Chapter Four · failure evidence

What Microencapsulation Technologies got wrong, from 32 dissertations

The records evaluate various microencapsulation formulations and processing techniques across drug delivery, self-healing materials, and thermal storage applications. Many investigated systems encountered failures including mechanical shell fracture during drying, poor retention leading to cargo leakage, and insufficient loading capacity. These records come from PhD theses at 14 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.

Shell rupture and morphological defects occur during microcapsule synthesis and drying

7 theses · 5 institutions

Microcapsule shells frequently ruptured, collapsed, or fractured when subjected to spray drying, antisolvent precipitation, or core volume expansion. Insufficient incubation or formulation imbalances such as absent surfactant also led to thin leaking walls, nonspherical tailed particles, and polymer aggregation.

Tried and failed

thermogelling polymer nanoemulsion formulation without surfactant applied to hydrophobic drug encapsulation hydrogels. Outcome: unstable. Reason: insufficient surfactant led to large droplet size and low viscosity, forming tailed particles instead of spheres

Nanoemulsion-Loaded Hydrogels For Advanced Pharmaceutical Formulations · MIT

Tried and failed

thin single-layer ALD oxide encapsulation applied to phase-change materials undergoing volume changes. Outcome: unstable. Reason: mechanical stress from volume expansion caused encapsulation failure, surface roughening, and material volatilization

Improving the reliability of optical phase change materials-based devices · MIT

Tried and failed

fatty alcohol phase change material coating applied to microcapsule pore sealing. Outcome: unstable. Reason: formed uneven, cracked layers that adhered poorly and detached easily

Bioinspired microrobotic systems for targeted and on-demand cargo delivery · Imperial

Tried and failed

sacrificial core dissolution in layer-by-layer assembly applied to hollow biopolymer microcapsule fabrication. Outcome: unstable. Reason: Core dissolution solvent caused irreversible bridging flocculation and aggregation of outer polymer layers

Platelet-inspired microparticles for targeted drug delivery to the atherosclerotic plaque · Imperial

Tried and failed

lower speed homogenization for Pickering emulsion templating applied to hollow microcapsule fabrication. Outcome: unstable. Reason: larger emulsion droplets formed fragile shells that ruptured during antisolvent precipitation

NOVEL STARCH MODIFICATIONS: FABRICATION AND APPLICATIONS · Cornell

Tried and failed

short-duration culture for bio-capsule shell synthesis applied to bacterial cellulose capsule formation. Outcome: unstable. Reason: insufficient incubation time resulted in thin, fragile shells that ruptured and leaked

Functional Materials Grown from Engineered Bacteria · Harvard

Considered and rejected

Considered and rejected: Rejected air drying and spray drying for fumed silica microcapsule powder preparation due to capsule collapse and high fracture rates

Synthesizing Semiconductor Nanowires in Hollow Microcapsules via the Geode Process · Georgia Tech

Tried and failed

spray drying applied to hollow inorganic microcapsules. Outcome: unstable. Reason: thermal and shear stresses caused extensive shell fracturing and particle breakage

Synthesizing Semiconductor Nanowires in Hollow Microcapsules via the Geode Process · Georgia Tech

Inadequate wall materials and processing methods lead to low encapsulation efficiency

6 theses · 4 institutions

Formulations relying on single wall materials, nanoprecipitation, or specific polymers such as PEG-PLGA and maltodextrin failed to achieve acceptable payload levels. Conventional double emulsion processes and unmodified liposomes also exhibited deficient loading capacity, excessive protein loss, or sub-therapeutic morpholino delivery.

Lost to a baseline

Untreated SFPC liposomes had slightly higher initial encapsulation efficiency for vitamin E (89 ± 3%) and vitamin C (72 ± 5%) compared to untreated MFGM liposomes (77 ± 5% and 65 ± 4%).

Synthesis and Characterization of Liposomes for pH-triggered Delivery of Hydrophilic and Lipophilic Bioactives · Cornell

Considered and rejected

Considered and rejected: Rejected conventional solvent extraction/evaporation double emulsion encapsulation due to resulting polydisperse microcapsules, low encapsulation efficiency, and excessive protein loss.

Microfluidic PLGA Microcapsules for the Sustained Delivery of Recombinant Human Bone Morphogenetic Protein 2 in 3D Printed PCL/βTCP Scaffolds · Penn

Considered and rejected

Considered and rejected: Rejected PEG-PLGA and maltodextrin (MDX) polymers for HB encapsulation due to low encapsulation efficiency (<5%) compared to CMC.

PROTECTIVE EFFECTS OF CYANIDIN-3-O-GLUCOSIDE-RICH HASKAP (LONICERA CAERULEA L.) BERRY AGAINST NITROSAMINE-INDUCED LUNG CARCINOGENESIS · DalSpace

Considered and rejected

Considered and rejected: Rejected using single wall material (such as maltodextrin alone) due to quick gastrointestinal release, deficient emulsification, and lower encapsulation efficiency.

Dietary supplementation of haskap berry (Lonicera caerulea L.) anthocyanin-rich fraction and probiotics attenuates the severity of dextran sulfate sodium-induced acute colitis in Balb/C mice · DalSpace

Considered and rejected

Considered and rejected: Rejected single-step traditional nanoprecipitation due to low drug encapsulation caps (<10 wt%).

Post Exposure Prophylaxis for HIV in the sexual exposure scenario (PEPSE): Development of a novel nanoformulation · University of Nottingham Repository

Considered and rejected

Considered and rejected: Abandoned polymersome encapsulation of antisense morpholinos for in vivo gene knockdown because released concentration was too low (~350 pmol/mL) to reach functional in vivo doses without aggregation.

Regulating Gene Expression With Light-Activated Oligonucleotides · Penn

Membrane permeability and phase separation cause premature cargo leakage and burst release

5 theses · 4 institutions

Encapsulated payloads frequently leaked into external phases or across carrier membranes because of low lipid phase transition temperatures or acidic deposition conditions. Polymer matrices exceeding entrapment capacity suffered liquid phase separation, while nanoparticle carriers exhibited rapid burst release that prevented functional delivery.

Tried and failed

double emulsion solvent evaporation encapsulation applied to hydrophilic small molecule drug loading. Reason: hydrophilic drug partitioned into external aqueous phase, resulting in zero encapsulation

Construction of a highly potent inhalable microparticles combination therapy to treat pulmonary tuberculosis · Imperial

Tried and failed

direct liposome encapsulation of proteins applied to protein delivery vehicle preparation. Reason: low phase transition temperature caused cargo leakage, while higher transition temperature lipids caused thermal artifacts

Development of tools and methods for protein identification: From single molecules to in vivo applications · EPFL

Tried and failed

freeze-thaw polymer hydrogel encapsulation of ionic liquids applied to drug delivery ionogel patches. Outcome: unstable. Reason: ionic liquid concentrations exceeding capacity could not be entrapped, leading to liquid phase separation onto surfaces

Overcoming Barriers in the Gastrointestinal Tract with Ionic Liquids · Harvard

Considered and rejected

Considered and rejected: Rejected calcium carbonate-PSS/PSS-PAH multilayer microcapsules due to ~58% cargo leakage during layer-by-layer polymer deposition at acidic pH

Bioengineered stimuli-responsive microcarriers for multi-drug delivery towards the treatment of bacterial infections · Imperial

Lost to a baseline

PAA NPs loaded with Dox via encapsulation failed to deliver Dox in vitro due to rapid burst release compared to PEI-functionalized NPs

Hierarchical Assemblies of Soft Matters From Polymers and Liquid Crystals on Structured Surfaces · Penn

Embedded self-healing microcapsules suffer mechanical destruction and degrade composite durability

5 theses · 4 institutions

Embedded healing capsules suffered premature destruction under high-shear mixing and degraded composite fatigue life or structural strength. Capsule systems also failed because self-healing chemicals were irreversibly consumed after initial repair or because strain energy dissipated before activating crack bridging.

Tried and failed

embedded deployable metamaterial capsules for mechanical actuation applied to crack bridging in polymer composites. Reason: strain energy dissipated completely before reaching actuation loads, preventing structural resilience under stress

Self-healing mechanism in polymer composite materials · Cranfield

Lost to a baseline

Capsule addition reduced unhealed fatigue cycles compared to neat asphalt at certain low loads (e.g., at 621 N, neat SMA resisted 5800 cycles vs 3900 cycles for capsule F)

Optimisation of encapsulated oil properties to maximise asphalt self-healing · University of Nottingham Repository

Considered and rejected

Considered and rejected: Extrinsic self-healing (microcapsules) was rejected due to vulnerability to destruction under high-shear mixing and short service lifespan for 20-25 year turbine applications.

Improved Material Formulations for Thick Adhesive Joints in Wind Turbine Blades · EPFL

Considered and rejected

Considered and rejected: Chemical self-healing mechanisms requiring microcapsules were rejected because self-healing agents are consumed during repair, preventing repeated autonomous healing.

Multifunctional flexible conductive materials for supercapacitors and biosensors · MSpace - University of Manitoba

Considered and rejected

Considered and rejected: Rejected vascular networks / embedded extrinsic capsule healing systems due to vascular network blockage over time and severe degradation of structural strength.

Self-Healing Polymer Nanocomposites for Composite Structure applications · Cranfield

Left open by the authors

Problems the authors named and did not get to.

Left open

Test non-pH responsive, PBS-soluble anticancer drugs for encapsulation and release in pH-responsive methacrylic polymersomes. Blocker: Requires a wet chemistry and biology lab to synthesize polymersomes and perform drug encapsulation/release assays

Self-assembled block copolymers: micelles, polymersomes and gels · Imperial

Left open

Optimize polymer composition and crosslinking density of poly(amine) microcapsules and evaluate their responsiveness in biologically relevant conditions. Blocker: Requires a wet lab, microfluidic devices, chemical synthesis, and biological testing assays.

Engineering Functional Microcapsules for Controlled Cargo Delivery · Harvard

Left open

Develop a single-capsule combined formulation of curcumin and ursolic acid lipid microspheres to reduce daily pill burden. Blocker: Requires a wet lab and pharmaceutical manufacturing equipment (hot-melt rotating disk and encapsulation tools).

Phase 1 clinical trial evaluating safety, bioavailability, and gut microbiome with a combination of curcumin and ursolic acid in lipid enhanced capsules · UT Austin

Left open

Develop encapsulation and on-demand release mechanisms for diverse antibacterial molecules using polyCu-MOF@AgNPs. Blocker: Requires a wet chemistry and biological testing laboratory to synthesize MOFs and test drug release.

New Metal Complexes and Metal-Organic Frameworks (MOFs) with Potential Biological Applications · IRIS - UNICAM - prod

Left open

Develop advanced encapsulation techniques such as nanocarriers, coacervation systems, and dual-phase emulsions to co-stabilize vitamin D and zinc. Blocker: Requires a wet chemistry/food science laboratory and sensory/bioavailability testing apparatus.

Fortified Foods with Vitamin D and Zinc · Cornell

Left open

Test nanoparticle treatment of chronic biofilm airway infections in βENaC-overexpressing transgenic mice without using artificial bead encapsulation. Blocker: Requires wet lab, animal facility access, and transgenic βENaC-overexpressing mouse models for in vivo infection experiments.

Controlling the Bio-Nano Interface via Engineered Layer-by-Layer Nanoparticles for Treatment of Biofilm-Based Infections · MIT

Left open

Optimize encapsulation efficiency of hydrophilic and hydrophobic payloads in DSPC liposomes across varying concentration gradients. Blocker: Requires wet lab equipment for liposome synthesis, extrusion, dialysis, and chemical encapsulation measurement

Biomimetic water-based lubrication: an exploration into vesicle lubrication · Imperial

Left open

Synthesize a microencapsulated phase change material with latent heat >=390 J/g and improved encapsulation for pavement thermal delay. Blocker: Requires chemical synthesis wet lab and encapsulation apparatus to produce and test the physical material.

Evaluation of Novel Asphalt Binder Modifiers and Additives to Improve Extreme Temperature Rheological Properties for Enhanced Pavement Performance · Texas Tech

Left open

Model layer-by-layer assembly and thermal heat transfer performance for phase change material microcapsules with more than two polyelectrolyte layers. Blocker: None

Development of Energy Systems Towards a Low Carbon Future: From Atoms to Policies · Cornell

Left open

Investigate phase separation kinetics and cargo diffusion pathways in PFH-hexane liquid-shell microcapsules under thermal stimuli. Blocker: Requires wet lab equipment, microfluidic devices, chemical synthesis, and specialized thermal imaging/characterization apparatus.

Engineering Functional Microcapsules for Controlled Cargo Delivery · Harvard

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