Bruker Anton Paar User Manual Download Page 24

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General Remarks

DOC-M88-EXX268_V1_12.2016

2.2.2.2

Temperature Calibration by Phase Transitions

Table 2.2: Some Samples with structural phase transitions useful for temperature calibration

Sample

Temperature

[°C]

Transition

Temperature

[°C]

Transition

Remark

TlNO

orh. → trig.

143

trig. → cub.

KNO

128

orh. → trig.

TlNO

143

trig. → cub.

CsNO

160

trig. → cub.

RbNO

164

trig. → cub.

219

cub. → tetr.

AgNO

165

orh. → trig.

RbNO

219

kub. → tetr.

291

tetr. → cub.

RbNO

291

tetr. → cub.

KClO

296

orh. → cub.

427

orh. → hex.

CsCl

476

SiO

(Qu.)

573

trig. → hex.

Scan range 25-27 °C

SO4

578

584

BaCO

812

Reacts with Pt, Ta, Mo

TlNO

orh. → trig.

143

trig. → cub.

Indium

157

melting

Reacts with Pt, Ta, Mo

Tin

232

melting

Reacts with Pt, Ta, Mo

Lead

327

melting

Reacts with Pt, Ta, Mo

Summary of Contents for Anton Paar

Page 1: ...Innovation with Integrity XRD Anton Paar Temperature Chambers for D8 ADVANCE D8 DISCOVER User Manual Original Instructions English ...

Page 2: ... in this manual are reviewed regularly and any necessary corrections are included in subsequent editions Suggestions for improvement are welcome 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 t...

Page 3: ...xpansion of MgO Periclase 21 2 2 2 1 1 Detailed Procedure for Temperature Determination 22 2 2 2 1 2 Shortened Procedure for Temperature Determination 23 2 2 2 2 Temperature Calibration by Phase Transitions 24 3 Vacuum Equipment 27 3 1 Installation of the Edwards High Vacuum Stage with TIC 27 3 1 1 Mounting of the Edwards High Vacuum Stage 27 3 1 2 Operation of the Edwards High Vacuum Stage 31 3 2...

Page 4: ...troduction 59 7 2 Mounting the Chamber to the Goniometer 59 7 3 Temperature Controllers and Water Circuit for CHC plus 60 7 3 1 Connecting the CCU Controller 65 7 3 2 Connecting the MHG for CHC plus 65 7 4 Configuring the Chamber in DIFFRAC MEASUREMENT CENTER 69 7 5 Operation 69 7 6 Alignment 72 8 Installation and Operation of the DCS 350 and DHS 1100 Chambers 73 8 1 Introduction 73 8 2 Mounting t...

Page 5: ...ion of the BTS 150 500 to the CPU1 Board 97 9 4 Configuring the Chamber in DIFFRAC MEASUREMENT CENTER 98 9 5 Operation and Alignment 98 10 Appendix Service Details 99 10 1 Vacuum Equipment 99 10 1 1 Programming of the Edwards High Vacuum Stage 99 10 2 Configuring a Chamber in DIFFRAC MEASUREMENT CENTER 100 10 2 1 HTK series TTK 600 XRK 900 and HPC 900 Chambers 100 10 2 2 CHC plus 107 10 2 2 1 CHC ...

Page 6: ...Contents 6 DOC M88 EXX268_V1_12 2016 ...

Page 7: ...on after rotation correction 39 Figure 4 3 Insert a deflection angle in CONFIGURATION for the temperature stage 40 Figure 4 4 Z scan over a wide range to roughly determine the right sample height 41 Figure 4 5 More accurate Z scan to determine the right sample height 42 Figure 4 6 Rocking curve at correct sample height 43 Figure 4 7 Inserting the temperature depending Z positions 46 Figure 5 1 Rem...

Page 8: ...rcuit 66 Figure 7 12 CPU board with USB connection of the Corio water bath 67 Figure 7 13 RS232 connections from UIOB to Julabo Heating Circulator and water connec tions 68 Figure 7 14 Water flow controller 69 Figure 7 15 Setting a new temperature and humidity with COMMANDER 71 Figure 7 16 Selecting the temperature mode in the COMMANDER 71 Figure 8 1 Fixing the DCS 350 onto the sample stage 74 Fig...

Page 9: ...lues from COMMANDER 91 Figure 8 21 Defining a sequence of measurements 92 Figure 8 22 Setting the drives for alignment for the each temperature 93 Figure 8 23 Create a job using the MeasureAlign cs script 94 Figure 9 1 Fixing screws for the BTS 150 500 adapter 96 Figure 9 2 USB connection of the BTS 150 500 to the CPU1 board in the USB1 slot 97 Figure 10 1 Import template from file 101 Figure 10 2...

Page 10: ...mplate in Measurement Center 118 Figure 10 24 Import section for CHC plus 118 Figure 10 25 Sections created for CHC plus 119 Figure 10 26 CHC_Stage Chamber Temperature Details 119 Figure 10 27 CHC_Stage Humidity Details 120 Figure 10 28 CHC_Stage Sample Temperature Details 121 Figure 10 29 CHC plus CPU Activation for USB Connection 121 Figure 10 30 CHC plus Controller Details 122 Figure 10 31 CHC ...

Page 11: ...or 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 129 Figure 10 44 Connecting serial lines to the CPU board 130 Figure 10 45 Import Template button 131 Figure 10 46 BTS 500 connector configuration 132 ...

Page 12: ...List of Figures 12 DOC M88 EXX268_V1_12 2016 ...

Page 13: ...nual by the warn ing symbols and are marked as follows according to the level of danger DANGER DANGER indicates a hazardous situation which if not avoided will result in death or serious injury This is the consequence of not following the warning 1 This is the safety condition u This is the safety instruction WARNING WARNING indicates a hazardous situation which if not avoided could result in deat...

Page 14: ...on designed to ensure efficient and smooth operation 1 2 Qualified Personnel The temperature chambers may only be set up and operated in conjunction with this man ual and the manual of the supplier of the temperature chamber Only qualified personnel should be allowed to work on this equipment The primary installation maintenance and repair of the temperature chamber must be car ried out only by pe...

Page 15: ... specifications within this manual Any use which exceeds or differs from the intended use shall be considered improper use No claims of any kind for damage will be entertained if such claims result from improper use 1 4 Disclaimer and Liability We have checked the contents of this manual for agreement with the hardware Instru ment Control Software and software described Since deviations cannot be ...

Page 16: ...ng liq uid nitrogen use personnel protective equipment CAUTION Extremely cold surface due to liquid Nitrogen Risk of severe burns when touching the surfaces u Use isolating gloves closed shoes and protective glasses Some temperature chambers are equipped with radiation outlet windows made from beryl lium Do not touch the radiation outlet window Fumes or the dust from beryllium and its compounds ca...

Page 17: ... heating chamber windows of some systems u Do not cut machine or handle beryllium in any way u It must not escape into the environment u Disposal of beryllium must comply with all applicable national state and local regulations u Strictly obey the applicable national state and local safety regulations Above about 1400 C UV radiation can be emitted by the heater Outside the temperature chamber at h...

Page 18: ...s 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 or cold surfaces ...

Page 19: ... 4 mbar up to 100 bar are possible Special chambers for humidity and reactive gases are available Some features of direct heaters are The easiest way of heating a sample is achieved by direct heating The heating filament is a flat ribbon of Pt Ta W or Graphite with AlN crucible High temperatures are accessible The sample is distributed on the heater A direct contact is given which allows fastest h...

Page 20: ...he device In the low temperature range around ambient temperature and down to 263 C Si diodes are used as sensors for measurements From LN2 temperature 196 C to 450 C Pt100 resistors and Type K thermocouples are widely used the latter are useful up to 1150 C Above ambient temperatures up to 1600 C Type S thermocouples Pt Pt 10 Rh are standard The recommended highest temperature ends at 1450 C beca...

Page 21: ...F 45 0946 for temperatures above ambient tempera tures up to 1000 C At higher temperatures sintering cannot be excluded Above 1000 C sintering of MgO cannot be excluded Another possibility is to use substances with a structural phase transition at defined tem peratures or melting points of metals see Table Some Samples with structural phase tran sitions useful for temperature calibration 24 Beware...

Page 22: ... 2 2 2 1 1 Detailed Procedure for Temperature Determination Put a small amount of MgO on the heater or the sample holder Start a scan at 30 C from 30 C to 130 C in 2θ Use the program DIFFRAC TOPAS 1 for refining the lattice con stant a0 a0 4 2109 3 at 25 C Refine the parameters for lattice constant and height never together with the zero shift for 2θ If the chamber height was adjusted correctly yo...

Page 23: ...nd the lattice constant with a0 24 d422 The influence of sample movement on the peak position due to expansion is neglected for this high angle reflection Comparing this lattice constant with the literature value figure below gives the temperature This procedure is well suited to recheck the temperature if the temperature dependence was previously investigated by the detailed procedure Figure 2 1 ...

Page 24: ... orh trig 143 trig cub KNO3 128 orh trig TlNO3 143 trig cub CsNO3 160 trig cub RbNO3 164 trig cub 219 cub tetr AgNO3 165 orh trig RbNO3 219 kub tetr 291 tetr cub RbNO3 291 tetr cub KClO4 296 orh cub Ag2SO4 427 orh hex CsCl 476 SiO2 Qu 573 trig hex Scan range 25 27 C Li2SO4 578 K2SO4 584 BaCO3 812 Reacts with Pt Ta Mo TlNO3 79 orh trig 143 trig cub Indium 157 melting Reacts with Pt Ta Mo Tin 232 me...

Page 25: ... DOC M88 EXX268_V1_12 2016 25 Sample Temperature C Transition Temperature C Transition Remark Aluminum 660 melting Reacts with Pt Ta Mo Silver 962 melting Reacts with Pt Ta Mo Copper 1085 melting Reacts with Pt Ta Mo ...

Page 26: ...General Remarks 26 DOC M88 EXX268_V1_12 2016 ...

Page 27: ...the D8 enclosure and the second shows how to install the Edwards backing pump 3 1 Installation of the Edwards High Vacuum Stage with TIC 3 1 1 Mounting of the Edwards High Vacuum Stage Connecting the vacuum tubes and the components 1 Connect vacuum tubes and components see the next 3 pictures 2 Mount the Edwards turbomolecular pump to the flexible bellow 3 Mount the Edwards backing pump backing pu...

Page 28: ...Vacuum Equipment 28 DOC M88 EXX268_V1_12 2016 Figure 3 1 Mounting the Edwards turbomolecular pump to the flexible bellow Figure 3 2 Connecting the vacuum tube to the HTK 1200N chamber ...

Page 29: ... 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 It is important to connect the red cable to and the black cable to for proper operation of the vent valve The communication cable has to be connected between the TIC and the relays box For proper operation the termination plug is very important If not plugged you ...

Page 30: ...ds turbomolecular instrument controller TIC left side and Edwards relay box right side 1 Mains supply 6 Terminator plug 2 WRG 7 Connection to TIC 3 Vent valve 8 Mains supply 4 Turbo pump 9 Backing pump 5 Connection to relay box 2 Check the oil level for the backing pump ð The vacuum stage is ready ...

Page 31: ... temperature chamber Figure 3 5 Starting screen for the TIC Controller 1 Switch on the Turbo Instrument Controller TIC programming is expected to be done 2 Press Cycle twice when Turbo OFF Back OFF is chosen The TMP and Backing pump will start 3 Switch back to the starting screen by pressing the Menu button Watch the vacuum pressure Channel 1 must be connected to Multi Wide Range Gauge MRG or WRG ...

Page 32: ...temperature chamber can be opened The ventilation will be done automatically It takes some minutes until the TMP speed has fallen below 50 For further information see the Edwards manuals 3 2 Installation of the Edwards Backing Pump Some applications only require a vacuum of about 10 2 mbar Therefore a backing pump is sufficient Bruker AXS offers the Edwards backing pump with 12 m3 h might be small...

Page 33: ...onnecting the vacuum tube to the heating chamber in the previous chapter 2 Connect the cables Choose head 1 Figure 3 7 Display and backside of the vacuum indicating instrument 3 Switch on the Edwards AGD 4 Check the oil level for the pump The vacuum stage is ready 5 Start the system by closing the valve and switching on the rotary pump 6 Start the temperature X ray measurements if the vacuum shows...

Page 34: ...Vacuum Equipment 34 DOC M88 EXX268_V1_12 2016 ...

Page 35: ...ze 0 006 LYNXEYE detector 0D mode with one opened strip 0D detector with receiving slit 0 1 mm use appropriate absorbers If the maximum position is not 0 0 01 mount the standard stage and repeat the glass slit adjustments Most chambers are supplied with a special tool It creates a small slit used for proper alignment of the chamber Chambers without this tool can be aligned by performing a pro cedu...

Page 36: ...have received an alignment slit with your chamber mount it as described in the An ton Paar Manual Preparation u Before mounting make sure that the diffractometer is well aligned 1 Align the chamber height roughly by eye so that the slit is positioned within the path of the X ray beam 2 Make sure that the X ray beam hits the slit 3 Align the chamber optically with the θ zero line 4 Fix the adapter ...

Page 37: ...k 1 Open the ratemeter COMMANDER Commander drop down menu Ratemeter and open the shutter 2 Mark the count rate or save it by clicking the Save as reference button 3 Close the shutter move the chamber using the manual adjustment screw and check the count rate again 4 Repeat until the maximum intensity has been found NOTE If no intensity is found make sure that the chamber rotation is not too far of...

Page 38: ...her 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 Align the rotation of the chamber by rotating the body on the alignment stage 2 Rotate chamber clockwise if the maximum is at negative values and vice versa see figure above A clockwise rotation is necessary here ...

Page 39: ...e 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 Rotation alignment by introducing a software offset Instead of physically rotating the chamber body one can introduce a deflection angle for the chamber into the measuremen...

Page 40: ... within the range of 0 0 02 4 Repeat step Height check for a final height check 4 1 2 Alternative Procedure Without Alignment Slit This method is less exact compared to the first one but more universal if no alignment slit is available It is important that the diffractometer is well aligned i e tube theta and detec tor in line at 0 position For correcting the chamber rotation only the method for i...

Page 41: ...the detector 0D detector or use all strips of the LYNXEYE detector in 0D mode 3 Move θ and 2θ angles to zero Height check u If you have a motorized Z stage perform a scan of the Z motor 1 Make the scan wide enough to ensure that the intensity is constant with distance at both ends of the curve 2 Move the stage to the position of 50 intensity If the scan was too course to accurately determine this ...

Page 42: ...u do not have a motorized Z stage 1 Open the ratemeter COMMANDER Commander drop down menu Ratemeter and open the shutter 2 Move the sample fully out of the beam 3 Mark the count rate or save it by clicking the Save as reference button 4 Close the shutter move the chamber using the manual adjustment screw and check the count rate again 5 Repeat until the ratemeter shows 50 of the direct beam intens...

Page 43: ...ine 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 temperature stage see figure above 3 Save the configuration and activate it 4 Repeat point 1 and 2 and check if the deviation is within the range of 0 0 02 5 Repeat step Height check for a final he...

Page 44: ...the direct beam sufficiently attenuated 10 kcps The correct Z position is at the half maximum intensity You must wait for all parts to warm up before the Z position can be determined which may take several minutes Step by step procedure 1 Align the chamber height and rotation under ambient conditions as described in chapter Alternative Procedure Without Alignment Slit 40 2 Heat up the chamber wait...

Page 45: ... D8 DOC M88 EXX268_V1_12 2016 45 Temperature C Z Position mm 600 0 22 700 0 1714 800 0 1262 900 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 ...

Page 46: ...s 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 The sample height is linearly interpolated for intermediate temperatures 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 47: ...onents the fitting position varies The controllers are coming in table top housings and can be mounted into the D8 enclo sure Use the mounting set to fix the controller in the 19 rack Steps to be taken 1 Loosen the screws on both sides of the controller base and remove the covers Figure 5 1 Removing the covers for rack mounting 2 Fix the guide bars on both sides of the controller Figure 5 2 Fixing...

Page 48: ...the plastic end caps Now the bottom cover can be pulled off 5 Press the central pin into the housing and take off the foot 6 You can remove the central pins plastics through the vent holes 7 Don t forget to mount the protecting earth wire and mount the bottom cover again Figure 5 3 Removing the supporting feet for rack mount ð The controller is now ready for mounting into the cabinet on supporting...

Page 49: ...mospheres HTK16N High temperature chamber using a strip heater to reach temperatures up to 1600 C in various atmospheres HTK 2000N High temperature chamber using a strip heater to reach temperatures up to 2300 C in vacuum or up to 1600 C in various atmospheres TTK 600 Low and high temperature chamber capable of reaching temperatures between 190 C and 600 C in vacuum or room temperature and 450 C i...

Page 50: ...e follow ing paragraph Figure 6 1 HTK 1200N mounted on a goniometer u It is assumed that the diffractometer is aligned before mounting the chamber 1 Set detector and source to a large 2θ to prevent them from restricting installation 2 Switch off mains supply 3 Feed all necessary cables and cooling water supply through the labyrinth for connecting them to the temperature chamber from the front of t...

Page 51: ...M88 EXX268_V1_12 2016 51 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 Fix the chamber mount using the three screw holes Figure 6 3 Fixing screws for the TTK 600 adapter ...

Page 52: ...com pressed air cooling vacuum gas and or liquid nitrogen cooling we refer to the Anton Paar Manual supplied with the chamber Figure 6 4 HTK 1200N mounted on a goniometer The turbomolecular pump is connected by a flexible bellow to the front of the chamber The backing pump is standing outside the enclosure and is connected by two 1 m flexible bellows DN10KF to the turbomolecular pump Alternatively...

Page 53: ...oller and the new CCU series Both versions can be mounted into the D8 cabinet in the same way Steps for doing this are given in chapter Mounting the Tem perature Controller into the D8 Enclosure 47 The steps for the software integration of both controllers are the same Instructions for this are given in chapter HTK series TTK 600 XRK 900 and HPC 900 Chambers 100 Figure 6 5 TCU series controller wi...

Page 54: ...o X1 via a Z cable A27D25 or X2 via a Y ca ble A27D26 of the Universal IO Board see figure below It is presupposed that the dialogue protocol is set to bisync normally done by Anton Paar The modbus protocol which is used for e g iTOOLS the control program of Eu rotherm only allows a connection via DIFFRAC MEASUREMENT CENTER if configured NOT standard Changing this protocol can be done only by hand...

Page 55: ...hambers DOC M88 EXX268_V1_12 2016 55 Figure 6 8 Connecting serial lines to the Universal IO Board 1 1st TCU CCU 6 UIOB X1 Z cable 2 RS232 I UIOB X1 7 UIOB X2 Y cable 3 RS485 UIOB X1 not used 8 3rd TCU CCU 4 RS232 II UIOB X1 9 RS232 I UIOB X2 5 2nd TCU CCU 10 RS232 II UIOB X2 ...

Page 56: ... 6 5 Operation NOTICE Working with some heaters requires a shielding of the Kapton window by a Graphite foil or other precautions Follow the instructions of your heater manual Check the status of the window foil and exchange it if looks burned to avoid breaking under vacuum NOTICE Substantial damage of the heater T W and Graphite heaters require a high vacuum or oxygen free atmosphere u Start the ...

Page 57: ...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 5 Press Set and wait until the temperature is reached see figures below The example shows a heating chamber with Z drive It automatically corrects the chamber height as function of...

Page 58: ...Installation and Operation of the HTK Series TTK 600 XRK 900 and HPC 900 Chambers 58 DOC M88 EXX268_V1_12 2016 ...

Page 59: ...equires additional controllers and has more operation modes which will be explained in this chapter Two controllers a TCU110C or CCU100 temperature controller and an MHG humidity controller and a water bath Julabo HE 4 or Corio need to be operated by DIFFRAC MEASUREMENT CENTER They are connected via RS232 or USB Corio ca bles to the universal IO board or CPU board Corio of the diffractometer For a...

Page 60: ...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 diffract...

Page 61: ...G for CHC plus 65 The steps for the software integration of the controllers are given in sec tion CHC plus 107 of the Appendix The Julabo water circuit must always stand outside the diffractometer enclosure close to the diffractometer on the back right side Figure 7 2 Front view of TCU110 Figure 7 3 Front view of a CCU100 Controller Figure 7 4 Front view of MHG controller ...

Page 62: ... for connecting the MHG controller to the mains board plugs X101 The Julabo HE 4 or Corio CD 201F heating circulator requires 230 V 100 V or 110 V Cooling water ca 4 l not destilled water for Julabo inner circle supply External cooling water ca 1 l min for Julabo HE 4 heating circulator Compressed air dry oil free ca 6 bar 120 l min for sample cooling or LN2 for cooling Transport gas N2 dry air He...

Page 63: ...Installation and Operation of the CHC plus Humidity Chamber DOC M88 EXX268_V1_12 2016 63 Figure 7 6 Power supply multiple socket Figure 7 7 MHG Power supply adapter ...

Page 64: ...HC plus Humidity Chamber 64 DOC M88 EXX268_V1_12 2016 Figure 7 8 Back side of Julabo Waterbath Corio CD 201F 1 USB Connection to CPU board 3 Water backflow from temperature controller 2 Connection to water cooler 4 Water out to CHC plus ...

Page 65: ...2 via a Y cable A27D26 of the Universal IO Board Figure 7 9 Back view of CCU100 The modbus protocol is used for communication 7 3 2 Connecting the MHG for CHC plus Figure 7 10 Back view of MHG controller The TCU 110C and MHG controllers require a null modem cable and the modbus proto col the Julabo HE 4 water circuit a special RS232 cable with more wires and the Julabo Corio water bath is connecte...

Page 66: ...ure 7 11 RS232 connection from UIOB to Temperature controller MHG controller and Julabo HE 4 water circuit 1 1st to TCU CCU 6 UIOB X1 Z cable 2 RS232 I UIOB X1 7 UIOB X2 Y cable 3 RS485 UIOB X1 not used 8 3rd to Julabo HE 4 4 RS232 II UIOB X1 9 RS232 I UIOB X2 5 2nd to MHG 10 RS232 II UIOB X2 ...

Page 67: ... 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 Figure 7 12 CPU board with USB connection of the Corio water bath ...

Page 68: ...g Circulator and water connections 1 to RS232 I UIOB X2 4 to relay box 2 Water bath inlet from CHC plus 5 Water bath outlet to CHC plus 3 Water bath outlet to drain 6 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 ...

Page 69: ...NTER 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 of the Appendix 7 5 Operation NOTICE Operation above 300 C requires vacuum Operation below am...

Page 70: ...l the booting process is finished Check for messages and follow the instructions 3 Switch on the diffractometer or reboot the diffractometer 4 If the chamber is configured the ICS connects automatically after some minutes to the controllers More details are described in the user s manual for your temperature controller Everything is now ready for operation 5 Activate the COMMANDER plugin in DIFFRA...

Page 71: ...us Humidity Chamber DOC M88 EXX268_V1_12 2016 71 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 ...

Page 72: ...eached before starting the scan Every time the Corio water bath was switched off leave it switched off for at least 20 seconds and then switch on again Without temperature dependent height correction peak positions might be wrong for temperature 25 C alignment temperature Meaning of the CHC plus modes Constant humidity keeps the rel humidity while changing the sample temperature This is a slow pro...

Page 73: ... to the Goniometer u It is assumed that the diffractometer is aligned before mounting the chamber 1 Set detector and source to a large 2θ to prevent them from restricting installation 2 Switch off mains supply 3 Feed all necessary cables and cooling water supply through the labyrinth for connecting them to the temperature chamber from the front of the goniometer 4 Screw the adapter plate delivered...

Page 74: ...CS 350 and DHS 1100 Chambers 74 DOC M88 EXX268_V1_12 2016 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 ...

Page 75: ...e 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 8 3 Temperature Controllers DC S350 and DHS 1100 The DCS 350 and DHS 1100 are controlled by TCU series controllers TCU 100 and TCU 200 respectively TCU 100 shown in Figure 8 3 with built in Eurotherm 2604 controller or by a CCU100 controller Figur...

Page 76: ... the D8 Enclosure 47 The steps for the software integration of both chambers are given in chapter DCS 350 and DHS 1100 126 of the Appendix Service Details 99 8 4 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 o...

Page 77: ...mple temperature Uncorrected sample height Z Position will lead to slightly wrong lattice parameters 8 5 1 Activating the Chamber in DA VINCI Contrary to chambers mounted in the diffractometer center domed stages are not recog nized by the OpCo system and have to be activated manually To do this 1 go to the DA VINCI plug in of the measurement software by clicking the DA VINCI tab in the line just ...

Page 78: ...field A drop down menu appears 3 Select the chamber you want to use 4 Click the field next to the drop down menu to activate the configuration Your sample stage field should now look like the right panel Magnification of the sample stage field with a DHS 1100 selected left Sample stage field after selecting DHS 1100 indicating with a green tick mark that everything is ok ...

Page 79: ...ing the Chamber To start using the chamber follow these steps 1 Open the water supply or compressed air for cooling 2 Switch on the controller and wait until the booting process is finished Check for messages and follow the instructions If problems are encountered check the Anton Paar Manual for your controller If the chamber is configured the ICS connects automatically to the controllers after so...

Page 80: ...amp rate but reaches the next temperature as fast as possible which risks uncontrolled heating and overshoot 5 Press Set and wait until the temperature is reached see figures below 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 Figure 8 8 Setting a new temperature and heating rate with COMMANDER Figure...

Page 81: ...n in chapter Adjustment of a Chamber on the D8 35 8 6 1 Aligning the Chamber for Automated Height Correction Dome chambers are generally mounted to a Eulerian Cradle XYZ or UMC stage These mounting bases include a Z drive which allows the chamber height to be automatically corrected for e g thermal expansion of the sample holder This requires a determination of chamber height for a number of tempe...

Page 82: ... the LYNXEYE detector in 0D mode 2 Move θ and 2θ angles to zero 3 Perform a scan of the Z motor Make the scan wide enough to ensure that the intensity is constant with distance at both ends of the curve Move the stage to the position of 50 intensity If the scan was too course to accurately determine this position next figure repeat the scan in a narrower range with a smaller step size second figur...

Page 83: ...on and Operation of the DCS 350 and DHS 1100 Chambers DOC M88 EXX268_V1_12 2016 83 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 ...

Page 84: ...ractometer there Then repeat point 4 and 5 until the sample height is ok 6 If the sample height is ok set theta to zero on the peak position using Reference And Offset Determination from the menu bar in COMMANDER Set theoretical position to 0 in the reference tab and click apply see figure above 7 Repeat point 5 and to check if the deviation is within the range of 0 0 02 8 Repeat point 4 for a fin...

Page 85: ...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 The sample height is linearly interpolated for intermediate temperatures ð Basic sample alignment in direct beam is finished Table 8 1 Z position as function of temperature for DHS 1100 in air Temperature C Z P...

Page 86: ... DCS 350 and DHS 1100 Chambers 86 DOC M88 EXX268_V1_12 2016 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 ...

Page 87: ...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 8 6 2 1 Optimizing Theta 1 Move the diffractometer to a known Bragg peak of your sample 2 Perform a rocking curve scan with open detector LYNXEYE or without detector slit 0D detector 3 Move theta to the peak...

Page 88: ...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 Move Two Theta to the peak position Figure 8 15 TwoTheta scan to align the Bragg angle ...

Page 89: ...ing 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 2 Move Psi to the peak position Figure 8 16 Psi scan to align the diffracting plane normal in the diffraction plane ...

Page 90: ...e 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 Create an HR XRD measurement for your sample Figure 8 18 Create an HR XRD measurement for your sample 3 Generate a sample definition for your sample as you would do for a normal HR XRD measurement ...

Page 91: ... 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 Figure 8 20 Import the centered values from COMMANDER 6 Define a measurement in the Method section 7 In the Sequences section define a temperature sequence by pressing the button Add new sequence ...

Page 92: ...nce 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 Normally a simple height correction should suffice but any motor alignment can be made ...

Page 93: ...n 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 Name the output file in the Result File Name column 11 Finally in the Script Name column select C ProgramData BrukerAXS Scripts MeasureAlign cs This is the script that will run the alignments during the measurement ...

Page 94: ...12 2016 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: ...her chambers in that they don t require an external controller This changes the way they are integrated into the diffractometer Changes with respect to the other chambers are given below For all other instructions we refer to the chapters Adjustment of a Chamber on the D8 35 and Installation and Operation of the HTK Se ries TTK 600 XRK 900 and HPC 900 Chambers 49 9 2 Mounting the Chamber to the Go...

Page 96: ...k into the designated holes in the mount 6 Feed the heater power cable the USB cable and the vacuum gas tubes optional through the labyrinth If necessary connect the vacuum tubes to a vacuum pump or to the desired gas source the chamber supports inert gases such as N2 and He as well as air The chamber takes 4 mm gas or vacuum tubing that can be plugged directly into the connectors at the top of th...

Page 97: ...tion 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 Figure 9 2 USB connection of the BTS 150 500 to the CPU1 board in the USB1 slot ...

Page 98: ...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 MENT CENTER 100 of the Appendix Service Details 99 9 5 Operation and Alignment Operation and alignment of the BTS series are done just as described in chapter Opera tion 56 an...

Page 99: ...e TIC to factory defaults 1 Press once Menu 2 Press 8 times Down Service Information 3 Press once Select 4 Press 9 times Down Reset TIC Default 5 Press once Select Reset Programming the TIC for automatic start and stop of the TMP and Backing pump Proceeding after resetting to factory defaults S W issue D39700640R 1 Press twice Down WRG New ID 2 Press once Select WRG and a pressure are indicated 3 ...

Page 100: ... 19 Press once Menu Turbo Off 20 Press Cycle twice for starting the system For further information on programming the TIC controller see the Edwards manuals See also 2 Operation of the Edwards High Vacuum Stage 31 10 2 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 ...

Page 101: ...ler 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 Figure 10 1 Import template from file 5 Choose Stage_PAAR_HTK1200_Motorized bfscn in C ProgramData Bruker AXS Instrument Configurations A25 D8_Advance Stages ...

Page 102: ...Appendix Service Details 102 DOC M88 EXX268_V1_12 2016 Figure 10 2 Select template 6 Press the Open button 7 Select entries by checking the boxes Figure 10 3 Import sections ...

Page 103: ...Service Details DOC M88 EXX268_V1_12 2016 103 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 ...

Page 104: ...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 ...

Page 105: ...ubsection 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 ...

Page 106: ...ting 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 ...

Page 107: ...troller the MHG controller and the Julabo water bath 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 5 Choose Stage_PAAR_CHCplus_LN2Cooling ...

Page 108: ...Appendix Service Details 108 DOC M88 EXX268_V1_12 2016 Figure 10 11 Import Section Stage_PAAR_CHCplus_LN2Cooling bfscn 7 Select entries by checking the boxes Figure 10 12 Import sections ...

Page 109: ...Appendix Service Details DOC M88 EXX268_V1_12 2016 109 In Goniometer Center CHC_Stage sections for the Sample stage next figures are inserted Figure 10 13 Sections created for CHC plus ...

Page 110: ...emperature 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: ...Appendix Service Details DOC M88 EXX268_V1_12 2016 111 Figure 10 15 CHC_Stage Sample Temperature Details ...

Page 112: ...tails 112 DOC M88 EXX268_V1_12 2016 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 ...

Page 113: ...Appendix Service Details DOC M88 EXX268_V1_12 2016 113 Figure 10 17 CHC plus Controller Details Figure 10 18 CHC plus Chamber Temperature and adjacent water temperatures ...

Page 114: ...Appendix Service Details 114 DOC M88 EXX268_V1_12 2016 Figure 10 19 CHC plus MHG Controller Details Figure 10 20 CHC plus TCU110 Controller Details ...

Page 115: ...ice Details DOC M88 EXX268_V1_12 2016 115 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 ...

Page 116: ...Appendix Service Details 116 DOC M88 EXX268_V1_12 2016 Figure 10 22 Control Rack UIOBoard serial connections for MHG TCU110 and Water Circuit Julabo HE 4 ...

Page 117: ... short instruction in its manual Press up and down at the same time for ca 5 seconds and set the communication to R ON 3 Switch on the diffractometer or reboot the diffractometer 4 Launch the DIFFRAC MEASUREMENT CENTER 4 program 5 Switch to the CONFIGURATION plugin 6 Open Device Goniometer Center and insert a template by pressing the right mouse button and selecting Import Template Figure 10 23 If...

Page 118: ...Appendix Service Details 118 DOC M88 EXX268_V1_12 2016 Figure 10 23 Import the CHCplus template in Measurement Center Figure 10 24 Import section for CHC plus ...

Page 119: ...dix Service Details DOC M88 EXX268_V1_12 2016 119 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 ...

Page 120: ...igured 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 Figure 10 27 CHC_Stage Humidity Details ...

Page 121: ...Appendix Service Details DOC M88 EXX268_V1_12 2016 121 Figure 10 28 CHC_Stage Sample Temperature Details Figure 10 29 CHC plus CPU Activation for USB Connection ...

Page 122: ...Appendix Service Details 122 DOC M88 EXX268_V1_12 2016 Figure 10 30 CHC plus Controller Details Figure 10 31 CHC plus Chamber Temperature and adjacent water temperatures ...

Page 123: ...Appendix Service Details DOC M88 EXX268_V1_12 2016 123 Figure 10 32 CHC plus MHG Controller Details Figure 10 33 CHC plus CCU100 Controller Details ...

Page 124: ...Appendix Service Details 124 DOC M88 EXX268_V1_12 2016 Figure 10 34 CHC plus Corio WaterCircuit Controller Details Figure 10 35 Control Rack UIOBoard serial connections for MHG and CCU100 controller ...

Page 125: ...Appendix Service Details DOC M88 EXX268_V1_12 2016 125 Figure 10 36 Control Rack CPUBoard USB connections for Corio Water Circuit Julabo Figure 10 37 TOOLS information for actual parameters of CHC plus ...

Page 126: ... 900 and HPC 900 Chambers 100 needs to be followed Figures 10 1 until 10 5 are still the same From there on take the following steps u As the dome stages are not mounted in the goniometer center but on sample stages they have to be activated as attachment on the mounted stage 1 To do this in Goniometer Center your mounted stage in the line AttachmentContainer column Connected to Component select D...

Page 127: ..._RS232_1 2 for SerialConnector If more chambers are configured SerialLine Power X1_RS232_2 SerialLine Full X2_RS232_1 2 Figure 10 40 Selecting SerialLine Full X2_RS232_1 2 for SerialConnector Direct connection to the slot CPU can be used figure Selecting SerialLine Full TTYS0 1 for SerialConnector 128 and figure Connecting serial lines to the Universal IO Board 129 Figure 10 41 Introducing the Boa...

Page 128: ... 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 130 ...

Page 129: ...onnecting serial lines to the Universal IO Board 1 1st Temperature controller 6 UIOB X1 Z cable 2 RS232 I UIOB X1 7 UIOB X2 Y cable 3 RS485 UIOB X1 not used 8 3rd Temperature controller 4 RS232 II UIOB X1 9 RS232 I UIOB X2 5 2nd Temperature controller 10 RS232 II UIOB X2 ...

Page 130: ...Appendix Service Details 130 DOC M88 EXX268_V1_12 2016 Figure 10 44 Connecting serial lines to the CPU board 1 TTYS1 Temperature controller 2 TTYS0 Temperature controller ...

Page 131: ...on the chamber 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 10 45 Import Template button 5 In the configuration tree select Device NonAmbient BTS500 and make sure the field under connected component is set to Device ControlRack CPUB...

Page 132: ...configuration 10 3 References Manual Document number 1 DIFFRAC TOPAS 5 Users Manual DOC M88 EXX065 2 DIFFRAC EVA User Manual DOC M88 EXX200 3 D8 ADVANCE_DISCOVER User Manual DOC M88 EXX153 4 DIFFRAC SUITE MEASUREMENT CENTER DOC M88 EXX191 5 DIFFRAC SUITE WIZARD User Manual DOC M88 EXX194 ...

Page 133: ...angle 40 43 H Humidity controller 59 60 I Inert gas 69 73 L LN2 20 59 62 107 117 120 M Modbus 54 65 Motorized Z stage 37 41 44 107 O Oil level 30 33 P Power cable 96 131 R Ramp rate 57 80 Rocking curve 37 40 81 83 87 RS232 55 59 65 106 126 128 129 S Sample height 41 46 56 70 77 81 84 Sample holder 20 22 35 44 50 81 95 Serial line 128 T Temperature calibration 21 24 Temperature controller 53 57 62 ...

Page 134: ...Index 134 DOC M88 EXX268_V1_12 2016 V Vacuum pump 27 56 W Water flow 69 Window foil 56 Z Z drive 57 72 80 81 Z position 44 56 70 77 81 85 Z scan 41 44 81 ...

Page 135: ...DOC M88 EXX268_V1_12 2016 135 ...

Page 136: ...Bruker Corporation info baxs bruker com www bruker com Order No DOC M88 EXX268 ...

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