The design and preparation of porous materials with controlled structures and functionalities is crucial to a variety of absorption‐ or separation‐relevant applications, including CO2 capture. Here, novel functional polymeric materials with three‐dimensionally ordered macroporous (3DOM) structures are prepared by using colloidal crystals as templates using relatively simple, rapid, and inexpensive approaches. These ordered structures are used for the reversible CO2 capture from ambient air by humidity swing. Typically, the colloidal crystal template is synthesized from polymer latex particles of poly(methyl methacrylate) (PMMA) or polystyrene (PS). To maintain the functionality of the material, it is important to prevent the porous structure collapsing, which can occur by the hydrolysis of the ester bonds in conventional crosslinkers under basic conditions. This hydrolysis can be prevented by using a water‐soluble crosslinker containing two quaternary ammonium moieties, which can be used to prepare stable porous crosslinked polymers with the monomer (vinylbenzyl)trimethylammonium chloride (VBTMACl) and using a PMMA‐based colloidal crystal template. The hydroxide‐containing monomer and dicationic crosslinker are synthesized from their chloride precursors, avoiding the ion‐exchange step which causes shrinkage of the pores. An analysis of different methods for infiltrating the monomer solution into the colloidal crystal template shows that infiltration using capillary forces leads to fewer defects than infiltration under a partial vacuum. In addition, functional macroporous films with micrometer thickness are prepared from a template of PS‐based colloidal crystals in a thin film. In general, the colloidal crystal templated materials showed improved CO2 absorption/desorption rates and swing sizes compared to a commercially available material with similar functional groups. This work could easily be extended to create a new generation of ordered macroporous polymeric materials with tunable functionalities for other applications.

Three‐dimensionally ordered macroporous (3DOM) hydrogels prepared by colloidal crystals templating display highly reversible shape memory properties, as confirmed by indirect electron microscopy imaging of their inverse replicas and direct nanoscale resolution X‐ray microscopy imaging of the hydrated hydrogels. Modifications of functional groups in the 3DOM hydrogels result in various materials with programmed properties for a wide range of applications.

X-ray microscopy instruments have the unique ability to achieve nondestructive imaging with higher spatial resolutions than traditional X-ray computed tomography (CT) systems. This unique ability is of interest to industrial quality control entities, as they deal with small features in precision manufactured parts. Since many of today’s technology and manufacturing companies demand increasingly higher levels of precision, accuracy, and reliability for dimensional measurements on feature sizes that are much smaller than 5mm, it would be ideal to further expand the imaging capabilities of X-ray microscopy to the field of precision metrology. To address such demand, this paper describes the development of a measurement workflow, through a package consisting of hardware and software, to improve the accuracy of dimensional data obtained with 3D X-ray microscopes (XRM). The workflow, called Metrology Extension (MTX), was designed to adjust and configure the XRM instrument work-zone to perform dimensional measurements. The main adjustments of an XRM instrument through MTX workflow, which must be implemented before scanning parts of interest for dimensional evaluation, include applying a distortion map correction on the image projections produced by the X-ray detector and a voxel scale correction prior to data reconstruction. The main purpose of this article is to present, evaluate, and analyze the experimental results of various measurement tests to verify the metrological performance of several XRM systems operating with the MTX workflow. The main results show that these systems can produce repeatable and reproducible measurements, with repeatability standard deviations of the order of 0.1μm, reproducibility standard deviations of less than 0.5μm, and measurement accuracies comparable to those offered by high-precision tactile coordinate measurement machines (with deviations within the range of ±0.95µm). Therefore, once the MTX workflow is executed, XRM instruments can be used to measure small volumes, in the order of (5mm)3 or less, with improved dimensional accuracy.

Three‐dimensionally ordered macroporous (3DOM) functional polymeric materials are synthesized by K. Matyjaszewski and co‐workers using colloidal crystal templating. These porous 3DOM materials are successfully used for reversible CO2 capture by humidity swing.

Today, 3D X-ray microscopes (XRMs) have the unique ability to achieve higher resolution, non-destructive imaging, within larger parts than traditional X-ray micro computed tomography (CT) systems. Such unique capability is, more and more, of interest to industrial quality control entities as they grapple with small features in precision manufactured parts for various industries such as automotive, electronics, aerospace, medical devices, and additive manufacturing, to name a few examples.