Panalytical X'pert Pro (XRD)
Status | UP |
Issue Date and Description | |
Estimated Fix Date and Comment | |
Responding Staff | Hakan Salihoglu |
iLab Name: XRD
iLab Kiosk: BRK Metrology Core
FIC: Mike Capano
Owner: Hakan Salihoglu
Location: BRK 2239
Maximum Wafer Size: 4"/100 mm Diameter, 11 mm maximum Z travel (sample thickness axis)
Highlights
4-bounce Ge Monochromator
Three sample stages (Standard, vacuum, and a heat controlled)
Point and Line focus options
0D, 1D, and 2D detectors
Goniometer with six degrees of freedom
High speed wide angle x-ray diffraction
Measurements up to 900 oC
X-ray diffractometry on films, crystals and polycrystalline (No powder XRD)
Fast mode reciprocal space mapping
Overview
X-RAYS ARE HARMFUL. THE X-RAY DIFFRACTION SYSTEM PRODUCES X-RAYS WHICH CAN BE DANGEROUS TO HEALTH IF THE PROPER PRECAUTIONS ARE NOT TAKEN.
IT IS IMPORTANT FOR THE HEALTH AND SAFETY OF THE OPERATOR THAT THE RECOMMENDATIONS GIVEN IN THE USER'S GUIDE, MANUALS, AND THE SAFETY MANUAL ARE CAREFULLY OBSERVED.
LOCAL SAFETY REGULATIONS MUST BE STRICTLY COMPLIED WITH.
NEVER OVERRIDE ANY SAFETY DEVICE.
Panalytical X'Pert Pro MRD System is perfectly safe if operated as described in the user guide.
General Description
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:
Three sample stages:
Standard 4” wafer mount
Anton Paar DHS 900 domed hot stage for data collection from RT up to 900 °C
Vacuum stage for wafers up to 4" in diameter
Incident beam optics:
5 arc sec Ge(440) point focus module (Bartels monochromator)
19 arc sec hybrid (combination x-ray mirror + channel cut Ge(220) monochromator) line focus module
X-ray mirror
Diffracted beam optics
Triple axis module with triple axis detector and rocking curve detector
Proportional detector
Parallel plate collimator
Technology Overview
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.
Equipment Overview
XRD Cabinet/Enclosure
X-rays ON lamp is lit whenever high tension is applied to the X-ray tube.
Experimental Space. Anything in this space can be exposed to high intensity X-rays.
Parts of the enclosure exposed to direct X-ray beam are 12 mm thick steel.
Interlocked lead glass sliding doors provide access and allow visibility of the sample and stages.
X-ray absorption equivalent to 1 mm of lead.
Instrument front control panel with the following buttons and displays:
Power On - Turns the power on to the instrument, not necessarily the X-ray tube.
Stand by - Turns off the high tension generator.
Light - Switches interior cabinet lighting ON/OFF
HT (Key) - Keyed lockout for the high tension generator.
Shutter close - Closes the shutter on the tube shield irrespective of the system's current operating state.
θ, 2θ, c/s - Displays the angle or intensity of the X-ray beam measured by the detector. The choice of information displayed is made in the data collector software.
kV, mA - Displays the high tension generator's voltage and current settings.
Shutter open - Displays a 1 if the shutter is open. Displays three dots if the safety interlocks are not met (i.e. - doors closed)
Anton Parr heated stage controller
Vacuum pump controller
XRD Lab Instrument control PC and data anlaysis PC
PC 1 is a non domain PC that does not require a log on. This PC is intended for you to use when accessing the iLab kiosk and to analyse your data, its use is free. Software available here includes Epitaxy, High Score, Reflectivity, and Data Viewer.
PC 2 is a Purdue domain PC that requires you to log on using your Purdue credentials (Career Account). This PC is interlocked in iLab and you must enable the tool to power on the monitor. This PC is used to control the XRD instrument during data collection.
XRD Components
Incident Beam Optics
X-ray Tube Shield (left) and X-ray Tube (right)
9430 922 00371 Special Ceramic Tube Cu LFF (Long Fine Focus)
Overview
High power ceramic diffraction X-ray tube with copper anode, specifically designed for use with X-ray mirrors and hybrid monochromators. An X-ray tube basically consists of an evacuated envelope containing an anode, a cathode (filament), a focusing cylinder and exit windows. When a current passes through the tungsten filament, electrons are thermally emitted and accelerated toward the anode by the high voltage differential. The electrons striking the anode cause emission of X-rays. For more information about X-ray tubes see the Wikipedia article https://en.wikipedia.org/wiki/X-ray_tube.
Specifications
Operational Settings: 45 kV, 40 mA
Idle Settings: 40 kV, 20 mA
Anode Material: Cu
Characteristic Wavelength Kα1: 1.54056 Å
Characteristic Wavelength Kα2: 1.54439 Å
Characteristic Wavelength Kα: 1.54184 Å
Maximum Power: 1.8 kW
Maximum Voltage: 60 kV
Maximum Current: 55 mA
The voltage on the HT cable, connected to the X-ray tube, decays slowly to zero when the generator is switched off. Do not disconnect the HT cable from the X-ray tube.
The X-ray tube has four beryllium windows. Beryllium is poisonous, fumes and dust from beryllium metal are hazardous if inhaled or swallowed. While the X-ray tube is installed in the tube shield there is no danger present.
Specifications:
Divergent monochromatic beam
Beam width 1.2 mm
Direct beam intensity > 16 x 106 cps @ 45 kV / 40 mA
FWHM < 0.0039° (As measured on (111) reflection of the Si (111) Single crystal reference sample)
PW3110/65 Ge(220) 4-crystal Monochromator
Overview
Provides monochromatic Cu Kα1 radiation. High resolution monochromators are based on two U-shaped blocks of single-crystal nearly perfect germanium. The crystals have (110) surfaces and are preset for Ge(220) Cu Kα1 reflections. The operation of this device uses Bragg's law interaction in Ge crystals to filter the x-ray wavelengths passed. These monochromators are commonly used for measurements on nearly perfect semiconductor crystals and epitaxial layers, and is suited for most routine semiconductor measurements.
Configuration
Anti Scatter Slit adjustment knob
Adjustable Beam Mask Control
Adjusting the beam size
The beam exiting the exiting the assembly has a width of 1.2 mm. You can adjust the beam size, thus the irradiated length of sample, by means of two knobs (one vertical and one horizontal) to allow a gap of between 0 and 10 mm to be set. The knob scales are graduated in steps of 0.02 mm. The horizontal knob controls the beam width, while the vertical knob controls the height of the beam. Since the width of the beam starts at 1.2 mm, adjustment of the horizontal knob between 1.2 mm and 10 mm is ineffective.
Adjustable Beam Mask control is used to shape the height of the beam via an adjustable horizontal slit. The control allows a gap of between 0 and 10 mm to be set. The knob scales are graduated in steps of 0.02 mm.
Adjustable Divergent Slit control is used to shape the width of the beam via an adjustable vertical slit. The control allows a gap of between 0 and 10 mm to be set. The knob scales are graduated in steps of 0.02 mm.
Specifications:
Quasi-parallel monochromatic beam
Beam width 0.08 to 1.3 mm depending on installed divergence slit.
Direct beam intensity > 3.4 x 109 cps @ 30 kV / 50 mA (using rocking curve optics)
Direct beam intensity > 3 x 109 cps @ 30 kV / 50 mA (using PPC, 0.27° optics)
Overview
The graded multi layer parabolic X-ray mirror is a special kind of beam conditioner which is able to convert the divergent X-ray beam from a line focus tube to an intense monochromatic quasi parallel beam. The mirror has a reflectivity factor of 65% for the Cu Kα1 and Cu Kα2 lines. The Cu Kβ is virtually eliminated, only 0.5% of the Kβ line is diffracted by the mirror. The equatorial divergence of the beam is less than 0.05%. The axial width and divergence are not controlled by the mirror.
Configuration
Automatic Attenuator electrical connection - This needs to be connected to the instrument even if you do not intend to use the attenuator. Failure to hook this up will result in the attenuation foil being placed in the beam during all measurements.
Anti Scatter Slit adjustment knob
Beam height adjustment knob
Attentuation foil / Beam mask install location
Divergent slit install location
Accessories
Fixed Divergent slits can be used to control the height of the X-ray beam coming out of the X-ray mirror and therefore the amount (length) of the sample that is irradiated. When the 1/2° divergence slit is used, the X-ray mirror is irradiated over its complete length by the X-ray tube's line focus. The width of the X-ray beam emitted by the mirror is then 1.3 mm.
Slit Marking | Width of Beam (mm) | Sample Irradiated Length (mm) | Image | |
|---|---|---|---|---|
1/2° | 1.3 | 0.10 + 1.3 / sin(ω) | | Click on chart above to enlarge |
1/4° | 0.65 | 0.10 + 0.65 / sin(ω) | | |
1/8° | 0.33 | 0.10 + 0.33 / sin(ω) | | |
1/16° | 0.16 | 0.10 + 0.16 / sin(ω) | | |
1/32° | 0.08 | 0.10 + 0.08 / sin(ω) | |
Attenuation Foils are used to reduce the intensity of the direct X-ray beam. Under typical operating conditions the beam from the X-ray mirror can have an intensity which is much greater than 1 million cps at which point the detectors become non linear in response and can potentially be damaged.
Attenuation Foil (thk) | Attenuation Factor | Image | Measured Using | |
|---|---|---|---|---|
Cu (0.1 mm) | 98.3 | | Cu Kα | Attenuation factor = Intensityno_attenuation / Inensityattenuated 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. |
Cu (0.2 mm) / Ni (0.02 mm) | 19,842 | |
Automatic Beam Attenuator contains a metal foil that can be set to be switched in and out of the X-ray beam at a preset angle or intensity. The device uses a 0.125 mm thick nickel foil with attenuation factor approximately equal to 200, the exact value is labeled on the attenuator. Its use is configured in the Data Collector software.
Beta-filter is used to keep as much as possible of the Kα radiation from the tube, while suppressing the Kβ and white radiation. By inserting a beta-filter with an appropriate absorption edge and thickness into the X-ray beam, the Kβ line almost disappears. The beta-filter is typically used when the sample fluoresces under characteristic radiation, leading to increased levels of background. If your sample contains high amounts of Cu, the same material as the anode, then it is best to place this filter in the incident beam path to reduce sample fluorescence.
X-ray Anode | Beta-filter | K absorption edge (Å) | Thickness (mm) | Kβ intensity reduction (%) | Kα intensity reduction (%) | Image |
|---|---|---|---|---|---|---|
Cu | Ni | 1.488 | 0.02 | 99 | 59 | |
Adjustable Beam Mask control is used to shape the height of the beam via an adjustable horizontal slit. Control allows a gap of between 0 and 10 mm to be set. The knob scales are graduated in steps of 0.02 mm.
Adjustable Anti Scatter Slit control is used to set the anti scatter slit width to the width of the beam. The appropriate setting is determined by the slit used, see table above. (example - if 1/2 slit is used, then set the vertical slit to 1.3 mm) Control allows a gap of between 0 and 10 mm to be set. The knob scales are graduated in steps of 0.02 mm.
Specifications:
Direct beam intensity > 1 x 108 cps (using rocking curve optics)
Direct beam intensity > 5 x 107 cps (using PPC, 0.27° diffracted beam optics)
Line focus
Parallel beam
Beam width 0.15 to 1.2 mm depending on installed divergence slit.
FWHM < 0.0052° (As measured on (111) reflection of the Si (111) Single crystal reference sample)
Overview
The hybrid monochromator 4X is an incident beam PreFIX module, consisting of a combination of an X-ray mirror and a 2-crystal Ge(220) 4-bounce monochromator. The acceptance angle from the line focus of the x-ray tube is 0.8. The Cu K radiation is suppressed to a level below 0.1%. The width of the x-ray beam is controlled by divergent slits. The height of the x-ray beam is controlled by beam masks or alternatively, beam attenuator foils or filters can be installed in this holder.
Configuration
Automatic Attenuator electrical connection
Attentuation foil / Beam mask install location
Divergent slit install location
Accessories
Fixed Divergent slits can be used to control the height of the X-ray beam coming out of the Hybrid Monochromator and therefore the amount (length) of the sample that is irradiated. When the 1/2° divergence slit is used, the Hybrid Monochromator is irradiated over its complete length by the X-ray tube's line focus. The width of the X-ray beam emitted by the mirror is then 1.2 mm.
Slit Marking | Width of Beam (mm) | Sample Irradiated Length (mm) | Image | |
|---|---|---|---|---|
1/2° | 1.2 | 1.2 / sin(ω) | | Click on chart above to enlarge |
1/4° | 0.6 | 0.6 / sin(ω) | | |
1/8° | 0.3 | 0.3 / sin(ω) | | |
1/16° | 0.15 | 0.15 / sin(ω) | | |
1/32° | 0.08 | 0.08 / sin(ω) | |
Attenuation Foils are used to reduce the intensity of the direct X-ray beam. Under typical operating conditions the beam from the Hybrid Monochromator can have an intensity which is much greater than 1 million cps at which point the detectors become non linear in response and can potentially be damaged.
Attenuation Foil (thk) | Attenuation Factor | Image | Measured Using | |
|---|---|---|---|---|
Cu (0.1 mm) | 98.3 | | Cu Kα | Attenuation factor = Intensityno_attenuation / Inensityattenuated 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. |
Cu (0.2 mm) / Ni (0.02 mm) | 19,842 | |
Automatic Beam Attenuator contains a metal foil that can be set to be switched in and out of the X-ray beam at a preset angle or intensity. The device uses a 0.125 mm thick nickel foil with attenuation factor approximately equal to 200, the exact value is labeled on the attenuator. Its use is configured in the Data Collector software.
Sample Platform or Stage
Horizontal X'Pert PRO Goniometer
The goniometer contains θ and 2θ axes, the basic axes in X-ray diffractometry. The goniometer also has specific mounting positions for the X-ray tube, the incident beam optics, the sample stage, the diffracted beam optics, and the X-ray detector.
Specifications
Goniometer Radius: 320 mm
Minimum step size in θ and 2θ: 0.0001°
Maximum step size in θ and 2θ: 1.27°
Configuration
Beam Path 1 detector mounting position (PW3120/60 Triple Axis and Rocking Curve Attachment shown mounted)
Divergent beam PreFIX module mounting position (PW3120/60 Triple Axis and Rocking Curve Attachment shown mounted)
All-Purpose MRD Cradle (Shown with no sample stage mounted)
Incident beam PreFIX module mounting position (PW3147/20 Hybrid Monochromator 4X mounted)
X-ray tube shield in standard position
PW3060/20 All-Purpose MRD Cradle
The all-purpose MRD cradle is a Eulerian cradle designed to accommodate large samples and provide five motorised axis (Φ, Ψ, X, Y, and Z).
Specifications