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WIDE ANGLE GONIOMETER ULTIMA + SYSTEM

X-ray diffractometersequipped witha wide ANGLE GONIOMETER are broadly used inmany industrial and research fields in order toconduct research and analysis of ceramic mate-rials, metals, minerals, semiconductors, fibers,chemical products, polymersand so on. Insome of these fields there is an increased de-mand for an optical SYSTEM which will permitgood peak resolution AND low backgrounds forthe low ANGLE region of2() variety of attachments for the wide anglegoniometers are also available to extend the an-alytical capabilities,responding to diversifiedapplications, thus making it possible to conductmeasurements at high and low temperatures orTHE 1993 Product InformationWIDE ANGLE GONIOMETER " ULTIMA +"SYSTEMT heta-Thetagoniometerequipped with Peltier Solid State Detector, high pressure, and measurements of thinfilms, fibres, stress, preferred orientationofcrystals, the field of X-ray detectors the standardscintillation counter is often being replaced bysolid-state detectors (SSD)

1. Introduction Powder X-ray diffractometers equipped with a wide angle goniometer are broadly used in many industrial and research fields in order to

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Transcription of WIDE ANGLE GONIOMETER ULTIMA + SYSTEM

1 X-ray diffractometersequipped witha wide ANGLE GONIOMETER are broadly used inmany industrial and research fields in order toconduct research and analysis of ceramic mate-rials, metals, minerals, semiconductors, fibers,chemical products, polymersand so on. Insome of these fields there is an increased de-mand for an optical SYSTEM which will permitgood peak resolution AND low backgrounds forthe low ANGLE region of2() variety of attachments for the wide anglegoniometers are also available to extend the an-alytical capabilities,responding to diversifiedapplications, thus making it possible to conductmeasurements at high and low temperatures orTHE 1993 Product InformationWIDE ANGLE GONIOMETER " ULTIMA +"SYSTEMT heta-Thetagoniometerequipped with Peltier Solid State Detector, high pressure, and measurements of thinfilms, fibres, stress, preferred orientationofcrystals, the field of X-ray detectors the standardscintillation counter is often being replaced bysolid-state detectors (SSD)

2 , Peltier SSDs, InelPSDs, area detectors and the like. As these de-tectors become more commonly utilized, it willno longer be necessary to use a scintillationcounter and a crystal monochromatorto pro-duce high quality monochromatized X-rays dif-fraction wide ANGLE goniometerULTIMA+has beendeveloped to meet the demands of researchersand operators calling for multiple can be used as a theta-theta GONIOMETER and39also as a vertical or horizontal GONIOMETER . At-tachments for theULTIMA+are also designed tobe used in common regardless of the goniome-ter Features Conversion to any of the configurations,theta-theta, vertical and horizontal, can be com-pleted easily by the user. The GONIOMETER radius can be set at severalpositions between 185 mm and 285 mm to se-lect optimum conditions of normal to high reso-lution.

3 Attachmentsare designed to be used ineach configuration with zero or minimal An optional curved crystal incident beammonochromator is available for each SYSTEM . Measurement with fixed slits or with op-tional paired continuously variable slits is possi-ble. Alignment of the GONIOMETER after conver-sion from one configuration to another, includ-ing the GONIOMETER angles, slits, and monochro-mator, is completed quickly with the aid of afully automated alignment Specifications~lVertical goniometerTheta-thetagoniometerHorizonta l goniometerTheta-ThetaVertical/Horizontal ConfigurationConfigurationDriving Axises,Od(independentor coupled0,20(independentor coupledaxis rotation)axis rotation)GoniometerRadius185mmMeasuring _79 -10 _158 (Os,Od)(20 )Fixed Step -50 -90 ContinuousScan -500 -1000/minSlew Speed(20)10000/min10000/min (Vertical)15000/min (Horizontal)Slit ExchangerAutomaticFixed Slit Exchanger SystemDS:1/2 , 1 ,2 , mm, OpenSS.

4 1/2 ,1 ,2 ,Absorber, , , , mm, OpenAutomaticAlignmentJigPaired knife edgeswith compacted silicon powder at jig centerOptics AlignmentFull AutomaticAlignmentand ControlOptical SystemGoniometerradius 185 mmGoniometerradius 185 mm(can be set at several positionsbetween 185 mm and 285 mm)Systematic ErrorComputer software automaticallycreates and corrects data baseCorrectionfor systematic errors/JFilterNickel (Standard),Others are optionalt40 The Rigaku JournalOptionsTheta-ThetaVertical/Horizo ntalConfigurationConfigurationIncident MonochromatorCurved Crystal (a-Si02 Johansson type)CoKa1, FeKa1,CuKa1, MoKa1, (CrKa1)ContinuouslyVariableVariable width: mmSlitsMaximum sample irradiation width:14 mm (for 185 mm radius) /pulse285 mm Radius -10 _165 SYSTEM (8s,8d)(2(;1)Encoder Mounting-Heidenhein encorder( Readout) Beam Monochromator MeasurementCurved Crystal Incident Beam MonochromatorThin Film MeasurementThin Film Attachment Preferred OrientationSpecimen Rotation Attachment Sample MeasurementSpecimen Rotation/Oscillation AttachmentMultiple Sample6-Position Sample Changer ASC-6 Exchanger43-Position Sample Changer ASC-43 High/Low TemperatureHigh Temperature Attachment: MeasurementAmbient-1500 CLow Temperature Attachment: -190-+50 CMedium/LowTemperature Attachment:-100-+300 CUltrahigh Temperature Attachment: Ambient-2500 CThin Film High Temperature Attachment:Ambient-1 OOO CLiquid Crystal HighTemperature Attachment:Ambient-240 CFiber Specimen Heating/Elongation Attachment.)

5 Ambient-300 CTexture MeasurementFiber Specimen Attachment Pole Figure Attachment Stress MeasurementStress Analysis Attachment Note 1: Temperature programmingfor each of the high, medium, and low temperatureattachmentsis made uti-lizing the programmingtemperaturecontroller 2: The .-markand the . -mark in the table indicate standard and special option availabilityfor these attachments are virtually interchangeablefor all three ExamplesExamples of actual measurements are shownin through 5. Each set of diffraction datawas obtained using a normal focus Copperanode X-ray tube set at a 6 take-off ANGLE . Nomonochromator was 1 through 3 show the measurement re-sults fora-Quartz. Fig. 2 shows data on the(100) diffraction peak fora-Quartz, in fixed timemode for 1 see/step.

6 As illustrated the Kal andKa2 peaks are separated to a slight degree, thusenabling complete separation by computer soft-ware enhancement of 3 showsthe diffractiondata for the (101) peak ofa-Quartz, in which the Kal and Ka2 peaks are su-perimposed on the raw sample shown in is a Lead Stearatepowder coated onto a sample peak ataround 28= can be seen 5 shows the diffraction scan on a synthet-ic multilayer sample. The 2d value of this sam-ple is approximately first peak is ob-served at approximately28= .A totalreflec-tion peak is located near 28= and the directbeam intensity rises around 28= .oRTE:5H11 PLE NH~Eq-~i02IR'iCUC"Val~ndCUR ~0KV40mR5 LlT505 IR5. ~5 55 I5U-1"1 SFEED~OEG/M! ~ ~RE~ ! ME20 SEe" IL ENAME!I I~ IDPESfiTQ,MU~IU2'I!jCOM'1E!'ITSMOOTH!NG , REOUCTI ONNO EXECUT IONOUTPUTFILEIIISMSamp I~Nc meR-Si02::::JouS.

7 Iii1~,~IIHigh Resolution GSpeCimenat:-8i02Lu,,--~AA~k~A~oniometer Fig. 1 wide Range Scan ofa-Quartz Rigaku ~-t( )Specimena-5i02uSF.'A.~:"':::~R:~::'!"P. :\G:':T'10:..e nd !~s:..r:sSCf:;'4 SP~:::)S:::?;SR ~e:..P::;:::S::T T!i~~:rr;".~~A~EOPf.;;;RTO:;:C0:1:~~~.r1 : q-5i02:C. 501':"';011I ,: JS 1 ~S ,05 S51S :J~.G;;~! J~GJS~:CVIOO: ;~UN::":?8S2iL5aHighResolution GONIOMETER ~,SI-OATf.;87, ~!NG~O.,0T~R:ESH.!r~iE~.:0(? !V,.0 C?S;(;)! "'1j)T~ :\: DUCT!O! ~~):!:Cl!:! !.3 TFl!T~J;" 2 Scan ofa-Quartz (100) Diffraction Peak5 Hlif' ~H::'<-So02,)Oul\r.~, ~E2\HiJi3ornqIrJ,~ ~E:2~ :r:(u1\,,2/I\ .!Il'liU4S1i'!'RfiT!O,4:J3 ZillR-Sl02 OflTE::IiHI-0-.~ ,a-5i02(101)ohs,{ka1ko<1ko<2Ka2)OFiTR[ :;U1 Mao~[ ,TRRNGU'::rJe]2~1iiINDEX:t1 0I)dl~aOqrKa,2 :. !'(rnsiriosu .e/FWH~ !G~AVIr rFCR!':TOP; ):JS;:E,.r; ;:)]Hl; ~nEw. l r rF ""h~l!NTECSRlINTENSI r s];u.}

8 'L~s~S1-~ . ~E:~;D, ..1.;). ':[ . ]ZF.,rjl:] 9~ 3 Scan ofa-Quartz (101) Diffraction peak (PeakSeparation)\\~. :LSU31 UISAMPLENAME: PbSllu\ ", ~~U(d.,) [d/ . e e ILRMBDR; :~.0 SOPERATOR:MUNE12 BSDATE:HODE1 :~tep scanMODE 2 AXIS. 2th/th{th-5/th-OJSTOP1~.U~~(do,) {deg] ~ASLlT2:0.~ 4 Low ANGLE Scanof Lead Stearate PowderNote 1:The sample was made available through thecourtesy of Organic Synthetic Materials Company, ownedsubsidiary of Energy Conversion Devices,Inc.!FILENRME:Lsra31~1(INTENSIHD ATA)NUMBER OFDATA"1000 \.29~. ,z=> 1 High .. ! '11'514 OPl~ATORR IGAKU/MUNEl28 SCOH!'1 ENiPHA- ,. "(PS/IOEGxOEGJeOEGNOEXECUT! 'IPI", 'fI/s:S~.3a~-,1stHigh ResolutionGoniometerx-,-"'Y"Re (I)(Specimenpresentedbycourtesyof Japan ) ~ }. 5 Low ANGLE Scanof W/Si Rigaku Journal}


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