X-ray diffraction for today and tomorrow X’Pert PRO X’Pert PRO is the new X-ray diffraction platform, developed by Philips Analytical. X’Pert PRO is X-ray diffraction for today and tomorrow. X-ray diffraction for today and tomorrow

Contents X-ray diffraction for today X-ray diffraction for tomorrow how can we make your work easier? X-ray diffraction for tomorrow the only thing constant in life is change What do we mean with “X-ray diffraction for today and tomorrow”? X-ray diffraction for today means: how can we make your work easier? How can we enable you to solve all your analytical problems with the appropriate diffraction system? X-ray diffraction for tomorrow means: how can we make your diffraction system future-proof? What will happen in five years? Will it be necessary to include new techniques to your diffractometer? Can you keep the existing functionality of the system when adding new applications? In this presentation we will discuss the answers to the questions posed here.

X’Pert PRO: X-ray diffraction for today Stress Flat samples Loose powders Phase analysis Diffractometer Rough samples Texture Small amounts Let us consider an example. The situation sketched above is typical for a university or a research laboratory, where several groups wish to do several types of analysis on different types of samples. The laboratory can afford only one diffraction system. In this particular case, there are the following sample types: flat samples loose powders samples with preferred orientation small amounts of samples, sensitive to humidity or poisonous large and irregularly shaped samples The following types of analysis are required: residual stress, preferred orientation (texture), phase identification and crystallography. Of course, this list can easily be extended, or changed for a specific set of demands: analysis of epitaxial layers, reflectivity, ... Crystallography Preferred orientation

The “ideal” diffraction system Fast exchange of : Tubes and tube focus positions Incident beam optics Sample platforms Diffracted beam optics Detectors without re-alignment ! If a diffraction system exist, capable of solving all questions shown on the previous slide, which properties should it have? It should be easy to exchange tubes and tube focus positions incident beam optics sample platforms diffracted beam optics detectors without laborious alignment procedures, or in other words: as fast as possible.

What is X’Pert PRO? Based on the PreFIX concept What is PreFIX? Pre-aligned Fast Interchangeable X-ray modules Exchange is easy, no re-alignment of hardware X’Pert PRO is our answer for the “ideal” diffraction system. It is based on the PreFIX philosophy: all components of the diffraction system are Pre-aligned Fast Interchangeable X-ray modules. The user can exchange items easily, without having to align the hardware. In the next slides we will show a - by no means complete - collection of PreFIX modules.

PreFIX incident beam optics Fixed divergence slit Programmable divergence slit X-ray mirror Hybrid monochromator X-ray lens Mono capillary … and more ... A large variety of incident beam PreFIX modules exists: from the simple fixed divergence slit module, to programmable slits, giving the user the possibility to choose between fixed illuminated length and fixed divergence angle... from slit optics with divergent X-ray beam to parallel beam optics using the X-ray mirror… the hybrid monochromator, which combines the X-ray mirror with a monochromator in one PreFIX module… the X-ray lens, generating a parallel beam from the point focus of the X-ray source… the monocapillary, for analysis of small spots on a sample… … and there is more! Think for instance about 4-crystal monochromators, crossed-slits collimators, and there is also more to come!

PreFIX sample platforms Fixed platforms Stage for large samples Non-ambient chambers Texture cradles Open Eulerian cradle Capillary spinner Spinner … and more ... Also the sample stages are exchangeable following PreFIX philosophy. From the simplest sample stage for flat solid samples, to non-ambient chambers, spinning sample stages and advanced stages capable of tilting and rotating the specimen in all directions, all stages are exchanged in minutes’ time. Again, there is more, and more to come!

PreFIX sample platforms New changer for 15 or 45 samples A special item is the PreFIX sample changer, used in conjunction with the sample spinner stage. Two versions exist: one with a single fifteen-position sample magazine and one with three of these magazines. Shown is the large sample changer, capable of storing 45 samples. Below each sample magazine is a separate position for a monitor sample. The small version is especially designed for intermittent usage: it is possible to push it aside in the enclosure in order to make room for large samples and complex sample stages, such as non-ambient chambers. When the sample changer is required, it is easily wheeled back to its position in front of the goniometer and locked in place without additional re-alignment.

PreFIX diffracted beam optics Programmable receiving slit Programmable or fixed anti-scatter slit Collimators of 0.27, 0.18 and 0.09 Position sensitive detector … and more ... Also on the diffracted beam side a lot of possibilities exist for choosing the best optical component for a given measurement: A receiving slit, optionally combined with fixed or programmable anti-scatter slits Parallel plate collimators with acceptance angles of 0.09 degrees, 0.18 degrees or 0.27 degrees A position-sensitive detector but there is more: a detector holder for recording rocking curves, an analyzer crystal for reciprocal space maps, and there is more to come!

Example of change between configurations Two systems: Capillary spinner system Standard phase analysis Contents of video presentation Start: bare system Build-up of capillary spinner system Change from capillary spinner to standard phase analysis system Enough talk about hardware, let us go to a specific example. Let’s consider that two types of samples need analysis. One is an analysis of small amounts of hazardous material, sealed in a glass capillary. The other is a standard powder sample. In the video presentation the change between a capillary spinner system and a standard phase analysis system is shown. But before starting the video, let us take a look at the differences between the two systems.

The capillary spinner Anti-scatter housing Soller slits Anti-scatter Hybrid monochromator housing Position Sensitive X-ray tube A photograph and a schematic beam path of a system optimized for the analysis of small amounts of hazardous materials in glass capillaries are shown on this slide. The heart of the system is - of course - the capillary sample, seen on its top. Because the amount of material analyzed is low, it is necessary to have a small, high-intensity beam on the sample. For this case, parallel beam optics is the best solution. Here the X-ray mirror is combined with a monochromator in order to have a beam containing only the K-Alpha1 component of the Copper radiation. In order to speed up the analysis time on the diffracted beam side, a Position-Sensitive Detector is used. As can be seen in the picture, on the incident as well as the diffracted beam side are anti-scatter devices, meant to shield the detector from stray photons. In this way, the data recorded with this configuration does not need any software correction (note for the speaker: Bruker needs this!). Detector (PSD) (line focus) Powder sample in D q = 18" - 25" capillary spinner Divergence slit

Conventional phase analysis Detector Soller slits Curved crystal Receiving slit monochromator (Graphite) X-ray tube Anti scatter slit Soller slits (line focus) The conventional system for phase analysis is well-known. The sample is flat and measured in reflection mode. Programmable divergence slits control the divergence of the X-ray beam. The slits can be operated in two modes, constant illumination angle or constant illuminated length. This last option is especially useful when measuring samples at low 2Theta angles. The sample can be spinned in order to improve particle statistics. The programmable anti-scatter slits follow the movement of the divergence slits. The X-ray beam is re-focused on the programmable receiving slit. This mode of operation is known as Bragg-Brentano geometry. After the receiving slit, a diffracted beam monochromator is mounted for suppression of the K-Beta line and the white radiation. Let us take a look at the video presentation to see the exchange from the previous configuration to this one. Note for the Speaker: The video presentation can now be started. Use only the first five minutes, in which the change described above is shown. Polycrystalline sample Beam mask Divergence slit

Another example A complete powder crystallography laboratory: capillary spinner for small amounts of powder with preferred orientation problems focusing incident beam monochromator for flat powder samples Is it possible to combine these systems? Now let us take a look at another example: a complete laboratory for crystallographic analysis of powder samples. One of the configurations is the capillary spinner system, as discussed before. The other one is a system with a focusing incident beam monochromator, for phase analysis in the Bragg-Brentano geometry with monochromatic radiation. Is it possible to combine these systems? Before answering this question, let us take a closer look to the focusing incident beam monochromator.

The 1-reflection system Soller slits Receiving slit Detector Soller slits Irradiation slit Anti scatter slit The Alpha-1 reflection system is a diffractometer that uses the Bragg-Brentano geometry, in which the divergent beam illuminating the sample is re-focused on the receiving slit. On the incident beam side, a curved Germanium monochromator is placed, which selects the Copper K-Alpha1 radiation and refocuses the beam. A focusing incident beam monochromator for Cobalt radiation is also available. X-ray tube (line focus) Polycrystalline sample Incident beam Programmable monochromator divergence slit

Can we combine these systems? Move tube tower from 1 to standard position It is possible to combine the two configurations shown in the previous slides, using the following steps: 1. Move the tube tower from the Alpha-1 position to the standard (Bragg-Brentano) position. The tube tower is PreFIX, it can be moved between two positions, depending on the necessity for monochromatic or “normal” radiation.

Can we combine these systems? Exchange the divergence slit for the hybrid monochromator Exchange the sample platform Exchange the receiving slit for a position sensitive detector The next steps to perform are: 2. Exchange of the incident beam optics, from a programmable divergence slit to a hybrid monochromator, 3. Exchange of the sample stage, from a spinner stage to a capillary spinner stage, 4. Exchange of the diffracted beam optics: from programmable slits to a position-sensitive detector. In this way, it is possible to combine these systems. This full exchange will cost you about ten minutes.

Conclusions X’Pert PRO gives you the ultimate flexibility for handling various types of X-ray analysis Today & Tomorrow With this presentation I intended to show you that X’Pert PRO gives you the ultimate flexibility for handling different types of X-ray diffraction analysis on one system. It may not be necessary to have this flexibility today. But it may be necessary tomorrow. Or next year. X’Pert PRO is future-proof. Thank you for your attention.