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iLab Name: XRD
iLab Kiosk: BRK Metrology Core
FIC: Mike Capano
Owner: Dmitry Zemlyanov
Location: BRK 1045
Maximum Wafer Size: 4"/100 mm Diameter, 11 mm maximum Z travel (sample thickness axis)
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Panalytical X'Pert Pro MRD System is perfectly safe if operated as described in the user guide.
The X'Pert PRO MRD (Materials Research Diffractometer) systems offer advanced and innovative X-ray diffraction solutions from research to process development and process control. Standard and in-plane geometries on one system offers a wide range of diffraction experiments for polycrystalline and highly perfect thin films. With the PreFIX concept, reconfiguring is easy and optics positioning is accurate.
Accessories:
X-ray diffraction is a method of analyzing the internal structure of materials based on the scattering pattern produced when a beam of x-rays interact with its crystal structure. A typical experiment consists of an x-ray source, various x-ray optics, a sample, and a detector. See the Wikipedia article X-ray crystallography for further information.
Vacuum pump controller
Cabinet construction conforms to the most stringent X-ray safety standards. The absorbed dose equivalent rate is less than 1 µSv/h at 10 cm distance from teh outside surface of the enclosure. |
IF EITHER OF THE WINDOWS IS BROKEN, SWITCH THE SYSTEM OFF IMMEDIATELY! |
*PreFIX - Pre-aligned Fast Interchangeable X-ray modules. These are factory aligned and can be dismounted from the system and mounted again without the need for system alignment by the user.
Application | Incident Beam Optics | Diffracted Beam Optics | Remarks |
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Phase analysis, Omega-stress, Crystoallography on ROUGH SAMPLES | XM | PPC | Default |
HM | PPC | Kα1 only | |
Phase analysis of THIN FILMS | XM | PPC | |
HM | PPC | Kα1 only | |
Reflectometry | XM | PPC | Use collimator slit |
HM | PPC | Thick layers, use collimator slit, Kα1 only | |
High Resolution Diffraction | HM | TA/RC | Line focus, copper radiation only |
Ge | TA/RC | Point focus | |
In-plane diffraction | Ge | PPC | Point focus, highest resolution, Kα1 only |
Phase identification is the most important application of X-ray diffraction. XRD is applied on polycrystalline solids and thin films. A phase is a crystalline solid with a regular 3-dimensional arrangement of the atoms. The measured diffraction peak positions and intensities are like a fingerprint of a particular crystalline phase. Identification is accomplished by comparison of the measured pattern with the entries in reference databases using a search-match algorithm. This is also known as qualitative phase analysis. An example where phase is criticle in application of nanomaterials is the devolpment and testing of sunscreen. The rutile phase of nano-titania is required for UV blocking applications whereas photocatalytic activity requires the anatase phase.
In measuring residual stress using X-ray diffraction (XRD), the strain in the crystal lattice is measured and the associated residual stress is determined from the elastic constants assuming a linear elastic distortion of the appropriate crystal lattice plane. Since X-rays impinge over an area on the sample, many grains and crystals will contribute to the measurement. The exact number is dependent on the grain size and beam geometry. Although the measurement is considered to be near surface, X-rays do penetrate some distance into the material: the penetration depth is dependent on the anode, material and angle of incidence. Hence the measured strain is essentially the average over a few microns depth under the surface of the specimen.
A technique used for determining the atomic and molecular structure of a crystal, in which the crystalline structure cause a beam of incident X-rays to diffract into many specific directions. By measuring the angles and intensities of these diffracted beams, a crystallographer can produce a three-dimensional picture of the density of electrons within the crystal. From this electron density, the mean positions of the atoms in the crystal can be determined, as well as their chemical bonds, their crystallographic disorder, and various other information.
X-Ray reflectometry, whish is essentially analysis of the specular reflection of the sample, can be used to non-destructively investigate film thickness (nm, +/- 0.5-1%), roughness of the layer interfaces (nm, model dependent, reproducible 3%), and density of the sample materials (g/cm3, +/- 1-2%). Futhermore, the scale of roughness parallel to the interface (lateral correlation) and perpendicular to the interface (lateral correlation) can be investigated using off-specular reflection of the sample. Since XRR relies on specular and off-specular reflection of the beam rather than Bragg's law diffraction, it works with most thin films including epitaxial, non-epitaxial, and even non-crystalline films.
In reflectivity experiments, the X-ray reflection of a sample is measured around the critical angle. This occurs around grazing incidence angles. Below the critical angle of total external reflection, X-rays penetrate only a few nanometers into the sample. Above this angle the penetration depth increases rapidly. At every interface where the electron density changes, a part of the X-ray beam is reflected. The interference of these partially reflected X-ray beams creates the oscillation pattern observed in reflectivity experiments. From these reflectivity curves, layer parameters such as thickness and density, interface and surface roughness can be determined, regardless of the crystallinity of each layer (single crystal, polycrystalline or amorphous).
Information Contained in a XRR measurement | Film property effects on Reflectivity Measurements | |
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The critical angle for a layer is a function of its electron density and composition. For a given composition, as the density of the film increases the critical angle often increases. | ||
The distance between interference fringes is inversely proportional to the thickness of the layer. Because of this, thicker films need better resolution and thinner films need more intensity. | ||
Roughness causes X-Rays to be scattered rather than reflected, producing a decay in the reflected beam intensity. |
This section describes the steps necessary to manually align a sample and collect X-Ray Reflectometry (XRR) measurements using the Panalytical X'Pert Pro MRD. This document is designed as a general guide to sample aligment and reflectometry measurement, adjustments may need to be made based on your sample.
For films < 100 nm thick, data must be collected at very high angles which requires high incident beam intensity, therefore the 76887839 PreFIX will be needed.
For films > 100 nm thick, data must be collected at very high angular resolution requiring the use of a monochromator, therefore the 76887839 PreFIX will be needed.
Install 1/32° 76887839 into the PreFIX module
Set the automatic attenuator for automatic control
Collect preliminary reflectivity curve
Set the automatic attenuator for automatic control if not already set
High-resolution X-ray diffraction (HRXRD) is a collection of application techniques for the non-destructive analysis of mostly layered, nearly-perfect crystalline structured materials. Film properties are largely determined by their compositional and structural parameters. Information such as layer thickness, composition, strain, relaxation and structural quality is obtained by measuring rocking curves and reciprocal space maps using high-resolution X-ray optics. The spatial distribution of defects can be visualized by X-ray diffraction imaging methods such as X-ray topography.
In-plane diffraction refers to the diffraction technique where the incident and diffracted beams are both nearly parallel to the sample surface. The penetration depth of the beam is limited to within about 100 nm of the surface and is used to examine surface layers. This method measures diffracted beams which are scattered nearly parallel to the surface, thus measuring planes that are perpendicular to the sample surface and are inaccessible with other techniques.
The following instructions are meant to be a guide, but many of the scan parameters may change based on your samples and experience. Please note that the optics are delicate; do not bump or drop the optic housing units. If the x-rays are off, NEVER attempt to turn them back on unless specifically instructed by a lab staff member.
Select the Incident Beam Optics tab and double click on one of the item lines:
a. PreFIX Module: Cu Mirror Module.
b. Divergence Slit: 1/32o divergence slit.
c. Beam Attenuator: Ni 0.15 mm automatic, Usage should be Do Not Switch and the Activated box should be checked. It is highly recommended to cycle from Activated → Deactivated → Activated to check if the attenuator is working properly.
Select the Diffracted Beam Optics tab and double click on one of the item lines:
a. PreFix Module: Parallel Plate Collimator.
b. Receiving Slit: Parallel Plate Collimator Slit.
c. Detector: Mini prop large window 1 and the Wavelength is K alpha 1.
Select the Instrument Settings tab, double click an item, select the X-ray tab, and set the Generator to 45 kV and 40 mA.
In this section, you will position the system so that the X-ray beam is aimed directly into the detector and you will determine the intensity of the direct X-ray beam.
An attenuation foil must be mounted in the housing slot in order to attenuate the beam whenever the measured intensity is expected to exceed the maximum count rate of the detector. |
The sample height must be adjusted within a couple of micrometers of the true zero, and the sample surface must be perfectly level with the X-ray tube and detector. In this section, you will position the system so that the X-ray beam is aimed directly into the detector in order to allow you to adjust the sample height and tilt (offset).
An attenuation foil must be mounted in the housing slot in order to attenuate the beam whenever the measured intensity is expected to exceed the maximum count rate of the detector. |
Large flat samples (> 1 cm2) are easiest to work with, other samples may be possible. Maximum penetration depth is about 1,000 nm.
Notes:
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See Initializing the XRD
Create process template for tool, allows a user to fill in the details of their process.
Rocking Curve - A scan where the detector (2Theta) is left stationary, while the omega axis is scanned. The data is plotted as intensity vs Omega.
Detector Scan (2Theta Scan) - A scan where the 2Theta axis is scanned, while other axis are stationary. The data is plotted as intensity vs 2Theta
Coupled Scan - A scan where both omega and 2Theta are scanned so that 2Theta = 2*Omega. The data is plotted as intensity vs 2Theta
Critical angle (Θc) - Below the critical angle the X-Ray beam is completely reflected (total external reflection). The critical angle for a layer is a function of its electron density and composition. For a given composition, as the density of the film increases the critical angle often increases. If either the composition or the density of a layer is known, the other can be determined using XRR.
Scott A Speakman, Ph.D - Center for Materials Science and Engineering at MIT
Joachim F. Woitok - Panalytical
XRD Quick Start Guide - September 2012.pdf