X射线衍射新技术介绍

1、杨林涛 博士, BRUKER AXS布鲁克AXS-2012用户会议，贵阳，2012-08-05布鲁克X射线衍射新技术介绍2Outlines New D8 ADVANCE & D8 DISCOVER 介绍 LYNXEYE XE能量色散阵列探测器 D2 PHASER 桌面衍射仪 SAXS新解决方案The New D8 with DAVINCI.DESIGNThe New D8 ADVANCE & DISCOVER开创XRD的新世纪The New D8 ADVANCEUnequalled Abundance of Innovations 元器件自动识别及配置元器件自动识别及配置 元器

2、件互换无需调整，弹指间实现光路互换元器件互换无需调整，弹指间实现光路互换 在一台设备上集成多功能，而且轻松实现功能互换在一台设备上集成多功能，而且轻松实现功能互换 系统智能纠错系统智能纠错新的D8 ADVANCE 衍射仪-世界上第一台真正的“智能化”衍射仪The New D8 ADVANCEwith DAVINCI.DESIGNDAVINCI.DESIGN: A revolutionary 3-level design1.DAVINCI.MODE元器件自动识别元器件自动识别2.DAVINCI.SNAP-LOCK无工具元器件互换无工具元器件互换3.DIFFRAC.DAVINCI虚拟测角仪技术虚拟

3、测角仪技术The New D8 ADVANCEDAVINCI.MODEDAVINCI.MODE=Component Recognition所有光学部件实现全自动实时识别所有光学部件实现全自动实时识别 每一个附件（狭缝及滤片外）每一个附件（狭缝及滤片外）拥有独特的拥有独特的IDID识别码识别码 狭缝及滤片通过类似光栅技术狭缝及滤片通过类似光栅技术进行识别进行识别真正的即插即用功能真正的即插即用功能ID ChipSpring contact connectorsBit mask with light barrier read-outThe New D8 ADVANCEDAVINCI.MODE所有附

4、件、附件互换、附件状态互换均实现系统实时自动识别所有附件、附件互换、附件状态互换均实现系统实时自动识别 所有光管，包括点或线焦斑识别所有光管，包括点或线焦斑识别 所有光学附件，包括狭缝及滤片所有光学附件，包括狭缝及滤片 所有的样品台，包括第所有的样品台，包括第3 3方附件，如高低温原位附件方附件，如高低温原位附件 所有的探测器，包括探测器所有的探测器，包括探测器 0 0/90/90设置设置每一个附件均在系统中保存了其全部的信息，包括调试信息及每一个附件均在系统中保存了其全部的信息，包括调试信息及功能功能 实现系统的全自动配置实现系统的全自动配置 光路补偿光路补偿 ( (如如G Gbelbel镜

5、镜) )将基于储存的对光信息进行全自动调整将基于储存的对光信息进行全自动调整所有笨拙的配置及调整一劳永逸的消除了！所有笨拙的配置及调整一劳永逸的消除了！The New D8 ADVANCEDAVINCI.SNAP-LOCKDAVINCI.SNAP-LOCK=Tool-free Change of OpticsHigh precision snap-lock mechanism: Tool-free change of optics in a second High-precision pre-alignment to optics mount with 3-point support3-poi

6、nt supportSNAP-LOCK: Fixing pin with bayonet lockThe New D8 ADVANCEDAVINCI.SNAP-LOCKAny change between different optics, instrument geometries and applications is literally childs playAlignment-free; all optics return to perfect alignment every timeFully automatic optics recognition and instrument c

7、onfiguration thanks to DIFFRAC.MODEEach optic is identified by an unique iconThe New D8 ADVANCEDAVINCI.SNAP-LOCKRepeated switch (5x) between Bragg-Brentano and parallel beam geometrySRM 1976aBragg-BrentanoParallel beam (Gbel mirror)D2q = 0.0025 2qD2q = 0.001 2qThe new D8 ADVANCEFully automatic optic

8、s changeThanks to TWIN-TWINThe New D8 ADVANCEDIFFRAC.DAVINCIDIFFRAC.DAVINCI=虚拟测角仪技术虚拟测角仪技术图形化的显示所有安装在测角图形化的显示所有安装在测角仪上的元器件及其状态仪上的元器件及其状态系统自动进行系统自动进行“冲突检测冲突检测”，确认光路的合理性确认光路的合理性The New D8 ADVANCEDIFFRAC.DAVINCI in Action1.) Component parameterisation, e.g. TWIN OpticPush-button switch between Bragg-Br

9、entano and parallel beam geometrySlit apertureComponent status: OKThe New D8 ADVANCEDIFFRAC.DAVINCI in ActionWrongly inserted slitComponent status: ERRORClear error messages3.) Conflict detection, e.g. wrongly inserted slitsThe new D8 ADVANCETWIN TWINPrimary TWINSecondary TWINLYNXEYESwitching modes:

10、n motorizedn software-controlledn alignment-freeThe new D8 ADVANCETWIN - TWINn TWIN optic for primary beam:n TWIN optic for secondary beam: Variable slit Gbel mirror Variable slit Equatorial soller 0.2The new D8 ADVANCETWIN TWIN for Bragg-BrentanoVariable slitVariable slitLYNXEYE 1DThe new D8 ADVANC

11、ETWIN TWIN for GIDGbel mirrorEquatorial sollerLYNXEYE 0DThe new D8 ADVANCETWIN TWIN for XRRGbel mirrorKECVariable slitLYNXEYE 0D turned 90The new D8 ADVANCETWIN TWIN for MicrodiffractionGbel mirrorMicro slitVariable slitLYNXEYE 1DThe new D8 ADVANCETWIST TUBELine FocusLine focusLoosen screwsTurn tube

12、 headtighten screwsPoint focusThe new D8 ADVANCEStress and Texturen Stress (iso-inclination mode)n Stress (side-inclination mode)n TexturePoint FocusThe new D8 ADVANCETWIN TWINBragg-BrentanoXRRGIDMicroThe New D8 ADVANCEDIFFRAC.DAVINCI不同功能之间的互换就象您玩游戏机一样的简单、快捷不同功能之间的互换就象您玩游戏机一样的简单、快捷！No problem with D

13、IFFRAC.DAVINCI !The New D8 ADVANCEDIFFRAC.DAVINCIDynamic list displaying all currently mounted componentsComponentComponent statusUnique icon of optical componentCurrent setting27D8 DISCOVERVNTEC-500 Outperforms all previous gaseous detectors.Thanks to our ingenious DAVINCI.DESIGN you will never los

14、e your smile.LYNXEYE II29High-Resolution Energy-Dispersive 1-D DetectorLYNXEYE XELYNXEYE II30The LYNXEYE XE is the first energy dispersive 1-dimensional detector operating at room temperature for ultra fast X-ray diffraction measurements.The LYNXEYE XE 全球率先推出的能量色散阵列探测器（工作条件为实验室室温条件） LYNXEYE XE能量色散阵列

15、探测器The LYNXEYE XE 超高强度与能量分辨首次完美结合！450倍的强度或者测试速度的提高 （相比常规的点探测器与石墨单色器系统）优秀的能量分辨率保证了不再需要K 滤片和石墨单色器完美的峰型（彻底消除残余K 影响） 布鲁克全球保证无任何缺陷通道完全免维护，室温实验室条件使用（无需电制冷、气氛） X-ray emission lines (Cr, Co, Cu, Mo, and Ag radiation)适合于小角衍射、小角散射、织构、应力、薄膜反射等非常规测试LYNXEYE II31USPUSPUSPLYNXEYE XE能量色散阵列探测器K-FiltersIntensity loss

16、 40-60% with respect to unfiltered radiationAbsorption edges, K level 0.5-1.5%Poor filtering of fluorescenseAbsorption Edge Modelling32LYNXEYE XE能量色散阵列探测器XRD单色化背景介绍 (Cu)K-FiltersIntensity loss 40-60% with respect to unfiltered radiationAbsorption edges, K level 0.5-1.5%Poor filtering of fluorescense

17、Absorption Edge Modelling33Before 2000, 90% of all instruments have been equipped with point detectors, 50% with (secondary) monochromatorsToday, 90% of all instruments are equipped with PSDs, 50% with mit K-FilterLYNXEYE XE能量色散阵列探测器XRD单色化背景介绍 (Cu)Absorption Edge Modelling34MonochromatizationEffect

18、of K-FilterPecharsky & Zavalij (2009)Remnantwhite radiationAbsorption Edge Modelling35K filters do leave some severe artefactsAbsorption edgesK level 0.5-1.5%Poor filtering of fluorescenseSevere absorption edge issues with any line profile fitting applications:Goodness-of-fit is poor as backgrou

19、nd function cant copeLYNXEYE XE能量色散阵列探测器XRD单色化背景介绍 (Cu)K-FiltersIntensity loss 40-60% with respect to unfiltered radiationAbsorption edges, K level 0.5-1.5%Poor filtering of fluorescenseMonochromatorsPrim.: Intensity loss 80-90% with respect to unfiltered rad.Sec. 0D: Intensity loss 70% with respect

20、 to unfiltered rad.Sec. 1D: Intensity loss 90% with respect to unfiltered rad.No absorption edges, no KExcellent filtering of fluorescenseSi(Li) detectorsNo intensity loss, best P/BNo absorption edges, no KExcellent filtering of fluorescenseLow linear range, low count rates, life time issuesOnly 0D!

21、Absorption Edge Modelling36LYNXEYE XE能量色散阵列探测器XRD单色化背景介绍 (Cu)LYNXEYE II37LYNXEYE XE能量色散阵列探测器XRD单色化背景介绍 (Cu)LYNXEYE II38MonochromatizationTraditional Si Strip / PixelLYNXEYE II39MonochromatizationTraditional Si Strip / PixelLYNXEYE II40MonochromatizationLYNXEYE XE荧光的过滤LYNXEYE II41LYNXEYE XE能量色散阵列探测器-

22、荧光的过滤LYNXEYE II42LYNXEYE XE能量色散阵列探测器-荧光的过滤Manganese Ore（锰矿）Fluorescense filtered completely LYNXEYE II43LYNXEYE XE能量色散阵列探测器-荧光的过滤Iron Ore （铁矿石）Fluorescense filtered completely LYNXEYE II44LYNXEYE XE能量色散阵列探测器-荧光的过滤Cobalt Ore （钴矿石）LYNXEYE II45LYNXEYE XE能量色散阵列探测器- K的过滤NIST SRM 1976a (Corundum)Square ro

23、ot scale to highlight detailsLYNXEYE XE, unfiltered radiationLYNXEYE XE, K filteringLYNXEYE XE, 0.0125 mm Ni FilterLYNXEYE XE, 0.02 mm Ni FilterLYNXEYE II46NIST SRM 1976a, Cu radiationK-alpha scanK-beta scan LYNXEYE XE能量色散阵列探测器- K的过滤K-alpha scanK-beta scan LYNXEYE II47Square root scale to highlight

24、detailsKa1,2WL1K3,1Ni EdgeWL2 + Kb(higher angle peak)LYNXEYE XE能量色散阵列探测器- K的过滤NIST SRM 1976a (Corundum)High-speed data acquisition up to 450 times faster than a conventional point detector system (point detector with secondary monochromator)See LYNXEYE XE Flyer (DOC-H88-EXS055)Maths:Intensity loss s

25、econdary monochromator 70%Intensity loss LYNXEYE XE K / fluorescense filtering 20-25%Factor3LYNXEYE is 150 times faster than a point detector system3 x 150 = 450Confirmed empirically by the data shown in the LYNXEYE XE flyerLYNXEYE II48LYNXEYE XE能量色散阵列探测器Speed-450 倍的强度或者速度获得Scinti with sec. monochro

26、matorLYNXEYE XE450Square root scaleLYNXEYE II49NIST SRM 1976a, Mo radiationLYNXEYE XE, 0.02 mm Zr filterLYNXEYE XE, K filteringLYNXEYE XE能量色散阵列探测器LYNXEYE II50NIST SRM 1976a, Mo radiationLYNXEYE XE能量色散阵列探测器LYNXEYE II51Remnant K peakZr absorption edgeRemnant K peakZr absorption edgeSpecimen peaks sitt

27、ing on top of an Zr absorption edgeK is below the detection limitMassive reduction of white radiationSquare root scale to highlight detailsNIST SRM 1976a, Mo radiationLYNXEYE XE能量色散阵列探测器LYNXEYE II52LYNXEYE XENIST SRM 1976a, Cu radiationK-alpha scanK-beta scan LYNXEYE II53LYNXEYE XETechnical DataUSPU

28、SPThe D2 PHASERXRD for Everyone - EverywhereThe D2 PHASERComponentsWorlds fastest desktop X-ray diffractometer LYNXEYE detector Scintillation counterInnovative high-end goniometer design (patent pending)Sample always horizontal Theta / Theta geometry(Bragg-Brentano)Sample spinner 1 rpm to 80 rpm Cho

29、ice of divergence and Soller slitsThe D2 PHASERCommon Sealed X-Ray Tube DesignStandard sealed X-ray tubeCompatible to standard tube dimensions Cr, Co, Cu radiation Cr KFL tube, 1.9 kW Co KFL tube, 1.8 kW Cu KFL tube, 2.2 kW Generator with 30 kV / 10 mA300 W power load, therefore: Virtually no tube a

30、geing Virtually infinite tube lifetimeThe D2 PHASERSample LoadingSimple sample loading Sample holders with industrial standard dimension (51.5mm)Compatible with the D4 and D8 diffractometer familiesThe D2 PHASER with LYNXEYEFast Lane Editionn Active area: 14.4x16 mm,5.5 2q angular coveragen Detector

31、 Guarantee:No dead strips!n Fluorescence suppression eliminating the need for secondary monochromatorsn More than 150 times faster / more intensity than a scintillation counterD2 PHASER with LYNXEYE The worlds fastest desktop X-ray diffractometerThe D2 PHASERPlugn AnalyzeMobile for on-location opera

32、tionNo pre-installation requirementsAll standard domestic wall sockets supported 90-250V 50-60HzInternal cooling system no water supply neededOperating temperature 5C - 35CXRD wherever you need it!The D2 PHASERPlugn Analyze No installation No alignment No instrument configuration2Th Degrees323028262

33、422201816141210Counts46 00044 00042 00040 00038 00036 00034 00032 00030 00028 00026 00024 00022 00020 00018 00016 00014 00012 00010 0008 0006 0004 0002 0000-2 000-4 000-6 000-8 000Quartz5.64 %Hematite8.59 %Gibbsite55.34 %Boehmite14.70 %Goethite8.77 %Anatase1.79 %Kaolinite (BISH) 5.17 %Quartz5.57 %He

34、matite8.95 %Gibbsite57.15 %Boehmite13.44 %Goethite8.69 %Anatase1.82 %Kaolinite (BISH) 4.37 %5/2/202261The D2 PHASER - Phase Quantification Fluorescent Material Agreement with round robin data: accuracy 1.5 wt-% Optimized discriminationresults in: Better quantification of minor constituents Higher ac

35、curacyNo Fe-discriminationwith Fe-discrimination样品E-30 D2和D8数据比较5/2/2022Bruker Confidential62Commander Sample ID - File: D2_10_70_4deg_1mm_0.03.raw - Type: Locked Coupled - Start: 9.9991 ? - End: 69.9890 ? - Step: 0.0304 ? - StCommander Sample ID - File: sample_4deg_per_min_0.03_5.1_2.5.raw - Type:

36、Locked Coupled - Start: 10.0001 ? - End: 70.0006 ? - Step: 0.Lin (Counts)01000020000300002-Theta - Scale152030405060黑线D8 （ 4度/分钟）红线D2（ 4度/分钟）测量基本参数相同D8 的强度高了大约一倍 5/2/2022Bruker Confidential63Commander Sample ID - File: D2_10_70_2deg_1mm_0.03.raw - Type: Locked Coupled - Start: 9.9991 ? - End: 69.989

37、0 ? - Step: 0.0304 ? - StCommander Sample ID - File: sample_4deg_per_min_0.03_5.1_2.5.raw - Type: Locked Coupled - Start: 10.0001 ? - End: 70.0006 ? - Step: 0.Lin (Counts)01000020000300002-Theta - Scale15203040506070样品E-30 D2和D8数据比较黑线D8 （4度/分钟）红线D2 （2度/分钟）强度和D8 非常接近January 21, 201264SAXS: Nanostar and MICRONanostarMICROBudget (indicative) 400 k 300 k Best used forMaterial Science , Physical TestingNanography BioSoft condensed matterPharma USPNanographyMICROcalioXKratky vs pin-hole collimationMICRO vs NanostarDefining slitsCleaning slitPin-hole : 360 field of vi