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Project Title:  Structure-Property-Processing Correlations in Freeze-Cast Biomimetic Materials: 80NSSC21K0039 Reduce
Images: icon  Fiscal Year: FY 2024 
Division: Physical Sciences 
Research Discipline/Element:
Physical Sciences: MATERIALS SCIENCE--Materials science 
Start Date: 09/29/2020  
End Date: 01/31/2025  
Task Last Updated: 07/01/2025 
Download Task Book report in PDF pdf
Principal Investigator/Affiliation:   Wegst, Ulrike  Ph.D. / Northeastern University 
Address:  Department of Physics 
 
Boston , MA 02115 
Email: u.wegst@northeastern.edu 
Phone:   
Congressional District:
Web:  
Organization Type: UNIVERSITY 
Organization Name: Northeastern University 
Joint Agency:  
Comments: NOTE: PI moved to Northeastern University from Dartmouth College in summer 2020. 
Co-Investigator(s)
Affiliation: 
Erb, Randall  Ph.D. Northeastern University 
Karma, Alain  Ph.D. Northeastern University 
Project Information: Grant/Contract No. 80NSSC21K0039 
Responsible Center: NASA MSFC 
Grant Monitor: Strutzenberg Littles, Louise  
Center Contact: (256) 544-0946 
louise.s@nasa.gov 
Unique ID: 14260 
Solicitation / Funding Source: 2015 NNH15ZTT002N MaterialsLab Open Science Campaigns for Experiments on the International Space Station 
Grant/Contract No.: 80NSSC21K0039 
Project Type: Flight 
Flight Program: ISS 
No. of Post Docs:
No. of PhD Candidates:
No. of Master's Candidates:
No. of Bachelor's Candidates:
No. of PhD Degrees:
No. of Master's Degrees:
No. of Bachelor's Degrees:
Program--Element: MATERIALS SCIENCE--Materials science 
Flight Assignment/Project Notes: End date changed to 01/31/2025 per PI and NSSC information (Ed., 9/20/23)

Task Description: NOTE: Continuation of "Structure-Property-Processing Correlations in Freeze-Cast Biomimetic Materials" (grant 80NSSC18K0305 at Dartmouth College), with the same Principal Investigator, Dr. Ulrike G. K. Wegst, due to PI move to Northeastern University July 1, 2020.

Strong, tough, and lightweight materials are needed for a myriad of structural and functional applications in Space systems and on Earth in diverse strategic fields that range from biomedical, to buildings, transportation and energy generation, or storage. These new, yet to be developed materials, should exhibit unprecedented combinations of strength and toughness, while being manufacturable at low cost and in high volume. Numerous processing techniques have been proposed to produce these materials, but frequently cannot provide the degree of microstructural control needed to manipulate and optimize the property profile, particularly of multifunctional materials. One technique, which holds great promise in fabricating novel materials with great structural control, is freeze-casting, a relatively inexpensive procedure which also provides a means to mimic complex, efficient natural materials with hierarchical designs over several length-scales. The fundamental science and understanding of this processing technique is limited, because, on Earth, convection and sedimentation complicate both the interpretation of experimental results and their comparison with theoretical predications. Avoiding these in space, following four scientific goals will be pursued. To reveal on Earth (Aim 1, completed, see Final Report) and in Space (Aim 2, to be performed, see Final Report) the underlying fundamental materials science of freeze casting and establish a realistic model for structure formation in multifaceted crystal nucleation and growth. Aim 3: Develop predictive models to identify the most promising material processing combinations and conditions to optimize material performance. Aim 4: Translate the results of (1-3) into structure-property-processing correlations for highly porous, freeze-cast scaffolds (polymer, ceramic, metal, and composite) made on Earth. Data obtained and computational models were made available to the NASA Physical Sciences Informatics to make the data accessible to the global community and help translate research into application for an accelerated pace of advanced-materials discovery, innovation, manufacture, and commercialization.

Research Impact/Earth Benefits: Our goal was to apply the fundamental knowledge gained through this study in the development of new and improved freeze-cast (ice-templated) materials that are strong, tough and lightweight and can be custom-designed for a given application. Such materials are required for applications that range from biomedical and tissue regeneration to filtration, catalysis, transportation, and energy generation and storage. Only with fundamental, physics-based models, systematic materials design and synthesis will this be possible. The results, first of the terrestrial (completed, see Final Report) and then the microgravity research (to be performed in the future, see Final Report), was collated, documented, and captured also in a visual format such as in, for example, structure-property-processing charts. With these we wish to enable a paradigm shift towards a more systematic approach in materials synthesis by pointing into particularly promising materials research directions.

Task Progress & Bibliography Information FY2024 
Task Progress: When aqueous solutions or slurries without additives are freeze cast, meaning directionally solidified, the ice crystals grow with their basal plane oriented parallel to the temperature gradient and along the crystallographic <11-20> direction. Because of this orientation, the structure of the typical wine-cork-like freeze-cast sample is lamellar once quasi-steady state solidification has been reached. The first two layers in a sample are dense and cellular in structure, only a few 100 µm thick, and initially formed during the first seconds of solidification, with cooling rates so high that no phase separation occurs, but the dissolved/suspended material is trapped within the ice crystals. In some cases, when water-based biopolymer solutions are freeze cast, the final freeze-cast materials and scaffolds exhibit features that are very unusual for directionally solidified materials; they exhibit, for example: i) highly aligned and regularly spaced ridges of uniform height, ‘jellyfish’-like caps and arrays, and ‘tentacles’-like features parallel to the direction of solidification, and ii) fibrillar pillars and bridges in fiber composites, and even enhanced iii) fibrillation, a form of self-assembly and structure formation in biopolymers such as collagen.

In our study of “Structure-Property-Processing Correlations in Freeze-Cast Biomimetic Materials,” we quantify both the to date little studied complex, dynamic ice crystal growth phenomena and the ice-templated hierarchical architecture of freeze-cast scaffolds as well as the various cell wall surface features, not only because they are of interest from a fundamental science point of view but also because the ridges, pillars, bridges, and fibrillation observed in freeze-cast biopolymer scaffolds frequently result in highly desirable features for biomedical applications. In peripheral nerve repair we observe, for example, that not only the highly aligned porosity, but also cell wall surface ridges serve as powerful structural cues to guide regenerating neurites from one end to the other of the freeze cast regenerative scaffold. While cell wall surface features, such as these regularly spaced ridges, had been observed under specific processing conditions in a range of freeze-cast biopolymers, we found that the fundamental science and underlying principles that govern their formation remain unknown ant that, in fact, more generally, ice crystal growth from the liquid phase and binary or ternary polymer solutions had hardly ever been studied and simulated. We therefore started to systematically study structure-property-processing correlations under well-defined conditions and complement experiments with phase-field (PF) simulations, which are essential to fully understand the observed phenomena and formulate robust and predictive structure-property-processing correlations for the design and manufacture of freeze-cast materials for a great variety of applications that range from biomedical to energy generation and storage, to catalysis, filtration, optical and acoustical absorption, and thermal insulation.

In the first instance, we experimentally determined structure-property-processing correlations for scaffolds freeze-cast from collagen- and chitosan-based scaffolds both in the dry and the fully hydrated states. The results obtained for both ‘smooth’ and ‘fibrillar’ polymer systems contributed to a better understanding of the likely sequence of events during the solidification process and the resulting ice-templated feature formation in the polymer phase. Noteworthy are also discoveries made with respect to the dependence of the mechanical properties, such as modulus, yield strength, and toughness, on processing conditions such as applied cooling rates and mold height, and the resulting structural features such as lamellar spacing (length of the short pore axis of the rectangular pores), and cell wall thickness, and scaffold reinforcing features such as ridges, bridges, and pillars, and preferential molecular alignment with the freezing direction.

These systematic experimental studies were key first steps on the path to our long-term goal of this study: to bridge the current critical knowledge gap, which is the lack of understanding of the fundamental mechanisms of structure formation, initially in freeze-cast polymers and later, also, in particle-based ceramic and metal systems. Knowing how the size and shape of the pores in freeze-cast materials are defined and can be controlled by controlling the ice crystal growth, the need for a better fundamental understanding of the physics of directional solidification in aqueous systems became even more obvious. We overcame the challenge of the absence of equilibrium phase diagrams and also determined concentration- and temperature-dependent diffusion coefficients and viscosities for our ternary chitosan-acetic acid-water system, and further reduced system complexity in support of the PF simulation effort by focusing in our 2D and 3D studies on the binary systems trehalose-water and sucrose-water systems, for which the fundamental properties are known and documented.

Since crystal growth in bulk samples are difficult to observe and characterize in situ, diffusive crystal growth under terrestrial conditions is typically studied in 2D with thin samples. While we initially focused on the traditional light microscopy perpendicular to the moving freezing front – primarily to observe both in aqueous and dimethyl sulfoxide (DMSO)-based systems the formation of Mullins-Sekerka instabilities, and their subsequent reorganization into an array of cells or dendrites, as a function of polymer concentration and cooling rates (which is equal to the product of velocity and thermal gradient in directional solidification) – we subsequently applied in situ X-ray tomoscopy, which is continuous, time-resolved tomography, as the more suitable tool to analyze in 3D the dynamics of both crystal growth and structure formation phenomena. With synchrotron-based tomoscopy, we were able to investigate and determine the kinetics of the ice-phase growth and the mechanisms by which the growing ice-crystals, thus ice phase, templates the polymer phase into a cellular solid with a range of cell wall surface features, while the polymer is increasingly upconcentrated and transitions from an aqueous solution to a glassy solid. Overall, our observation is that 2D thin film experiments should, whenever possible, be complemented by 3D in situ tomoscopy experiments, because it is frequently impossible to extrapolate structure formation phenomena from 2D thin film observations to bulk materials; DMSO is an excellent example for that.

As critical as 3D in situ X-ray tomoscopy is for our quantitative studies, and the observation also of transient events during the directional solidification in freeze casting, are the 3D PF simulations, which were performed for aqueous and DMSO-based systems. Remarkably, the PF simulations of anisotropic, faceted ice crystal growth binary aqueous systems with a dilute impurity (trehalose, sucrose in the case of water, and water in the case of DMSO), reproduced for the first time the various salient features of freeze-cast structures: from the cellular scaffold structure with their characteristic lamellar spacing to the cell wall surface features, such as ridges, which are templated by secondary instabilities on the ice crystal’s basal plane. The value of the 3D phase-field simulations is immense, since they enable us to investigate little studied and not yet modeled mechanisms of hierarchical microstructure formation and cell wall material self-assembly, both of which define anisotropy, property profile, and overall performance of freeze-cast materials. Our results highlight the crucial role of both the solid-liquid interface free-energy and the interface kinetics in structure formation. They also highlight other potentially important physical effects neglected in the phase-field model, such as fluid flow generated by the expansion of ice, which may play a more secondary role in structure formation. From a practical point of view, the ability to accurately predict the detailed temporal evolution of interface structures under prescribed growth conditions is highly informative for optimizing processing routes and material properties.

In preparation of the System Requirements Review (SRR) and microgravity experiments, two Science Requirements Documents (SRDs) were prepared for the CASTing project: first, one for the Pore Formation and Mobility Investigation (PFMI) Insert supported by Redwire Space; then a second, insert-agnostic version, to explore also a newly available platform, MaRVIn of Tec-Masters, Inc. (TMI). A successful System Requirements Review (SRR) to determine flight readiness took place at the Marshall Space Flight Center (MSFC) on October 16, 2024.

Bibliography: Description: (Last Updated: 07/14/2025) 

Show Cumulative Bibliography
 
Articles in Peer-reviewed Journals Wegst UGK, Kamm PH, Yin K, García-Moreno F. "Freeze casting." Nat Rev Methods Primers. 2024 Apr 25;4(1):28. https://doi.org/10.1038/s43586-024-00307-5 , Apr-2024
Articles in Peer-reviewed Journals Kamm PH, Yin K, Neu TR, Schlepütz CM, Garcia-Moreno F, Wegst UGK. "Freeze casting biomimetic materials: X-ray tomoscopy reveals the dynamics of ice templating and structure formation." Microsc. Microanal. 2024 Jul 24;30(1):ozae044.471. https://doi.org/10.1093/mam/ozae044.471 , Jul-2024
Patents PCT/US2024/012288 (WO 2024/155961). Published July 25, 2024. Jul-2024 Jowett N, Wegst UGK. "Viral Vector Functionalized Core-Shell Scaffold."
Patents US 12,230,437 B2. Issued February 18, 2025. Feb-2025 Reese BA, Wegst UGK, Sullivan CR. "Freeze-cast Magnetic Flake Composites."
Significant Media Coverage Wallen H. "PrimeView: Freeze casting." Illustrated summary of Dr. Wegst's research, Nat Rev Methods Primers, 2024 Apr 25;4(1):29. https://doi.org/10.1038/s43586-024-00316-4 , Apr-2024
Significant Media Coverage Rötger A. (Wegst UGK interview). "Freeze casting - A guide to creating hierarchically structured materials." Science Highlight, Helmholtz Centre Berlin for Materials and Energy GmbH website, April 25, 2024. https://www.helmholtz-berlin.de/pubbin/news_seite?nid=26686 ;sprache=en , Apr-2024
Significant Media Coverage Rötger A. (Wegst UGK interview for news release). "Freeze casting – A guide for complex structured materials." News release on IDW website, April 25, 2024. https://idw-online.de/de/news832601 , Apr-2024
Significant Media Coverage Bioengineer. (Wegst UGK interview). "Freeze casting – A guide to creating hierarchically structured materials. " Science News feature on Bioengineer.org website, April 25, 2024. https://bioengineer.org/freeze-casting-a-guide-to-creating-hierarchically-structured-materials/ , Apr-2024
Significant Media Coverage Science News: Chemistry. (Wegst UGK interview). "Freeze casting – A guide to creating hierarchically structured materials." Scienmag Science Magazine. 25 April 2024. https://scienmag.com/freeze-casting-a-guide-to-creating-hierarchically-structured-materials/ , Apr-2024
Significant Media Coverage Helmholtz Association of German Research Centres. (Wegst UGK interview). "Freeze casting—A guide to creating hierarchically structured materials." News feature on Phys.org website, April 25, 2024. https://phys.org/news/2024-04-hierarchically-materials.html , Apr-2024
Significant Media Coverage Helmholtz-Zentrum Berlin für Materialien und Energie. "Freeze casting: A guide to creating hierarchically structured materials." Science News feature on ScienceDaily, April 25, 2025. https://www.sciencedaily.com/releases/2024/04/240425131419.htm , Apr-2024
Significant Media Coverage innoreports. (Wegst UFK interview). "Freeze casting – A guide for complex structured materials." Innovations Report, April 26, 2024. https://www.innovations-report.de/technik/materialwissenschaften/gefriergussverfahren-eine-anleitung-fuer-komplex-strukturierte-materialien/ , Apr-2024
Significant Media Coverage News. (Wegst UFK interview). "Freeze casting: A guide to creating hierarchically structured materials." Pract. Metallogr. May 25, 2024;61(6):412-13. https://doi.org/10.1515/pm-2024-0035 , May-2024
Significant Media Coverage Helmholtz-Zentrum Berlin für Materialien und Energie. "Guide to Hierarchically Structured Materials via Freeze Casting" Science feature on MirageNews website, April 25, 2024. https://www.miragenews.com/guide-to-hierarchically-structured-materials-1222392/ , Apr-2024
Significant Media Coverage NASA. "Image of freeze-cast biopolymer scaffolds. Featured with the month of May in NASA's 2024 Science calendar. Image and text credit: Yin K, Littles L, Wegst UGK, Troy A." NASA Science Calendar 2024. https://eospso.nasa.gov/sites/default/files/publications/2024%20NASA%20Science%20Calendar%20508.pdf , Jan-2024
Project Title:  Structure-Property-Processing Correlations in Freeze-Cast Biomimetic Materials: 80NSSC21K0039 Reduce
Images: icon  Fiscal Year: FY 2023 
Division: Physical Sciences 
Research Discipline/Element:
Physical Sciences: MATERIALS SCIENCE--Materials science 
Start Date: 09/29/2020  
End Date: 01/31/2025  
Task Last Updated: 03/11/2024 
Download Task Book report in PDF pdf
Principal Investigator/Affiliation:   Wegst, Ulrike  Ph.D. / Northeastern University 
Address:  Department of Physics 
 
Boston , MA 02115 
Email: u.wegst@northeastern.edu 
Phone:   
Congressional District:
Web:  
Organization Type: UNIVERSITY 
Organization Name: Northeastern University 
Joint Agency:  
Comments: NOTE: PI moved to Northeastern University from Dartmouth College in summer 2020. 
Co-Investigator(s)
Affiliation: 
Erb, Randall  Ph.D. Northeastern University 
Karma, Alain  Ph.D. Northeastern University 
Project Information: Grant/Contract No. 80NSSC21K0039 
Responsible Center: NASA MSFC 
Grant Monitor: Strutzenberg Littles, Louise  
Center Contact: (256) 544-0946 
louise.s@nasa.gov 
Unique ID: 14260 
Solicitation / Funding Source: 2015 NNH15ZTT002N MaterialsLab Open Science Campaigns for Experiments on the International Space Station 
Grant/Contract No.: 80NSSC21K0039 
Project Type: Flight 
Flight Program: ISS 
No. of Post Docs:
No. of PhD Candidates:
No. of Master's Candidates:
No. of Bachelor's Candidates:
No. of PhD Degrees:
No. of Master's Degrees:
No. of Bachelor's Degrees:
Program--Element: MATERIALS SCIENCE--Materials science 
Flight Assignment/Project Notes: End date changed to 01/31/2025 per PI and NSSC information (Ed., 9/20/23)

Task Description: NOTE: Continuation of "Structure-Property-Processing Correlations in Freeze-Cast Biomimetic Materials" (grant 80NSSC18K0305 at Dartmouth College), with the same Principal Investigator, Dr. Ulrike G. K. Wegst, due to PI move to Northeastern University July 1, 2020.

Strong, tough, and lightweight materials are needed for a myriad of structural and functional applications in Space systems and on Earth in diverse strategic fields that range from biomedical, to buildings, transportation and energy generation, or storage. These new, yet to be developed materials, should exhibit unprecedented combinations of strength and toughness, while being manufacturable at low cost and in high volume. Numerous processing techniques have been proposed to produce these materials, but frequently cannot provide the degree of microstructural control needed to manipulate and optimize the property profile, particularly of multifunctional materials. One technique, which holds great promise in fabricating novel materials with great structural control, is freeze-casting, a relatively inexpensive procedure which also provides a means to mimic complex, efficient natural materials with hierarchical designs over several length-scales. To date, the fundamental science and understanding of this processing technique is limited, because, on Earth, convection and sedimentation complicate both the interpretation of experimental results and their comparison with theoretical predications. Avoiding these in space, following four scientific goals will be pursued. To reveal on Earth (Aim 1) and in Space (Aim 2) the underlying fundamental materials science of freeze casting and establish a realistic model for structure formation in multifaceted crystal nucleation and growth. Aim 3: Develop predictive models to identify the most promising material processing combinations and conditions to optimize material performance. Aim 4: Translate the results of (1-3) into structure-property-processing correlations for highly porous, freeze-cast scaffolds (polymer, ceramic, metal, and composite) made on Earth. Data obtained and computational models will be made available to the NASA Physical Sciences Informatics to make the data accessible to the global community and help translate research into application for an accelerated pace of advanced-materials discovery, innovation, manufacture, and commercialization.

Research Impact/Earth Benefits: Our goal is to apply the fundamental knowledge gained through this study in the development of new and improved freeze-cast (ice-templated) materials that are strong, tough and lightweight and can be custom-designed for a given application. Such materials are required for applications that range from biomedical and tissue regeneration to filtration, catalysis, transportation, and energy generation and storage. Only with fundamental, physics-based models, systematic materials design and synthesis will this be possible. The results, first of the terrestrial and then the microgravity research, will be collated, documented, and captured also in a visual format such as in, for example, structure-property-processing charts. With these we wish to enable a paradigm shift towards a more systematic approach in materials synthesis by pointing into particularly promising materials research directions.

Task Progress & Bibliography Information FY2023 
Task Progress: When aqueous solutions or slurries without additives are freeze cast, meaning directionally solidified, the ice crystals grow with their basal plane oriented parallel to the temperature gradient and along the crystallographic <112 ¯0> direction. Because of this orientation, the structure of the typical wine-cork-like freeze-cast sample is lamellar once quasi-steady state solidification has been reached. The first two layers in a sample are dense and cellular in structure, only a few 100 µm thick, and initially formed during the first seconds of solidification, with cooling rates so high that no phase separation occurs, but the dissolved/suspended material is trapped within the ice crystals.

In some cases, when water-based biopolymer solutions are freeze cast, the final freeze-cast materials and scaffolds exhibit features that are very unusual for directionally solidified materials; they exhibit, for example: i) highly aligned and regularly spaced ridges of uniform height, ‘jellyfish’-like caps and arrays, and ‘tentacles’-like features parallel to the direction of solidification; ii) fibrillar pillars and bridges in fiber composites; and iii) even enhanced fibrillation, a form of self-assembly and structure formation in biopolymers such as collagen.

In our study of “Structure-Property-Processing Correlations in Freeze-Cast Biomimetic Materials,” we quantify both the (to date) little studied, complex, dynamic ice crystal growth phenomena and the ice-templated hierarchical architecture of freeze-cast scaffolds, as well as the various cell wall surface features, not only because they are of interest from a fundamental science point of view but also because the ridges, pillars, bridges, and fibrillation observed in freeze-cast biopolymer scaffolds frequently result in highly desirable features for biomedical applications. In peripheral nerve repair we observe, for example, that not only the highly aligned porosity, but also cell wall surface ridges, serve as powerful structural cues to guide regenerating neurites from one end to the other of the freeze cast regenerative scaffold. While cell wall surface features, such as these regularly spaced ridges, had been observed under specific processing conditions in a range of freeze-cast biopolymers, we found that the fundamental science and underlying principles that govern their formation remain unknown and that, in fact more generally, ice crystal growth from the liquid phase and binary or ternary polymer solutions had hardly ever been studied and simulated. We therefore started to systematically study structure-property-processing correlations under well-defined conditions and complement experiments with phase-field (PF) simulations, which are essential to fully understand the observed phenomena and formulate robust and predictive structure-property-processing correlations for the design and manufacture of freeze-cast materials for a great variety of applications that range from biomedical, to energy generation and storage, to catalysis, filtration, optical and acoustical absorption, and thermal insulation.

In the first instance, we experimentally determined structure-property-processing correlations for scaffolds freeze-cast from collagen- and chitosan-based scaffolds both in the dry and the fully hydrated states. The results obtained for both ‘smooth’ and ‘fibrillar’ polymer systems contributed to a better understanding of the likely sequence of events during the solidification process and the resulting ice-templated feature formation in the polymer phase. Noteworthy are also discoveries made with respect to the dependence of the mechanical properties, such as modulus, yield strength, and toughness, on processing conditions such as applied cooling rates and mold height, and the resulting structural features such as lamellar spacing (length of the short pore axis of the rectangular pores), and cell wall thickness, and scaffold reinforcing features such as ridges, bridges, and pillars, and preferential molecular alignment with the freezing direction.

These systematic experimental studies were key first steps on the path to our long-term goal of this study: to bridge the current critical knowledge gap, which is the lack of understanding of the fundamental mechanisms of structure formation, initially in freeze-cast polymers and later also in particle-based ceramic and metal systems. Knowing how the size and shape of the pores in freeze-cast materials are defined and can be controlled by controlling the ice crystal growth, the need for a better fundamental understanding of the physics of directional solidification in aqueous systems became even more obvious. We overcame the challenge of the absence of equilibrium phase diagrams and also determined concentration- and temperature-dependent diffusion coefficients and viscosities for our ternary chitosan-acetic acid-water system, and further reduced system complexity in support of the PF simulation effort by focusing in our 2D and 3D studies on the binary systems trehalose-water and sucrose-water systems, for which the fundamental properties are known and documented.

Since crystal growth in bulk samples is difficult to observe and characterize in situ, diffusive crystal growth under terrestrial conditions is typically studied in 2D with thin samples. While we initially focused on the traditional light microscopy perpendicular to the moving freezing front primarily to observe both in aqueous and DMSO-based systems the formation of Mullins-Sekerka instabilities and their subsequent reorganization into an array of cells or dendrites as a function of polymer concentration and cooling rates, which is equal to the product of velocity and thermal gradient in directional solidification, we now apply in situ X-ray tomoscopy, which is continuous, time-resolved tomography, as the more suitable tool to analyze in 3D the dynamics of both crystal growth and structure formation phenomena. With synchrotron-based tomoscopy, we have since Year 3 been able to investigate and determine the kinetics of the ice-phase growth and the mechanisms by which the growing ice-crystals, thus ice phase, templates the polymer phase into a cellular solid with a range of cell wall surface features, while the polymer is increasingly upconcentrated and transitions from an aqueous solution to a glassy solid. Overall, our observation is that 2D thin film experiments should, whenever possible, be complemented by 3D in situ tomoscopy experiments, because it is frequently impossible to extrapolate structure formation phenomena from 2D thin film observations to bulk materials; DMSO is an excellent example.

As critical as 3D in situ X-ray tomoscopy is for our quantitative studies and the observation also of transient events during the directional solidification in freeze casting, are the 3D PF simulations, which started in Year 2 for aqueous systems. Remarkably, the PF simulations of anisotropic, faceted ice crystal growth binary aqueous systems with a dilute impurity (trehalose, sucrose), reproduced for the first time the various salient features of freeze-cast structures: from the cellular scaffold structure with their characteristic lamellar spacing to the cell wall surface features such as ridges, which are templated by secondary instabilities on the ice crystal’s basal plane. The value of the 3D phase-field simulations is immense, since they enable us to investigate little studied and not yet modeled mechanisms of hierarchical microstructure formation and cell wall material self-assembly, both of which define anisotropy, property profile, and overall performance of freeze-cast materials. Our results highlight the crucial role of both the solid-liquid interface free-energy and the interface kinetics in structure formation. They also highlight other potentially important physical effects neglected in the phase-field model, such as fluid flow generated by the expansion of ice may play a more secondary role in structure formation. The PF-modelling effort was in 2022 (Year 5) extended to DMSO-based material systems; first results were reported in 2023 (Year 6). From a practical point of view, the ability to accurately predict the detailed temporal evolution of interface structures under prescribed growth conditions is critical for optimizing processing routes and material properties. In preparation for the microgravity experiments, two Science Requirements Documents (SRDs) have been prepared for the CASTing project: one for the Pore Formation and Mobility Investigation (PFMI) Insert and a second insert-agnostic version.

Bibliography: Description: (Last Updated: 07/14/2025) 

Show Cumulative Bibliography
 
Abstracts for Journals and Proceedings Kamm PH, Yin K, Neu TR, Schlepütz CM, Garcia-Moreno F, Wegst UGK. "X-Ray tomoscopy reveals the dynamics of ice templating." MRS Fall Meeting 2022, Boston, MA, USA, November 27 - December 2, 2022. Sponsored by the Materials Research Society (MRS).

Abstracts. MRS Fall Meeting 2022, Boston, MA, USA, November 27 - December 2, 2022. Symposium CH01. , Nov-2022

Abstracts for Journals and Proceedings Qiu K, Wegst UGK. "Excellent mechanical and electrical properties of anisotropic freeze-cast native and carbonized bacterial cellulose-alginate foams." MRS Fall Meeting 2022, Boston, MA, USA, November 27 - December 2, 2022. Sponsored by the Materials Research Society (MRS).

Abstracts. MRS Fall Meeting 2022, Boston, MA, USA, November 27 - December 2, 2022. Symposium EN09. , Nov-2022

Abstracts for Journals and Proceedings Yin K, Divakar P, Wegst UGK. "Plant-derived nanocellulose as structural and mechanical reinforcement of freeze-cast chitosan scaffolds for biomedical applications." MRS Fall Meeting 2022, Boston, MA, USA, November 27 - December 2, 2022. Sponsored by the Materials Research Society (MRS).

Abstracts. MRS Fall Meeting 2022, Boston, MA, USA, November 27 - December 2, 2022. Symposium EN09. , Nov-2022

Abstracts for Journals and Proceedings Wegst UGW. "Biogenic and bioinspired functional materials for sustainability." MRS Fall Meeting 2022, Boston, MA, USA, November 27 - December 2, 2022. Sponsored by the Materials Research Society (MRS).

Abstracts. MRS Fall Meeting 2022, Boston, MA, USA, November 27 - December 2, 2022. Symposium EN09. , Nov-2022

Abstracts for Journals and Proceedings Yin K, Reese BA, Sullivan CR, Wegst UGK. "Magnetic nacre-superior mechanical and magnetic performance of highly anisotropic sendust-flake composites freeze cast in a uniform magnetic field." MRS Fall Meeting 2021, Boston, MA, USA, November 29 - December 2, 2021. Sponsored by the Materials Research Society (MRS).

Abstracts. MRS Fall Meeting 2021, Boston, MA, USA, November 29 - December 2, 2021. Symposium SB09. , Nov-2021

Abstracts for Journals and Proceedings Yin K, Reese BA, Sullivan CR, Wegst UGK. "Mechanical and magnetic performance of highly anisotropic sendust-flake composites freeze cast in a uniform magnetic field." EuroMat 2021, Graz, Austria, September 12-16, 2021.

Abstracts. EuroMat 2021, Graz, Austria, September 12-16, 2021. , Sep-2021

Abstracts for Journals and Proceedings Yin K, Ji K, Strutzenberg L, Trivedi R, Karma A, Wegst UGK. "Experimental observations of mechanisms of pattern formation during freeze casting" 2021 TMS Annual Meeting & Exhibition, Virtual, March 15-18, 2021. Sponsored by The Minerals, Metals & Materials Society (TMS).

Abstracts. 2021 TMS Annual Meeting & Exhibition, Virtual, March 15-18, 2021. , Mar-2021

Abstracts for Journals and Proceedings Ji K, Yin K, Strutzenberg L, Trivedi R, Wegst UGK, Karma A. "Phase-field simulations of pattern formation during freeze casting." 2021 TMS Annual Meeting & Exhibition, Virtual, March 15-18, 2021. Sponsored by The Minerals, Metals & Materials Society (TMS).

Abstracts. 2021 TMS Annual Meeting & Exhibition, Virtual, March 15-18, 2021. , Mar-2021

Abstracts for Journals and Proceedings Wegst UGK. "Nature-inspired materials science – Challenges and opportunities." PittCon Conference & Expo, Atlanta, Georgia, USA, March 8-12, 2021.

Abstracts. PittCon Conference & Expo, Atlanta, Georgia, USA, March 8-12, 2021. , Mar-2021

Abstracts for Journals and Proceedings Wegst UGK, Ji K, Silva M, Strutzenberg LL, Trivedi R, Shubitidze F, Karma A, Yin K. "From fundamental science to tissue scaffolds: Mechanisms of structure formation in ice-templated materials." 8th International Conference on Mechanics of Biomaterials and Tissues (ICMOBT), Waikoloa, HI, December 15-19, 2019.

Abstracts. 8th International Conference on Mechanics of Biomaterials and Tissues (ICMOBT), Waikoloa, HI, December 15-19, 2019. , Dec-2019

Abstracts for Journals and Proceedings Yin K, Mylo MD, Speck T, Wegst UGK, "Bamboo-inspired porous tubes: Permeability, flow, and water purification." 8th International Conference on Mechanics of Biomaterials and Tissues (ICMOBT), Waikoloa, HI, December 15-19, 2019.

Abstracts. 8th International Conference on Mechanics of Biomaterials and Tissues (ICMOBT), Waikoloa, HI, December 15-19, 2019. , Dec-2019

Abstracts for Journals and Proceedings Yin K, Priemel T, Divakar P, Harrington MJ, Wegst UGK. "Fibrillation and alignment of plant-derived nanocellulose, chitosan, and collagen in freeze-cast scaffolds." 8th International Conference on Mechanics of Biomaterials and Tissues (ICMOBT), Waikoloa, HI, December 15-19, 2019.

Abstracts. 8th International Conference on Mechanics of Biomaterials and Tissues (ICMOBT), Waikoloa, HI, December 15-19, 2019. , Dec-2019

Abstracts for Journals and Proceedings Yin K, Divakar P, Wegst UGK. "Plant-derived nanocellulose as structural and mechanical reinforcement of freeze-cast chitosan scaffolds for biomedical applications." MRS Fall Meeting 2019, Boston, MA, December 1-6, 2019. Sponsored by the Materials Research Society (MRS).

Abstracts. MRS Fall Meeting 2019, Boston, MA, December 1-6, 2019. Symposium MS03. , Dec-2019

Abstracts for Journals and Proceedings Ji K, Yin K, Strutzenberg LL, Trivedi R, Shubitidze F, Wegst UGK, Karma A. "3D phase-field simulations explain experimental observations of structure formation in ice-templated materials." MRS Fall Meeting 2019, Boston, MA, December 1-6, 2019. Sponsored by the Materials Research Society (MRS).

Abstracts. MRS Fall Meeting 2019, Boston, MA, December 1-6, 2019. Symposium MT06. , Dec-2019

Abstracts for Journals and Proceedings Yin K, Ji K, Silva M, Strutzenberg LL, Trivedi R, Shubitidze F, Karma A, Wegst UGK. "Mechanisms of structure formation in ice-templated materials: Experimental observations." MRS Fall Meeting 2019, Boston, MA, December 1-6, 2019. Sponsored by the Materials Research Society (MRS).

Abstracts. MRS Fall Meeting 2019, Boston, MA, December 1-6, 2019. Symposium MT06. , Dec-2019

Abstracts for Journals and Proceedings Wegst UGK. "Porous metals by freeze casting: Challenges and opportunities." TMS MetFoam 2019, Dearborn, MI, August 20-23, 2019. Sponsored by The Minerals, Metals & Materials Society (TMS).

Abstracts. TMS MetFoam 2019, Dearborn, MI, August 20-23, 2019. , Aug-2019

Abstracts for Journals and Proceedings Wegst UGK. "Biogenic and bioinspired functional materials for sustainability and a more circular economy." Nano-Micromaterials for Circular Economy and Sustainability, National University of Singapore, Singapore, August 29 - September 1, 2019.

Abstracts. Nano-Micromaterials for Circular Economy and Sustainability, National University of Singapore, Singapore, August 29 - September 1, 2019. , Sep-2019

Abstracts for Journals and Proceedings Yin K, Divakar P, Mohan S, Sundback, CA, Jowett N, Wegst UGK. "Structure-property-processing correlations and in vivo performance of freeze-cast chitosan-nanocellulose scaffolds." 9th International Plant Biomechanics Conference, Montreal, Quebec, Canada, August 9-14, 2018.

Abstracts. 9th International Plant Biomechanics Conference, Montreal, Quebec, Canada, August 9-14, 2018. , Aug-2018

Abstracts for Journals and Proceedings Wegst UGK. "Bioinspired materials and devices and their assessment in vitro and in vivo." 2nd Bioinspired Interfacial Materials and Devices Conference, Beihang University, Beijing, China, June 22–24, 2018.

Abstracts. 2nd Bioinspired Interfacial Materials and Devices Conference, Beihang University, Beijing, China, June 22–24, 2018. , Jun-2018

Abstracts for Journals and Proceedings Wegst UGK. "Architecture of natural and freeze-cast materials." Gordon Research Conference on Thin Film and Small Scale Mechanical Behavior, Micro- and Nano-Mechanics as a Tool for Materials Design, Lewiston, ME, July 15-20, 2018.

Abstracts. Gordon Research Conference on Thin Film and Small Scale Mechanical Behavior, Micro- and Nano-Mechanics as a Tool for Materials Design, Lewiston, ME, July 15-20, 2018. , Jul-2018

Abstracts for Journals and Proceedings Wegst UGK. "Freeze casting – The controlled solidification of water for the manufacture of new and improved materials." NUconvergence 2018: Frontiers in Aerospace Materials, Microgravity Materials Research, Northeastern University, Boston, MA, May 18-19, 2018.

Abstracts. NUconvergence 2018: Frontiers in Aerospace Materials, Microgravity Materials Research, Northeastern University, Boston, MA, May 18-19, 2018. , May-2018

Abstracts for Journals and Proceedings Wegst UGK, Divakar P, Yin K, Moodie KL, Hoopes PJ, Theiler R, Sundback C, Matthew M, Jowett N, Rosen J. "Biological materials, biomaterials, and biomimetics: Emulating performance-defining features in bulk with a fast and easy production process." 7th International Conference on Mechanics of Biomaterials and Tissues (ICMOBT), Big Island, HI, December 10-14, 2017.

Abstracts. 7th International Conference on Mechanics of Biomaterials and Tissues (ICMOBT), Big Island, HI, December 10-14, 2017. , Dec-2017

Abstracts for Journals and Proceedings Wegst UGK. "Employing the complex dynamics of ice templating to tailor performance-defining features in biomedical materials." 9th International Conference on Mechanics of Biomaterials and Tissues (ICMOBT), Waikoloa, HI, December 16 - 20, 2023.

Abstracts: 9th International Conference on Mechanics of Biomaterials and Tissues (ICMOBT), Waikoloa, HI, USA, December 16 - 20, 2023. , Dec-2023

Abstracts for Journals and Proceedings Wegst UGK. "Freeze casting peptide-enabled biomaterials for tissue regeneration." MRS Fall Meeting 2023, Boston, MA, November 26 - December 1, 2023. Sponsored by the Materials Research Society (MRS).

Abstracts. MRS Fall Meeting 2023, Boston, MA, November 26 - December 1, 2023. Symposium SB03. , Nov-2023

Abstracts for Journals and Proceedings Kamm PH, Yin K, Neu TR, Schlepütz CM, Garcia-Moreno F, Wegst UGK. "Ice crystal growth and the dynamics of ice templating by X-ray tomoscopy." MRS Fall Meeting 2023, Boston, MA, USA, November 26 - December 1, 2023. Sponsored by the Materials Research Society (MRS).

Abstracts. MRS Fall Meeting 2023, Boston, MA, USA, November 26 - December 1, 2023. Symposium SF02. , Nov-2023

Abstracts for Journals and Proceedings Ji K, Zhong M, Yin K, Littles LS, Trivedi R, Wegst UGK, Karma A. "Phase-field modeling of ice-templated hierarchical structures." MRS Fall Meeting 2023, Boston, MA, November 26 - December 1, 2023. Sponsored by the Materials Research Society (MRS).

Abstracts. MRS Fall Meeting 2023, Boston, MA, November 26 - December 1, 2023. Symposium SF02. , Nov-2023

Articles in Peer-reviewed Journals Kamm PH, Yin K, Neu TR, Schlepütz CM, Garcia-Moreno F, Wegst UGK. "X-ray tomoscopy reveals the dynamics of ice templating." Adv. Funct. Mater. 2023 Nov;33(48):2304738. https://doi.org/10.1002/adfm.202304738 , Nov-2023
Articles in Peer-reviewed Journals Yin K, Ji K, Strutzenberg Littles L, Trivedi R, Karma A, Wegst UGK. "Hierarchical structure formation by crystal growth-front instabilities during ice templating." PNAS. 2023 Jun 6;120(23):e2210242120. https://doi.org/10.1073/pnas.2210242120 , Jun-2023
Articles in Peer-reviewed Journals Caruso I, Yin K, Divakar P, Wegst UGK. " Tensile properties of freeze-cast collagen scaffolds: How processing conditions affect structure and performance in the dry and fully hydrated states." J. Mech. Behav. Biomed. Mater. 2023 Aug 1;144:105897. https://doi.org/10.1016/j.jmbbm.2023.105897 , Aug-2023
Dissertations and Theses Ji K. "Phase-field modeling of microstructural pattern dormation during ice templating and alloy solidification." Dissertation, Northeastern University, November 2021. , Nov-2021
Dissertations and Theses Yin K. "Freeze casting: From the fundamentals to applications." Dissertation, Thayer School of Engineering, Dartmouth College, May 2020. , May-2020
NASA Technical Documents Radlinska A, Bracker G, Collins P, Edmunson J, Edwards D, Fiske M, Phillips B, Sperl M, Sansoucie M, Shulman H, Strutzenberg L, Weber R, Wegst UGK. "Manufacturing from regolith." Huntsville, AL : Marshall Space Flight Center, 2021. NASA/20210023598. https://ntrs.nasa.gov/api/citations/20210023598/downloads/Manufacturing%20from%20Regolith%20-%20Concept%20Paper%20-%20Radlinska%20FINAL.pdf , Oct-2021
Project Title:  Structure-Property-Processing Correlations in Freeze-Cast Biomimetic Materials: 80NSSC21K0039 Reduce
Images: icon  Fiscal Year: FY 2022 
Division: Physical Sciences 
Research Discipline/Element:
Physical Sciences: MATERIALS SCIENCE--Materials science 
Start Date: 09/29/2020  
End Date: 12/31/2023  
Task Last Updated: 11/10/2022 
Download Task Book report in PDF pdf
Principal Investigator/Affiliation:   Wegst, Ulrike  Ph.D. / Northeastern University 
Address:  Department of Physics 
 
Boston , MA 02115 
Email: u.wegst@northeastern.edu 
Phone:   
Congressional District:
Web:  
Organization Type: UNIVERSITY 
Organization Name: Northeastern University 
Joint Agency:  
Comments: NOTE: PI moved to Northeastern University from Dartmouth College in summer 2020. 
Co-Investigator(s)
Affiliation: 
Erb, Randall  Ph.D. Northeastern University 
Karma, Alain  Ph.D. Northeastern University 
Project Information: Grant/Contract No. 80NSSC21K0039 
Responsible Center: NASA MSFC 
Grant Monitor: Strutzenberg Littles, Louise  
Center Contact: (256) 544-0946 
louise.s@nasa.gov 
Unique ID: 14260 
Solicitation / Funding Source: 2015 NNH15ZTT002N MaterialsLab Open Science Campaigns for Experiments on the International Space Station 
Grant/Contract No.: 80NSSC21K0039 
Project Type: Flight 
Flight Program: ISS 
No. of Post Docs:
No. of PhD Candidates:
No. of Master's Candidates:
No. of Bachelor's Candidates:
No. of PhD Degrees:
No. of Master's Degrees:
No. of Bachelor's Degrees:
Program--Element: MATERIALS SCIENCE--Materials science 
Task Description: NOTE: Continuation of "Structure-Property-Processing Correlations in Freeze-Cast Biomimetic Materials" (grant 80NSSC18K0305 at Dartmouth College), with the same Principal Investigator, Dr. Ulrike Wegst, due to PI move to Northeastern University in summer 2020.

Strong, tough, and lightweight materials are needed for a myriad of structural and functional applications in Space systems and on Earth in diverse strategic fields that range from biomedical, to buildings, transportation and energy generation, or storage. These new, yet to be developed materials, should exhibit unprecedented combinations of strength and toughness, while being manufacturable at low cost and in high volume. Numerous processing techniques have been proposed to produce these materials, but frequently cannot provide the degree of microstructural control needed to manipulate and optimize the property profile, particularly of multifunctional materials. One technique, which holds great promise in fabricating novel materials with great structural control, is freeze-casting, a relatively inexpensive procedure which also provides a means to mimic complex, efficient natural materials with hierarchical designs over several length-scales. To date, the fundamental science and understanding of this processing technique is limited, because, on Earth, convection and sedimentation complicate both the interpretation of experimental results and their comparison with theoretical predications. Avoiding these in space, following four scientific goals will be pursued. To reveal on Earth (Aim 1) and in Space (Aim 2) the underlying fundamental materials science of freeze casting and establish a realistic model for structure formation in multifaceted crystal nucleation and growth. Aim 3: Develop predictive models to identify the most promising material processing combinations and conditions to optimize material performance. Aim 4: Translate the results of (1-3) into structure-property-processing correlations for highly porous, freeze-cast scaffolds (polymer, ceramic, metal, and composite) made on Earth. Data obtained and computational models will be made available to the NASA Physical Sciences Informatics to make the data accessible to the global community and help translate research into application for an accelerated pace of advanced-materials discovery, innovation, manufacture, and commercialization.

Research Impact/Earth Benefits: Our goal is to apply the fundamental knowledge gained through this study in the development of new and improved freeze-cast (ice-templated) materials that are strong, tough and lightweight and can be custom-designed for a given application. Such materials are required for applications that range from biomedical and tissue regeneration to filtration, catalysis, transportation, and energy generation and storage. Only with fundamental, physics-based models, systematic materials design and synthesis will this be possible. The results of the terrestrial and microgravity research will be collated, documented, and captured also in a visual format such as in, for example, structure-property-processing charts. With these we wish to enable a paradigm shift towards a more systematic approach in materials synthesis by pointing into particularly promising materials research directions.

Task Progress & Bibliography Information FY2022 
Task Progress: When aqueous solutions or slurries without additives are freeze-cast, meaning directionally solidified, the ice crystals grow with their basal plane oriented parallel to the temperature gradient and along the crystallographic <11-20> direction. Because of this orientation, the structure of the typical wine-cork-like freeze-cast sample is lamellar once quasi-steady state solidification has been reached. The first two layers in a sample are dense and cellular in structure, only a few 100 µm thick, and initially formed during the first seconds of solidification, with cooling rates so high that no phase separation occurs, but the dissolved/suspended material is trapped within the ice crystals.

In some cases, when water-based biopolymer solutions are freeze-cast, the final freeze-cast materials and scaffolds exhibit features that are very unusual for directionally solidified materials; they exhibit, for example: i) highly aligned and regularly spaced ridges of uniform height, ‘jellyfish’-like caps and arrays, and ‘tentacles’-like features parallel to the direction of solidification, and ii) fibrillar pillars and bridges in fiber composites, and even enhanced iii) fibrillation, a form of self-assembly and structure formation in biopolymers such as collagen.

In our study of “Structure-Property-Processing Correlations in Freeze-Cast Biomimetic Materials,” we quantify both the (to date, little studied) complex, dynamic ice crystal growth phenomena and the ice-templated hierarchical architecture of freeze-cast scaffolds, as well as the various cell wall surface features, not only because they are of interest from a fundamental science point of view but also because the ridges, pillars, bridges, and fibrillation observed in freeze-cast biopolymer scaffolds frequently result in highly desirable features for biomedical applications. In peripheral nerve repair, we observe, for example, that not only the highly aligned porosity, but also cell wall surface ridges serve as powerful structural cues to guide regenerating neurites from one end to the other of the freeze-cast regenerative scaffold. While cell wall surface features, such as these regularly spaced ridges, had been observed under specific processing conditions in a range of freeze-cast biopolymers, we found that the fundamental science and underlying principles that govern their formation remain unknown and that, in fact, more generally, ice crystal growth from the liquid phase and binary or ternary polymer solutions had hardly ever been studied and simulated. We therefore started to systematically study structure-property-processing correlations under well-defined conditions and complement experiments with phase-field (PF) simulations, which are essential to fully understand the observed phenomena and formulate robust and predictive structure-property-processing correlations for the design and manufacture of freeze-cast materials for a great variety of applications that range from biomedical to energy generation and storage, to catalysis, filtration, optical and acoustical absorption, and thermal insulation.

In the first instance, we experimentally determined structure-property-processing correlations for scaffolds freeze-cast from collagen- and chitosan-based scaffolds, both in the dry and the fully hydrated states. The results obtained for both ‘smooth’ and ‘fibrillar’ polymer systems contributed to a better understanding of the likely sequence of events during the solidification process and the resulting ice-templated feature formation in the polymer phase. Noteworthy are also discoveries made with respect to the dependence of the mechanical properties, such as modulus, yield strength, and toughness, on processing conditions such as applied cooling rates and mold height, and the resulting structural features such as lamellar spacing (length of the short pore axis of the rectangular pores), and cell wall thickness, and scaffold reinforcing features such as ridges, bridges, and pillars, and preferential molecular alignment with the freezing direction.

These systematic experimental studies were key first steps on the path to our long-term goal of this study: to bridge the current critical knowledge gap, which is the lack of understanding of the fundamental mechanisms of structure formation, initially in freeze-cast polymers, and later also in particle-based ceramic and metal systems. Knowing how the size and shape of the pores in freeze-cast materials are defined and can be controlled by controlling the ice crystal growth, the need for a better fundamental understanding of the physics of directional solidification in aqueous systems becomes even more obvious. We overcame the challenge of the absence of equilibrium phase diagrams and, even more important, the non-equilibrium state diagrams, which describe the metastable ‘states’ fundamental to an understanding of these systems; we determined concentration- and temperature-dependent diffusion coefficients and viscosities for our ternary chitosan-acetic acid-water system; and further reduced system complexity in support of the PF simulation effort by focusing our 2D and 3D studies on the binary systems trehalose-water and sucrose-water systems, for which the fundamental properties are known and documented.

Since crystal growth in bulk samples are difficult to observe and characterize in situ, diffusive crystal growth under terrestrial conditions is typically studied in 2D with thin samples. These thin samples are designed so that the solidification conditions can be controlled carefully and only a single, two-dimensional (2D) array of dendrites (or cells) forms, and the solid-liquid interface, interface dynamics, and the formation of instabilities can be observed. Initially (in Years 1-3), we focused on the traditional light microscopy perpendicular to the moving freezing front primarily in the trehalose-water and sucrose-water systems. To observe the formation of Mullins-Sekerka instabilities and their subsequent reorganization into an array of cells or dendrites as a function of polymer concentration and cooling rates (which is equal to the product of velocity and thermal gradient in directional solidification), we discovered X-ray tomoscopy, which is continuous, time-resolved tomography, as the more suitable tool for crystal growth phenomena.

With synchrotron-based tomoscopy, we have in Years 3 and 4 been able to investigate and determine the kinetics of the ice-phase growth and the mechanisms by which the growing ice crystals (thus ice phase), templates the polymer phase into a cellular solid with a range of cell wall surface features, while the polymer is increasingly upconcentrated and transitions from an aqueous solution to a glassy solid. Overall, our observation is that 2D thin film experiments should, whenever possible, be complemented by 3D in situ tomoscopy experiments, because it is impossible to extrapolate structure formation phenomena from thin film observations to bulk materials, in which the third dimension and grain or domain interactions play an important role.

As critical as 3D in situ X-ray tomoscopy has become for our study for the quantitative 3D imaging and observation also of transient events during the directional solidification in freeze-casting, are the 3D PF simulations, which started in Year 2. Remarkably, the PF simulations of anisotropic, faceted ice crystal growth binary aqueous systems with a dilute impurity (trehalose, sucrose), reproduced for the first time the various salient features of freeze-cast structures: from the cellular scaffold structure with their characteristic lamellar spacing to the cell wall surface features such as ridges, which are templated by secondary instabilities on the ice crystal’s basal plane. The value of the 3D phase-field simulations is immense, since they enable us to investigate little studied and not yet modeled mechanisms of hierarchical microstructure formation and cell wall material self-assembly, both of which define anisotropy, property profile, and overall performance of freeze-cast materials. Our results highlight the crucial role of both the solid-liquid interface free-energy and the interface kinetics in structure formation. They also highlight that other potentially important physical effects neglected in the phase-field model, such as fluid flow generated by the expansion of ice, may play a more secondary role in structure formation.

From a practical point of view, the ability to accurately predict the detailed temporal evolution of interface structures under prescribed growth conditions is critical for optimizing processing routes and material properties.

Bibliography: Description: (Last Updated: 07/14/2025) 

Show Cumulative Bibliography
 
Articles in Peer-reviewed Journals Yin K, Divakar P, Wegst UGK. "Plant-derived nanocellulose as structural and mechanical reinforcement of freeze-cast chitosan scaffolds for biomedical applications." Biomacromolecules. 2019 Aug 27;20(10):3733-45. https://doi.org/10.1021/acs.biomac.9b00784 ; PMID: 31454234; PMCID: PMC6800197 , Aug-2019
Articles in Peer-reviewed Journals Yin K, Mylo MD, Speck T, Wegst UGK. "Bamboo-inspired tubular scaffolds with functional gradients." J Mech Behav Biomed Mater. 2020 Oct;110:103826. https://doi.org/10.1016/j.jmbbm.2020.103826 ; PMID: 32957175 , Oct-2020
Articles in Peer-reviewed Journals Yin K, Mylo MD, Speck T, Wegst UGK. "2D and 3D graphical datasets for bamboo-inspired tubular scaffolds with functional gradients: micrographs and tomograms." Data Brief. 2020 Jun 17;31:105870. https://doi.org/10.1016/j.dib.2020.105870 ; PMID: 32642506; PMCID: PMC7334595 , Jun-2020
Articles in Peer-reviewed Journals Yin K, Reese BA, Sullivan CR, Wegst UGK. "Superior mechanical and magnetic performance of highly anisotropic sendust-flake composites freeze cast in a uniform magnetic field." Adv. Funct. Mater. 2020 Dec 3. https://doi.org/10.1002/adfm.202007743 , Dec-2020
Articles in Peer-reviewed Journals Yin K, Divakar P, Wegst UGK. "Structure-property-processing correlations of longitudinal freeze-cast chitosan scaffolds for biomedical applications." J Mech Behav Biomed Mater. 2021 Sep;121:104589. https://doi.org/10.1016/j.jmbbm.2021.104589 ; PMID: 34126508 , Sep-2021
Articles in Peer-reviewed Journals Qiu K, Wegst UGK. "Excellent specific mechanical and electrical properties of anisotropic freeze-cast native and carbonized bacterial cellulose-alginate foams." Adv. Funct. Mater. 2021 Jun 11;32(1):2105635. https://doi.org/10.1002/adfm.202105635 , Jun-2021
Dissertations and Theses Yin K. "Freeze casting: From the fundamentals to the applications." PhD Thesis, Thayer School of Engineering, Dartmouth College, May 2020. , May-2020
Dissertations and Theses Ji K. "Phase-field modeling of microstructural pattern formation during ice templating and alloy solidification." PhD Thesis. Department of Physics, Northeastern University, October 2021. , Oct-2021
Project Title:  Structure-Property-Processing Correlations in Freeze-Cast Biomimetic Materials: 80NSSC21K0039 Reduce
Images: icon  Fiscal Year: FY 2021 
Division: Physical Sciences 
Research Discipline/Element:
Physical Sciences: MATERIALS SCIENCE--Materials science 
Start Date: 09/29/2020  
End Date: 12/31/2023  
Task Last Updated: 03/11/2024 
Download Task Book report in PDF pdf
Principal Investigator/Affiliation:   Wegst, Ulrike  Ph.D. / Northeastern University 
Address:  Department of Physics 
 
Boston , MA 02115 
Email: u.wegst@northeastern.edu 
Phone:   
Congressional District:
Web:  
Organization Type: UNIVERSITY 
Organization Name: Northeastern University 
Joint Agency:  
Comments: NOTE: PI moved to Northeastern University from Dartmouth College in summer 2020. 
Co-Investigator(s)
Affiliation: 
Erb, Randall  Ph.D. Northeastern University 
Karma, Alain  Ph.D. Northeastern University 
Project Information: Grant/Contract No. 80NSSC21K0039 
Responsible Center: NASA MSFC 
Grant Monitor: Strutzenberg Littles, Louise  
Center Contact: (256) 544-0946 
louise.s@nasa.gov 
Unique ID: 14260 
Solicitation / Funding Source: 2015 NNH15ZTT002N MaterialsLab Open Science Campaigns for Experiments on the International Space Station 
Grant/Contract No.: 80NSSC21K0039 
Project Type: Flight 
Flight Program: ISS 
No. of Post Docs:
No. of PhD Candidates:
No. of Master's Candidates:
No. of Bachelor's Candidates:
No. of PhD Degrees:
No. of Master's Degrees:
No. of Bachelor's Degrees:
Program--Element: MATERIALS SCIENCE--Materials science 
Task Description: NOTE: Continuation of "Structure-Property-Processing Correlations in Freeze-Cast Biomimetic Materials" (grant 80NSSC18K0305 at Dartmouth College), with the same Principal Investigator, Dr. Ulrike Wegst, due to PI move to Northeastern University in summer 2020.

Strong, tough, and lightweight materials are needed for a myriad of structural and functional applications in Space systems and on Earth in diverse strategic fields that range from biomedical, to buildings, transportation and energy generation, or storage. These new, yet to be developed materials, should exhibit unprecedented combinations of strength and toughness, while being manufacturable at low cost and in high volume. Numerous processing techniques have been proposed to produce these materials, but frequently cannot provide the degree of microstructural control needed to manipulate and optimize the property profile, particularly of multifunctional materials. One technique, which holds great promise in fabricating novel materials with great structural control, is freeze-casting, a relatively inexpensive procedure which also provides a means to mimic complex, efficient natural materials with hierarchical designs over several length-scales. To date, the fundamental science and understanding of this processing technique is limited, because, on Earth, convection and sedimentation complicate both the interpretation of experimental results and their comparison with theoretical predications. Avoiding these in space, following four scientific goals will be pursued. To reveal on Earth (Aim 1) and in Space (Aim 2) the underlying fundamental materials science of freeze casting and establish a realistic model for structure formation in multifaceted crystal nucleation and growth. Aim 3: Develop predictive models to identify the most promising material processing combinations and conditions to optimize material performance. Aim 4: Translate the results of (1-3) into structure-property-processing correlations for highly porous, freeze-cast scaffolds (polymer, ceramic, metal, and composite) made on Earth. Data obtained and computational models will be made available to the NASA Physical Sciences Informatics to make the data accessible to the global community and help translate research into application for an accelerated pace of advanced-materials discovery, innovation, manufacture, and commercialization.

Research Impact/Earth Benefits: Our goal is to apply the fundamental knowledge gained through this study in the development of new and improved freeze-cast (ice-templated) materials that are strong, tough and lightweight and can be custom-designed for a given application. Such materials are required for applications that range from biomedical and tissue regeneration to filtration, catalysis, transportation, and energy generation and storage. Only with fundamental, physics-based models, systematic materials design and synthesis will this be possible. The results of the terrestrial and microgravity research will be collated, documented, and captured also in a visual format such as in, for example, structure-property-processing charts. With these we wish to enable a paradigm shift towards a more systematic approach in materials synthesis by pointing into particularly promising materials research directions.

Task Progress & Bibliography Information FY2021 
Task Progress: The basis of freeze casting is a phase-separation-induced solvent templating of a second phase (polymers, particles, or both). Templating involves a large number of process-defining parameters. Four categories of parameters determine the structure and properties of the freeze-cast material: i) the chemistry of the solution or slurry system (e.g., polymer and/or particle composition and properties such as charge, size and shape); ii) additives and impurities (and their effects on either the solvent, polymer or particles); iii) processing conditions (e.g., cooling rate, temperature field); and iv) the physics of solvent nucleation and growth. Empirically over the past 20-25 years, strategies have been developed to control some of these parameters in an attempt to custom-design and manufacture, in a single processing step, material over several length-scales. Lacking are quantitative, predictive, mesoscopic models. Phase-field (PF) simulations parallel our systematic experiments with experimentally relevant parametric ranges. Critical for the performance of freeze-cast materials is their hierarchical architecture, which is ice-templated during the process of directional solidification. The formation of instabilities, (initially dendrites, later also secondary structures such as ridges and other surface features on the cell walls), play a critical role in governing the solute segregation pattern that controls the property and reliability of the freeze-cast materials or scaffold. Fundamental and key parameters and the physics that govern dendritic growth in the directional solidification of aqueous systems remain little understood; similarly, the origin and subsequent dynamic structural evolution. The main goal of our research and study is to quantitatively establish the fundamental physics that critically control the spatiotemporal organization of structural features and their interaction under directional solidification conditions. Our project addresses several outstanding issues that still remain open in our understanding of the complex dendritic microstructure formed during freeze casting. We focused in Years 1-3 on Research Aims 1, 3 and 4, and on water-based systems, and started working on dimethyl sulfoxide (DMSO)-based systems.

A discovery made, in Years 2-4, through 3D PF simulations is the significance of the anisotropy of the water-ice system for the initiation of formation of performance-defining features and patterns in freeze-cast materials, which consist of primary dendrites and secondary structures such as ridges or other surface side branches and might be further enhanced by interdendritic solute flow and forces resulting from the 9% volumetric expansion of water upon solidification. The value of such 3D phase-field simulations is immense, since they enable us to investigate little studied and not yet modeled mechanisms of hierarchical microstructure formation and cell wall material self-assembly, both of which define anisotropy, property profile, and overall performance of freeze-cast materials.

Bibliography: Description: (Last Updated: 07/14/2025) 

Show Cumulative Bibliography
 
 None in FY 2021
Project Title:  Structure-Property-Processing Correlations in Freeze-Cast Biomimetic Materials: 80NSSC21K0039 Reduce
Images: icon  Fiscal Year: FY 2020 
Division: Physical Sciences 
Research Discipline/Element:
Physical Sciences: MATERIALS SCIENCE--Materials science 
Start Date: 09/29/2020  
End Date: 12/31/2023  
Task Last Updated: 01/27/2021 
Download Task Book report in PDF pdf
Principal Investigator/Affiliation:   Wegst, Ulrike  Ph.D. / Northeastern University 
Address:  Department of Physics 
 
Boston , MA 02115 
Email: u.wegst@northeastern.edu 
Phone:   
Congressional District:
Web:  
Organization Type: UNIVERSITY 
Organization Name: Northeastern University 
Joint Agency:  
Comments: NOTE: PI moved to Northeastern University from Dartmouth College in summer 2020. 
Co-Investigator(s)
Affiliation: 
Erb, Randall  Ph.D. Northeastern University 
Karma, Alain  Ph.D. Northeastern University 
Project Information: Grant/Contract No. 80NSSC21K0039 
Responsible Center: NASA MSFC 
Grant Monitor: Strutzenberg Littles, Louise  
Center Contact: (256) 544-0946 
louise.s@nasa.gov 
Unique ID: 14260 
Solicitation / Funding Source: 2015 NNH15ZTT002N MaterialsLab Open Science Campaigns for Experiments on the International Space Station 
Grant/Contract No.: 80NSSC21K0039 
Project Type: Flight 
Flight Program: ISS 
No. of Post Docs:  
No. of PhD Candidates:  
No. of Master's Candidates:  
No. of Bachelor's Candidates:  
No. of PhD Degrees:  
No. of Master's Degrees:  
No. of Bachelor's Degrees:  
Program--Element: MATERIALS SCIENCE--Materials science 
Task Description: NOTE: Continuation of "Structure-Property-Processing Correlations in Freeze-Cast Biomimetic Materials" (grant 80NSSC18K0305 at Dartmouth College), with the same Principal Investigator, Dr. Ulrike Wegst, due to PI move to Northeastern University in summer 2020.

Strong, tough, and lightweight materials are needed for a myriad of structural and functional applications in Space systems and on Earth in diverse strategic fields that range from biomedical, to buildings, transportation and energy generation, or storage. These new, yet to be developed materials, should exhibit unprecedented combinations of strength and toughness, while being manufacturable at low cost and in high volume. Numerous processing techniques have been proposed to produce these materials, but frequently cannot provide the degree of microstructural control needed to manipulate and optimize the property profile, particularly of multifunctional materials. One technique, which holds great promise in fabricating novel materials with great structural control, is freeze-casting, a relatively inexpensive procedure which also provides a means to mimic complex, efficient natural materials with hierarchical designs over several length-scales. To date, the fundamental science and understanding of this processing technique is limited, because, on Earth, convection and sedimentation complicate both the interpretation of experimental results and their comparison with theoretical predications. Avoiding these in space, following four scientific goals will be pursued. To reveal on Earth (Aim 1) and in Space (Aim 2) the underlying fundamental materials science of freeze casting and establish a realistic model for structure formation in multifaceted crystal nucleation and growth. Aim 3: Develop predictive models to identify the most promising material processing combinations and conditions to optimize material performance. Aim 4: Translate the results of (1-3) into structure-property-processing correlations for highly porous, freeze-cast scaffolds (polymer, ceramic, metal, and composite) made on Earth. Data obtained and computational models will be made available to the NASA Physical Sciences Informatics to make the data accessible to the global community and help translate research into application for an accelerated pace of advanced-materials discovery, innovation, manufacture, and commercialization.

Research Impact/Earth Benefits: Our goal is to apply the fundamental knowledge gained through this study in the development of new and improved freeze-cast (ice-templated) materials that are strong, tough and lightweight and can be custom-designed for a given application. Such materials are required for applications that range from biomedical and tissue regeneration to filtration, catalysis, transportation, and energy generation and storage. Only with fundamental, physics-based models, systematic materials design and synthesis will this be possible. The results of the terrestrial and microgravity research will be collated, documented, and captured also in a visual format such as in, for example, structure-property-processing charts. With these we wish to enable a paradigm shift towards a more systematic approach in materials synthesis by pointing into particularly promising materials research directions.

Task Progress & Bibliography Information FY2020 
Task Progress: New project for FY2020.

NOTE: Continuation of "Structure-Property-Processing Correlations in Freeze-Cast Biomimetic Materials" (grant 80NSSC18K0305 at Dartmouth College), with the same Principal Investigator, Dr. Ulrike Wegst, due to PI move to Northeastern University in summer 2020.

Bibliography: Description: (Last Updated: 07/14/2025) 

Show Cumulative Bibliography
 
 None in FY 2020