第4章 X射线衍射仪实验技术与应用
Beijing China , 2010.09
He Chong Zhi
1. D8 X射线衍射仪系列系统与功能简介
2. 核心部件与功能
3. Bragg-Brentano 衍射几何
4. 光学系统及其参数选择对采集数据质量影响
5. 平行光束-Geobel 镜和掠射入射衍射
6. X射线透镜
7. 探测器
8. 控测、采集数据与测量条件
9. 非常态结构动态衍射分析
10. 应用X射线衍射仪衍射关心的具体问题
1. D8 X射线衍射仪系列系统与功能简介
配置光学编码器的测角仪
高精度的Dovetail导轨, 模块化的
光学器件快速互换
射线防护好：0.2 Sv/h 通过欧
洲安全论证，2 套安全电路
配置各种特殊功能的附件，即
可组成具有各种功能的衍射
仪系统，如高低温及不同气氛
与压力下的结构变化的动态
分析等。
在 D8 Advance 基础上,组建 D8 X射
线衍射仪系列产品。
D8 Advance
D8 DISCOVER
单晶外延膜、薄膜分析高分辨衍射分析单晶外延膜的结构特征，
用Bond法超精度地测点阵参数、点阵错
配、化学组份，用Rocking曲线测定测算
嵌镶结构、取向,作倒易空间测绘; 用
于分析薄膜的厚度、密度、表面与界面
粗糙度等。
高精度的尤拉环
高强度的织构及应力测量
D8 GADDS 系统Fast phase ID microdiffraction percent crystallinity 功能:Powders, Texture, Stress,SAXS.
特点:Fast speed,Micro-diffraction, Versatility.
fast stress
fast texture
2D SAXS
GADDS - all applications with ONE instrument
18Kw 转靶 X射线衍射仪
X射线光源: X射线发生器最大输出功率≥18kW ;额定
电压20-
60kV; 最大额定电流450 mA;电流电压稳定度优于
±0.01% (外电压波动10%时), X光源自旋转阳极; 光
源震动0.2 微米以下; 焦斑尺寸0.5 x 10 mm
测角仪: 扫描方式 θ/2θ测角仪，测角仪垂直放置;
测角仪采用光学编码器技术;角度重现性 0.0001?, 驱动方式：步进马达驱动; 最高定位速度：1500?/min
狭缝系统：包括索拉狭缝、发散狭缝、防散射狭缝、
接受狭缝等
闪烁计数器；线性范围：≥2 x 106 cps; 背底噪声：
＜0.5 cps,可配备闪烁计数器、万特探测器、固体探测器、面探测器
等。
循环水冷系统:要求连续工作; 控温精度≤±2℃;
供水流量, 满足发生器要求, 进水度可调; 过
热保护
最新X射线衍射技术-The New D8 ADVANCE
with DAVINCI.DESIGN
DAVINCI.DESIGN: A revolutionary 3-level design
DAVINCI.MODE
Component Recognition
DAVINCI.SNAP-LOCK
Tool-free Change of Optics
DIFFRAC.DAVINCI
The Virtual Goniometer
DIFFRAC.DAVINCI=The Virtual Goniometer ?Graphical representation of the actual goniometer showing all mounted components plus their status
?Software validated instrument configuration with real-time conflict detection
Dynamic list displaying all currently mounted
components
Component
Component
status
Unique icon of
optical component Current setting
1.) Component
parameterisation
3.) Conflict 2.) Component detection
selection
1) Component parameterisation, e.g. TWIN Optic
Component
status: OK Push-button switch between
Bragg-Brentano and parallel
beam geometry
Slit aperture
2) Component selection, e.g. slits
Component
status: HINT
Push-button selection of any of the slits configured for the present instrument, e.g.
- Absorber
- Filter
- Divergence slit
- No slit
- ... HINT: No slit inserted! - By intention?
- By mistake?
The new D8 ADVANCE
TWIST TUBE Line
focus
Loosen
screws
Point
focus
tighten
screws Turn tube
head
Secondary
TWIN
Primary
LYNXEYE TWIN
TWIN optic for primary beam: TWIN optic for secondary beam: ? Variable slit ? Variable slit
? G?bel mirror ? Equatorial soller 0.2°
Switching modes:
motorized
software-controlled
alignment-free
The new D8 ADVANCE
TWIN - TWIN for Bragg-Brentano
LYNXEYE 1D Variable slit Variable slit
The new D8 ADVANCE
TWIN - TWIN for GID
LYNXEYE 0D
G?bel mirror
Equatorial
soller
The new D8 ADVANCE
TWIN - TWIN for XRR
LYNXEYE 0D
G?bel
KEC turned 90°mirror
Variable slit
The new D8 ADVANCE TWIN - TWIN for Microdiffraction G?bel LYNXEYE 1D
mirror
Variable slit
Micro
slit
15000 14000 13000 12000 11000 10000 9000 8000 7000 6000 5000 4000 3000 2000 1000
15
Compare
Greem: D8 ADVANCE+LYNXEYE
Blue: D2 PHASER+ LYNXEYE
Red D8 ADVANCE+SC
20 30 40 50 60 70 8
2-Theta - Scale
File: LFP-02(SUZHOU)_SC.raw - Type: 2Th/Th locked - Start: 15.000 ? - End: 79.993 ? - Step: 0.020 ? - Step time: 0.5 s - Temp.: 25 ? (Room) - Time Started: 3 s - 2-Theta: 15.000 ? - Theta: 7.500 ? -
Operations: Import
Commander Sample ID - File: BJLTP010.6s.raw - Type: Locked Coupled - Start: 14.999 ? - End: 79.991 ? - Step: 0.020 ? - Step time: 0.6 s - Temp.: 25 ? (Room) - Time Started: 0 s - 2-Theta: 14.999
Operations: Import
Commander Sample ID - File: BJLTP022.4s.raw - Type: Locked Coupled - Start: 14.999 ? - End: 79.991 ? - Step: 0.020 ? - Step time: 2.4 s - Temp.: 25 ? (Room) - Time Started: 0 s - 2-Theta: 14.999
Operations: Import