Development of Combinatorial Chemistry Methods for Coatings:  High-Throughput Optimization of Curing Parameters of Coatings Libraries

Abstract

An automated analytical system has been implemented for the high-throughput optimization of processing conditions such as curing parameters in fabrication of UV-cured automotive organic protective coatings. Selection of optimum process conditions of combinatorial arrays of coatings is essential to correlate the high-throughput screening and conventional processes and to achieve the desired physical properties of coatings. For monitoring of curing conditions of each coating in the array, a viscosity-sensitive fluorophore 4,4'-bis(2-benzoxazolyl)stilbene was incorporated into coating formulations. This fluorescence tagging approach permitted us to combine a gradient temperature heater and a UV curing system with the full capabilities of our high-throughput screening system, including generation of spectroscopic data and its analysis. This investigation demonstrated the possibility of rapid decoupling of temperature and radiation effects in curing of UV-curable coating formulations by using multiple coatings and process conditions at once. While the system described here was implemented for high-throughput optimization of temperature conditions of radiation curing of arrays of organic protective coatings for automotive applications, this system can be further applied for a variety of other applications where optimization of process parameters can be studied in situ or off-line using optical spectroscopic tools.

Combinatorial and High‐Throughput Materials Science

“…The concept satisfies the essential needs of high data compatibility and versatility together with convenient data import and export. Potyrailo and co-workers [121][122][123] presented a centralized data-management and storage system for their work on organic polymer and hybrid coatings. One important fact of their approach is the sharing of information from synthesis, testing, and evaluation by the database.…”

High‐Throughput Experimentation in Organic Coating and Thin Film Research: State‐of‐the‐Art and Future Perspectives

“…Recently, Potyrailo et al reported a combinatorial tool for investigating UV-curing as a function of temperature. [10] Acrylated aliphatic urethane oligomers were doped with a fluorophore (4,4 0 -bis(2-benzoxazolyl)stilbene), applied on a gradient heater and exposed to a curing radiation (Figure 2, top and right). The fluorophore probe alters its emission spectrum as a function of the curing conditions.…”

“…Set-up for the measurement of the cross-linking behavior of polymer films as a function of UV curing conditions (taken from ref. [10] ).…”

“…Establishing quantitative structure-property relationships enabling prediction and design of material performance remains a challenge for coatings and coating formulations. [1,6,10] b) Close the loop: There is wide agreement that step changes in R&D effectiveness and efficiency are only achieved if all elements of a high-throughput screening work-flow are in place. Design of experiment, formulation, film application, film property testing, and data analysis need to go hand in hand.…”

Techniques and Instrumentation for Combinatorial and High‐Throughput Polymer Research: Recent Developments

“…[2] Optimal curing conditions of doped acrylated aliphatic urethanes were determined by Potyrailo et al with respect to curing temperature and curing radiation. [3] High-throughput techniques for materials testing, such as e.g., abrasion resistance, [4] adhesion, [5] and wettability [6] have also been established.…”