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Inorganic Chemistry

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Single Crystal and Powder X-ray Diffraction

Single Crystal and Powder X-ray Diffraction



X-ray diffraction is a common analytical technique used in materials science and biochemistry to determine the structures of crystals.

It traces the paths of X-rays through crystals to probe the structure. There are two major techniques. Powder X-ray diffraction determines the phases and purity of a crystalline species. Single X-ray diffraction identifies the atoms in a crystal and their locations, as well as electron densities, bond lengths, and angles.

This video illustrates the operation of an X-ray diffractometer, procedures for both single-crystal and powder X-ray diffraction, and discusses a few applications.

We'll start by examining the concept of crystal structure, and exploring how X-rays interact with crystals.

A crystal is a periodic configuration of atoms, that is, a geometric pattern of atoms that repeat at regular intervals. The smallest repeating element of a crystal is called a "unit cell." It is described by its packing structure, dimensions and bond angles. "Miller indices" describe any fictitious planar cross sections of the unit cell.

X-rays are a form of electromagnetic waves whose wavelengths are similar to the atomic spacing in crystals. When a single X-ray strikes an individual atom, it is diffracted. When two coherent X-rays strike atoms in different planes, the diffracted X-rays interfere, resulting in constructive or destructive signals.

The diffraction pattern of a powder crystalline sample is comprised of intense spots, which form rings of constructive interference. The angles at which these spots occur correspond to the spacing of atoms in that plane. The spacing can be determined using Bragg's Law.

Now that we have learned about crystals and X-ray diffraction patterns, let's look at how an X-ray diffractometer works.

An X-ray diffractometer consists of three basic components: an X-ray source, a specimen, and a detector. All components are oriented in a coplanar, circular arrangement with the sample holder at the center. The source usually contains a copper target, that, when bombarded by electrons, emits a beam of collimated X-rays. The beam is directed at the sample, which refracts the X-rays. The sample and the detector are then rotated in opposite directions, until the angles of X-ray intensity are determined.

High X-ray intensity corresponds to constructive interference by a crystallographic plane in both single-crystal and powder X-ray diffraction. Powder X-ray diffraction reveals the crystal structure of the sample, while single-crystal X-ray diffraction additionally reveals the chemical content and locations of atoms.

Now, let us see a practical example of X-ray diffractometry.

Single-crystal X-ray diffraction requires high-quality crystals without impurities, grain boundaries, or other interfacial defects. Bring the crystals of the organo-molybdenum compound to the light microscope to analyze it.

Begin by adding a drop of paratone oil to a clean glass slide. Then add a small amount of paratone oil to a spatula, and scoop some crystals from the crystallization vial onto a slide.

Examine the crystals under the microscope, and select a crystal with uniform, well defined edges. Once an ideal crystal is chosen, use a Kapton loop to pick up the crystal, ensuring little oil sticks to the crystal.

Next, open the diffractometer doors to load the sample. Attach the Kapton loop to the gonoimeter head, centering the crystal with respect to the X-ray beam. Then close the doors.

Open the X-ray crystallography software and run a short data collection sequence that establishes the structure of the unit cell. Based on this data, select a data collection strategy and run full data collection. Once a full data set has been collected, work up the data using a suitable program and refine it.

In comparison to single crystal X-ray diffraction, powder X-ray diffraction is a bulk characterization technique that does not require single crystals.

Choose an appropriately-sized sample holder and a diffraction plate that will not affect the readings at the angles of interest.

Place a fine mesh sieve over the diffraction plate. Carefully add 20 mg of sample to the sieve, keeping the sample over the plate. Tap the sieve on the benchtop until a monolayer of powder forms.

Secure the diffraction plate in the sample holder. Open the diffractometer doors and mount the sample. If the sample mount has locking pins, ensure the pins are engaged and the sample holder is secure before closing the doors.

Using a suitable software, load a standard data collection method. Enter a range of scan angles suitable for the material. Then enter the scan time; a longer scan time allows for better resolution. Then press "start".

Now, let's compare the results obtained from the single crystal and powder X-ray diffraction of the organo-molybdenum complex.

From the single crystal X-ray data, a structural model of the electron density map is generated, which is used to obtain experimentally determined bond lengths and angles within the structure.

Furthermore, the powder XRD provides additional information about the compound. The flat baseline of the spectrum indicates, that the sample used is highly crystalline, whereas curved baselines are indicative of amorphous materials.

X-ray diffraction is a valuable characterization tool in virtually every field of material science, and therefore plays a role in diverse applications.

A major component of heritage art conservation includes understanding how works of art were produced and why they corrode. Recent developments in X-ray diffraction study corrosion by destructively testing less than 1 mg of sample. Since corrosion products are rarely monocrystalline, powder X-ray diffraction is required. Typical analyses occur at 2θ between 5-85º degrees over 20 hours. The locations of atoms within the crystal may be optimized algorithmically, providing insight into the location and nature of chemical attacks.

Films of material ranging from nanometers to micrometers in thickness have unique protective, electrical, and optical abilities that differ from those of bulk materials. X-ray diffraction provides information on film thickness, density, and surface texture. It is used to determine film stress, and the likelihood of film failure and breakage. It also helps characterize the optical behavior of films, since absorption largely depends on crystal structure. It is therefore used to characterize thin film light sensors and photovoltaic cells.

You've just watched JoVE's introduction to single-crystal and powder X-ray diffraction. You should now be familiar with the principles of X-ray diffractometry, a procedure for obtaining diffraction patterns, and some applications. As always, thanks for watching!

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