Chapter Four · failure evidence
What Surface Modification & Plasma Treatment got wrong, from 68 dissertations
Surface modification and plasma treatments frequently encounter failures stemming from energetic particle damage, chemical self-polymerization, and mechanical surface degradation. Process challenges also emerge from the rapid hydrophobic recovery of activated surfaces and adverse interfacial adhesion during bonding or demolding. These records come from PhD theses at 25 institutions, 2021 to 2026. Each links to its thesis. They were extracted by language models reading the full text, so treat each as a lead to read, not a verdict.
Plasma exposure and energetic bombardment cause physical and chemical damage to delicate substrates and thin films
Energetic plasma ion bombardment and reactive species erode underlying polymer matrices, reduce metal oxides, and degrade electrical transport in sensitive semiconductor channels. Exposure to oxygen or hydrogen plasmas also induces defect states, damages photoresists, and leads to surface morphology degradation across fragile nanostructures.
Tried and failed
argon plasma pre-etch surface treatment applied to nanomaterial contact interface formation. Outcome: worse than baseline. Reason: Excessive plasma bombardment damaged the sensitive nanomaterial channel, degrading electrical transport properties
Lab-to-Fab Monolithic 3D Integrated Carbon Nanotube Transistors: Scaling and Reliability · MIT
Tried and failed
increasing plasma power during dry etching applied to metal contact performance during recess etching. Outcome: worse than baseline. Reason: higher RF power caused plasma-induced damage degrading ohmic contact resistance
GaN Complementary-Metal-Oxide-Semiconductor (CMOS) Technology · MIT
Tried and failed
oxygen plasma treated PEG-DA hydrogel membranes applied to flexible microfluidic polymer devices. Outcome: unstable. Reason: membranes became brittle after plasma treatment and burst under applied pressure
Tried and failed
plasma pre-treatment before dielectric deposition applied to ultrathin barrier semiconductor heterostructures. Outcome: worse than baseline. Reason: plasma ion bombardment damaged the thin barrier layer and degraded two-dimensional electron gas conductivity
HIGH-SPEED, HIGH-POWER TRANSISTORS ON SINGLE-CRYSTAL ALUMINUM NITRIDE PLATFORM · Cornell
Tried and failed
prolonged high-power oxygen plasma surface treatment applied to carbon-fiber reinforced polymer composites. Outcome: worse than baseline. Reason: excessive plasma exposure caused matrix over-erosion and fiber damage, leading to premature interlaminar failure
An investigation into the surface pre-treatment of CFRPs prior to adhesive bonding · Imperial
Tried and failed
oxygen plasma etching or cleaning applied to chalcogenide glass nanostructures. Outcome: unstable. Reason: direct low-power oxygen plasma exposure caused severe material degradation of the particles
All-Dielectric Nanophotonic via Glass Fluid Instabilities · EPFL
Tried and failed
pulsed laser deposition on 2D material interlayers applied to oxide thin film growth on graphene. Reason: harsh plasma plume damaged and etched the 2D layer, preventing mechanical exfoliation
Nanoscale Engineering for Mixed-Dimensional Heterostructure Growth and Integration · MIT
Tried and failed
PECVD dielectric coating deposition applied to metal oxide contact layers. Outcome: worse than baseline. Reason: Plasma-generated atomic hydrogen chemically reduced the underlying transition metal oxide layer, degrading device performance.
Tried and failed
oxygen plasma surface treatment applied to ferroelectric oxide thin films. Reason: direct exposure caused dense nanoparticle formation and surface morphology degradation
Conductive ferroelectric domain walls in Pb(Zr,Ti)O3 for neuromorphic applications · EPFL
Tried and failed
direct PECVD dielectric deposition without buffer layer applied to nanomaterial transistor channels. Outcome: worse than baseline. Reason: Plasma damage during deposition caused severe current degradation and large parameter variations.
Considered and rejected
Considered and rejected: Rejected pure reactive O2 sputtering for encapsulating Ag/Cu nanowires because plasma-induced oxygen species oxidize and corrode the metallic nanowires, adopting reactive N2 sputtering with residual H2O/O2 instead.
Rapidly-Deployable Materials Processing Approaches for Energy Applications and Chemical Separations · MIT
Considered and rejected
Considered and rejected: Rejected O2 plasma-based oxidation for ALE because it damages photoresist, causes high porosity in MACE Si nanostructures, and lacks selectivity to high-surface-area features.
Considered and rejected
Considered and rejected: Rejected hydrogen plasma treatment for introducing -OH groups to repair nano-cracks because high-energy plasma damaged the surface and induced unwanted defect states.
Investigation of Transport Properties in β-Ga2O3 Nanomembranes Under Mechanical Strain · DSpace at SUNY Buffalo
Considered and rejected
Considered and rejected: Rejected using an oxygen plasma source during initial oxide nucleation on GaAs because it oxidizes the GaAs surface into amorphous Ga and As oxides; used molecular oxygen instead.
Integration of Multi-Functional Oxide Thin Film Heterostructures with III-V Semiconductors · TXST Digital Repository
Considered and rejected
Considered and rejected: Decided against using O2 plasma etching for TMD pore creation because it oxidizes and degrades monolayer MoS2
Nanostructure Engineering In Two-Dimensional Materials Beyond Graphene · Penn
Surface modifications cause unintended adhesion anomalies, excessive stiction, or catastrophic delamination
Oxygen plasma, silanization, and chemical etching can inadvertently suppress required cell attachment or increase stiction to the point of tearing hydrogels and elastomeric molds during release. In other instances, treatments disperse contaminants deeper into substrates or leave residual interfacial oxides, leading to poor bonding repeatability and film peeling.
Tried and failed
oxygen plasma surface treatment for hydrophilicity applied to PDMS substrates for stem cell adhesion. Reason: plasma treatment prevented human embryonic stem cell adhesion to the substrates
Tried and failed
plasma surface modification for demoulding release applied to photopolymerised micro-moulded hydrogels. Reason: insufficient anti-stiction without silanisation caused hydrogel tearing during mould release
Considered and rejected
Considered and rejected: Rejected using oxygen plasma treatment prior to spin-coating the polymer film destined for delamination, because it prevented spontaneous delamination in water.
Tried and failed
hydrofluoric acid surface etching applied to silicone elastomer substrates. Reason: increased surface hydrophobicity degraded subsequent sputtered metal film adhesion and caused peeling
Development of stencil lithography for stretchable interconnects · EPFL
Tried and failed
atmospheric pressure plasma surface treatment applied to silicone-contaminated polymer composites. Outcome: worse than baseline. Reason: treatment dispersed and drove silicone contaminants deeper into the substrate instead of removing them, reducing bond strength
Atmospheric pressure plasma surface engineering to improve polymer matrix composite bonding · Cranfield
Tried and failed
polyvinyl alcohol surface coating applied to cell adhesion on silicone microfluidics. Outcome: worse than baseline. Reason: PVA surface modification significantly reduced epithelial cell attachment compared to untreated controls
Development of a biomicrofluidic model of the gastrointestinal-lymphatic interface · Imperial
Tried and failed
dielectric barrier discharge plasma surface treatment applied to silicone-contaminated polymer matrix composites. Reason: failed to remove silicone, instead oxidising residual contamination into silica and masking desired surface functionalisation
Atmospheric pressure plasma surface engineering to improve polymer matrix composite bonding · Cranfield
Tried and failed
thin film deposition without thermal surface deoxidation applied to heterostructure growth on silicon carbide. Outcome: unstable. Reason: residual native surface oxide causes thin film delamination during high-temperature annealing
Ballistic transport in hexagonal boron nitride/epigraphene/silicon carbide heterostructures · Georgia Tech
Lost to a baseline
Silanized composites (AI-Sil and AI-Cu-Sil) yielded lower hbMSC cell attachment and metabolic activity than pristine untreated polymer AI-pristine due to increased surface hydrophobicity (contact angle 96° vs 0°).
Design of advanced biobased photocurable formulations: from dynamic covalent network to composite scaffold for tissue engineering · IRIS - POLITO - prod
Considered and rejected
Considered and rejected: Rejected hydrophobic silicon-to-silicon wafer bonding due to high sensitivity to surface cleanliness and poor repeatability vs hydrophilic bonding
3D Heterogeneous Integration for RF/mmWave Electronics · Georgia Tech
Considered and rejected
Considered and rejected: Abandoned trilayer graphene insertion under PEDOT:PSS due to poor adhesion and large sheet resistance non-uniformity (14 Ω/sq to 4 kΩ/sq) induced after oxygen plasma treatment.
Considered and rejected
Considered and rejected: Rejected standard dual-surface oxygen plasma bonding for PDMS-to-gel attachment because plasma exposure degrades substrate-bound ssDNA patterns.
GUIDED ORGANOGENESIS USING MOSAIC PATTERNS OF PROGENITORS · ScholarlyCommons at Penn
Tried and failed
oxygen plasma treatment with polymer coating applied to elastomeric micromolding release. Reason: caused severe adhesion leading to demolding failure, broken products, and torn molds
Microneedle Patch Delivery of Controlled-Release Microspheres to the Skin · Georgia Tech
Mechanical polishing and abrasive treatments destroy critical surface microstructures and protective passive films
Abrasive grinding and polishing frequently smooth away the microscale and nanoscale topography essential for superhydrophobic and superoleophobic performance. Additionally, excessive mechanical treatment introduces microcracks, leaves microscopic voids, and strips protective passive films without allowing adequate repassivation.
Tried and failed
manual surface abrasion of polymer substrates applied to printed conductive silver traces. Outcome: worse than baseline. Reason: abrasion left microscopic surface voids, failing to eliminate voids and degrading electrical conductivity
Developing Intelligent Structures and Functional Devices Using Novel Smart Materials and Multi-Material Multi-Method (m4) 3D Printing · Georgia Tech
Tried and failed
silane sol-gel surface modification applied to cellulosic fabrics for superhydrophobic coating. Outcome: unstable. Reason: mechanical abrasion wore away the surface coating and degraded superhydrophobic wettability
Functional cellulosic materials in precision oil-water separation for fatberg point source control · Imperial
Tried and failed
mechanical abrasion durability testing via sandpaper grinding applied to superhydrophobic coated mesh. Reason: continuous mechanical friction destroyed the micro- and nanoscale surface topography essential for superhydrophobicity
Functional cellulosic materials in precision oil-water separation for fatberg point source control · Imperial
Tried and failed
mechanical surface polishing applied to austenitic stainless steel corrosion resistance. Outcome: worse than baseline. Reason: polishing removed native protective passive film without sufficient repassivation compared to as-received surface
Bromide induced corrosion of stainless steels and Ni-based alloys · Imperial
Tried and failed
differential abrasive polishing for selective phase removal applied to polymer matrix composite surfaces. Reason: failed to selectively erode matrix to expose reinforcing fibers, causing high measurement scatter and poor bonding
Tried and failed
fine grit mechanical polishing applied to underwater superoleophobic ceramic substrates. Outcome: worse than baseline. Reason: polishing smoothed the required microscale surface roughness, degrading anti-oil performance
Bio-inspired functional materials with special interfacial properties · Imperial
Considered and rejected
Considered and rejected: Rejected relying solely on surface roughening/mechanical interlocking, because high adhesive viscosity fails to fill features, creating built-in pre-cracks that sharply lower detachment stress.
Considered and rejected
Considered and rejected: Rejected aggressive mechanical substrate surface treatments (jackhammering/chipping) because they induce >2x higher microcrack densities in normal substrates compared to sandblasting.
Considered and rejected
Considered and rejected: Rejected dry scrubbing brushes for solar panels because contact abrasion causes irreversible surface scratching that degrades optical transmittance over time.
Charged interfaces and their applications in energy sustainability · MIT
Considered and rejected
Considered and rejected: Rejected sandblasting and physical carving for waveguide surface modification due to inability to programmably generate continuous gradient surface roughness distributions.
Light, fluidics and their applications in global sustainability and health · Cornell
Considered and rejected
Considered and rejected: Rejected mechanical surface grooving/patterning (diamond saw) to promote structural adhesion because it destroys the thin (200nm) Si3N4 passivation coating.
Optimising laser stereolithography for constructing electronic packages onto novel substrates · University of Nottingham Repository
Silane functionalization suffers from uncontrolled self-polymerization, aggregation, and unstable interfacial grafting
Silane precursors frequently undergo self-condensation and uncontrollable cross-linking, producing aggregates, gels, and cracked coatings instead of uniform monolayers. These unstable silane multilayers easily wash off or delaminate under fluid shear stress and aqueous exposure, undermining sensor stability and bonding.
Tried and failed
Extended vapor-phase silane surface functionalization applied to silicon micro/nanostructures for anti-stiction. Reason: Prolonged exposure causes excessive silane polymerization and residue buildup around nanofeatures
Nanoscale Strain Gauges in Flexible Polymer for Biological Cell Force Measurement · Georgia Tech
Tried and failed
epoxysilane surface functionalization applied to silica optical microresonator biosensors. Outcome: unstable. Reason: Silane formed unstable multilayers that washed off under fluid flow, degrading optical quality factor
Engineering and characterisation of optical nucleic acid sensors · Imperial
Tried and failed
silane surface functionalisation for polymer bonding applied to bonding PET membrane to PDMS. Outcome: unstable. Reason: membrane delaminated upon exposure to aqueous media
Development of a biomicrofluidic model of the gastrointestinal-lymphatic interface · Imperial
Tried and failed
Aqueous silanization for polymer surface functionalization applied to PET membranes for microfluidic bonding. Outcome: unstable. Reason: Silane self-polymerization in aqueous solution led to poor adhesion and delamination under fluid shear stress
An Organ-on-a-chip model of pulmonary arterial hypertension · Imperial
Tried and failed
high-concentration silane surface functionalization applied to optical sensor substrates. Outcome: worse than baseline. Reason: silane self-condensation produced surface aggregates and induced substrate cracking
All-Dielectric Nanophotonic via Glass Fluid Instabilities · EPFL
Tried and failed
One-pot surface functionalization by amine-silane substitution applied to cellulose nanocrystals. Outcome: unstable. Reason: Silane cross-linked uncontrollably into an irreversible gel instead of grafting to the particle surface
Scalable Approaches to Manufacturing Nanocellulose-Glass-Fiber Reinforced Composites · Georgia Tech
Tried and failed
chlorotrimethylsilane surface silanization applied to porous boron nitride adsorbents. Outcome: worse than baseline. Reason: monolayer formation reduced average pore size without significantly enhancing hydrophobicity
Tried and failed
silane-assisted surface coating of porous media applied to flow-through reactive contaminant remediation. Outcome: unstable. Reason: active reagent rapidly leached under continuous flow, precipitating inactive secondary sludge within minimal pore volumes
Considered and rejected
Considered and rejected: Liquid-phase silane immersion without sonication/optimisation was rejected due to excessive ambient moisture causing silane polymerisation and surface inhomogeneities
Functionalised organic field-effect transistors as biosensors for circulating-tumour DNA detection · Imperial
Considered and rejected
Considered and rejected: Liquid-phase OTES silanization rejected due to uncontrolled silane polymerization bridging unhydroxylated sites and interfering with surface assays.
Methods for High-Contrast Photoluminescence and Label-Free Surface-Sensitive Detection · Publikationssystem UB Tuebingen
Plasma-activated surfaces suffer from rapid hydrophobic recovery and environmental instability
Hydrophilic activation generated by oxygen plasma often dissipates quickly within minutes in ambient air or degrades irreversibly upon exposure to moisture. This rapid loss of surface wettability undermines sustained capillary flow and compromises long-term microfluidic bonding and packaging yields.
Lost to a baseline
Untreated control sensors had higher 30-day packaging yield (20%) than oxygen-plasma-treated sensors (12%).
A robust sensor design for measuring sweat chloride · JScholarship
Considered and rejected
Considered and rejected: Rejected plasma activation of PDMS for long-term culture comparisons due to hydrophobic recovery over time.
Development of a biomicrofluidic model of the gastrointestinal-lymphatic interface · Imperial
Considered and rejected
Considered and rejected: Rejected PDMS/oxygen plasma and standard thermoplastic bonding due to sensitivity to ambient conditions, temperature, humidity, and cleanliness, opting for H2-plasma-treated PTFE
Considered and rejected
Considered and rejected: Rejected plasma treatment for PDMS bonding to glass coverslips during anaerobic microfluidics chip assembly.
Considered and rejected
Considered and rejected: Rejected UV/plasma etching alone because it only creates nanometer roughness, resulting in fast hydrophobic recovery without sustained capillary flow.
Surface Modification of Thermoplastic Polymers for Lateral Flow Assay Applications · TXST Digital Repository
Tried and failed
plasma oxidation of polymer precursor films applied to gas separation membranes. Outcome: unstable. Reason: irreversible degradation in permeance and selectivity upon exposure to water vapor
Nanoengineering Polyorganosilica (POSi) Nanomembrane for Hydrogen Purification · DSpace at SUNY Buffalo
Tried and failed
unpassivated porous silicon as hydrophobic adsorbent applied to volatile organic compound preconcentration. Outcome: unstable. Reason: ambient moisture oxidised the surface over time, causing severe loss of hydrophobicity
Nanoporous Silicon in Gas Preconcentration and Sensing · Cambridge
Considered and rejected
Considered and rejected: Rejected relying on oxygen-plasma-treated surfaces for underwater oleophobicity because hydrophilicity dissipates rapidly within minutes in air compared to robust PAA grafts.
Fabrication Of Superhydrophilic Nanostructured Membranes For Oil/water · Penn
Plasma cleaning and discharge treatments fail due to insufficient reactive species or substrate contamination
Using inert gas plasmas or dry discharge treatments often yields insufficient reactive species to eliminate organic soils and leaves behind unwanted surface species compared to wet chemical treatments. Furthermore, plasma can infiltrate porous thin films to degrade pattern fidelity or oversaturate coatings with substrate elements.
Considered and rejected
Considered and rejected: Rejected dry plasma/UV surface activation for glass coverslips in favor of wet piranha solution to avoid depositing undesired species and achieve deeper cleaning.
Novel crystallization platforms for drugs and biomolecules: self-assembled surface functionalization and gels · IRIS - POLITO - prod
Tried and failed
inert gas cold atmospheric plasma applied to surface bacterial decontamination. Outcome: worse than baseline. Reason: pure nitrogen and helium mixtures generated lower reactive species concentrations than ambient air plasma
Microbial Decontamination of Egg Surface via Cold Plasma · HARVEST
Tried and failed
atmospheric pressure dielectric barrier discharge plasma cleaning applied to soiled optical glass surfaces. Reason: plasma treatment alone failed to remove sufficient soil to meet required optical reflectance thresholds
Considered and rejected
Considered and rejected: Rejected oxygen plasma alone or Ar-O2 plasma without vacuum baking prior to Ti/Cu sputtering because they failed to significantly increase seed-layer adhesion to polymer dielectrics.
Design and Demonstration of Mechanical and Electrical Reliability of 1-micron Redistribution Layers · Georgia Tech
Tried and failed
reactive ion etching post-calcination applied to porous mesostructured thin films. Reason: plasma infiltrated the void spaces of the porous oxide, degrading pattern fidelity
QUANTUM METAMATERIALS DIRECTED BY BLOCK COPOLYMER SELF-ASSEMBLY VIA ADVANCED MANUFACTURING · Cornell
Considered and rejected
Considered and rejected: Plasma-sprayed deposition was rejected in favor of gel-binder doctor blade application because thin coatings became oversaturated with substrate elements and could not eliminate voids.
MICROSTRUCTURAL EVOLUTION AND REACTION MECHANISMS IN MULTI-PHASE METAL SYSTEMS · JScholarship
Left open by the authors
Problems the authors named and did not get to.
Left open
Apply plasma treatment or surface polymer grafting with alternative nanomaterials to produce superhydrophilic nanofibrous membranes. Blocker: Requires a wet chemistry lab, electrospinning equipment, and plasma treatment/chemical synthesis apparatus
Development of Multifunctional Nanofibrous Membrane Material for Biological Wastewater Treatment · YorkSpace
Left open
Perform in vitro biophysical characterization of purified full-length PLEKHA4 or isolated C-terminal domains to analyze plasma membrane puncta formation. Blocker: Requires wet lab facilities for protein purification and in vitro biophysical assays
Left open
Modify PDMS microfluidic channel surfaces with surfactant coatings, grafting, or hydrophilic polymers to reduce protein adsorption during flow. Blocker: Requires a wet lab and microfluidic fabrication equipment to perform chemical surface modifications and flow experiments.
Left open
Investigate time-dependent efficacy degradation of textured condenser surfaces. Blocker: Requires experimental aging data, physical degradation testing, or specialized material fouling studies
Technoeconomic Analysis of Textured Surfaces for Improved Condenser Performance in Thermoelectric Power Plants · Virginia Tech
Left open
Evaluate chemical etching and automated polishing methods for Small Punch Test sample preparation and measure their impact on surface finish. Blocker: Requires a physical metallography laboratory, chemical etching chemicals, polishing apparatus, and surface profilometry equipment.
Exploration of the Additive Manufacturing Process Development Space using High-throughput Mechanical Property Assays · Georgia Tech
Left open
Modify specimen cutting and machining processes to eliminate surface-exposed centerline shrinkage porosity in cast steel fatigue specimens. Blocker: Requires physical casting, machining, and metallurgical laboratory apparatus.
A process and investigation into the influence of cast surface condition on fatigue life · Iowa State
Left open
Prevent semiconductor surface oxidation in aqueous solution and enhance micromotor compatibility with high-ionic-strength media. Blocker: Requires a wet lab and materials/chemical apparatus to modify surface chemistry and test in liquid media.
Light modulation of electric field driven semiconductor micromotors · UT Austin
Left open
Implement surface modifications (PVA, PEG, LbL) or switch to thermoplastics (PC, PMMA, COC) to preserve long-term microchannel wettability. Blocker: Requires a wet lab, microfabrication facilities, and chemical reagents for surface treatment.
Capillary-driven Microfluidic Biosensing Platforms for Digital Biomolecule Detection · Texas Tech
Left open
Evaluate the long-term durability and hydrophobic performance of micro-textured cementitious surfaces under real-world environmental exposure conditions. Blocker: Requires physical cement samples, fabrication tools, outdoor weathering exposure, and physical testing equipment.
Cement-based materials with hydrophobic micro-textured surface · Imperial
Left open
Couple weathering rates to fluid transport through micro-cracks and reactive surface exposure dynamically in a finite element homogenization framework. Blocker: Lacks specific governing equations, reaction kinetics formulations, or validation datasets defined in the thesis summary.
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