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SmartLab: Automated Multipurpose X-ray Diffractometer

Sample Holders

Use a sample holder when measuring samples that require preparation, such as
powder and bulk samples.

For information on preparing samples, refer to Section 2.8 of the “Quick theta/2-theta
measurement (BB)” or “Quick 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

Aluminum sample holder

Use this sample holder to measure powder samples or small bulk samples.

Aluminum sample holder

Transmission SAXS sample holder (option: 2680J111)

Use this sample holder to measure fibrous or film samples by the transmission
method.

Transmission SAXS sample holder

Содержание 2080A211

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

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 8: ......

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

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

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

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

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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...

Страница 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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