide to metallization [20].
    • Clearfield, Furman, Callegari 1994 "The Role of Physical and Chemical Structure in the Long-term Durability of Metal/Polyimide Interfaces" International Journal of Microcircuits and electronic Packaging 17(3), pp. 228-35.