3D printed high-throughput hydrothermal reactionware for discovery, optimization, and scale-up.

Area of Science:

• Materials Science
• Chemical Engineering
• Crystallography

Background:

• Traditional reactionware limits experimental flexibility and scalability.
• Hydrothermal synthesis requires specialized, often custom-designed, equipment.

Purpose of the Study:

• To design and fabricate sealed, monolithic reactors using 3D printing for hydrothermal synthesis.
• To demonstrate the utility of 3D printed reactors in materials discovery and synthesis optimization.
• To assess the scalability of synthesis using 3D printed reactors.

Main Methods:

• Digital design and 3D printing of monolithic reactors.
• Direct introduction of reaction mixtures during reactor fabrication.
• High-throughput screening using 3D printed reactor arrays.
• Optimization and scale-up of coordination polymer synthesis.

Main Results:

• Successful fabrication of sealed, monolithic reactors with tailored geometries and scales.
• Discovery of two new coordination polymers using high-throughput 3D printed reactors.
• Optimization and successful scale-up of a new coordination polymer's synthesis.
• Production of phase-pure MIL-96 and HKUST-1 in comparable yields to traditional methods.

Conclusions:

• 3D printing provides a versatile platform for creating custom reactionware for hydrothermal synthesis.
• This approach accelerates materials discovery and enables efficient synthesis optimization and scale-up.
• 3D printed reactors offer a viable alternative to traditional apparatus for producing advanced materials.