think forward

Bruker AXS

D8 DISCOVER with GADDS

XRD

XRD2 Solutions

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Squaring the circle or achieving what seems to be impossible – that’s what work is like in many areas of research and development today. As the frontiers of science are extended, researchers are engaged in the development of new active ingredients, materials and processes, and in monitoring quality.

The urge to find out what makes things tick has always been the driving force behind progress. To satisfy curiosity you look for causal connections; you want to know why a thing works the way it does and which parameters are crucial.

Anyone whose day-to-day work involves achieving the impossible, needs an extremely practical, highly flexible, and absolutely reliable measuring instrument to analyze and test actual objects. This instrument would have to work super fast while, at the same time, registering and taking into account all aspects – both known and unknown – of the object under examination. It would have to measure atomic positions and analyze the microscopic properties of samples at the same time. It should be able to virtually take the sample apart, right down to the very last detail, without altering it in any way.

Impossible? No! There is an ideal method and there are perfect solutions that resolve all the apparent contradictions and meet all the requirements: the method is called XRD2, the solutions are provided by the D8 DISCOVER with GADDS.

Sensitivity

Functionality

Flexibility

Useability

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XRD – squaring the circle

Power

Speed

Accuracy

Reliability

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Open your eyes using XRD –discover the g-information

Single Crystals

Micro Samples

Textured Materials

Powders

Strained Materials

Debye Ring

Debye Cone

Incident Beam

Sample

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XRD2 – X-ray analysis by means of a 2-dimensional detector – is the ideal, non-destructive, analytical method for examining samples of all kinds. With XRD2 you can simultaneously identify all the crystalline phases present in a sample without the need for time-consuming preparations. This is particularly important because several phases are normally present in a sample. In general, each sample contains a wide variety of crystals of different sizes. These crystallites frequently show preferred orientation and, in addition, their structure may be under stress.

For many other analytical methods, these real-life samples present an immense challenge – but not for XRD2. For a complete characterization, the smallest detail is important. But measuring every detail by counting every photon – doesn’t that take an incredibly long time? No, because in addition to detecting every signal, the greatest advantage of the XRD2 method is its incredible speed. The complete XRD2 Pattern of the diffracted X-rays is measured simultaneously in the 2-Theta and Gamma directions. Only together, this 2-Theta and Gamma information provide a complete picture of the sample structure. All you have to do is decipher this ”fingerprint“ and extract the relevant parameters. Here’s how it works:

The sample structure is determined �from the position and intensity of the reflections.

By comparing this pattern with known �patterns, the crystalline phases are identified.

In addition, the respective quantities of �those phases can also be determined.

Measured intensities are also used to �quantify the orientation distribution of the crystallites.

Last but not least, residual stress and �external stresses are determined from shifts in the XRD2 Pattern.

You may not always want to use all the information at once. Therefore, we made it easy to pick out the relevant facts, allowing you to focus on the solution and not on the analytical method – D8 DISCOVER with GADDS.

Structural informationlattice parameterscrystalline structuresymmetrycoordination andcorrelation

Phase identificationcrystalline phasesamorphous contentphase transitionpolymorphism

Phase quantificationcrystalline phasesphase mixtures% crystallinity

Orientation quantificationpreferred orientationtexture componentspole figuresorientation distribution

Residual stressmicrostraindeformationstress tensorhard coating

XRD Pattern

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The Keys to the world of XRD

To apply the XRD2 method, it is essential to precisely align your sample and to detect 2-dimensional data with high speed, accuracy, and sensitivity. The key components to success:

The patented laser/video microscopeIt provides a simple method for accurate �alignment and positioning of any type of sample. Without touching the surface, the sample is automatically positioned in the exact center of the diffractometer, ensuring that the X-ray beam hits the selected spot of your sample.

Simply zoom in on the region of interest and �move your sample to the desired XY-position. Control your sample height by monitoring the relative positions of the laser spot and microscope crosshair and start your measurement.

Multiple sample positions can be defined �either in ”pick-target“ mode or by clicking on the sample image.

For automatic operation, the VIDEO program �allows you to auto-align sample heights for the selected measurement spots. It detects the laser spot in the video image and brings the laser spot and the crosshair into coincidence

Correct Sample Position

Video

Laser

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Applications

Phase Identification

TaskCrystalline phase identification of solid or liquid samples

MeasurementMeasure intensity distribution of XRD2 Pattern

EvaluationIdentify crystalline phases by matching with known data sets

Key FeaturesSuper speed phase identifi- �cation in millisecondsExcellent data quality even �from non-ideal samples due to 2D samplingEnhanced match qualification �using 2D diffraction details

Micro Diffraction

TaskMicroanalysis of small or inhomogeneous samples

MeasurementMeasure XRD2 Pattern with micron accuracy

EvaluationIntegrate spotty data and extract desired sample information

Key FeaturesEvidential results from traces �for forensic studies and threat detectionSpot analysis down to microns �Valuable diffraction information �even from a small number of grains

Phase Quantification

TaskCrystalline or amorphous �phase quantification of solid or liquid samples

MeasurementMeasure relative intensities of �XRD2 Pattern

EvaluationQuantify the volume fractions �from the ratio of the diffracted intensities

Key FeaturesSuper speed phase quantifi- �cation in millisecondsReliable data from spot sizes �down to 10 micronsObtain accurate results for any �sample geometry from non-ideal samples

Mapping

TaskMapping of inhomogeneous and structured samples

MeasurementAutomatically collect XRD2 Patterns from multiple locations

EvaluationAutomated extraction and mapping of specific sample properties

Key FeaturesMapping of samples up to �300 mm x 300 mmClear 2D and 3D mapping �display1- and 2-dimensional sampling �using free grids

Texture

TaskOrientation identification and quantification of crystallites in solid samples

MeasurementCollect intensity distribution in XRD2 Patterns as a function of sample orientation

EvaluationDetermine orientation distribution

Key FeaturesSimultaneously record multiple �high resolution pole figures and full back-groundIntuitive modeling of texture �using the component methodDescriptive and graphical �presentation of individual texture components

Reciprocal Space Mapping

TaskOrientation and quality of epitaxial layers

MeasurementMeasure diffracted intensity as a function of incident and exit angle

EvaluationDetermine layer structure and epitaxial relationship

Key FeaturesLarge set of reflections �covered simultaneously with 2D detectorCollect a large section of �reciprocal space with only one sample rotationFull picture of reciprocal space �without blind spots or missed reflections

Stress

TaskResidual stress determination

MeasurementMeasure shifts in XRD2 Patterns as a function of sample orientation

EvaluationDetermine the 3D stress and strain

Key FeaturesSimultaneously record multiple �reflections and full backgroundBetter statistics by monitoring �the shape of the Debye ringEasy stress determination on �curved samples with small spot sizes down to microns

Non- Ambient

TaskChange of structural properties as a function of sample environment

MeasurementCollect XRD2 Patterns under varying conditions

EvaluationDetermine structural parameters as a function of sample environment

Key FeaturesDomed temperature stage for �maximum angular coverageSoftware-controlled �temperature profilingComprehensive graphical �display and report

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Single Crystal Diffraction

TaskCrystallographic structure from small single crystals

MeasurementCollect a large number of reflections in multiple XRD2 Patterns

EvaluationIndex the reflections and solve the crystal structure

Key FeaturesPrecise lattice parameter �determinationEasy determination of crystal �orientationFull structure analysis from �crystals down to microns

High Resolution X-ray Diffraction

TaskThickness, composition, mismatch, relaxation, and defects for epitaxial layers

MeasurementMeasure rocking curves, radial scans, and reciprocal space maps

Absolute lattice parameter using Bond method

EvaluationSimultaneous evaluation of several reflections

Key FeaturesFully automatic sample �alignmentAdjustable detection resolution �with Pathfinder

Small Angle X-ray Scattering

TaskNanostructure analysis including particle shape, size, distribution, and particle orientation

MeasurementMeasure small angle X-ray scattering signals in XRD2 Patterns

EvaluationModel the data and determine nano structural properties

Key FeaturesStraightforward determination �of anisotropic sample parametersCapillary mode for liquids �Low background with He �beam-path due to minimized air scattering

Reflectometry

TasksThickness, roughness, and density of crystalline and amorphous layers down to 0.1 nm

Lateral and vertical roughness correlation

MeasurementMeasure specular scans, diffuse scans, and reciprocal space maps

EvaluationUnified evaluation of XRR and HRXRD

Key FeaturesNine orders of magnitude �dynamic range using a Göbel mirror and knife edge collimatorThird generation Göbel mirror �for perfect incident beam conditions

High-Throughput Screening

TaskRapid analysis of multiple samples in combinatorial research, development and quality control

MeasurementAutomatically collect XDR2 Patterns from sample libraries and arrays

EvaluationAutomated extraction and screening of specific sample parameters

Key FeaturesAutomatic sample alignment �using the laser/video microscopeHorizontal sample mount for �reflection and transmission geometryOperator-ready display of the �results

Grazing Incidence Diffraction

TaskPhase identification, parallel mismatch, crystal quality, symmetry, and orientation of very thin layers

MeasurementMeasure in-plane reflections with very small incident and exit angle

EvaluationDetermine lattice parameters and phases

Key FeaturesAutomatic alignment of lattice �planes with tilt stageCharacterization of layers down �to 1 nmDepth profiling by changing the �incidence angle

Phase Identification

Phase Quantification

Texture

Stress

Single Crystal Diffraction

Small Angle X-ray Scattering

High-Throughput Screening

Micro Diffraction

Mapping

Reciprocal Space Mapping

Non-Ambient

High Resolution X-ray Diffraction

Reflectometry

Grazing Incidence Diffraction

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Accept no limits – tailored solutionsfor your applications and samples

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Unlimited potential – being able to examine every conceivable type of sample, in the best possible way and using a wide variety of methods.

Unlimited freedom – being able to select from a vast number of perfectly coordinated components and to move, effortlessly, between completely different geometries.

Unlimited versatility – a Diffraction Solution which can perform any number of tasks successfully with great ease.

Tailored solution – the perfect combination of hardware and software, of innovation and experience, of service and consultation.

More simply said – D8 DISCOVER with GADDS!

High-flux optics from �graphite monochromator to focusing PolyCap™

Sample handling from �capillary to 300 mm wafers

Choice of detector from �dynamic scintillation counter, innovative VÅNTEC-1 to unique 2D HI-STAR

Accessories: Alignment �tools, non-ambient sample chambers, sample spinners, beamstops

Pioneering MULTEX AREA �for texture analysis

Unique DIFFRAC �plus

EVA / SEARCH for phase identification

Innovative PILOT for full �automated high-throughput screening

Universal DIFFRAC �plus

LEPTOS for thin film analysis

Award winning DIFFRAC �plus

TOPAS for profile fitting and structure investigation

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Don’t miss a single phase – XRD

Adjustable sample-to detector distance for �optimized angular resolution

Motorized stages for easy sample handling �

Contact-free alignment with laser/video and �manual control box

Sample

HI-STAR Detector

Laser/Video Microscope

UBC Source

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Non-ambient temperatures from -180 °C up to 1100 °C �

PILOT software for intuitive powder diffraction strategy �

Vertical Theta/Theta geometry for easy sample placement �

Challenging samples, like a few small grains or textured material – anything other than ideal powder – the D8 DISCOVER with GADDS analyzes these samples in real-time at or in dimensions that no diffractometer could do before.

Preparation is quick and easy: place your sample, zoom in with the laser/video microscope and center your sample – nothing else required. Then start the data collection with PILOT software. It suggests an optimized measurement strategy. For example, it proposes the best settings for optimized data collection in different geometries. Choose a start and end angle, measurement time, and resolution. Then go! The system starts to collect a series of XRD2 Patterns and displays it in a Debye-view. The large size of the HI-STAR detector ensures that you get all the reflections.

The Debye view allows you to identify Debye rings with similar properties in terms of spottiness, texture, and other identifying characteristics. Only the Debye rings with identical characteristics can belong to the same crystalline phase. This information can make all the difference in getting the right answer, and it’s only available in XRD2!

Use our unique SEARCH to identify the present phases by matching the data to the more than 100,000 entries of the ICDD database within seconds. That makes the D8 DISCOVER with GADDS the ideal choice for fast qualitative and quantitative phase analysis.

Domed sample stages for controlled non-ambient conditions take full advantage of the HI-STAR detector, because intensities can be collected in any direction.

Another outstanding feature is the high detection speed that allows you to collect instant snapshots and full XRD2 movies. During phase transition studies, you will never miss a single phase.

Phase Transition

Phase 2Phase 3Phase 1

Conventional XRD

XRD2 Movie

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Small spot analysis down to microns �

Non-destructive trace analysis for forensic �applications

Scanning diffraction microscope �functionality

Up to 300 mm mapping of large samples �

As modern trends move toward smaller samples and spot sizes, XRD2 microdiffraction once again gets right to the point. The point is: small samples require larger detection areas and higher sensitivity. The D8 DISCOVER with GADDS is unrivaled for its microdiffraction capacity. It features our unique laser/video microscope alignment in combination with high performance X-ray technology to precisely hit the sample with micron accuracy.

The small number of grains in the X-ray beam produces very spotty, incomplete Debye rings.

Data integration of the 2-dimensional XRD2 Pattern makes sure that you don’t miss the reflections from these single grains. No photon will be wasted!

The small spot size in combination with the automated alignment system allows you to map entire sample regions. Just click on the video image and define individual spots or a whole grid for your analysis.

After data collection, strong mapping and analysis software routines allow you to extract whatever XRD feature you need to explore, from material composition to percent crystallinity, from stress to texture. The D8 DISCOVER with GADDS – get right to the point!

Small Sample Amounts

Montel Mirror

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Get right to thepoint – XRD

Small Spots

Focusing PolyCapTM

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Graphical definition of time- and �resolution-optimized measurements using MULTEX AREA

Intuitive link between 2-dimensional �measurement data and high resolution pole figures

Calculated full pole figures of individual �texture components

Unique quantitative evaluation of texture �components with MULTEX AREA

Focus on the relevant – XRD

Two-Position Chi Stage

Graphite Monochromator

MonoCap™

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Whether you are designing new anisotropic materials with new capabilities or your are developing a new process to create a cer tain required texture in your material, whether you are working with metals, superconductors, coatings, fibers, polymers, nano-materials, thin films, or wires: with the D8 DISCOVER with GADDS you can solve the complete texture of your sample in an easy and elegant way.

A primary advantage is our straight-forward MULTEX AREA software, which supports you in all steps of texture analysis. From optimizing the data collection strategy through interactive evaluation, to transparent results and the final reporting, it simultaneously collects multiple pole figures and complete background, taking full advantage of the XRD2 technology. Interactively solving your texture with MULTEX AREA works like this:

First you build a model of your sample �by selecting the texture components via drag and drop.

Then the software refines it and �represents the results in a pie chart.

Click on a slice and you get a 3D �picture and full information for that texture component.

Focused on the relevant – �D8 DISCOVER with GADDS and MULTEX AREA.

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RandomTexture Component

Fiber Texture Component

PreferredOrientation Components Texture with XRD

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When stress is an important factor affecting performance or lifetime of your samples, the D8 DISCOVER with GADDS is the answer to getting reliable stress measurement results.

It is the only solution when you have to deal with complex geometries, heavy samples and textured and inhomogeneous materials. Precisely define your measurement location using the unique laser/video microscope.

XRD2 allows you to analyze the smallest sample features with an X-ray beam collimated down to 10 microns. Finally, generate a 1- or 2-dimensional stress map using the high precision motorized xyz stages. For example, to control the welding process you can easily determine the stress distribution across a weld along a line of measuring points. Then, determine the local stresses with the sin2(psi) method and display the results in a map.

With the XRD2 method you directly measure stress-induced deformation of the Debye cone. This improves your data because you are simultaneously collecting measurement points from multiple inclination angles. Altogether total stress control with D8 DISCOVER with GADDS.

Optimum data quality with the optimum wavelength: �Cu, Co, Fe or Cr

Improved results with elastic constants calculated �with ELASTIX software

XRD �2 stress analysis on samples with texture or with a

small number of grains

Easy handling of large and heavy samples – no sample �preparation required

Small spot analysis on complex parts: inhomogeneous �or curved samples, etc.

Stressed Sample

Exchangeable X-ray Source

uniaxial

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XRD – get Stressunder control

Unstressed Debye Ring

Stressed Debye Ring

Unstressed Reflection

sheer

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Master the floodof samples: XRD

Full support of CFR 21 Part 11 regulations �

Well established XQ procedures for �consistent throughput

Reflection and transmission geometry �available

Patented, retractable Knife Edge Collimator �(KEC) for optimum data quality

PILOT software for straightforward �measurement set-up

Screening samples / materials

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High-throughput screening systems need to probe hundreds of samples rapidly and in a non-destructive fashion. High precision sample positioning, automated data acquisition, handling, and evaluation are indispensable. XRD2 has the capability to simultaneously and unambiguously determine sample properties such as phase composition, polymorphism, structure, percent crystallinity, particle size, texture, and residual stress.

The D8 DISCOVER with GADDS is the unique solution for high-throughput screening in terms of speed, sensitivity, and data quality. In addition, the GADDSplus software suite provides the tools to rapidly screen and analyze sample libraries of any format. To detect unpredictable sample features, the innovative PolySNAP software compares full XRD2 Patterns. It mines through thousands of datasets by marking and sorting deviating samples. This method will automatically identify samples with identical phases and detect mixtures.

For quality control, samples can be automatically flagged based on a pass/fail criteria.

The D8 DISCOVER with GADDS is also easily integrated into large workflows. It plays in concert with other analytical methods. For example, the results can include video images as well as imported general sample information. Another plus is that the data can be ported to other data mining software.

Rapid screening with the D8 DISCOVER with GADDS is the optimum solution to master your highthroughput needs.

Sample array / libraries

Screening criteria

Screening result Pass / fail result

and / or

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Montel Mirror for a highly intense, �point-like parallel beam

Helium beampath for reduction of air �scattering

Compact Centric Eulerian cradle for �maximum access to reciprocal space

Multiscale structure analysis �

Helium Beampath

Beamstop

Dimensions and Structures analyzed by SAXS

Dimensions and Structures analyzed by XRD2

Dimensions and Structures analyzed by SCD

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Micro – Nano – Sub Angstrom –

pick your scale with XRD2

Modern material research and nanotechnology rely on structural investigations to design and optimize new materials. The detailed knowledge of structural properties allows you to understand and predict electrical, optical, and mechanical properties that affect material performance.

The D8 DISCOVER with GADDS provides a broad and comprehensive picture of structural aspects from atomic positions to particle sizes, from epitaxial relationships to particle shapes.

XRD2 covers the whole range of length-scales: large scale features that result in Small Angle X-ray Scattering (SAXS) signals and arrangement of individual atoms in a single crystal that result in Bragg diffraction signals. Consequently, the D8 DISCOVER with GADDS can characterize structures in the nano-range, molecular structures in single crystals, and heterostructures in thin films.

Due to the unique combination of extremely low background and single photon detection of the HI-STAR detector, 2D SAXS patterns from anisotropic samples can be detected in real-time.

In addition, these HI-STAR features mean that crystal structures from samples as small as 20 microns can be solved.

Maps of large reciprocal space sections can be accomplished in a very short time due to the high spatial resolution and the large active area of the detector.

D8 DISCOVER with GADDS analyzes every structural aspect of your sample – pick your scale.

Small

Large

Inhomogeneous

Preferred Orientation

Weakly Diffracting

Powder

Complex Geometries

Heavy

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Ewald Sphere

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SamplesSmall Large Inhomo-

geneousPreferred

OrientationWeakly

DiffractingPowder Complex

GeometriesHeavy

Small

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Inhomogeneous

Preferred Orientation

Weakly Diffracting

Powder

Complex Geometries

Heavy

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Patented laser/video microscope �

Automated, contact-free sample �alignment and monitoring

Unique HI-STAR detector with real-time 2-dimensional �data display

Ultra sensitive, noise free, single photon detection �

VÅNTEC-2000 with patented MikroGap �TM technology

The video camera adds an extra benefit to your daily work: the recorded video pictures can be used for documentation, report writing, and even other optical applications like birefringes method, polarized light microscopy, optical sample screening, and more.

The patented 2-dimensional HI-STAR detectorThis detector features an up to 65° 2-Theta and large Gamma active area while providing an unrivalled single photon sensitivity and high dynamic range. This long list of features makes the HI-STAR a unique XRD2 detector covering the entire range of X-ray diffraction applications ranging from powder diffraction, micro diffraction, texture, and stress to Small Angle X-ray Scattering (SAXS) and single crystal diffraction.

The HI-STAR is the most sensitive detector for laboratory diffraction experiments, enabling millisecond measurement time. This is the reason why the HI-STAR is one of Bruker AXS’ most popular SUPER SPEED components.

1.000 x 1.000measuring pointswithin oneXRD2 Pattern

Traditionalone pointmeasurement

Single Photon Detection

Technical DataConfiguration Horizontal and vertical,

Theta/2-Theta and Theta/Theta geometry (can be reconfigured on-site)

Angular range 360° (without accessories)

Max. usable angular range (depends on accessories and set up)

-160.5° < 2-Theta ≤ 120°

X-ray optics Flat graphite monochromatorUBC Göbel Mirrors2-D Montel Mirror Focusing PolyCap™ 500 μm spotCollimators 1 mm down to 50 μmMonoCap™ optics 1 mm down to 10 μmFocusing Micro lens for beam size down to 100 µm

Sample stages Fixed-chi stageTwo-position chi stageCentric Eulerian cradle¼-circle Eulerian cradleXYZ stagesUMC 300

HI-STAR detector Real-time data collection and displayTrue photon counting11.5 cm diameter active area2-Theta coverage: 65° at 6 cm sample-to-detector distance 18° at 30 cm sample-to-detector distance

Optional detectors Scintillation counterEnergy dispersive Sol-XE1-dimensional VÅNTEC-12-dimensional VÅNTEC-2000 with 14 x 14 cm2 active area

Accessories Optical microscopeLaser/Video microscopeSample rotation stagesCapillary spinnerHigh and low temperature chambers: -180 °C up to 1100 °CRetractable Knife Edge CollimatorBeamstop and beampath for SAXS

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Bruker AXS GmbH

Karlsruhe, Germany Phone +49 (7 21) 5 95-28 88 Fax +49 (7 21) 5 95-45 87 info@bruker-axs.de www.bruker-axs.de

Bruker AXS Inc.

Madison, WI, USA Phone +1 (800) 234-XRAY Tel. +1 (608) 276-3000 Fax +1 (608) 276-3006 info@bruker-axs.com www.bruker-axs.com

D8 and DIFFRAC are registered trademarks of the US Office of Patents and Trademarks.The Laser/Video system, the VÅNTEC and LynxEye technology, the Pathfinder, the Göbel Mirror, and LEPTOS are protected by patents of the US or EP Offices of Patents and Trademarks.

www.bruker-axs.com