Ongoing software developments for creating three-dimensional (3D) printed crystallographic models seamlessly from Crystallographic Information Framework (CIF) data (*.cif files) are reported. Color versus monochrome printing is briefly discussed. Recommendations are made on the basis of our preliminary printing efforts. A brief outlook on new materials for 3D printing is given.

A statistically sound procedure for the unambiguous identification of the underlying Bravais lattice of an image of a 2D periodic array of objects is described. Our Bravais lattice detection procedure is independent of which type of microscope has been utilized for the recording of the image data. It is particularly useful for the correction of Scanning Tunneling Microscope (STM) images that suffer from a blunt scanning probe tip artifact, i.e. simultaneously recording multiple mini-tips. The unambiguous detection of the type of translation symmetry presents a first step towards making objective decisions about which plane symmetry a 2D periodic image is best modeled by. Such decisions are important for the application of Crystallographic Image Processing (CIP) techniques to images from Scanning Probe Microscopes (SPMs).

Complementing a multitude of activities around the International Year of Crystallography, we report here on a few resources that are helpful for integrating basic crystallography into interdisciplinary college education. We concentrate on four resources with which we are directly involved. The Crystallography Open Database (COD) features currently more than 295,000 entries and has over the last decade developed into the world’s premier open-access source for the structures of small molecules and small to medium sized unit cell crystals. ‘Educational offshoots’ of the COD with approximately a thousand entries combined provide structural information on small molecules, selected macromolecules, crystal structures, grain boundaries, and crystal morphologies in the well documented Crystallographic Information Framework (CIF) file format. This information can be displayed interactively on the website http://nanocrystallography.research.pdx.edu and freely downloaded. Files that allow for the printing of selected database entries on any 3D printer have been added to this site and are also freely downloadable. These files were created with the programs Cif2VRML and WinXMorph that convert CIF files directly into 3D printing files. Interested college educators are invited to visit our open access crystallography resource portal and suggest other resources that should receive wider exposure over this portal.

An automated technique for the mapping of nanocrystal phases and orientations in a transmission electron microscope (TEM) is briefly described. It is primarily based on the projected reciprocal lattice geometry that is extracted automatically from precession electron diffraction (PED) enhanced spot patterns. The required hardware allows for a scanning-precession movement of the primary electron beam on the crystalline sample and can be interfaced to any newer or older mid-voltage TEM. Comprehensive open-access crystallographic databases that may be used in support of this technique are mentioned.

Strategies for the structurally identification of nanocrystals from Precession Electron Diffraction (PED) patterns in a Transmission Electron Microscope (TEM) are outlined. A single-crystal PED pattern may be utilized for the structural identification of an individual nanocrystal. Ensembles of nanocrystals may be fingerprinted structurally from “powder PED patterns”. Highly reliable “crystal orientation & structure” maps may be obtained from automatically recorded and processed scanning-PED patterns at spatial resolutions that are superior to those of the competing electron backscattering diffraction technique of scanning electron microscopy. The analysis procedure of that automated technique has recently been extended to Fourier transforms of high resolution TEM images, resulting in similarly effective mappings. Open-access crystallographic databases are mentioned as they may be utilized in support of our structural fingerprinting strategies.

We present a quantitative investigation of data quality using electron precession, compared to standard selected-area electron diffraction (SAED). Data can be collected on a CCD camera and automatically extracted by computer. The critical question of data quality is addressed – can electron diffraction data compete with X-ray diffraction data in terms of resolution, completeness and quality of intensities?

GeSn alloy nanocrystals were formed by implantation of Ge and Sn ions into an amorphous SiO2 matrix and subsequent thermal annealing. High resolution transmission electron microscopy (HRTEM) and scanning transmission electron microscopy (STEM) with a high angle annular dark field (HAADF) detector were used to show that phase-segregated crystalline bi-lobe nanocrystals were formed. Rapid melting and solidification using a single excimer laser pulse transformed the bi-lobe structure into a homogeneously mixed amorphous structure. Raman spectroscopy was used to monitor the crystalline nature and approximate grain size of the Ge portion of the nanocrystals after each heat treatment, and the Raman spectra were compared with the TEM images.

Gallium nitride powders and zinc oxide powders were each calcined with a few weight percent of copper oxide and/or magnesium oxide either in air or N2. Powder X-ray diffractometry, transmission electron microscopy, energy dispersive X-ray spectroscopy, and electron energy loss spectroscopy were performed in order to observe calcination induced structural effects on these wurtzite type semiconductors. We note that our earlier magnetic results on Cu doped GaN are qualitatively consistent with recent first principle calculations [Wu et al., Appl. Phys. Lett. 89 (2006) 62505].

A novel method for the structurally identification of a nanocrystal from a single high resolution (HR) transmission electron microscopy (TEM) micrograph is described. Components of this method are demonstrated on both experimental and simulated HRTEM images. On the experimental side, the structural information that can be extracted from a HRTEM image is the projected reciprocal lattice geometry, the plane symmetry group, a few structure factor amplitudes and phases, and an outline of the projected atomic structure to the limited resolution of the HRTEM (via a Fourier synthesis of the structure factors). Searching for this information in a comprehensive database and matching it with high figures of merit to that of candidate structures should allow for highly discriminatory identifications of nanocrystals, even without additional chemical information as obtainable in analytical TEMs.

Gallium nitride powders were calcined with copper oxide in either air or N2 and analyzed by means of powder X-ray diffraction (XRD), high-resolution parallel illumination (HRTEM) and scanning probe transmission electron microscopy (STEM), energy dispersive X-ray spectroscopy (EDXS), and electron energy loss spectroscopy (EELS) in order to address the structural and electronic effects of Cu-incorporation into GaN. Gallium oxide and multiple copper oxide phases corresponding to the calcination environment were detected. Significant changes in the lattice parameters and electronic structure of the N2-processed GaN indicate incorporation of both copper and oxygen into the GaN lattice as well as changes in the chemical bonding due to the calcinations process. SQUID magnetometer measurements at 300 K demonstrated ferromagnetism in selected samples.

Because a great deal of nanoscience and nanotechnology relies on crystalline nanometer sized or nanometer structured materials, crystallographers have to provide their specific contributions to the National Nanotechnology Initiative. Here we review two open access internet-based crystallographic databases, the Crystallography Open Database (COD) and the Nano-Crystallography Database (NCD), that store information in the Crystallographic Information File (CIF) format. Having more than ten thousand crystallographic data sets available on the internet in a standardized format allows for many kinds of internet-based crystallographic calculations and visualizations. Examples for this that are dealt with in this paper are interactive crystal structure visualizations in three dimensions (3D) and calculations of theoretical lattice-fringe fingerprint plots for the identification of unknown nanocrystals from their atomic-resolution transmission electron microscopy images.

Powder X-ray diffraction analyses of Mn-and Cu-doped ZnO powders calcined at 500˚C, show shifts in the wurtzite type semiconductor's lattice constants and unit cell volume which correspond to the nominal concentrations of transition metal dopants. Marked reductions in the a-lattice constant and unit cell volume for a small concentration of Cu dopants, which is not maintained upon increased Cu concentration, suggest a change in the copper ion hybridization state due to the dopant concentration. In all the samples, only ZnO and CuO phases were detected, aiding the ascertainment of any ferromagnetic response from the samples as arising from the formation of a true dilute magnetic semiconductor.

Crystallographic databases for inorganic materials that are freely accessible over the internet are reviewed. The Nano-Crystallography Database project is described. Instructions are given on how to visualize in three dimensions the atomic arrangements of the several thousand entries of the Crystallography Open Database.