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X
TECHNICAL DESCRIPTION scintillator
Taper
CCD cooling electronics
Be
Figure 4.2.1 Schematic of a fibre-optic-coupled CCD detector for x-rays
X-rays enter the vacuum detector enclosure through a Be window. The photons are intercepted by a scintillation screen, which transforms the X-rays to visible light. The light is conducted towards the
CCD detector via a fibre optic taper. The CCD chip integrates the light dose received from the taper.
Its electric signal is then amplified and digitised in a readout circuit.
The central component of the detector is the CCD chip, which is situated in a vacuum enclosure.
The vacuum enclosure isolates the chip thermically and protects it from condensation in the cooled state. The CCD chip requires cooling to reduce its dark current.
The chip is cooled by a Peltier cooler, which dissipates its heat into a Cu heat sink, which is water cooled by the CCD water chiller. The Peltier is powered with 100W to maintain the CCD chip at an operating temperature of –45 to –50ºC. A number of security systems ensure that the Peltier will not overheat the detector due to lack of cooling. The CCD detector power supply is supplied by the
CCD water chiller, which checks the water flow rate and temperature. In the case of loss of cooling water the chiller shuts down the CCD power supply. Additionally there are two heat sensor on the heat sink, which shut down the system, when the heat sink is >40ºC.
The CCD chip has a size of approximately 25 x 25mm arranged in 1024 x 1024 pixels.
In order to obtain an X-ray sensitive area of 62 x 62mm the chip is coupled to fibre-optic taper. The taper is characterised by its reduction ratio. The reduction ratio of the taper is measured in a factory calibration procedure and is typically 2.45-2.5:1. The large end of the taper is covered with scintillation screen. The screen is composed of GdOS
2
:(Tb), which is the most efficient screen material with respect to stopping power and light output. Note that the screen thickness determines the resolution of the detector.
4.2.1 Beryllium Window
The 0.5mm Beryllium window is the entrance for the X-ray photons into the detector unit. The detector unit is held under vacuum to provide thermal isolation for the Peltier cooled CCD chip. The
Be window absorbs incoming X-ray photons in the following way:
Radiation Pure Be
Absorption coeff.
(mm
-1
)
Be with 0.1% contamination (Cu)
Transmission (%) Absorption coeff.
(mm
-1
)
Transmission
(%)
Cu
Mo
Version 1.4 Xcalibur_Manual_v1.4
Page 16
Xcalibur
USER MANUAL
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Table of contents
- 10 1. Health and Safety Information
- 10 1.1 General
- 11 1.2 Electrical Safety
- 11 1.2.1 Potential Electrical Hazards
- 11 1.2.2 Recommended Precautions
- 11 1.2.3 First Aid
- 12 1.3 Mechanical Handling Safety
- 12 1.4 Safe Mechanical Practice
- 12 1.5 Moving Parts
- 12 1.6 X-ray Radiation
- 13 1.7 Extreme Temperatures
- 14 1.8 Vacuum
- 14 1.9 High Pressures
- 14 1.10 Hazardous or Toxic Materials
- 14 1.11 Modifications and Service
- 15 2. Introduction
- 15 2.1 Scope
- 15 2.2 How To Use This Manual
- 15 2.3 System Overview
- 16 3. Specifications
- 16 3.1 Environmental Requirements
- 16 3.2 Services
- 16 3.2.1 Electrical Supply
- 16 3.2.2 Water Cooling
- 17 3.2.3 Helium Gas Supply (where applicable)
- 17 3.3 Performance Data
- 17 3.3.1 X-ray Tube (Typical Operating Conditions)
- 18 3.3.2 Sapphire 2 CCD Detector
- 19 3.3.3 Sapphire 3 CCD Detector
- 20 3.3.4 Onyx CCD Detector
- 20 Onyx CCD Detector Theta and Resolution Ranges
- 21 3.3.5 PC CCD Interface
- 21 3.3.6 Four-circle Kappa Geometry X-ray Goniometer
- 22 4.4 Electrical Data
- 23 4. Technical Description
- 23 4.1 Overview
- 24 4.2 CCD Detector Technology
- 25 4.2.1 Beryllium Window
- 26 4.2.2 Phosphor
- 26 4.2.3 Taper
- 26 4.2.4 CCD
- 26 4.2.5 Readout Speed
- 26 4.2.6 Binning
- 27 4.2.7 Dark Current and MPP Mode
- 27 4.2.8 Radiation Damage
- 27 4.2.9 Full Well Depth and 18-bit Digitisation
- 27 4.2.10 Anti-blooming
- 27 4.2.11 Vacuum
- 27 4.2.12 Fast Shutter
- 28 4.2.13 Zingers and Cosmic Ray Events
- 28 4.3 Four-Circle Kappa Geometry Goniometer
- 29 4.4 X-ray Generator
- 30 4.5 Software
- 30 4.5.1 Directory Structure
- 31 4.5.2 Basic Menu Philosophy
- 31 4.6 KMW200CCD Chiller
- 31 4.7 KMW3000C Chiller
- 31 4.8 Low Temperature Option
- 31 4.9 Safety Features
- 32 5. Handling, Installation, Storage and Transit Information
- 32 5.1 Reception and Handling
- 32 5.1.1 Delivery
- 32 5.1.2 Unpacking
- 33 5.1.3 Mechanical Handling
- 33 5.1.3.1 Weights, Dimensions and Lifting Points
- 34 Delivery
- 34 5.2 Installation and Setting to Work
- 34 5.2.1 Preparation of Site and Services
- 34 5.2.1.1 Environmental Requirements
- 34 5.2.1.2 System Layout
- 35 5.2.1.3 Electrical Services
- 36 5.2.1.4 Water Supply
- 36 5.2.1.5 Low Temperature Option
- 36 5.2.1.6 CCD Camera Pumping
- 36 5.2.1.7 Helijet Option
- 37 5.2.2 Setting to Work
- 37 5.2.2.1 Equipment Required
- 37 5.2.2.2 Personnel Required for Installation
- 37 5.2.2.3 Setting up Procedures
- 39 Storage
- 40 6. Operation
- 40 6.1 Controls and Indicators
- 41 6.2 Initial Switch on Procedure
- 42 6.3 X-ray Tube Warm-up Procedure
- 43 6.4 Software
- 43 6.4.1 Software Updates
- 44 6.4.2 Software Installation
- 44 6.4.2.1 MGC interface software
- 45 6.4.2.2 CrysAlis Software
- 45 6.4.3 Changing Machine Correction and Set-up Files
- 46 6.5 Normal Operation
- 46 6.5.1 General Commands
- 48 6.5.2 Changing Xcalibur Settings
- 52 6.5.3 Standard Diffraction Experiment
- 52 6.5.3.1 Crystal Mounting and Alignment
- 54 6.5.3.2 Diffraction Photographs to Determine Crystal Quality
- 55 6.5.3.3 Unit Cell Determination
- 57 6.5.3.4 Data Collection
- 58 6.5.3.5 Data Processing and Reduction
- 59 6.5.3.5.1 Orientation Matrix
- 60 6.5.3.5.2 Run List
- 61 6.5.3.5.3 Scan Width
- 61 6.5.3.5.4 Background Evaluation
- 62 6.5.3.5.5 Special Corrections
- 63 6.5.3.5.6 Outlier Rejection
- 64 6.5.3.5.7 Output Format
- 65 6.5.3.6 Changing the Output Format from Data Reduction
- 66 6.5.3.7 Absorption Correction
- 74 6.5.3.8 GRAL - Space Group Determination
- 80 6.5.3.9 Structure Solution and Refinement
- 80 6.5.4 Ewald explorer
- 86 6.5.5 Dc Movie - Replay of Data Collection Movie
- 87 6.5.6 Reconstruction of Precession Photographs
- 91 6.5.7 Dc opti - Optimisation of Data Collection Strategy
- 96 6.5.8 Indexing and Data Reduction of Incommensurate Samples
- 97 6.5.9 Indexing and Data Reduction of Twinned Samples
- 99 6.5.10 Extracting Data from Powder Samples
- 100 6.5.11 Refining of Machine Parameter File
- 103 6.5.12 Glossary of CrysAlis Commands
- 110 6.6 Normal Shutdown
- 110 6.7 Emergency Shutdown
- 111 6.7.1 Emergency Shutdown Procedure
- 112 7. Mechanical Changeover of Detectors and X-ray Sources
- 112 7.1 Interchange of CCD Detectors
- 112 7.1.1 Installation of a Sapphire 2 and Sapphire 3 CCD detectors
- 113 7.1.2 Removal of a Sapphire 2 and Sapphire 3 CCD detectors
- 113 7.1.3 Installation of the Onyx CCD camera
- 116 7.1.4 Removal of the Onyx CCD camera
- 117 7.2 Procedure for Interchange of the Molybednum and Copper Enhance X-ray Source
- 121 8. Maintenance Schedules
- 121 8.1 Introduction
- 121 8.2 Weekly Maintenance Schedule
- 121 8.3 Monthly Maintenance Schedule
- 122 8.4 Six Monthly Maintenance Schedule
- 122 8.5 Yearly Maintenance Schedule
- 123 8.6 10,000 Hours Maintenance Schedule
- 124 9. Maintenance Instructions
- 124 9.1 Special Tools
- 124 9.2 Refining the Machine Parameter File
- 125 9.3 Changing the X-ray Tube of Enhance
- 126 9.4 Changing the X-ray Tube of Enhance ULTRA
- 128 9.5 X-ray Beam Stop Alignment
- 129 9.6 Changing the Collimator of Enhance
- 130 9.7 Changing the Collimator of Enhance Ultra
- 130 9.8 Aligning the X-ray Collimator of Enhance
- 130 9.9 Aligning the Enhance X-ray Source
- 133 9.10 Aligning the Enhance Ultra X-ray Source
- 133 9.10.1 X-ray Beam Alignment of Enhance Ultra
- 135 9.10.2 Optic Alignment of Enhance Ultra
- 136 9.10.3 Collimator Alignment of Enhance Ultra
- 136 9.10.4 Aligning the beam to the centre of the goniometer – Enhance Ultra
- 137 9.11 Checking the Door Safety Interlocks
- 137 9.12 Checking the Emergency stop
- 138 9.13 Checking the X-ray Radiation Levels
- 138 9.14 CCD Detector – Pumping Out Vacuum
- 140 9.15 Dismantling Xcalibur
- 143 10. Trouble Shooting
- 146 11. Spares
- 148 12. Disposal Instructions
- 148 12.1 X-ray Tube and CCD Detector
- 148 12.2 Third Party Equipment
- 149 13. Additional Information
- 149 13.1 Third Party Information
- 150 13.2 Drawings
- 150 13.2.1 Mechanical Drawings
- 150 Xcalibur Suggested Layout
- 150 System and Component Dimensions
- 152 13.2.2 Electrical Drawings
- 154 14. CE Conformity notice
- 155 Appendices
- 155 Appendix 1 X-ray Tubes Wave Lengths
- 155 Appendix 2 Standard Crystal Parameters
- 155 Appendix 3 Temperature Scales Conversion
- 155 Appendix 4 Maintenance Records
- 160 Appendix 5 Example of Local Rules for the Xcalibur System Set Up at Oxford Diffraction