High Throughput Methods in the Synthesis, Characterization, and Optimization of Porous Materials

Abstract

Notwithstanding these impediments, in many fields of materials science, solutions are being designed to mitigate hindrances to the efficient sampling of chemical space and improving the robustness of computational screening models through a combination of high throughput synthesis (HTS), characterization, and machine learning. In this review, we highlight key developments in high throughput approaches pertinent to porous materials. Specifically, we focus on developments in the field of zeolitic materials, metal-organic frameworks (MOFs), and touch upon covalent organic frameworks (COFs). Although superficially these classes of materials have little in common, there are structural links such as topology which allow for the consideration of how high throughput methods contrast with one another. By contrasting developments in different fields, we identify some underutilized approaches which could be leveraged in the future. We target structurally ordered materials because the exploration of chemical and topological space is more straightforward to enumerate, though similar approaches could be applied to disordered materials. The scale of the problem faced in materials science of targeted structure and function [1] is by no means unique; in drug discovery, HTS and chemoinformatic approaches have been used for more than 40 years in an attempt to accelerate the discovery of druggable molecules. [2,3] Unlike the drug discovery process, where Lipinski's "rule of 5" [4] provides a reliable top level sift for viable targets, identifying the most promising material for a target application requires very particular properties that may be intertwined in complex and contradictory ways. For example, thermoelectrics require high electrical conductivity and low thermal conductivity and yet these properties are typically correlated unless they can be separated. [5] Given the large scope of potential applications, the advent of the Materials Genome Initiative (MGI) [6,7] in the United States has undoubtedly helped to promote ways to solve the aforementioned obstacles and numerous others. Similarly there are major initiatives within the EU (e.g., NOMAD [8] and BIGmax [9]) and Switzerland (MARVEL [10]). In the MGI, nanoporous materials, including zeolites and MOFs, have been specifically targeted [11] and in this review, we seek to highlight particular challenges in the field of porous materials and how researchers have sought to overcome these challenges. We focus primarily on the methods used in HTS and rapid throughput/screening computational approaches. Aspects of high throughput computation applied to porous materials have been reviewed before, [12-14] as has high throughput experimentation (HTE) [15,16] but here we focus on their combination within an integrated workflow. Porous materials are widely employed in a large range of applications, in particular, for storage, separation, and catalysis of fine chemicals. Synthesis, characterization, and pre-and post-synthetic computer simulations are mostly carried out in a piecemeal a...

Exploring and expanding the Fe-terephthalate metal–organic framework phase space by coordination and oxidation modulation

“…It is both surprising and intriguing to have discovered a new structure in a phase space which has already been explored so extensively, but also that it possesses a rarely seen topology. This highlights how much phase complexity is perhaps missed, or even omitted, during many conventional synthetic studies, and we expect that with the arrival and implementation of automation 51 and machine learning 52 in combination with new modulated self-assembly protocols, 35 that this will become even more evident for other MOF systems.…”

“…This highlights how much phase complexity is perhaps missed, or even omitted, during many conventional synthetic studies, and we expect that with the arrival and implementation of automation 51 and machine learning 52 in combination with new modulated self-assembly protocols, 35 that this will become even more evident for other MOF systems.…”

Advancement in Organic Synthesis Through High Throughput Experimentation

“…This review focuses on HTE efforts to guide organic synthesis and understand the challenges and potential future areas of development that have been reported between January 2016 to January 2021. Publications describing high throughput discovery strategies [5] such as DNA-encoded libraries, [6] PROTAC based HTE, [7] biocatalytic transformations [8] in continuous flow synthesis, [9] kinetic data acquisition in catalytic transformations, [10] or optimization of porous inorganic materials [11] are outside the scope of this review. A recent article [12] has provided insight into high throughput experimen- tation from an industrial standpoint; however, this Minireview focuses on the use of HTE tools to develop new methodologies and optimization of key transformations in target oriented synthesis.…”

Recent Advances of Porous Materials Based on Cyclodextrin

“…However, there are few reviews on porous materials based on CDs although porous materials have been reviewed by many researchers. [ 22–24 ]…”