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Optics

SmartLab: Automated Multipurpose X-ray Diffractometer

Receiving optics unit # 2

This unit attaches to before receiving slit box # 2. A parallel slit can be installed
in receiving optics unit # 2.

Receiving parallel slit adaptor (RPS adaptor)

This adaptor is used to install a parallel slit.
A parallel slit is installed so that the plates inside are mounted vertically
controlling axial divergence for the theta_d axis.

Receiving parallel slit adaptor

Attach the receiving parallel slit adaptor to the rail of the theta_d arm.

Secure it in place with the Allen wrench provided.

Summary of Contents for 2080A211

Page 1: ...Automated Multipurpose X ray Diffractometer Instruction Manual...

Page 2: ...ual has to be purchased for each product If there are any missing or incorrectly collated pages in the delivered instruction manual please contact the sales representative who you purchased the instru...

Page 3: ...anslate any part of this manual you must obtain our written approval before doing so for each specific case 4 In general unless special agreements are reached each product unit is provided with a copy...

Page 4: ...ademarks of Microsoft Corporation in the United States and or other countries Pentium is a registered trademark of Intel Corporation Other company names and product names are trademarks or registered...

Page 5: ...l software SmartLab Guidance 6 Two slit SAXS optics 7 In plane optics 2080B212 7 Names of Parts 9 Main unit 9 Goniometer 11 X ray tube 13 Theta_s arm 14 Theta_d arm 15 Detector mounting bracket 16 Sam...

Page 6: ...ceiving optical device adaptor ROD adaptor 49 2 bounce analyzer option 52 Receiving optics unit 2 54 Receiving parallel slit adaptor RPS adaptor 54 Receiving slit box 2 57 Standard receiving slit box...

Page 7: ...SAXS sample holder option 2680J111 93 Accessories 95 Examples of Sample Mounting 97 Powder samples 97 Bulk samples 97 Sample for transmission SAXS measurements 97 Wafer shaped samples 98 Measurements...

Page 8: ......

Page 9: ...lm analysis SmartLab system Para focusing method Parallel beam SAXS Micro area 4 bounce monochromator 2 bounce analyzer 2 bounce analyzer Ni filter Diffracted beam monochromator PSA PSA Soller slit So...

Page 10: ...se wavelengths are quite close Although this does not pose serious problems for ordinary measurement of powder samples for phase identification ID analysis optimal results can be achieved by using onl...

Page 11: ...y developed connector allows easy changing of attachments X ray generator Even with a horizontal sample mount goniometer with a moving x ray source the product can incorporate a state of the art high...

Page 12: ...ors and 2 bounce analyzers have built in adjustment mechanisms that enable automatic adjustment via control software hereinafter referred to as SmartLab Guidance Crystal adjustment positions are prese...

Page 13: ...with variable slit and length limiting slit Receiving optics system The following mechanisms enable selection of a broad range of resolution characteristics for specific purposes A parallel slit analy...

Page 14: ...guides the user through required measurement procedures and condition setting processes in addition to providing conventional SmartLab control functions Optical device configurations optics alignment...

Page 15: ...attachment enables measurements of in plane diffraction by maintaining grazing incidence conditions during sample rotation This allows the measurement of diffraction from lattice planes perpendicular...

Page 16: ...at appear as a background in the K filter method is proportional to the square of the tube voltage and is also proportional to the tube current This means that an optimum tube voltage value exists for...

Page 17: ...eft 2080A211 2080B211 2080A411 2080B411 Right 2080B212 1 Rotary pump Pump for maintaining the vacuum in the x ray generator 2080A211 2080A411 2 Control PC PC used to control SmartLab Main unit Front v...

Page 18: ...onnector External power supply connects here 7 Connector for control PC The LAN cables used to control SmartLab connect here 8 Connectors for rotary pump The power supply for the rotary pump connects...

Page 19: ...tics Optical device for achieving desired incident x ray conditions 4 Theta_d arm Arm for controlling the x ray detector angle 5 Receiving optics Optical device for achieving desired x ray receiving c...

Page 20: ...deg Ge 220 x2 etc Receiving optical device adaptor analyzer PSA Soller slit 5 0 deg In plane PSA 0 5 deg etc Receiving parallel slit adaptor Soller slit in plane PSA Scintillation counter D teX ultra...

Page 21: ...g source 3 Shutter Controls x ray emissions 4 Filament replacement window Window for replacing the filament 5 Ion gauge Measures the vacuum in the x ray generator 6 Turbo molecular pump TMP Vacuates t...

Page 22: ...ta_s arm 1 Incident connector box The control cable of the optical device connects here 2 Cross beam optics CBO unit Optics unit for switching optics 3 Incident optics unit Soller units monochromators...

Page 23: ...for the optical devices connect here 2 Receiving slit box 1 Variable slit on receiving side 3 Receiving optics unit 1 Receiving optical devices analyzer are installed here 4 Receiving optics unit 2 So...

Page 24: ...t 1 Base Used to secure the detector in place 2 Detector adaptor Used to attach the detector Sample stage and attachments Sample stage and attachments 1 Sample stage Sample attachment unit 2 Attachmen...

Page 25: ...such as RSM pole figure etc Performs simple data processing Analysis software options PDXL 9240J702 9240J703 9240J710 Performs the additional functions such as phase ID analysis quantitative analysis...

Page 26: ...060 Si 2 42 2 6 44 60 6 93 3 189 1 48 0 157 0 102 0 050 SiO2 2 65 2 3 71 34 5 53 1 108 2 34 0 252 0 164 0 080 CaCO3 2 71 2 8 02 70 9 107 205 1 06 0 120 0 079 0 041 Fe2O3 5 26 2 27 3 216 42 7 86 5 0 16...

Page 27: ...RATE lamp blinks while SmartLab is starting up and when an error occurs For more information see Appendix Using the OPERATE Lamp Starting SmartLab Guidance 1 Click the Start button Select All Programs...

Page 28: ...mp make sure the cooling water is flowing properly If the cooling water is not flowing or the amount pressure of water are incorrect an alarm will be issued and remain active for three minutes after t...

Page 29: ...Halting the cooling water supply in less than three minutes may result in damage to SmartLab For more information on the shutdown procedure refer to Section 2 6 of the CBO Maintenance Package Measure...

Page 30: ...to exit SmartLab Guidance Turning off SmartLab If SmartLab is unused for a while New Year Holidays etc turn off SmartLab according to the following procedure 1 Check the SmartLab status e g confirm t...

Page 31: ...nd close the door by the following procedure Opening the door Under normal conditions the door is locked and cannot be opened 1 Press the DOOR LOCK button on the door 2 The shutter will close and the...

Page 32: ...cy stop switch EMO Press this switch in the event of an emergency to cut off the power supply to the main unit To cancel the emergency stop status turn the button clockwise After confirming safety pre...

Page 33: ...can also be converted into a narrow beam for small angle scattering measurements or a small beam for micro area measurements Fine adjustments of the multilayer mirror can be performed from SmartLab Gu...

Page 34: ...X ray Diffractometer 1 Attach the CBO unit to the shutter Press the CBO unit against the surface in the back and secure the unit in place with the Allen wrench provided 2 Insert the cable into the CB...

Page 35: ...CBO unit for Cu target SmartLab Automated Multipurpose X ray Diffractometer 27 3 Insert a selection slit into the slit box of the CBO unit...

Page 36: ...the CBO Cu and CBO Cu Co units CBO Cu CBO Cu Co PB For convergent beam included in the CBO E unit CBO E CB For micro area measurements option 2431C302 CBO Cu CBO Cu Co PB03 For small angle scattering...

Page 37: ...0 3 mm PB03 Parallel beam 2431C301 0 1 mm PB01 Point source x rays 1 2431C202 0 3 mm BB03 Point source x rays 1 2431C201 0 1 mm BB01 1 Switchable to the point source x rays only using the sealed tube...

Page 38: ...optical device from three types parallel slit 2 bounce monochromator and 4 bounce monochromator Incident parallel slit adaptor IPS adaptor This adaptor is used to install a parallel slit Incident par...

Page 39: ...ptics unit SmartLab Automated Multipurpose X ray Diffractometer 31 2 Connect the cable to the MONO ADPT connector on the incident connector box 3 Install the parallel slit on the adaptor and secure it...

Page 40: ...ller_Slit_open Soller slit 5 Soller_Slit_5 0 deg Soller slit option 2680D114 2 5 Soller_Slit_2 5 deg In plane PSC Parallel Slit Collimator option 2680D113 1 0 In plane_PSC_1 0 deg In plane PSC option...

Page 41: ...d x ray beam using a 2 bounce channel cut crystal Fine alignment of the channel cut crystal are performed from SmartLab Guidance A dedicated parallel slit can be installed after the channel cut crysta...

Page 42: ...mated Multipurpose X ray Diffractometer 2 Connect the cable to the MONO ADPT connector on the incident connector box 3 Install a parallel slit on the 2 bounce monochromator Secure it in place with the...

Page 43: ...type of installed crystal can be identified from SmartLab Guidance Table Parallel slits for 2 bounce monochromator Type Divergence Abbreviation Illustration Open provided with the unit None Soller_sl...

Page 44: ...ochromatized x ray beam using two 2 bounce channel cut crystals Fine alignment of the channel cut crystals can be performed from SmartLab Guidance 4 bounce monochromator 1 Attach the 4 bounce monochro...

Page 45: ...er 37 2 Connect the cable to the MONO ADPT connector on the incident connector box Table 4 bounce monochromators Crystal Diffraction plane Abbreviation Illustration Ge option 2680B211 220 Ge 220 x4 Ge...

Page 46: ...longitudinal direction onto the sample The optical device is used for the measurements of micro amount of a sample and of micro area Fine alignment of the CBO f unit is performed from SmartLab Guidan...

Page 47: ...rd incident optics unit SmartLab Automated Multipurpose X ray Diffractometer 39 2 Connect the cable to the MONO ADPT connector on the incident connector box The type of installed crystal can be identi...

Page 48: ...trol the beam divergence angle for the para focusing method or the beam width for the parallel beam method For small angle scattering measurements this slit guards against parasitic scattering A lengt...

Page 49: ...box SmartLab Automated Multipurpose X ray Diffractometer 41 2 Connect the cable to the SLIT connector on the incident connector box 3 Insert a length limiting slit to control beam length along the lon...

Page 50: ...type of inserted length limiting slit can be identified from SmartLab Guidance Collimator holder option Some types of pinhole collimators can be installed for micro area measurements K filter for Cu c...

Page 51: ...se X ray Diffractometer 43 Table Incident filter option Name Illustration Absorber case 2431H101 K filter for Cu 2431H201 K filter for various wavelength can be supplied Please contact the sales repre...

Page 52: ...Automated Multipurpose X ray Diffractometer 1 Install the collimator holder to the Zs axis and secure it in place with the Allen wrench provided 2 Connect the cable to the SLIT connector on the incid...

Page 53: ...0 05 mm 2431E101 0 05 CAUTION Do not use the pinhole collimator option with the XY 4 phi attachment When using the pinhole collimator with the XY 4 phi attachment the end of the pinhole collimator co...

Page 54: ...slit width to reduce the level of background scatter from the sample For parallel beam optics it functions as the first slit in a double slit receiving system The slit width can be controlled from Sm...

Page 55: ...ox 3 A K filter may be inserted Check whether a K filter is inserted from SmartLab Guidance K filter Ni foil The K filter reduces the K characteristic x rays by approximately 90 while only reducing th...

Page 56: ...Optics 48 SmartLab Automated Multipurpose X ray Diffractometer 4 The installation position can be read from the scale on the theta_d arm...

Page 57: ...ing optics unit 1 Receiving optical device adaptor ROD adaptor This adaptor is used to install a parallel slit analyzer PSA A parallel slit analyzer is installed so that the plates inside are mounted...

Page 58: ...Automated Multipurpose X ray Diffractometer 2 Connect the cable to the ADPT1 connector on the receiving connector box 3 Attach a parallel slit analyzer to the adaptor Secure it in place with the Alle...

Page 59: ...11 90 mm PSA_0 114 deg Open 90 mm PSA_open The standard configuration of SmartLab cannot incorporate either the PSA 0 114 deg or PSA open 90 mm in conjunction with a receiving parallel slit In order t...

Page 60: ...ution on the 2 theta axis by only allowing diffracted x rays that satisfy the diffraction condition for the analyzer crystal to enter the detector Fine alignment of the channel cut crystal can be perf...

Page 61: ...ect the cable to the ADPT1 connector on the receiving connector box Table Crystal types Crystal Diffraction plane Abbreviation Illustration Ge option 2680C111 220 Ge 220 x2 Ge option 2680C112 400 Ge 4...

Page 62: ...cs unit 2 Receiving parallel slit adaptor RPS adaptor This adaptor is used to install a parallel slit A parallel slit is installed so that the plates inside are mounted vertically controlling axial di...

Page 63: ...2 SmartLab Automated Multipurpose X ray Diffractometer 55 2 Connect the cable to the ADPT2 connector on the receiving connector box 3 Attach a parallel slit to the adaptor Secure it in place with the...

Page 64: ...er_slit_5 0 deg Soller slit option 2680F114 2 5 Soller_slit_2 5 deg In plane PSA option 2680F113 1 0 In plane_PSA_1 0 deg In plane PSA use of PSA 0 5 deg 0 5 In plane_PSA_0 5 deg In plane PSA use of P...

Page 65: ...ains the variable receiving slit and controls measurement resolution in the para focusing and double slit receiving configurations If a double slit receiving system is used it will function as the sec...

Page 66: ...58 SmartLab Automated Multipurpose X ray Diffractometer When using the para focusing method set the installation position to 300 mm 2 Connect the cable to the SLIT2 connector on the receiving connect...

Page 67: ...types of attenuators on a rotating disc Attenuators for optics alignment are also built in The type of attenuator can be switched from SmartLab Guidance Attenuators can be switched automatically for v...

Page 68: ...Connect the cable to the ATT connector on the receiving connector box The attenuator types used during actual measurements are as follows Open 1 70 1 1000 1 10000 The attenuator types used during ali...

Page 69: ...ing onto the theta_d arm It achieves the ultrahigh resolution of the X ray diffraction beam from a sample The positions of the analyzer crystals and detector can be aligned from SmartLab Guidance CALS...

Page 70: ...rtLab Automated Multipurpose X ray Diffractometer 3 Secure it in place with the Allen wrench provided 4 Connect the ADPT1 ADPT2 and SLIT2 cable to the ADPT1 ADPT2 and SLIT2 connector on the receiving...

Page 71: ...b Automated Multipurpose X ray Diffractometer 63 Receiving parallel slit Install the parallel slit in a manner such that the stacking direction of the foils should be the same as the direction of the...

Page 72: ...on Soller slit 5 0 Soller slit 5 0deg Soller slit option 2 5 Soller slit 2 5deg In plane PSA option 1 0 In plane PSA 1 0deg In plane PSA use of PSA 0 5deg 0 5 In plane PSA 0 5deg In plane PSA use of P...

Page 73: ...condition the X ray beams Table Beam conditioner Type Abbreviation Use Illustration Knife edge KE Cuts off the scattering X rays from the sample in data measurements reference Receiving slit ARS Used...

Page 74: ...ay Diffractometer Dtector D teX Ultra Detects X rays diffracted from CALSA D teX Ultra 1 Connect the power cable and LAN cable to D teX Ultra 2 Attach D teX Ultra to the detector adaptor of CALSA Secu...

Page 75: ...Multipurpose X ray Diffractometer 67 Detector Detector adaptor Used to attach the detector Detector adaptor 1 Attach the detector adaptor to the rail of the theta_d arm Secure it in place with the All...

Page 76: ...Detector 68 SmartLab Automated Multipurpose X ray Diffractometer 2 Connect the cable to the COUNTER connector on the receiving connector box...

Page 77: ...tector adaptor It detects x rays received by the receiving optics Check whether the scintillation counter is installed from SmartLab Guidance Scintillation counter 1 When detecting x rays from the rec...

Page 78: ...rtLab Automated Multipurpose X ray Diffractometer 2 Attach the base to the detector adaptor Secure it in place with the Allen wrench provided 3 The installation position can be read from the scale on...

Page 79: ...ochromating crystal from Bent para focusing geometry to Flat parallel beam geometry by rotating the dial on the top of the monochromator housing DBM diffracted beam monochromator unit for Cu Diffracte...

Page 80: ...position can be read from the scale on the theta_d arm When using the monochromator in Bent mode with para focusing optics the unit must be installed at a specific position for a specific target given...

Page 81: ...eter 73 4 Insert the monochromator slit RSm into the unit The presence absence of the slit can be confirmed from SmartLab Guidance Use the RSm only when using the monochromator in Bent mode for the pa...

Page 82: ...Ultra is installed from SmartLab Guidance D teX Ultra 1 When detecting x rays from the receiving optics directly in absence of the diffracted beam monochromator install D teX Ultra to the base with th...

Page 83: ...in place with the Allen wrench provided When the measurement is made in para focusing optics install the detector adaptor at position 351 mm 4 Connect the power cable and communication cable to the c...

Page 84: ...Ultra option 2726P101 This unit is used to monochromatize the diffracted beam such that only K x rays are detected DBM diffracted beam monochromator unit for Cu for D teX Ultra 1 Install D teX Ultra o...

Page 85: ...ceiving parallel slit adaptor see Receiving parallel slit adaptor RPS adaptor standard receiving slit box 2 see Standard receiving slit box 2 and standard attenuator see Standard attenuator 3 Install...

Page 86: ...742A101 PILATUS is a low noise high sensitivity semi conductor hybrid 2D detector Attach PILATUS to the PILATUS holder and install the PILATUS holder 2431J101 to SmartLab PILATUS can be placed either...

Page 87: ...ight alignment unit To install a sample stage join the stage with the rail of the sample height alignment unit as shown in the following figure and slide it from top down Make sure that the stage is p...

Page 88: ...an be used in combination with attachments Standard sample stage sample stage option 2430B101 This can be used in combination with attachments The rotational axis on the sample surface plane enables t...

Page 89: ...thereby averaging the variation of particle sizes Auto sample changer ASC 6 Table Standard accessories Name Illustration Al sample holder with base 0 5 for ASC 2455E445 Height alignment jig for ASC G...

Page 90: ...455E463 is also necessary for this measurement Loosen the left lever and rotate the turntable 180 degrees clockwise for the vertical transmission geometry Switch to the vertical transmission geometry...

Page 91: ...X ray Diffractometer 83 Table Accessories Name Illustration Transmission film sample holder Center slit for ASC Incident knife edge INC KE Extended base for ASC Direct beam stopper DBS Receiving knif...

Page 92: ...AntonPaar sample stages equipped with temperature adjustment mechanism The stages are HTK1200N HTK16 HTK2000 XRK900 TTK450 and CHC For information of how to use the sample stage and pipe arrangement...

Page 93: ...hanging attachments 1 Click Manual Control under the Control menu Move the chi axis to 0 and the phi axis to 0 2 Release the hook 3 Open the clasps for the right and left sides Remove the attachment 4...

Page 94: ...attachment cannot be used with 8 inch wafer sample plates XY 4 phi attachment option 2680A212 This attachment has 50 mm provides X and Y translation axes which are perpendicular to each other It is u...

Page 95: ...ion SAXS sample plate option 2680J111 A transmission SAXS sample holder is inserted into the transmission SAXS sample plate The transmission SAXS sample plate is placed directly on the attachment Tran...

Page 96: ...lder are 1 0 mm 0 7 mm etc Use the appropriate size for the capillary to be used Capillary spin attachment and capillary holder Wafer sample plates and sample spacers A wafer sample plate is used in m...

Page 97: ...center of the x ray beam Since the thickness range for which the Z axis can be adjusted is 3 mm you must select the appropriate sample spacer based on the thickness of the sample to be measured Table...

Page 98: ...6 mm 6 9 mm 9 12 mm 12 15 mm 15 18 mm black stamped mark 4 inch wafer sample plate 6 inch wafer sample plate 1 8 inch wafer sample plate 1 0 3 mm 3 6 mm 6 9 mm 9 12 mm 12 15 mm 15 18 mm 4 inch wafer...

Page 99: ...ttachment align the sections indicated by the arrows in the figure below then turn the sample spacer clockwise to secure it in place Installing the sample spacer on the attachment To remove the sample...

Page 100: ...align the sections indicated by the arrows in the figure below then turn the sample plate clockwise to secure it in place The wafer sample plate can be removed by turning it counterclockwise Installin...

Page 101: ...k theta 2 theta measurement PB PSA Help Topic of the online help section of the SmartLab Guidance software Glass sample holder Use this sample holder to measure powder samples Glass sample holder Alum...

Page 102: ...nd B intersect on the sample The only difference is that the shape of the multilayer mirror used in the CBO E unit is ellipsoidal while the mirror shape used for CBO is parabolic The ellipsoidal multi...

Page 103: ...tomated Multipurpose X ray Diffractometer 95 Accessories Table Accessories Name Illustration Center slit Si powder reference sample Si wafer reference sample Tool for installation of optical devices A...

Page 104: ...and resolutions of incident monochromator crystals Type of crystal Resolution FWHM Applications Ge 220 x2 crystal 0 008 For applications requiring monochromatized K 1 x rays or for measurements of ma...

Page 105: ...mple plate to measure bulk samples Select the appropriate sample spacer and sample plate based on sample thickness For detailed information refer to Wafer sample plates and sample spacers Place the sa...

Page 106: ...ng the sample horizontally Place the sample at the center of the sample plate Use the magnets provided to hold the sample in place The magnets can be used with samples that are up to 3 mm thick For in...

Page 107: ...paring for measurements 1 Make sure that the OPERATE lamp on the main panel is lighting up in green 2 Launch SmartLab Guidance Click Package Measurement under the Task menu 3 Click the Startup button...

Page 108: ...rd receiving slit box 2 and detector adaptor and enter the correct corresponding values Selecting a Package Measurement 1 Click Package Measurement under the Task menu 2 Registered Package measurement...

Page 109: ...easurements after HV PHA adjustments The characteristics of the detector will change over time Replacement of the detector is required when it reaches the end of its service life However you can minim...

Page 110: ...ou purchased the instrument from When contaminant tungsten from the filament from the electron gun filament adheres to the target metal surface you may observe characteristic x rays from the contamina...

Page 111: ...Lab Guidance after the SmartLab is restarted 3 SmartLab stops abruptly during measurement or other operation Make sure the OPERATE lamp on the main panel has turned to red SmartLab may have stopped du...

Page 112: ...n for 10 to 20 seconds After that when the lamp lights up in green SmartLab is ready to use If the OPERATE lamp does not turn green flashing red instead after startup or if the lamp turns green but ch...

Page 113: ...generator XG See 4 in Troubleshooting Attachment connecting cover is open The cover of the attachment connection cable is open in the radiation enclosure Close the cover Communication error A communi...

Page 114: ...elength platinum For efficient absorption of K x rays only select an element as a K filter with its absorption edge wavelength located between the K x ray and K x ray wavelengths Those elements will h...

Page 115: ...tion Rigaku Americas Corporation Rigaku Europe SE Head Office 3 9 12 Matsubara cho Akishima shi Tokyo 196 8666 Japan Phone 81 42 545 8189 Fax 81 42 544 9223 e mail rinttyo rigaku co jp 9009 New Trails...

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