High-Throughput Methods in Materials Science (Part I): A Review of Chemical and Physical Methods and Automated Sample...

Artificial intelligence (AI) and machine learning (ML) algorithms possess the capability to accelerate the design of novel materials; however, their advancement in materials science is severely hindered by a fundamental deficit of experimental data, commonly referred to as data starvation. Unlike solution-based chemistry, where high-throughput (HT) technologies are a well-established standard, the automated synthesis of solid materials-particularly polymers and multicomponent composites-poses an extreme engineering challenge. Furthermore, the traditional, manual research model is inherently flawed by human bias, notably the systematic non-publication of negative results, which deprives AI models of critical boundary information regarding the design space. This paper is the first in a three-part review series defining the architecture of a fully automated, unbiased "data factory" for closed-loop discovery. This section focuses on the physical foundations of the HT workflow: experimental planning, automated synthesis, and material management. Emphasis is placed on the paradigm shift from classical, discrete Design of Experiments (DoE) to the novel concept of Continuous Gradient DoE. It reviews how robotic platforms utilizing precise gravimetric and volumetric feeders, integrated with extruders and in-line capillary rheology, enable the seamless, high-throughput manufacturing of thermoplastics and composites. Moreover, an innovative approach to sample logistics is presented, redefining classical storage patterns through the implementation of Continuous Material Management. This encompasses direct physical tagging (e.g., inkjet marking on continuous filaments or films), spool-based transport systems, and precise, real-time metadata mapping. As demonstrated, the integration of these systems yields an order-of-magnitude increase in productivity (generating tens of thousands of novel material variants annually), a radical reduction in unit costs, and the production of terabytes of standardized, machine-readable data. Establishing this reliable hardware and analytical infrastructure represents the essential first step toward unlocking the full potential of artificial intelligence in advanced materials engineering.