Library · Materials, chemistry & fabrication
What Solid-State Synthesis got wrong, from 31 theses
Summary written by a model from the records below: The records describe synthesis attempts and design choices across solid-state materials including perovskites, solid electrolytes, and layered oxides. Many investigations encountered failures stemming from persistent secondary phase formation, precursor decomposition, volatile component loss, or poor densification during thermal processing. These records come from graduate theses, 2021 to 2025, each labeled with its degree where the repository states it, and 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.
Plus 10 problems the authors left open, listed at the end.
Failure modes, by theses reporting them
Select a mode to jump to its records.
Direct solid-state reactions fail to achieve phase purity due to persistent precursors and competing secondary phases
Solid-state sintering and calcination frequently produced multiphase mixtures, unreacted starting precursors, and thermodynamically favored competing phases instead of the target composition. High-temperature solid-state firing of complex perovskites, MAX phases, and argyrodites suffered from substantial phase segregation and poor sample homogeneity.
Tried and failed
high-temperature solid-state sintering applied to polyanion disordered rocksalt cathode synthesis. Reason: failed to achieve phase purity, retaining persistent precursor impurities and degrading electrochemical performance
Polyanionizing rocksalt cathodes for lithium-ion batteries · MIT · PhD
Tried and failed
flux-free solid-state synthesis applied to multinary metal oxide precursor synthesis. Reason: failed to form target phase, yielding incongruent secondary phases instead
Advanced electrochemical materials for sustainable energy conversion and storage · UT Austin · PhD
Tried and failed
direct reaction of pre-synthesized intermetallics with carbon applied to MAX phase ceramic synthesis. Reason: formed unwanted competing ternary carbide phases instead of the target MAX phase
Fundamental Formation mechanisms of the MAX phase Zr3AlC2 and small scale mechanical properties of the MAX phases · Imperial · PhD
Tried and failed
transition metal substitution in mechanochemical synthesis applied to polyanion-doped disordered rocksalt cathode materials. Reason: substitution hindered target phase formation, leaving unreacted precursor impurities
Polyanionizing rocksalt cathodes for lithium-ion batteries · MIT · PhD
Tried and failed
solid-state synthesis of double perovskite oxides applied to strontium neodymium iridate compositions. Outcome: unstable. Reason: the composition failed to form a phase-pure perovskite crystal structure during synthesis
The Effectiveness of Perovskites for the Oxygen Evolution Reaction in Acid · UT Austin
Tried and failed
solid-state direct synthesis via calcination applied to single-halide argyrodite solid electrolytes. Reason: failed to form the target crystalline phase upon thermal annealing up to 450 °C
Design and Development of High-Performance Solid Electrolyte for All-Solid-State Lithium Ion Batteries · Georgia Tech · PhD
Tried and failed
conventional solid-state reaction synthesis applied to complex perovskite nickelate ceramics. Reason: produced inhomogeneous samples with ~50% impurity phases despite repeated high-temperature high-pressure oxygen anneals
Metal-insulator transition in yttrium- and neodymium-doped lanthanum nickelates · UT Austin · PhD
Tried and failed
high-temperature direct solid-state synthesis applied to layered perovskite oxide target phase. Reason: formed a thermodynamically favored competing binary phase instead of the target ternary composition
Cation exchange chemistry as a route to induce noncentrosymmetry in layered perovskite oxides · Oxford · PhD
Tried and failed
conventional furnace solid-state reaction applied to yttrium aluminum perovskite phase synthesis. Reason: formed competing intermediate oxide phases (YAG and YAM) instead of phase-pure perovskite
Thermal and Optical Properties of Oxide Coatings for High-Temperature Applications · Harvard · PhD
Sol-gel and wet precursor routes produce secondary phases or suffer from contamination and stoichiometry deviations
Sol-gel Pechini methods and wet precursor processing struggled with inconsistent phase purity, forming carbonate or fluoride impurities and metastable non-stoichiometric phases. Absence of appropriate complexing agents or optimal water ratios led to side reactions, poor reproducibility, and disrupted powder morphology during subsequent calcination.
Tried and failed
modified Pechini sol-gel synthesis applied to gallium-doped garnet solid electrolytes. Reason: failed to reliably yield secondary-phase- and impurity-free products reproducibly
Using advanced surface analysis techniques to investigate the solid-solid interfaces in solid state batteries · Imperial · PhD
Tried and failed
Sol-gel synthesis of ceramic solid electrolytes applied to garnet-type lithium lanthanum zirconium oxide. Outcome: unstable. Reason: Rapid degradation from ambient air exposure and secondary impurity phase formation during synthesis.
Recovering materials from end-of-life lithium-ion batteries · Imperial · PhD
Tried and failed
sol-gel chemical synthesis applied to catalyst candidate material synthesis. Reason: insufficient network formation in the gel prevented synthesis
Optimization Algorithms for Quantum and Digital Annealers · Harvard · PhD
Tried and failed
fluoropolymer labware in sol-gel synthesis applied to metal oxide nanoparticle synthesis. Reason: leached fluorine from PTFE formed unwanted metal fluoride impurity phases during calcination
NOVEL AND ENHANCED FUNCTIONAL MATERIALS PROPERTIES VIA BLOCK COPOLYMER STRUCTURE DIRECTED POROSITY · Cornell · PhD
Considered and rejected
Considered and rejected: Rejected sol-gel Pechini-type synthesis of Ga-LLZO because achieving impurity- and secondary-phase-free material consistently was unreliable compared to commercial Toshima powder.
Using advanced surface analysis techniques to investigate the solid-solid interfaces in solid state batteries · Imperial · PhD
Considered and rejected
Considered and rejected: Rejected using 1:1 Ba/Ti molar ratio in wet sol-gel synthesis because it produced non-stoichiometric metastable phases (BaTi2O5, Ba2Ti5O11, Ba4Ti13O30).
Exploring the Potential of Polymer-Ceramic Nanocomposites for Energy Harvesting: The Role of Particle Functionalization in Enhancing Dielectric and Piezoelectric Properties · University of Trento · PhD
Considered and rejected
Considered and rejected: Rejected completely water-free sol-gel synthesis because it resulted in ~10 wt% SrCO3 impurities; required 4.5 vol% H2O.
NOVEL AND ENHANCED FUNCTIONAL MATERIALS PROPERTIES VIA BLOCK COPOLYMER STRUCTURE DIRECTED POROSITY · Cornell · PhD
Considered and rejected
Considered and rejected: Rejected Ga-LLZO due to less consistent synthesis of monophasic powder and intermediate CTE between Al-LLZO and Ta-LLZO.
Fabrication of laminated solid electrolytes with compressive surface stresses for lithium batteries · Oxford · Master's
Molten salt fluxes and melt synthesis cause flux decomposition, unreacted residues, or phase separation
Molten salt fluxes decomposed at elevated synthesis temperatures, introduced insoluble contaminants like carbonates and sulfates, or triggered severe phase separation into unreacted binary oxides. Direct melt synthesis routes failed to form homogeneous liquid solutions below liquidus temperatures or reacted destructively with substrate materials.
Tried and failed
direct single-step molten-salt flux synthesis applied to layered oxide cathode materials. Reason: caused severe phase separation into unreacted binary oxides and undesired polymorphs instead of target phase
Deciphering the degradation mechanisms of layered oxide cathodes for sodium-ion batteries · UT Austin · PhD
Tried and failed
sulfate molten-salt flux synthesis applied to sodium-ion layered oxide cathodes. Reason: Sulfate flux decomposed at high temperatures, forming nickel sulfate and persistent secondary phase impurities.
Deciphering the degradation mechanisms of layered oxide cathodes for sodium-ion batteries · UT Austin · PhD
Tried and failed
binary alkali carbonate molten salt flux synthesis applied to single crystal cathode materials. Outcome: worse than baseline. Reason: carbonate impurities were insoluble during washing, causing high polarization and rapid capacity fade
Insights on the synthesis, properties, and performance of high-nickel layered oxide cathodes · UT Austin · PhD
Tried and failed
melt synthesis doping below liquidus temperature applied to solid-state electrolyte halide mixtures. Reason: reactants failed to form a molten homogeneous solution at target temperature, leading to incomplete doping
Borohydride-based solid electrolytes and polymer composite separators for lithium-ion batteries · Georgia Tech · PhD
Tried and failed
reactive infiltration of binary ceramic with molten metal applied to ternary carbide MAX phase synthesis. Outcome: no signal. Reason: direct high-temperature reaction between pre-formed carbide and molten metal did not initiate phase formation
Fundamental Formation mechanisms of the MAX phase Zr3AlC2 and small scale mechanical properties of the MAX phases · Imperial · PhD
Tried and failed
molten salt shielded synthesis applied to Zr3AlC2 MAX phase synthesis. Reason: produced unwanted binary phases and heavy zirconium oxide contamination instead of the target ternary phase
Fundamental Formation mechanisms of the MAX phase Zr3AlC2 and small scale mechanical properties of the MAX phases · Imperial · PhD
Tried and failed
supporting molten salt sorbents on alumina substrates applied to high-temperature carbon capture. Outcome: unstable. Reason: destructive solid-state reaction between molten salt and substrate formed inactive ternary compounds, destroying sorption capacity
Molten Alkali Metal Borates for High Temperature Carbon Capture · MIT · PhD
Tried and failed
molten salt ion exchange at high temperature applied to layered transition metal oxide synthesis. Outcome: unstable. Reason: thermal decomposition and structural degradation into rock-salt and spinel secondary phases
Study of iron-based cathode materials for lithium-ion batteries · Oxford · PhD
Tried and failed
direct single-step melting of multicomponent powder mixture applied to multicomponent sulfide electrolyte synthesis. Reason: failed to form a homogeneous melt, requiring multi-step pre-melting
New Methodology to Model Metal Chemistry at High Temperature · MIT · Doctorate
High temperatures cause precursor volatilization, structural decomposition, or unwanted phase changes upon cooling
Prolonged heating or high temperatures caused volatile constituents to sublime or boil off, while target phases suffered thermal decomposition into elemental or degraded species. Several high-temperature phases decomposed or hydrated during cooling, and excessive thermal processing induced unwanted grain coarsening.
Tried and failed
solid-state high-temperature reaction of precursor salts applied to synthesis of pure anti-perovskite phases. Outcome: unstable. Reason: thermodynamic instability prevented pure phase formation from precursor mixtures
Low melting point solid electrolytes for scalable manufacturing of all-solid-state li-ion batteries · Georgia Tech · PhD
Tried and failed
direct thermal synthesis doping with volatile precursors applied to high-temperature ceramic semiconductor synthesis. Outcome: no signal. Reason: dopant precursors sublimed below the synthesis temperature required for host lattice formation
Investigating the effect of nonmetal functionalisation on the chemical, sorptive, optoelectronic and photocatalytic properties of semiconducting boron and carbon nitride materials · Imperial · Doctorate
Tried and failed
solid-state synthesis of mixed-anion crystalline phase applied to argyrodite solid electrolyte synthesis. Outcome: unstable. Reason: the target phase was thermodynamically stable only at high temperature and decomposed upon cooling
Design and Development of High-Performance Solid Electrolyte for All-Solid-State Lithium Ion Batteries · Georgia Tech · PhD
Tried and failed
extended high-temperature solid-state metathesis applied to chromium nitride synthesis from oxide. Outcome: unstable. Reason: prolonged thermal exposure at high temperature caused product decomposition into elemental metal
SYNTHESIS, CHARACTERIZATION, AND PHOTOTHERMAL PROPERTIES OF PLASMONIC METAL NITRIDE NANOPARTICLES · Dalhousie · PhD
Considered and rejected
Considered and rejected: Solid-state reaction synthesis was rejected in favour of the sol-gel citric-nitrate method due to excessive volatile RuO2 loss and chemical degradation above 1200°C.
Lanthanum nickel oxide based double perovskites and their exsolution phenomena · Imperial · PhD
Considered and rejected
Considered and rejected: High-temperature metallurgical/annealing methods were rejected due to particle sintering/coarsening, phase diagram restrictions, and Bi boiling during synthesis.
ELECTROCHEMICAL SYNTHESIS OF INTERMETALLIC ELECTROCATALYSTS · Johns Hopkins · PhD
Considered and rejected
Considered and rejected: Discarded 3-step solid-state reaction synthesis due to high processing temperatures, long annealing times, and excessive grain growth causing high thermal conductivity.
Development of Cu2SnS3 based thermoelectric materials and devices · University of Trento · PhD
Considered and rejected
Considered and rejected: Rejected slow cooling of NaKCo2TeO6 and Li3Co2SbO6 after high-temperature synthesis due to undesired hydration/decomposition and formation of the orthorhombic polymorph, respectively.
Probing Kitaev Behavior in the Cobaltate Honeycomb Lattice · Johns Hopkins · PhD
Exceeding dopant solubility limits or using incompatible precursors causes phase segregation and poor densification
Exceeding solid solution solubility limits or introducing sub-stoichiometric precursor ratios precipitated insulating secondary phases and caused phase separation. Incompatible precursor decomposition products and excessive dopant substitutions created high porosity and poor densification, while crucible interactions altered cation stoichiometry.
Tried and failed
aliovalent cation doping to increase ionic conductivity applied to solid-state electrolyte crystalline lattices. Outcome: worse than baseline. Reason: exceeded the solid solution solubility limit, precipitating insulating impurity phases
Design and Development of High-Performance Solid Electrolyte for All-Solid-State Lithium Ion Batteries · Georgia Tech · PhD
Tried and failed
solid-state melt synthesis of substituted chalcogenides applied to iron-deficient quaternary sulfide solid solutions. Reason: sub-stoichiometric iron compositions separated into distinct quaternary and binary phase mixtures
Murunskite - a new class of functional material · EPFL · PhD
Tried and failed
high dopant substitution in solid-state sintering applied to ceramic proton conductors. Outcome: worse than baseline. Reason: excessive dopant substitution caused poor densification and high porosity, degrading electrochemical conductivity
Investigation of structure and conductivity of LaNb0.9Mo0.1O4.05 based materials · Imperial · PhD
Considered and rejected
Considered and rejected: Rejected traditional high-temperature solid-solution synthesis because large nucleation barriers prevent trapping metastable misfit phases.
Utilizing Nanoconfinement and Surface Stabilization to Synthesize Metastable Phases of Iron-Containing Selenides · University of Oregon · PhD
Considered and rejected
Considered and rejected: Rejected transition-metal acetates as precursors in SC1 synthesis because C2H3O2 decomposition products generate high powder porosity that limits chemical conversion.
Deciphering the degradation mechanisms of layered oxide cathodes for sodium-ion batteries · UT Austin · PhD
Considered and rejected
Considered and rejected: Rejected alumina crucibles for high-temperature synthesis of high-entropy perovskite oxides because metal ions leach into alumina, using platinum crucibles instead to preserve cation stoichiometry
Left open by the authors
Problems the authors named and did not get to.
Left open
Develop and synthesize cathode composite architectures containing zero added solid-state electrolyte for solid-state lithium batteries. Blocker: Requires a physical wet lab, chemical synthesis, and battery testing facilities
Probing Interfacial Dynamics in Solid-State Lithium Metal Batteries · Georgia Tech · PhD
Left open
Investigate failure mechanisms causing resistive interfaces at anode/sulfide and halide/sulfide electrolyte boundaries in solid-state sodium batteries. Blocker: Requires wet lab electrochemical synthesis and advanced characterization tools to examine battery interface degradation.
Tailoring the electrochemical properties of catholytes for solid-state sodium batteries · UT Austin · PhD
Left open
Develop new sodium- and potassium-ion solid-state electrolytes and explore the interfacial stability model for solid-state batteries. Blocker: Requires materials synthesis, wet lab experimental electrochemistry, and characterization facilities
Fusible alloy electrodes and multi-cation interfacial chemistry in alkali metal batteries · UT Austin · PhD
Left open
Investigate FeF3-based solid-state sodium-ion batteries using solid electrolytes to reduce cathode dissolution. Blocker: Requires a wet/materials chemistry laboratory and experimental apparatus for synthesizing solid electrolytes and assembling solid-state battery cells
IMPROVING ELECTROCHEMICAL PERFROMANCE OF IRON TRIFLUORIDE (FeF3) IN SODIUM-ION BATTERIES · Georgia Tech · PhD
Left open
Screen hetero-element dopants or additives to improve sulfide solid-state electrolyte properties and assess economically viable manufacturing procedures. Blocker: Requires experimental synthesis, physical battery validation, and industrial manufacturing assessment
First-principles exploration and design of sulfide-based electrolytes for lithium metal batteries · UT Austin · PhD
Left open
Pair surface-protected sulfur cathodes with low-concentration electrolytes and evaluate battery performance. Blocker: Requires wet lab synthesis of coated cathodes, electrolyte preparation, and physical battery testing
TUNING ELECTROLYTE COMPOSITION FOR ENHANCED PERFORMANCE OF LITHIUM-SULFUR BATTERIES · Georgia Tech · PhD
Left open
Synthesize polyanionized disordered rocksalt cathodes via solid-state sintering using alternative phosphorus precursors like Li3P or elemental phosphorus. Blocker: Requires a physical materials synthesis and characterization lab with solid-state sintering equipment and chemical handling capabilities.
Polyanionizing rocksalt cathodes for lithium-ion batteries · MIT · PhD
Left open
Synthesize and evaluate single-crystal morphology and surface coatings on high-Ni NMA cathode materials to reduce reactivity and cracking. Blocker: Requires a wet-chemistry battery synthesis lab, precursors, calcination furnaces, and electrochemical cell testing apparatus.
Comprehensive evaluation of cobalt-free, high-nickel layered oxide cathodes for lithium-ion batteries · UT Austin · PhD
Left open
Develop and optimize 3D nanohybrid gyroidal full-cell architectures to overcome sulfur cathode performance limitations. Blocker: Requires a wet lab and materials synthesis/fabrication facilities to construct 3D nanohybrids and coin cells
AN ELECTROANALYTICAL ASSESSMENT OF ORGANIC REDOX TRANSFORMATIONS IN BATTERY AND ELECTROSYNTHETIC APPLICATIONS · Cornell · PhD
Left open
Develop electrolytes and interphases that lower the bulk-to-surface diffusivity ratio to prevent ion piling-up at the electrolyte/electrode interface. Blocker: Requires wet lab chemical synthesis and electrochemical characterization apparatus
Electrodeposition and reversibility of Lithium metal in liquid electrolytes · Cornell · PhD
Who has worked on this
Authors of the public theses cited on this page, most-cited first.
- Yimeng Huang · MIT · PhD · 2023
Polyanionizing rocksalt cathodes for lithium-ion batteries - Jack Lyons · Imperial · PhD · 2022
Fundamental Formation mechanisms of the MAX phase Zr3AlC2 and small scale mechanical properties of the MAX phases - Zhantao Liu · Georgia Tech · PhD · 2021
Design and Development of High-Performance Solid Electrolyte for All-Solid-State Lithium Ion Batteries - William Moore · Cornell · PhD · 2025
NOVEL AND ENHANCED FUNCTIONAL MATERIALS PROPERTIES VIA BLOCK COPOLYMER STRUCTURE DIRECTED POROSITY - Mohammed Nabi · Imperial · PhD · 2023
Using advanced surface analysis techniques to investigate the solid-solid interfaces in solid state batteries - Fischer Harvel · University of Oregon · PhD · 2025
Utilizing Nanoconfinement and Surface Stabilization to Synthesize Metastable Phases of Iron-Containing Selenides - Ioanna Itskou · Imperial · Doctorate · 2024
Investigating the effect of nonmetal functionalisation on the chemical, sorptive, optoelectronic and photocatalytic properties of semiconducting boron and carbon nitride materials - Victor Kenneth Champagne III · Harvard · PhD · 2024
Thermal and Optical Properties of Oxide Coatings for High-Temperature Applications - Yidong Han · Imperial · PhD · 2024
Investigation of structure and conductivity of LaNb0.9Mo0.1O4.05 based materials - S Mahato · Oxford · PhD · 2024
Study of iron-based cathode materials for lithium-ion batteries - Aashray Narla · Georgia Tech · PhD · 2023
Borohydride-based solid electrolytes and polymer composite separators for lithium-ion batteries - Jia Guo · Imperial · PhD · 2023
Lanthanum nickel oxide based double perovskites and their exsolution phenomena
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