Bruker Anton Paar User Manual
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Bruker Anton Paar User Manual

Temperature chambers for d8 advance / d8 discover
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Anton Paar
Temperature Chambers
for D8 ADVANCE / D8 DISCOVER
User Manual
Original Instructions (English)
XRD
Innovation with Integrity

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  • Page 1 Anton Paar Temperature Chambers for D8 ADVANCE / D8 DISCOVER User Manual Original Instructions (English) Innovation with Integrity...
  • Page 2 All configurations and specifications are subject to change without notice. Order no. DOC-M88-EXX268 V1. Dec 20, 2016. © 2016 Bruker AXS GmbH, Karlsruhe, Germany. All trademarks and registered trademarks are the sole property of their respective owners. Printed in the Federal Republic of Germany.

  • Page 3: Table Of Contents

    Contents Contents List of Figures.......................... 7 Safety Guidelines ........................ 13 About this Manual ...................... 13 Qualified Personnel...................... 14 Correct and Intended Usage.................. 15 Disclaimer and Liability .................... 15 General Safety Precautions .................. 15 Signage........................ 18 General Remarks ........................ 19 Heating Principles ...................... 19 Temperature Measurement and Calibration .............. 20 2.2.1 Temperature Measurement .................. 20 2.2.2...
  • Page 4 Installation and Operation of the HTK-Series, TTK 600, XRK 900, and HPC 900 Chambers .............................. 49 Introduction ........................ 49 Mounting the Chamber to the Goniometer.............. 50 Temperature Controllers for Anton Paar Chambers ............ 53 6.3.1 Connecting the TCU Controller.................. 54 Configuring the Chamber in DIFFRAC.MEASUREMENT CENTER...... 56 Operation ........................ 56...
  • Page 5 Contents 8.6.2 Optimizing Theta, Two Theta and Psi................ 87 8.6.2.1 Optimizing Theta...................... 87 8.6.2.2 Optimizing Two Theta .................... 88 8.6.2.3 Optimizing Psi: ...................... 89 8.6.3 Creating a Temperature Dependent Measurement Using the WIZARD...... 90 Installation and Operation of the BTS 150 and BTS 500 Chambers ........ 95 Introduction ........................ 95 Mounting the Chamber to the Goniometer.............. 95 USB Connection of the BTS 150/500 to the CPU1 Board ........... 97...
  • Page 6 Contents DOC-M88-EXX268_V1_12.2016...

  • Page 7: List Of Figures

    List of Figures List of Figures Figure 2.1: Temperature dependence of lattice parameter a0 of MgO........Figure 3.1: Mounting the Edwards turbomolecular pump to the flexible bellow......Figure 3.2: Connecting the vacuum tube to the HTK 1200N chamber ........Figure 3.3: Mounting the Edwards backing-pump to the flexible vacuum line ......
  • Page 8 List of Figures Figure 6.8: Connecting serial lines to the Universal IO-Board ........... Figure 7.1: CHC plus chamber fully mounted on vertical diffractometer........Figure 7.2: Front view of TCU110....................Figure 7.3: Front view of a CCU100 Controller................Figure 7.4: Front view of MHG controller ................... Figure 7.5: Julabo Waterbath (Corio CD-201F) ................
  • Page 9 List of Figures Figure 8.10: Z-scan at 25 °C over a wide range to determine roughly the height position ..Figure 8.11: Z-scan at 25 °C with determination of height position ..........Figure 8.12: Rocking-curve scan at 25 °C with determination of rotation error ......Figure 8.13: Inserting the temperature depending Z-positions and activating them ....
  • Page 10 List of Figures Figure 10.12: Import sections ......................108 Figure 10.13: Sections created for CHC plus ................109 Figure 10.14: CHC_Stage Chamber Temperature Details ............110 Figure 10.15: CHC_Stage Sample Temperature Details............... 111 Figure 10.16: TOOLS information for actual parameters of CHC plus .......... 112 Figure 10.17: CHC plus Controller Details..................
  • Page 11 List of Figures Figure 10.39: Selecting SerialLine/Power X1_RS232_1/-2 for SerialConnector ......127 Figure 10.40: Selecting SerialLine/Full X2_RS232_1/-2 for SerialConnector........ 127 Figure 10.41: Introducing the Board CPU to the controllers section ..........127 Figure 10.42: Selecting SerialLine/Full TTYS0/1 for SerialConnector ........... 128 Figure 10.43: Connecting serial lines to the Universal IO-Board ...........
  • Page 12 List of Figures DOC-M88-EXX268_V1_12.2016...

  • Page 13: Safety Guidelines

    This manual and the manual of the supplier contain general information and guidelines about the Bruker AXS instruments, which have to be observed to ensure personal safety, as well as to protect the product. These notices are highlighted in this manual by the warn- ing symbols and are marked as follows according to the level of danger.

  • Page 14: Qualified Personnel

    The primary installation, maintenance and repair of the temperature chamber must be car- ried out only by personnel who are authorized by Bruker AXS. All repairs, adjustments and alignments performed at any component of the system...

  • Page 15: Correct And Intended Usage

    Correct function of the instrument The instrument can only function correctly and safely if it is transported, stored, setup, and installed correctly, and if it is operated and maintained as recommended by Bruker AXS and the manufacturer of the temperature chamber.
  • Page 16 Safety Guidelines CAUTION Extremely hot and cold surfaces from -190 °C to 2300 °C on internal components Risk of severe burns when touching the surfaces. u Turn off the device and wait until components have cooled down! u Do not touch the sample holder or internal shieldings before ambient conditions are reached Some temperature chambers need liquid Nitrogen (LN ) for operation.
  • Page 17 Safety Guidelines WARNING Beryllium Beryllium is carcinogenic and causes diseases of the skin, splenic, liver and lungs. u Never touch, inhale or incorporate fumes, dust or pieces of beryllium. u Wear personal protective equipment (PPE). u Do not touch any part of the instrument which contains beryllium, e.g. X-ray tube radiation outlet window, the detector front window or the heating chamber windows of some systems.

  • Page 18: Signage

    Safety Guidelines Signage The following symbols and information signs can be found or displayed on the instrument. They refer to their immediate surroundings. Strictly obey all instructions and warning text printed on the labels which are attached to the various parts of the equipment. Symbol Meaning of the Symbol Danger of freezing or burning due to hot...

  • Page 19: General Remarks

    • Heating / cooling devices can be roughly divided into two groups: direct heaters and environmental heaters. • Anton Paar chambers cover the range from RT up to 2300 °C for heating systems. • Additional cooling increases the range down to –193 °C.

  • Page 20: Temperature Measurement And Calibration

    General Remarks Some features of environmental heaters are: • Convection (at lower temperatures without vacuum) and radiation heating (at high temperatures or under vacuum) are used. • A crucible can be used to hold the sample. • Different chemically inert sample holders are provided. •...

  • Page 21: Temperature Calibration

    General Remarks 2.2.2 Temperature Calibration The temperature sensor used for controlling can indicate a wrong value for the sample, because the position of the sensor differs from the sample position. Another reason is the reduced contact of the sample and the sample holder. These effects are increasing for ex- treme temperatures.

  • Page 22: Detailed Procedure For Temperature Determination

    General Remarks The accuracy of temperature determination with MgO is ± 20 °C below 500 °C, ± 30 °C up to 1000 °C and less than ± 40 °C up to 1400 °C. (0.001 Å change in lattice parameter cor- responds to a temperature change of 17 °C). Table 2.1: Reflections of MgO (a = 4.2112 Å), CuK -rad.

  • Page 23: Shortened Procedure For Temperature Determination

    General Remarks 2.2.2.1.2 Shortened Procedure for Temperature Determination Put a small amount of MgO on the heater or the sample holder. Start a scan for the reflec- tion (422) at about 126 °C. The program DIFFRAC.EVA [2] allows the determination of the peak position (λ=1.5405 Å) and the d-value d and the lattice constant with a =√24*d...

  • Page 24: Temperature Calibration By Phase Transitions

    General Remarks 2.2.2.2 Temperature Calibration by Phase Transitions Table 2.2: Some Samples with structural phase transitions useful for temperature calibration Sample Temperature Transition Temperature Transition Remark [°C] [°C] TlNO orh. → trig. trig. → cub. orh. → trig. TlNO trig. → cub. CsNO trig.
  • Page 25 General Remarks Sample Temperature Transition Temperature Transition Remark [°C] [°C] Aluminum melting Reacts with Pt, Ta, Mo Silver melting Reacts with Pt, Ta, Mo Copper 1085 melting Reacts with Pt, Ta, Mo DOC-M88-EXX268_V1_12.2016...
  • Page 26 General Remarks DOC-M88-EXX268_V1_12.2016...

  • Page 27: Vacuum Equipment

    Vacuum Equipment Vacuum Equipment Two examples for the installation of vacuum pumps for heating chambers are presented. One concerns the Edwards turbomolecular pump and its mounting in the front of the D8 enclosure and the second shows how to install the Edwards backing pump. Installation of the Edwards High Vacuum Stage with TIC 3.1.1 Mounting of the Edwards High Vacuum Stage...

  • Page 28: Figure 3.1: Mounting The Edwards Turbomolecular Pump To The Flexible Bellow

    Vacuum Equipment Figure 3.1: Mounting the Edwards turbomolecular pump to the flexible bellow Figure 3.2: Connecting the vacuum tube to the HTK 1200N chamber DOC-M88-EXX268_V1_12.2016...

  • Page 29: Figure 3.3: Mounting The Edwards Backing-Pump To The Flexible Vacuum Line

    Vacuum Equipment Figure 3.3: Mounting the Edwards backing-pump to the flexible vacuum line Connecting the cables to the TIC controller and the relays box An extension has to be connected between the TIC controller and the turbo pump and feed through the labyrinth of the D8 radiation safety enclosure, see next 2 pictures. Fur- ther connections are the interface cable for the WRG (wide range gauge) and the vent valve (which has to be installed in the TMP body).

  • Page 30: Figure 3.4: Back Sides Of: Edwards Turbomolecular Instrument Controller (Tic, Left Side) And Edwards Relay Box (Right Side)

    Vacuum Equipment 1. Connect the cables: Figure 3.4: Back sides of: Edwards turbomolecular instrument controller (TIC, left side) and Edwards relay box (right side) Mains supply Terminator plug Connection to TIC Vent valve Mains supply Turbo pump Backing pump Connection to relay box 2.

  • Page 31: Operation Of The Edwards High Vacuum Stage

    Vacuum Equipment 3.1.2 Operation of the Edwards High Vacuum Stage Five soft keys on the Turbo Instrument controller (TIC) front are used to control and pro- gram the TIC. In the figure below the starting screen is shown and the soft keys are de- scribed, programming is expected to be done.

  • Page 32: Installation Of The Edwards Backing-Pump

    Installation of the Edwards Backing-Pump Some applications only require a vacuum of about 10  mbar. Therefore a backing-pump is sufficient. Bruker AXS offers the Edwards backing pump with 12 m /h (might be smaller in actual systems) intake volume. Figure 3.6: Vacuum sensor, flooding valve, tube to chamber and mist-filter mounted...

  • Page 33: Figure 3.7: Display And Backside Of The Vacuum Indicating Instrument

    Vacuum Equipment It is connected to the chamber with DN25KF flexible metal hoses and equipped with a vacuum sensor and a manually operated flooding valve. The mist filter absorbs accessing oil. The vacuum indicating instrument can be placed in - or outside the D8 enclosure. 1.
  • Page 34 Vacuum Equipment DOC-M88-EXX268_V1_12.2016...

  • Page 35: Adjustment Of A Chamber On The D8

    Adjustment of a Chamber on the D8 Adjustment of a Chamber on the The Anton Paar chamber has to be installed on the goniometer as described in chapter 5 and onward. This chapter discusses general alignment procedures. For chamber specific details, we refer to the chapter discussing the chamber of interest.

  • Page 36: Adjustment Procedure With Alignment Slit

    4. Fix the adapter to the goniometer. Alignment Then proceed as following (see your Anton Paar Manual for chamber specifics): 1. Insert absorbers to ensure a count rate of <10 kcps in the direct beam. Open the receiving slit of the detector (0D-detector) or use all strips of the LYNXEYE detector in 0D mode.
  • Page 37 Adjustment of a Chamber on the D8 Height check u If you have a motorized Z-stage, proceed as follows for height check: 1. Perform a scan of the Z-motor and move the chamber to the position of maximum intensity. u If you do not have a motorized Z-stage, proceed as follows for height check: 1.

  • Page 38: Figure 4.1: Rocking Curve To Check Chamber Rotation Error

    Adjustment of a Chamber on the D8 Figure 4.1: Rocking curve to check chamber rotation error The alignment of the rotation of the chamber may be done either by physically rotating the chamber body or by introducing a sofware offset. See the 2 following subchapters Rotation alignment by physical adjustment of the chamber 1.

  • Page 39: Figure 4.2: Final Position After Rotation Correction

    Adjustment of a Chamber on the D8 Figure 4.2: Final position after rotation correction 3. Repeat steps Performing a rocking curve and Physical adjustment of the chamber rotation iteratively until the angular offset is 0° ± 0.05° (see figure above). 4. Repeat the step Height check for a final height check. The scans might look different and a change in the parameters can be necessary due to different slit sizes or small differences between temperature chambers.

  • Page 40: Alternative Procedure Without Alignment Slit

    Adjustment of a Chamber on the D8 Figure 4.3: Insert a deflection angle in CONFIGURATION for the temperature stage 1. Determine the ZI-value (figure ) and insert it as a deflection angle in CONFIGURATION | Basic instrument information | Device | Goniometer | Center | PAAR_Z_HTK1200 for the temperature stage (see figure Rocking curve to check chamber rotation error [} 38]...

  • Page 41: Figure 4.4: Z-Scan Over A Wide Range To Roughly Determine The Right Sample Height

    Adjustment of a Chamber on the D8 Alignment 1. Make sure that the diffractometer in the setup that will be used for the non-ambient measurements is well aligned. 2. Insert absorbers to ensure a count rate of <10 kcps in the direct beam. Open the receiving slit of the detector (0D detector) or use all strips of the LYNXEYE detector in 0D mode.

  • Page 42: Figure 4.5: More Accurate Z-Scan To Determine The Right Sample Height

    Adjustment of a Chamber on the D8 3. repeat the scan in a narrower range with a smaller step size Figure 4.5: More accurate Z-scan to determine the right sample height u If you do not have a motorized Z-stage, 1. Open the ratemeter (COMMANDER | Commander drop-down menu | Ratemeter) and open the shutter.

  • Page 43: Figure 4.6: Rocking Curve At Correct Sample Height

    Adjustment of a Chamber on the D8 Alignment - Continuation 1. Perform a rocking curve scan from -2° to 2°, with a 0.01° step size. Figure 4.6: Rocking curve at correct sample height 2. Determine the ZI-value (figure Rocking curve to check chamber rotation error [} 38]) and insert it as a deflection angle in CONFIGURATION | Basic instrument information | Device | Goniometer | Center | PAAR_Z_HTK1200 for the...

  • Page 44: Using Automated Height Correction

    Adjustment of a Chamber on the D8 4.1.3 Using Automated Height Correction If your alignment stage is equipped with a motorized Z-translation, the chamber height can be automatically corrected for e.g. thermal expansion of the sample holder. This requires a determination of chamber height for a number of temperatures by the procedure de- scribed in chapter Alternative Procedure Without Alignment Slit [} 40].
  • Page 45 Adjustment of a Chamber on the D8 Temperature [°C] Z-Position [mm] 0.22 0.1714 0.1262 0.07 1000 0.0024 1100 -0.0495 1200 -0.0992 Note: The elements in the list for temperatures and Z-Position must have exactly the same length. DOC-M88-EXX268_V1_12.2016...

  • Page 46: Figure 4.7: Inserting The Temperature Depending Z-Positions

    Adjustment of a Chamber on the D8 Figure 4.7: Inserting the temperature depending Z-positions After saving the configuration, activating it and reconnecting, these values become active. The Z-position can no longer be set independently, but it will now be set automatically (in COMMANDER and WIZARD) according to its calibrated positions at the working tempera- ture.

  • Page 47: Mounting The Temperature Controller Into The D8 Enclosure

    Mounting the Temperature Controller into the D8 Enclosure Four height units are required to mount the Anton Paar controller into the rack. Depending on other components, the fitting position varies. The controllers are coming in table top housings and can be mounted into the D8 enclo- sure.

  • Page 48: Figure 5.3: Removing The Supporting Feet For Rack Mount

    Mounting the Temperature Controller into the D8 Enclosure 3. To remove the supporting feet: Remove the four screws in the corners of the back side of the controller. 4. Take off the plastic end caps. ´ Now the bottom cover can be pulled off. 5.

  • Page 49: Installation And Operation Of The Htk-Series, Ttk 600, Xrk 900, And Hpc 900 Chambers

    Introduction This chapter contains all relevant user information for installing and operating a range of Anton Paar temperature chambers that are all mounted in the goniometer center and have similar modes of operation. Chambers that are included are the following: •...

  • Page 50: Mounting The Chamber To The Goniometer

    Installation and Operation of the HTK-Series, TTK 600, XRK 900, and HPC 900 Chambers Mounting the Chamber to the Goniometer All Anton Paar chambers discussed in this chapter have the same interface for mounting them into the goniometer center. How to mount these chambers is described in the follow- ing paragraph.

  • Page 51: Figure 6.2: Red Dots For The Bayonet Fixture In The "Locked" Position

    Installation and Operation of the HTK-Series, TTK 600, XRK 900, and HPC 900 Chambers 5. Insert it by aligning the red dots on chamber and diffractometer and then rotating clockwise. Figure 6.2: Red dots for the bayonet fixture in the “locked” position 6.

  • Page 52: Figure 6.4: Htk 1200N Mounted On A Goniometer

    DIFFRAC.DA VINCI if your machine is equipped with this. For detailed instructions on connecting the chamber to the controller, cooling water, com- pressed air cooling, vacuum/gas, and/or liquid nitrogen cooling, we refer to the Anton Paar Manual supplied with the chamber.

  • Page 53: Temperature Controllers For Anton Paar Chambers

    Installation and Operation of the HTK-Series, TTK 600, XRK 900, and HPC 900 Chambers Temperature Controllers for Anton Paar Chambers Anton Paar supplies two temperature controller versions: the TCU series with built-in Eu- rotherm 2604 controller and the new CCU series. Both versions can be mounted into the D8 cabinet in the same way.

  • Page 54: Connecting The Tcu Controller

    Installation and Operation of the HTK-Series, TTK 600, XRK 900, and HPC 900 Chambers 6.3.1 Connecting the TCU Controller Figure 6.7: Front view of TCU110C mounted in a D8 DISCOVER Physically, the serial lines are connected to X1 (via a Z-cable, A27D25) or X2 (via a Y-ca- ble, A27D26) of the Universal IO-Board (see figure below).

  • Page 55: Figure 6.8: Connecting Serial Lines To The Universal Io-Board

    Installation and Operation of the HTK-Series, TTK 600, XRK 900, and HPC 900 Chambers Figure 6.8: Connecting serial lines to the Universal IO-Board TCU/CCU UIOB X1 / Z-cable RS232-I | UIOB X1 UIOB X2 / Y-cable RS485 | UIOB X1 (not used) TCU/CCU RS232-II | UIOB X1 RS232-I | UIOB X2...

  • Page 56: Configuring The Chamber In Diffrac.measurement Center

    Configuring the Chamber in DIFFRAC.MEASUREMENT CENTER Normally, Anton Paar stages come preinstalled with a new system or will be installed by a Bruker technician upon purchase. They should therefore be ready to use. If this is not the case, or for some reason the chamber needs to be reinstalled in DIFFRAC.MEASURE-...

  • Page 57: Alignment

    Installation and Operation of the HTK-Series, TTK 600, XRK 900, and HPC 900 Chambers To start using the chamber, follow these steps: 1. Open the water supply. 2. Switch on the controller and wait until the booting process is finished. Check for messages and follow the instructions.
  • Page 58 Installation and Operation of the HTK-Series, TTK 600, XRK 900, and HPC 900 Chambers DOC-M88-EXX268_V1_12.2016...

  • Page 59: Installation And Operation Of The Chc Plus Humidity Chamber

    The mounting of the CHC plus is the same as for the chambers in chapter 5. For instruc- tions, see para-graph Mounting the Chamber to the Goniometer [}  50]. A picture of a mounted CHC plus is shown below. For connection of all the cables, see the Anton Paar Manual. DOC-M88-EXX268_V1_12.2016...

  • Page 60: Temperature Controllers And Water Circuit For Chc Plus

    Humidity sensor Temperature Controllers and Water Circuit for CHC plus Anton Paar supplies two temperature controller versions: the TCU series with built-in Eu- rotherm 2604 controller and the new CCU series. Both versions, as well as the humidity controller (Figure 7.4) can be mounted into the D8 enclosure in the same way or in a sep- arate rack (close to the diffractometer on the back right side) powered by the diffractome- DOC-M88-EXX268_V1_12.2016...

  • Page 61: Figure 7.2: Front View Of Tcu110

    Installation and Operation of the CHC plus Humidity Chamber ter supply line voltage. Steps for doing this are given in section Connecting the MHG for CHC plus [} 65]. The steps for the software integration of the controllers are given in sec- tion CHC plus [} 107] of the Appendix.

  • Page 62: Figure 7.5: Julabo Waterbath (Corio Cd-201F)

    Installation and Operation of the CHC plus Humidity Chamber Figure 7.5: Julabo Waterbath (Corio CD-201F) Operation of the CHC plus requires: • Electrical supply: – TCU110  / CCU100 temperature controllers and MHG must be connected to the mains board plugs X101. –...

  • Page 63: Figure 7.6: Power Supply Multiple Socket

    Installation and Operation of the CHC plus Humidity Chamber Figure 7.6: Power supply multiple socket Figure 7.7: MHG Power supply adapter DOC-M88-EXX268_V1_12.2016...

  • Page 64: Figure 7.8: Back Side Of Julabo Waterbath (Corio Cd-201F)

    Installation and Operation of the CHC plus Humidity Chamber Figure 7.8: Back side of Julabo Waterbath (Corio CD-201F) USB Connection to CPU board Water backflow from temperature controller Connection to water cooler Water out to CHC plus DOC-M88-EXX268_V1_12.2016...

  • Page 65: Connecting The Ccu Controller

    Installation and Operation of the CHC plus Humidity Chamber 7.3.1 Connecting the CCU Controller The serial lines from the controller are connected to X1 (via a Z-cable, A27D25) or X2 (via a Y-cable, A27D26) of the Universal IO-Board. Figure 7.9: Back view of CCU100 The modbus protocol is used for communication.

  • Page 66: Figure 7.11: Rs232 Connection From Uiob To Temperature Controller, Mhg Controller And Ju

    Installation and Operation of the CHC plus Humidity Chamber Figure 7.11: RS232 connection from UIOB to Temperature controller, MHG controller and Julabo HE-4 water circuit to TCU/CCU UIOB X1 / Z-cable RS232-I | UIOB X1 UIOB X2 / Y-cable RS485 | UIOB X1 (not used) to Julabo HE-4 RS232-II | UIOB X1 RS232-I | UIOB X2...

  • Page 67: Figure 7.12: Cpu Board With Usb Connection Of The Corio Water Bath

    Installation and Operation of the CHC plus Humidity Chamber Adapter cable A24D25 is used for plug UIOB X1 which supports two RS232 (null modem) and one RS485 ports. Adapter cable A24D26 is used for plug UIOB X2 which supports two RS232 ports (with hardware handshake and power lines). Do not change the connectors A25D25 and A25D26.

  • Page 68: Figure 7.13: Rs232 Connections From Uiob To Julabo Heating Circulator And Water Connections

    Water bath outlet to CHC plus Water bath outlet (to drain) Water bath inlet (from tap) The Julabo controller configuration was set to ‘remote’ at Bruker AXS to allow operation by the DIFFRAC.Measurement software, no further changes are required. DOC-M88-EXX268_V1_12.2016...

  • Page 69: Configuring The Chamber In Diffrac.measurement Center

    Configuring the Chamber in DIFFRAC.MEASUREMENT CENTER Normally, Anton Paar stages come preinstalled with a new system or will be installed by a Bruker technician upon purchase. They should therefore be ready to use. If this is not the case, or for some reason the chamber needs to be reinstalled in DIFFRAC.MEASURE- MENT CENTER, we refer to chapter CHC plus [} 107]...
  • Page 70 Installation and Operation of the CHC plus Humidity Chamber For small temperature changes or temperature settings close to the limits choose a small ramping rate e.g. 1°/s or less to avoid over/undershoot of the sample temperature. Uncorrected sample height (Z-Position) will lead to slightly wrong lattice parameters! To start using the chamber, follow these steps: 1.

  • Page 71: Figure 7.15: Setting A New Temperature And Humidity With Commander

    Installation and Operation of the CHC plus Humidity Chamber Figure 7.15: Setting a new temperature and humidity with COMMANDER 7. Press Set and wait until the temperature and humidity are reached. Figure 7.16: Selecting the temperature mode in the COMMANDER DOC-M88-EXX268_V1_12.2016...

  • Page 72: Alignment

    Installation and Operation of the CHC plus Humidity Chamber ´ This may take some minutes if the water bath has to he heated or cooled for a new sample temperature ´ The example shows a heating chamber with Z-drive. It automatically corrects the chamber height as function of temperature (height at 25 °C is 1 mm).

  • Page 73: Installation And Operation Of The Dcs 350 And Dhs 1100 Chambers

    Installation and Operation of the DCS 350 and DHS 1100 Chambers Installation and Operation of the DCS 350 and DHS 1100 Chambers Introduction The DHS  1100 and DCS  350 (Domed Hot Stage and Domed Cooling Stage) chambers are designed for heating and/or cooling samples that have to be mounted on four-circle goniometers or on XYZ-stages.

  • Page 74: Figure 8.1: Fixing The Dcs 350 Onto The Sample Stage

    Installation and Operation of the DCS 350 and DHS 1100 Chambers NOTICE Due to the fragility of the chamber dome, it is recommended to remove this before mounting the chamber to avoid breakage. Figure 8.1: Fixing the DCS 350 onto the sample stage DOC-M88-EXX268_V1_12.2016...

  • Page 75: Temperature Controllers Dc S350 And Dhs 1100

    Figure 8.2: Fixing the DHS 1100 onto the sample stage For detailed instructions on connecting the chamber to the controller, cooling water, com- pressed air cooling, vacuum/gas, and/or liquid nitrogen cooling, we refer to the Anton Paar Manual supplied with the chamber.

  • Page 76: Configuring The Chamber In Diffrac.measurement Center

    Configuring the Chamber in DIFFRAC.MEASUREMENT CENTER Normally, Anton Paar stages come preinstalled with a new system or will be installed by a Bruker technician upon purchase. They should therefore be ready to use. If this is not the case, or for some reason the chamber needs to be reinstalled in DIFFRAC.MEASURE- MENT CENTER, we refer to chapter DCS 350 and DHS 1100 [} 126]...

  • Page 77: Operation

    Installation and Operation of the DCS 350 and DHS 1100 Chambers Operation This paragraph describes basic operation of the chamber. More advanced features, in- cluding automatic alignment and temperature programming are discussed in upcoming sections. For small temperature changes or temperature settings close to the limits choose a small ramping rate e.g.

  • Page 78: Figure 8.5: Da Vinci Overview With Sample Stage

    Installation and Operation of the DCS 350 and DHS 1100 Chambers Figure 8.5: DA VINCI overview with sample stage 2. Click the arrow next to this field. ´ A drop down menu appears. 3. Select the chamber you want to use. 4.

  • Page 79: Operating The Chamber

    Installation and Operation of the DCS 350 and DHS 1100 Chambers Figure 8.6: DA VINCI with DHS 1100 selected 5. The fields for temperature control should now appear in the bottom left of the COMMANDER plug-in (next figure). Figure 8.7: Temperature control field in COMMANDER 8.5.2 Operating the Chamber To start using the chamber, follow these steps:...

  • Page 80: Figure 8.8: Setting A New Temperature And Heating Rate With Commander

    Installation and Operation of the DCS 350 and DHS 1100 Chambers 4. Insert a new temperature (°C) and a ramp rate (°C/s) in the according fields, use mode Set Temperature with Rate (the mode Set Temperature does NOT allow to use a ramp rate but reaches the next temperature as fast as possible, which risks uncontrolled heating and overshoot).

  • Page 81: Alignment

    Installation and Operation of the DCS 350 and DHS 1100 Chambers 1. If this works successfully, you can start automatic measurements as described in your temperature controller manual and in the manuals for DIFFRAC.SUITE [4] and WIZARD [5]. 2. Check box to wait for temperature reached before starting the scan. Without temperature dependent height correction, peak positions might be wrong for temperature >25 °C (alignment temperature).

  • Page 82: Figure 8.10: Z-Scan At 25 °C Over A Wide Range To Determine Roughly The Height Position

    Installation and Operation of the DCS 350 and DHS 1100 Chambers u Make sure that the diffractometer in the setup that will be used for the non-ambient measurements is well aligned. 1. Insert absorbers to ensure a count rate of <10 kcps in the direct beam. Open the receiving slit of the detector (0D detector) or use all strips of the LYNXEYE detector in 0D mode.

  • Page 83: Figure 8.11: Z-Scan At 25 °C With Determination Of Height Position

    Installation and Operation of the DCS 350 and DHS 1100 Chambers Figure 8.11: Z-scan at 25 °C with determination of height position 4. Perform a rocking curve scan from ‑2° to 2°, with a 0.01° step size. DOC-M88-EXX268_V1_12.2016...

  • Page 84: Figure 8.12: Rocking-Curve Scan At 25 °C With Determination Of Rotation Error

    Installation and Operation of the DCS 350 and DHS 1100 Chambers Figure 8.12: Rocking-curve scan at 25 °C with determination of rotation error 5. If you get a plateau instead of a broad peak, the sample height is too low. The sample height is ok if peak intensity is half of the maximum intensity (if the detector is not saturated).
  • Page 85 Installation and Operation of the DCS 350 and DHS 1100 Chambers 10.Transfer these values to the CONFIGURATION and check the box for Automatic Correction. ´ After saving the configuration, activating it and reconnecting, these values become active. The Z-position can no longer be set independently, but it will now be set automatically (in COMMANDER and WIZARD) according to its calibrated positions at the working temperature.

  • Page 86: Figure 8.13: Inserting The Temperature Depending Z-Positions And Activating Them

    Installation and Operation of the DCS 350 and DHS 1100 Chambers Figure 8.13: Inserting the temperature depending Z-positions and activating them Note: The elements in the list for temperatures and Z-Position must have exactly the same length. DOC-M88-EXX268_V1_12.2016...

  • Page 87: Optimizing Theta, Two Theta And Psi

    Installation and Operation of the DCS 350 and DHS 1100 Chambers 8.6.2 Optimizing Theta, Two Theta and Psi Alignment of additional motor positions (Psi, Theta, Two Theta, etc.) can make sense for e.g. single crystal heating or cooling experiments. Pre-alignment of the sample is necessary before starting the experiment. Further opti- mizations can then be performed automatically by the software at each temperature if the aligned positions are transferred to or edited in the WIZARD in HR-XRD mode.

  • Page 88: Optimizing Two Theta

    Installation and Operation of the DCS 350 and DHS 1100 Chambers 8.6.2.2 Optimizing Two Theta u When using a 1D detector, use a single strip. When using a 0D detector, use a 0.1 mm detector slit. 1. With Theta positioned at the peak position measured previously, scan Two Theta. 2.

  • Page 89: Optimizing Psi

    Installation and Operation of the DCS 350 and DHS 1100 Chambers 8.6.2.3 Optimizing Psi: u When using a 1D detector, use a single strip. When using a 0D detector, use a 0.1 mm detector slit. 1. With Theta and Two Theta positioned at the peak positions measured previously, scan Psi.

  • Page 90: Creating A Temperature Dependent Measurement Using The Wizard

    Installation and Operation of the DCS 350 and DHS 1100 Chambers 8.6.3 Creating a Temperature Dependent Measurement Using the WIZARD u In COMMANDER, make sure that all drives are at the aligned position for the desired reflection. 1. Click COMMANDER | Transmit Drive Positions. Figure 8.17: Transmit drive positions from COMMANDER to WIZARD 2.

  • Page 91: Figure 8.19: Selecting The Aligned Sample Reflection

    Installation and Operation of the DCS 350 and DHS 1100 Chambers 4. In the Alignment section, choose the aligned Bragg reflection. The positions to be aligned must be set to Required. Figure 8.19: Selecting the aligned sample reflection 5. Import the aligned motor positions from COMMANDER by pressing the Import from COMMANDER button.

  • Page 92: Figure 8.21: Defining A Sequence Of Measurements

    Installation and Operation of the DCS 350 and DHS 1100 Chambers Figure 8.21: Defining a sequence of measurements 8. In the Sequence details list in the top right section of the screen, you can now define motors that have to be aligned at each temperature. This can be done by setting their entry in the Alignment column to Required.

  • Page 93: Figure 8.22: Setting The Drives For Alignment For The Each Temperature

    Installation and Operation of the DCS 350 and DHS 1100 Chambers Figure 8.22: Setting the drives for alignment for the each temperature 9. When the scan is set up, save it as a .bsml file. 10.In the START JOBS plug in of DIFFRAC.MEASUREMENT CENTER, load the job by selecting the .bsml file in the Experiment Name column.

  • Page 94: Figure 8.23: Create A Job Using The Measurealign.cs Script

    Installation and Operation of the DCS 350 and DHS 1100 Chambers Figure 8.23: Create a job using the MeasureAlign.cs script 12.The job can now be run by pressing Start Jobs in the bottom right corner of the screen. Note: The Z-Position will only be updated if a new temperature outside the temperature detection window (± 1 K for most chambers) is set.

  • Page 95: Installation And Operation Of The Bts 150 And Bts 500 Chambers

    Introduction The Benchtop Heating Stages BTS 150 and BTS 500 are the smallest XRD non-ambient stages available from Anton Paar and are designed for use in small spaces and ease-of- use. The BTS 500 uses a resistance heater to operate in the temperature range between room temperature and 500 °C.

  • Page 96: Figure 9.1: Fixing Screws For The Bts 150/500 Adapter

    Installation and Operation of the BTS 150 and BTS 500 Chambers Figure 9.1: Fixing screws for the BTS 150/500 adapter 5. Attach the chamber to the mount by inserting the micrometer screws in the back into the designated holes in the mount. 6.

  • Page 97: Usb Connection Of The Bts 150/500 To The Cpu1 Board

    Installation and Operation of the BTS 150 and BTS 500 Chambers USB Connection of the BTS 150/500 to the CPU1 Board As the BTS series chambers do not have external controllers, the only thing that has to be done is to connect the USB cable to the USB port in the CPU1 board of the diffractometer housing.

  • Page 98: Configuring The Chamber In Diffrac.measurement Center

    Configuring the Chamber in DIFFRAC.MEASUREMENT CENTER Normally, Anton Paar stages come preinstalled with a new system or will be installed by a Bruker technician upon purchase. They should therefore be ready to use. If this is not the case, or for some reason the chamber needs to be reinstalled in DIFFRAC.MEASURE- MENT CENTER, we refer to paragraph Configuring a Chamber in DIFFRAC.MEASURE-...

  • Page 99: 10 Appendix / Service Details

    Vacuum Equipment 10.1.1 Programming of the Edwards High Vacuum Stage The programming was done at Bruker already. If necessary use the following procedure to program Edwards TIC controller, S/W issue: D39700640R. All settings will be reset by this procedure! Resetting the TIC to factory defaults: 1.

  • Page 100: Configuring A Chamber In Diffrac.measurement Center

    10.2.1 HTK-series, TTK 600, XRK 900, and HPC 900 Chambers The following procedure is suitable for the Anton Paar chambers HTK 2000N, HTK 16N, HTK 1200N, TTK 600, XRK 900 and HPC 900. For this example, the configuring of an HTK 1200N chamber is described.

  • Page 101: Figure 10.1: Import Template From File

    Appendix / Service Details 1. Switch on the Anton Paar controller and wait until the booting process is finished. Follow the instructions on the controller. 2. Launch the DIFFRAC.MEASUREMENT CENTER [4] program. 3. Switch to the CONFIGURATION plugin. 4. Open Device | Goniometer | Center and insert a template by pressing the right mouse button and selecting Import Template (figure below).

  • Page 102: Figure 10.2: Select Template

    Appendix / Service Details Figure 10.2: Select template 6. Press the Open button 7. Select entries by checking the boxes Figure 10.3: Import sections DOC-M88-EXX268_V1_12.2016...

  • Page 103: Figure 10.4: Section For Htk1200N In Goniometer/Center/Paar_Z_Htk1200

    Appendix / Service Details ð In Goniometer | Center | PAAR_Z_HTK1200 sections for the Sample stage (next 2 figures) are inserted: Figure 10.4: Section for HTK1200N in Goniometer/Center/PAAR_Z_HTK1200 DOC-M88-EXX268_V1_12.2016...

  • Page 104: Figure 10.5: Section Htk1200N In Goniometer/Center/Paar_Z_Htk1200/Htk1200

    Appendix / Service Details Figure 10.5: Section HTK1200N in Goniometer/Center/PAAR_Z_HTK1200/HTK1200 1. Check the Automatic Movement box if you want to corect height automatically with temperature (see chapter Using Automated Height Correction [} 44]). ´ In Configuration | Configuration Tree | Non Ambient the controller (here TCU1000) is inserted (next 2 pictures): Figure 10.6: Section for NonAmbient Controller DOC-M88-EXX268_V1_12.2016...

  • Page 105: Figure 10.7: Subsection Tcu1000_Controller For Nonambient Controller

    Appendix / Service Details Figure 10.7: Subsection TCU1000_Controller for NonAmbient Controller 2. Checking the box for Unlimited Ramping ignores the Max. Heating Rate, (shown in the figure above), in mode Set Temperature. If unchecked, Max. Heating Rate, here 60, is used in mode Set Temperature, shown in the next figure. DOC-M88-EXX268_V1_12.2016...

  • Page 106: Figure 10.8: Setting A New Temperature And Heating Rate With Commander

    Appendix / Service Details Figure 10.8: Setting a new temperature and heating rate with COMMANDER 3. For SerialConnector you have 4 possibilities to connect the RS232 communication line. Standard is SerialLine/Power X1_RS232_I, see figure below: Figure 10.9: Selecting SerialLine/Power X1_RS232_I/-II for SerialConnector DOC-M88-EXX268_V1_12.2016...

  • Page 107: Chc Plus

    Do not change the connectors A25D25 and A25D26 The following procedure is suitable for the Anton Paar chambers. 1. Switch on the Anton Paar controller, the MHG controller, and the Julabo water bath and wait until the booting process is finished. Follow the instructions on the controller.

  • Page 108: Figure 10.11: Import Section Stage_Paar_Chcplus_Ln2Cooling.bfscn

    Appendix / Service Details Figure 10.11: Import Section Stage_PAAR_CHCplus_LN2Cooling.bfscn 7. Select entries by checking the boxes Figure 10.12: Import sections DOC-M88-EXX268_V1_12.2016...

  • Page 109: Figure 10.13: Sections Created For Chc Plus

    Appendix / Service Details ´ In Goniometer | Center | CHC_Stage sections for the Sample stage (next figures) are inserted: Figure 10.13: Sections created for CHC plus DOC-M88-EXX268_V1_12.2016...

  • Page 110: Figure 10.14: Chc_Stage Chamber Temperature Details

    Appendix / Service Details Figure 10.14: CHC_Stage Chamber Temperature Details 8. All CHC plus templates are configured for cooling with LN2. If you plan to use compressed air cooling, the minimum temperature must be limited to ‑5 °C. This can be done by changing the Min. Temperature setting in Device | Goniometer | Center | CHC_Stage | SampleTemperature to ‑5 °C.

  • Page 111: Figure 10.15: Chc_Stage Sample Temperature Details

    Appendix / Service Details Figure 10.15: CHC_Stage Sample Temperature Details DOC-M88-EXX268_V1_12.2016...

  • Page 112: Figure 10.16: Tools Information For Actual Parameters Of Chc Plus

    Appendix / Service Details Figure 10.16: TOOLS information for actual parameters of CHC plus In Configuration | Configuration Tree | Non Ambient the controllers (here MHG, TCU110 and WaterCircuit controller) are inserted: DOC-M88-EXX268_V1_12.2016...

  • Page 113: Figure 10.17: Chc Plus Controller Details

    Appendix / Service Details Figure 10.17: CHC plus Controller Details Figure 10.18: CHC plus Chamber Temperature and adjacent water temperatures DOC-M88-EXX268_V1_12.2016...

  • Page 114: Figure 10.19: Chc Plus Mhg Controller Details

    Appendix / Service Details Figure 10.19: CHC plus MHG Controller Details Figure 10.20: CHC plus TCU110 Controller Details DOC-M88-EXX268_V1_12.2016...

  • Page 115: Figure 10.21: Chc Plus Watercircuit Controller Details

    Appendix / Service Details Figure 10.21: CHC plus WaterCircuit Controller Details The next figure shows the serial connections for MHG, TCU110 and Water Circuit (Julabo HE-4) on the Control Rack UIOBoard: DOC-M88-EXX268_V1_12.2016...

  • Page 116: Figure 10.22: Control Rack Uioboard Serial Connections For Mhg, Tcu110 And Water Circuit (Julabo He-4)

    Appendix / Service Details Figure 10.22: Control Rack UIOBoard serial connections for MHG, TCU110 and Water Circuit (Julabo HE-4) DOC-M88-EXX268_V1_12.2016...

  • Page 117: Chc Plus With Ccu100 And Corio Water Bath

    The following procedure is suitable for the Anton Paar chamber CHC plus with CCU 100 controller and Corio water bath. 1. Switch on the Anton Paar controller, the MHG controller and the Julabo water bath. Wait until the booting process is finished. Follow the instructions on the controller.

  • Page 118: Figure 10.23: Import The Chcplus Template In Measurement Center

    Appendix / Service Details Figure 10.23: Import the CHCplus template in Measurement Center Figure 10.24: Import section for CHC plus DOC-M88-EXX268_V1_12.2016...

  • Page 119: Figure 10.25: Sections Created For Chc Plus

    Appendix / Service Details 1. Confirming creates CHC_Stage und three substages under Center: Figure 10.25: Sections created for CHC plus Figure 10.26: CHC_Stage Chamber Temperature Details DOC-M88-EXX268_V1_12.2016...

  • Page 120: Figure 10.27: Chc_Stage Humidity Details

    Appendix / Service Details 2. All CHC plus templates are configured for cooling with LN2. If you plan to use compressed air cooling, the minimum temperature must be limited to ‑5 °C. This can be done by changing the Min. Temperature setting in Device | Goniometer | Center | CHC_Stage | SampleTemperature (Figure 10.28) to ‑5 °C.

  • Page 121: Figure 10.28: Chc_Stage Sample Temperature Details

    Appendix / Service Details Figure 10.28: CHC_Stage Sample Temperature Details Figure 10.29: CHC plus CPU Activation for USB Connection DOC-M88-EXX268_V1_12.2016...

  • Page 122: Figure 10.30: Chc Plus Controller Details

    Appendix / Service Details Figure 10.30: CHC plus Controller Details Figure 10.31: CHC plus Chamber Temperature and adjacent water temperatures DOC-M88-EXX268_V1_12.2016...

  • Page 123: Figure 10.32: Chc Plus Mhg Controller Details

    Appendix / Service Details Figure 10.32: CHC plus MHG Controller Details Figure 10.33: CHC plus CCU100 Controller Details DOC-M88-EXX268_V1_12.2016...

  • Page 124: Figure 10.34: Chc Plus Corio Watercircuit Controller Details

    Appendix / Service Details Figure 10.34: CHC plus Corio WaterCircuit Controller Details Figure 10.35: Control Rack UIOBoard serial connections for MHG and CCU100 controller DOC-M88-EXX268_V1_12.2016...

  • Page 125: Figure 10.36: Control Rack Cpuboard Usb Connections For Corio Water Circuit (Julabo)

    Appendix / Service Details Figure 10.36: Control Rack CPUBoard USB connections for Corio Water Circuit (Julabo) Figure 10.37: TOOLS information for actual parameters of CHC plus DOC-M88-EXX268_V1_12.2016...

  • Page 126: Dcs 350 And Dhs 1100

    Appendix / Service Details 10.2.3 DCS 350 and DHS 1100 CAUTION Risk of severe burns when touching the PEEK Dome u Do not touch the PEEK Dome. u Do not touch the PEEK Dome because it breaks very easy under vacuum. For configuring the DCS 350 and DHS 1100 stages, a slightly different procedure from the one described in paragraph HTK-series, TTK 600, XRK 900, and HPC 900 Chambers...

  • Page 127: Figure 10.39: Selecting Serialline/Power X1_Rs232_1/-2 For Serialconnector

    Appendix / Service Details Don’t forget to set the RS232 com port where you have connected the temperature controller to. • Standard is SerialLine/Power X1_RS232_1. Figure 10.39: Selecting SerialLine/Power X1_RS232_1/-2 for SerialConnector • If more chambers are configured, SerialLine/Power X1_RS232_2, SerialLine/Full X2_RS232_1 / -2.

  • Page 128: Figure 10.42: Selecting Serialline/Full Ttys0/1 For Serialconnector

    Appendix / Service Details Figure 10.42: Selecting SerialLine/Full TTYS0/1 for SerialConnector Physically, the serial lines are connected to X1 (via a Z-cable, A27D25) or X2 (via a Y-ca- ble, A27D26) of the Universal IO-Board (see figure below) or to the RS232 connectors on the slot CPU connected to the 9pin Sub-D on top of the slot CPU, see figure Connecting serial lines to the CPU board...

  • Page 129: Figure 10.43: Connecting Serial Lines To The Universal Io-Board

    Appendix / Service Details Figure 10.43: Connecting serial lines to the Universal IO-Board Temperature controller UIOB X1 / Z-cable RS232-I | UIOB X1 UIOB X2 / Y-cable RS485 | UIOB X1 (not used) Temperature controller RS232-II | UIOB X1 RS232-I | UIOB X2 Temperature controller RS232-II | UIOB X2 DOC-M88-EXX268_V1_12.2016...

  • Page 130: Figure 10.44: Connecting Serial Lines To The Cpu Board

    Appendix / Service Details Figure 10.44: Connecting serial lines to the CPU board TTYS1 Temperature controller TTYS0 Temperature controller DOC-M88-EXX268_V1_12.2016...

  • Page 131: Bts 150 And Bts 500

    Appendix / Service Details 10.2.4 BTS 150 and BTS 500 1. Plug in the BTS 150/500 power cable. Turn on the chamber by pressing the power button in the bottom right of the panel on the chamber. 2. Launch the DIFFRAC.MEASUREMENT CENTER [4] program. 3.

  • Page 132: References

    Appendix / Service Details Figure 10.46: BTS 500 connector configuration 10.3 References Manual Document number DIFFRAC.TOPAS 5 Users Manual DOC-M88-EXX065 DIFFRAC.EVA User Manual DOC-M88-EXX200 D8 ADVANCE_DISCOVER User Manual DOC-M88-EXX153 DIFFRAC.SUITE MEASUREMENT CENTER DOC-M88-EXX191 DIFFRAC.SUITE WIZARD User Manual DOC-M88-EXX194 DOC-M88-EXX268_V1_12.2016...

  • Page 133: Index

    Modbus.............  54, 65 Absorber ...........  35, 81 Motorized Z-stage ......  37, 41, 44, 107 Adjustment ........ 35, 36, 38, 42 Anton Paar Manual.... 36, 52, 59, 69, 75 Automatic correction.........  44, 85 Oil level.............  30, 33 Backing pump...........  27, 32 Bayonet ............
  • Page 134 Index Vacuum pump ..........  27, 56 Water flow ............ 69 Window foil .............  56 Z-drive ..........  57, 72, 80, 81 Z-position...... 44, 56, 70, 77, 81, 85 Z-scan.......... 41, 44, 81 DOC-M88-EXX268_V1_12.2016...
  • Page 135 DOC-M88-EXX268_V1_12.2016...
  • Page 136 ● Bruker Corporation info.baxs@bruker.com www.bruker.com Order No: DOC-M88-EXX268...

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