Chapter Four · failure evidence
What Electrochemical Deposition & Synthesis got wrong, from 39 dissertations
The compiled records demonstrate various operational and material challenges encountered during electrochemical deposition and synthesis processes. These failures frequently stem from morphological instabilities, substrate corrosion, mechanical delamination, and unoptimized electrochemical control parameters. These records come from PhD theses at 15 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.
Uncontrolled synthesis conditions lead to precipitation, phase segregation, and degraded product quality
Omitting buffers, coordinating ligands, or appropriate precursor control during electrodeposition caused unwanted precipitates, basification, and poor elemental incorporation. Overcharging, interlayer screening, or unconstrained polymerization similarly resulted in non-uniform phases, isolated particles, or inferior sensing response compared to solution baselines.
Tried and failed
omitting buffer in electrochemical oxidation applied to electrochemical alkene difunctionalization. Outcome: unstable. Reason: solution basification caused catalyst degradation and lower yields
Tried and failed
pulsed co-electrodeposition without coordinating ligands applied to bimetallic catalyst synthesis. Outcome: unstable. Reason: loss of active transition metal ions due to insoluble precipitate formation and uncontrolled oxidation
Selective Electrochemical Nitrate Reduction to Ammonia over Cobalt-based Catalysts · Queens University Institutional Repository
Lost to a baseline
Electrochemically synthesised Cu3(HHTP)2 showed only 3.4% resistance decrease to 5 ppm NO2 compared to 19.6% and 8.7% for solution-synthesised a-Cu3(HHTP)2 and n-Cu3(HHTP)2.
Two-dimensional metal-organic frameworks for gas sensing · Oxford
Tried and failed
direct potentiostatic electrodeposition applied to metal selenide thin film deposition. Reason: produced isolated amorphous elemental selenium particles rather than a uniform nickel selenide film
Practical understanding of oxygen evolution electrocatalysis in alkaline electrolyte · UT Austin
Tried and failed
electrodeposition using specialty precursor salts applied to noble metal surface coatings. Outcome: unstable. Reason: narrow operational window across current densities prevented reproducible deposition
Manufacture of novel intermetallic bond coats from the electroplating of ionic liquids · Cranfield
Tried and failed
remote epitaxy through multilayer 2D interlayers applied to metal electrodeposition on substrates. Outcome: no signal. Reason: interlayer thickness screened substrate potential field, resulting in randomly oriented polycrystalline deposits
Understanding Atomic Interactions through Layered Materials during Metal Electrodeposition · Georgia Tech
Lost to a baseline
Mo1 electrodeposited onto NiO|P1 using a 3-fold higher charge (36 mC) resulted in worse photoelectrocatalytic performance compared to lower charge deposition due to surface oversaturation.
Design and study of organic-inorganic hybrids as photocatalysts for energy and environmental applications · DSpace-CRIS at TU Wien
Considered and rejected
Considered and rejected: Rejected electrochemically initiated chain-growth polymerization because it causes uncontrolled polymer formation and precipitation away from 3D micro-architected surfaces.
Tried and failed
potentiostatic template electrodeposition applied to alloy nanowire synthesis. Outcome: unstable. Reason: current spikes caused working electrode deformation and poor iron incorporation, preventing magnetic response
Gold-iron nanowires for magneto-mechanical and radiation therapy of glioblastoma multiforme · Imperial
Substrates and deposited layers suffer premature dissolution and corrosion under applied electrochemical conditions
Applying electrochemical biases in acidic, reactive, or high-temperature media triggered severe dissolution of underlying metal substrates, nanowires, or catalyst layers. Parasitic substrate oxidation, high-voltage field-accelerated etching, and diffuse coatings also led to electrode cracking, corrosion, and interference with the intended electrodeposition.
Tried and failed
electrochemical delamination with metal sacrificial layer applied to 2D material transfer from metal substrate. Outcome: unstable. Reason: the thin aluminium layer prematurely dissolved in the electrolyte under the applied electrochemical bias
Synthesis and Applications of Large-Area Monolayer Graphene · MIT
Tried and failed
electrochemical deposition on a matching metal cathode applied to acidic metal leaching solution. Outcome: unstable. Reason: zinc cathode spontaneously redissolved in the acidic electrolyte
Analyse et traitement des métaux lourds des rejets industriels Développement de méthodes chimiques électrochimiques et membranaires · DSpace at the University of Batna 1
Tried and failed
electrophoretic deposition on metal nanowires applied to graphene oxide coating on silver nanowires. Outcome: unstable. Reason: applied positive bias caused the metal nanowires on the electrode to undergo anodic dissolution
Development of Solution-Processed Stable Silver Nanowire Networks for Transparent Electrodes · MIT
Tried and failed
electrodeposition of metal oxide overlayers applied to acidic oxygen evolution reaction catalysts. Outcome: unstable. Reason: underlying catalyst layer underwent rapid dissolution in acidic electrolyte
A Journey to the Center of the Earth Abundant Metal Oxide Catalysts · Harvard
Tried and failed
metal electroplating of graphite electrodes applied to molten salt electrosynthesis. Outcome: unstable. Reason: metal coatings dissolved into the high-temperature melt without providing catalytic enhancement over bare graphite
Towards Sustainable Electrosynthesis of Industrially Valuable Small Molecules · MIT
Tried and failed
electrodeposition using reactive metal working electrodes applied to metal recovery in deep eutectic solvents. Outcome: unstable. Reason: parasitic substrate oxidation and electrode dissolution interfered with the target electrodeposition process
Toward lead recovery from lead waste acid batteries by deep eutectic solvents · Imperial
Tried and failed
electrodeposition of gold coatings applied to copper substrate redox electrodes. Outcome: unstable. Reason: diffuse coating caused poor electrolyte wetting, irreversible redox kinetics, and rapid substrate corrosion
Conceptualization, Thermodynamics, Kinetics, and Prototyping of Continuous Electrochemical Refrigeration · Georgia Tech
Tried and failed
electrochemical anodization at high voltage and fluoride applied to metal foam electrode morphologic engineering. Outcome: unstable. Reason: local field-accelerated dissolution caused non-uniform localized spots and cracking
Practical understanding of oxygen evolution electrocatalysis in alkaline electrolyte · UT Austin
Dendrite formation and uneven metal plating cause severe battery short circuits and stripping overpotentials
Metal electrodeposition on bare current collectors or without protective interfacial coatings produced porous morphologies, water electrolysis, and random crystallographic growth. These rough deposits guided dendrites toward the separator, reduced coulombic efficiency, and induced rapid short circuits or extreme stripping overpotentials.
Tried and failed
bare metal substrate for electrodeposition applied to anode-free solid and liquid batteries. Outcome: unstable. Reason: non-uniform deposition and contact loss voiding during stripping caused rapid short circuits within five cycles
Investigating the Interfacial Evolution of Lithium Metal in Anode-Free Batteries with Liquid and Solid-State Electrolytes · Georgia Tech
Tried and failed
unprotected metal electrodeposition without interfacial coatings applied to zinc metal battery anodes. Outcome: unstable. Reason: parasitic hydrogen evolution, uncontrolled passivation byproduct accumulation, and dendrite-induced short circuits
UNDERSTANDING AND DESIGNING INTERPHASE IN ZINC AND LITHIUM ANODES · Cornell
Tried and failed
high current density fast-charging electrodeposition applied to metal and alloy anodes. Outcome: unstable. Reason: severe dendrite formation and low coulombic efficiency at high current densities
UNDERSTANDING AND DESIGNING INTERPHASE IN ZINC AND LITHIUM ANODES · Cornell
Tried and failed
front-side nucleophilic coating on porous substrate applied to metal anode electrodeposition. Outcome: unstable. Reason: guided deposition toward separator rather than rear, causing aggressive short-circuiting dendrite growth
Tried and failed
low current density electrodeposition applied to zinc metal anodes. Outcome: unstable. Reason: random crystallographic orientation and dendritic growth caused early cell short-circuits
Investigation on Electrodeposition of Metals and Alloys with Advanced Characterizations · Georgia Tech
Tried and failed
high overpotential electrochemical additive manufacturing applied to localized metal electrodeposition. Outcome: unstable. Reason: ion diffusion depletion and water electrolysis caused severe dendritic and porous morphology
Electrochemical metal 3D printing · Imperial
Tried and failed
direct electrodeposition onto bare current collectors applied to alkali metal anode plating. Outcome: unstable. Reason: rough, porous initial deposition caused extreme stripping overpotentials approaching 4 V
Substrate incompatibility and non-uniform coverage prompt rejection of direct electrodeposition
Electrodepositing onto high-resistance supports, carbon paper, or nanowire arrays generated discrete island growth, electrical leakage short circuits, or inadequate nanoparticle coverage. Additionally, high parasitic hydrogen evolution on certain electrodeposited metals made direct electrodeposition inferior to electroless, galvanic, or chemical bath methods.
Considered and rejected
Considered and rejected: Rejected direct electrodeposition of porous Au foam due to high catalytic hydrogen evolution activity on deposited Au; substituted with galvanic replacement of NiSn sacrificial templates in Au bath.
3d Porous High Areal Capacity Lithium-Ion Micro-Batteries · Penn
Considered and rejected
Considered and rejected: Electrochemical deposition of platinum was rejected in favor of electroless deposition due to substantially lower nanoparticle coverage (2.04% vs 67.30% Pt mass)
Rapid and low-cost sensors based on nanostructured carbon materials for health and agricultural applications · Iowa State
Considered and rejected
Considered and rejected: Rejected electrodeposition of NiO onto ITO-PET due to high sheet resistance (30 Ω/sq) and surface heterogeneity causing non-uniformity, choosing chemical bath deposition instead.
Reversible Metal Electrodeposition and Ion Intercalation for Dynamic Windows · unevada
Considered and rejected
Considered and rejected: Rejected electrodeposition using Ti precursors instead of EPD because it frequently resulted in less porous coatings with variable particle sizes after sintering.
Considered and rejected
Considered and rejected: Rejected carbon paper supports for Bi electrodeposition because BiOBr grew discretely on carbon fibers rather than forming a homogeneous film, yielding poor ECR selectivity (45.4% FE).
Rational Design of Electrocatalytic Materials for Stable and Selective CO2 Reduction · Queens University Institutional Repository
Tried and failed
metal electrodeposition onto semiconductor nanowire arrays applied to generator-collector electrode fabrication. Reason: conductive leakage pathway formed between the substrate and metallic layer causing electrical shorting
Electrochemical CO2 Reduction with Well-Defined Electrodes · Harvard
Excessive deposition rates, extended durations, and aggressive potential sweeps trigger film delamination and peeling
Prolonged deposition times and high cathodic current densities generated mechanical stress, discontinuous cluster layers, and rapid film detachment. Similarly, wide potential sweeping or rapid oxidation caused deposited nanoparticles and large crystals to peel, strip, or show faster physical degradation than baseline techniques.
Tried and failed
extended cathodic electrodeposition duration applied to electrocatalyst films on porous substrates. Outcome: unstable. Reason: excessive deposition time caused film delamination and peeling during synthesis and electrochemical testing
Tried and failed
cathodic electrodeposition at high current density applied to protective coating deposition on alloy substrates. Outcome: unstable. Reason: High current density caused poor nucleation, film discontinuity, and detachment of deposited cluster layers
Protection of magnesium alloys from corrosion using magnesium rich surfaces. · Cranfield
Lost to a baseline
CuAg catalyst prepared by electrodeposition (CuAgdep/Cu) exhibited faster activity degradation (-0.146 vs -0.044 degradation rate slope) and physical detachment compared to galvanically prepared CuAgglv/Cu.
Profitable and sustainable use of biomass in developing technologies · Iowa State
Tried and failed
electrochemical deposition via wide potential sweeping applied to noble metal on transition metal oxide. Outcome: unstable. Reason: wide potential sweeping caused deposited nanoparticles to peel and strip off the support
Sub-Stoichiometric Titania as a Viable Support for Pt Electrodes · Georgia Tech
Tried and failed
sacrificial metal dual-working-electrode anodic electrodeposition applied to conductive metal-organic framework thin films. Outcome: unstable. Reason: rapid oxidation produced large detached crystals rather than coherent thin films on the substrate
Synthesis and characterisation of conductive metal-organic framework materials · Oxford
Left open by the authors
Problems the authors named and did not get to.
Left open
Develop non-vacuum deposition techniques like dip or suspension coating for sub-micron bilayer electrolyte protection in solid oxide cells. Blocker: Requires a physical materials synthesis and electrochemical wet laboratory.
Enhancing the Stability and Performance of Solid Oxide Cells by Tailoring Surfaces and Interfaces through Surface Modification · Georgia Tech
Left open
Investigate whether non-uniform lithium deposition improves high-current cycling performance when deposits maintain electronic percolation. Blocker: Requires a wet-lab battery fabrication and electrochemical characterization facility
Quantitative Solid Electrolyte Interphase-Based Descriptors for Lithium Liquid Electrolyte Design · MIT
Left open
Print SOFC electrodes using electrostatic spray deposition and optimize anode-supported substrates. Blocker: Requires a wet lab, synthesis materials, and physical deposition equipment (e.g., electrostatic spray deposition setup).
Left open
Develop design rules for optimal battery anode coating chemistries across use-cases such as fast charging and anode-free systems. Blocker: Requires wet-lab synthesis, material characterization, and electrochemical battery testing.
CRYSTALLOGRAPHIC CONTROL AND INTERFACE DESIGN STRATEGIES FOR SODIUM-BASED SECONDARY BATTERY ANODES · Cornell
Left open
Optimize ALD coating thickness and alternative chemistries (HfO2, SiO2, ZrO2, TiO2, nitrides) on battery electrodes to improve solid electrolyte wetting. Blocker: Requires atomic layer deposition (ALD) equipment, specialized battery materials, and wet-lab physical testing facilities.
Low melting point solid electrolytes for scalable manufacturing of all-solid-state li-ion batteries · Georgia Tech
Left open
Fabricate dimensionally stable anodes by coating etched titanium mesh with Pd-Pt mixed oxides baked above 400 °C to sustain high current densities. Blocker: Requires wet lab fabrication equipment and electrochemical testing apparatus.
Electrochemical Alkene Epoxidation Using Water as the Oxygen Source · MIT
Left open
Develop interlayer engineering schemes to accommodate alloy transformation and homogeneously re-form the alloy layer during battery stripping. Blocker: Requires wet-lab battery fabrication, thin-film deposition, and specialized operando/cryo-FIB characterization facilities.
Investigating the Interfacial Evolution of Lithium Metal in Anode-Free Batteries with Liquid and Solid-State Electrolytes · Georgia Tech
Left open
Design the interface contact between the active material and conductive/binder phases to prevent microscopic detachment and side reactions in battery electrodes. Blocker: Requires wet lab chemical synthesis, battery electrode fabrication, and experimental electrochemical testing.
Hierarchical porous architecture design in battery electrodes for scalable high-energy battery systems · UT Austin
Left open
Optimize semi-crystalline pPFDA coatings for lithium metal anode protection in aqueous environments. Blocker: Requires wet lab electrochemistry equipment and chemical vapor deposition apparatus (iCVD)
UNDERSTANDING AND DESIGNING INTERPHASE IN ZINC AND LITHIUM ANODES · Cornell
Left open
Perform comparative electrodeposition using different deep eutectic solvents, ionic liquids, and aqueous media to evaluate catalyst morphology and crystal structure. Blocker: Requires a physical wet chemistry lab, electrodeposition setup, and characterization equipment (e.g., SEM, XRD)
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