2013. 2. 26.2013. 2. 26.
XRF XRF XRF XRF XRF source X- -
Sample Crystal Detector K lines & L lines Intensity Ratio
Data FP (Fundamental Parameter Method) FP Mapping (Max 250 μm) Qualitative analysis Quantitative analysis
XRF XRF XRF XRF XRF source X- -
1. XRF ?
X-ray fluorescence
is the emission of characteristic "secondary" (or fluorescent) X-rays from a material that has been excited by bombarding with high-energy X-rays or gamma rays. The phenomenon is widely used for elemental analysis and chemical analysis, particularly in the investigation of metals, glass, ceramics and building materials, and for research in geochemistry, forensic science and archaeology. ( Wikipedia)
Electron transitions
Sequential typeSequential typeSimultaneous Simultaneous typetype
Energy dispersive spectrometry
3. XRF
KS D 1654 KS D 1655 X KS D 1686 X KS D 1898 X KS D 1898 X KS D 2597 X KS D 2597 X KS D 2710 X KS D ISO 4503 X KS D ISO 4883 X KS E 3045 KS E 3075 KS E 3076 KS E ISO 9516-1 X1 KS L 3316 X KS L 5222 X KS M 0017 X
KS D ISO 14706 X-(TXRF)

KS M ISO 14596 ---X
KS M ISO 14597 X
KS M ISO 15597 X
KS M ISO 20847 X
KS M ISO 20884 X
KS M ISO 5938 (Na3AlF6)
X-ray
KS M ISO 12980 X
4. XRF
thin Beryllium window 75m or 125m
+Voltage
+Voltage
Tube head cooling
Ring shaped cathode
- Filament filament target X
- = 0.2 %( )
Rh target Rh - Cd
Cr target Cl - Ti Cr, Mn
X-ray
50 kV-75 mA 26Fe - 92U
30 kV-130 mA 4Be - 8O
X-ray
50 kV-55 mA 26Fe - 92U
30 kV-95 mA 4Be - 8O
Targrt
5. XRF source 2 - Rh, Cr, W, Mo, Pt, Au , Ag, Cu
X
Energie-range [keV] Wavelenghts Description < 10-7 cm to km Radio-waves < 10-3 mm to cm Microwaves < 10-3 mm to mm Infrared
0.0017 - 0.0033 380 to 750 nm Visible light 0.0033 - 0.1 10 to 380 nm Ultraviolett light 0.11 0.11 -- 100100 0.01 to 11.3 nm0.01 to 11.3 nm XX--raysrays 10 - 5000 0.0002 to 0.12 nm gamma radiation
Electromagnetic radiationElectromagnetic radiation
- - (ZnS, CdS, NaI ) - - = 1 - - (, ) - ,
6. X-

-
-
- -
0 )
Aperture : 1 mm ~ 30 mm
Filter : Al, Ti, Ni, Cu, Zr
Primary X-ray Filter
Al Cl, Rh, Cd
Ti Cr – Fe
Ni Zn, As, Hf, Pb, Bi ,
Cu As, Hf, Pb, Bi
Zr Ru – Cd (Rh-target) ,
8. Sample

Standard
High Resolution ClKα RhLα, MnKα CrKβ

X-, crystal ,
Bragg
, () ()
Slit
LiF(420) Lithiumfluoride / from Co 0.1801 LiF(220) Lithiumfluoride / from V 0.2848 LiF(200) Lithiumfluoride / from K 0.4028
Ge Germanium / P, S, Cl 0.653 InSb Indiumantimonide / Si 0.7481 PET Pentaerythrit / Al - Ti 0.874 AdP Ammonium dihydrogen phosphate / Mg 1.0648 TlAP Thalliumhydrogenphtalate / F, Na 2.5760
OVO-55 Multilayer (W/Si) / (C) O - Si 5.5 OVO-160 Multilayer (Ni/C) / B, C, N 16 OVO-N Multilayer (Ni/BN) / N 11 OVO-C Multilayer (V/C) / C 12 OVO-B Multilayer (Mo/B4C) / B (Be) 20
EDX & WDX
10. Detector
12. Intensity Ratio
Data FP (Fundamental Parameter Method) FP Mapping (Max 250 μm) Qualitative analysis Quantitative analysis
Qualitative/quantitative analysis, FP , Mapping
- Qualitative/Quantitative (Empirical Correction Method) analysis , , /
- FP (Fundamental Parameter Method)
- FP (Film Thickness Measurement and Thin Film Analysis) Film thickness measurement and inorganic component analysis for high-polymer thin films with background FP method
- Mapping : Max 250 µm point analysis
13. Data
- ( ) , - , Fundamental Parameter - , .
- FP –
. .
→ (Fixed), Balance Net .
Background , , Balance
14. FP (Fundamental Parameter Method)

,
2
Film Thickness Measurement and Thin Film Analysis 15. FP
16. Mapping (Max 250 µm)
Ammonite Ca, P, Si, Fe
- (crystal) .
- () -Ray tube Target Rh - .
(X-Ray RhKα, RhKβ, RhLα, Compton RhKαC, RhKβC) Peak . () .
, SbKα SbKβ, PbLαPbLβ1 . . , - ~
.
- () WDX : EDX : WDX .
Escape, SUM Net : ( →FP)
WDX : , EDX : , , ,
17. Qualitative analysis
Qualitative analysis()
•• :: C, Si, Al, Ca, Fe, C, Si, Al, Ca, Fe, BaBa, Mg, K, S,, Mg, K, S, P
•• : Mo, Ti, V, : Mo, Ti, V, MnMn, Ni, , Ni, SrSr, Zn, U, , Zn, U, ZrZr, , Cu, Y, Cu, Y, NbNb, , CoCo
5 10 15 20 25 30 35 40 45 50 55 60 65 2Theta (°)
0
25
100
225
400
625
•• Graphite • Quartz • Augite • Uranocircite • Tremolite, Amphibole • Pylite • Dravite
F.C SiO2 Al2O3 Fe2O3 CaO MgO Na2O BaSO4 K2O TiO2 MnO P2O5
35.10 28.44 6.89 4.31 6.75 2.71 0.15 4.95 1.38 0.50 0.08 0.83
( n >= 2 ) 1 ( n = 1 )
,3 3
,2 2
2

X-, , Bragg . , ()() .
- Simultaneous type WDX WDX
, Bragg (2dsinθ=nλ) X-
X-, , Bragg . , () .


.
FP (Fundamental Parameter) , .
- (CRM/RM) - (Glass Disk) - Intensity : Glass Disk /Flux - (Belt grinder) - 3
- 2θ, background point, PHA
-
(α,α ) X-Ray(Target, kV, mA) 1 X-
Aperture size Slit(Standard, High Sensitivity, High Resolution) Crystal (LiF, Ge, PET, TAP ) Detector (SC,FPC)
: Background level/
Spectrometer condition(Air, Vacuum, He )
Kα Lα
XRF
PHA(PHD)
- : peak - : peak
K2O 12 % K2O 0.2 %
Detectors: Proportional counter (Flow counter) E ∞ Pulse height of X-ray quants
HV: + 1400 V - 2000 V
Preampliefier
counterwire
e- e- e-
I+ I+ I+
e- + O2 O2 -
Detectors: Proportional counter - Pulse Height Analysis (PHA)
Ar + 10% CH4
Pulse height [Volts] Pulse hight [Volts] Energy [keV] Energy [keV]
Escape
Encapsulated
Scintillation
Crystal-NaI(Tl)
Energy [keV]
Fe KA1
The resulting light strikes a photocathode from which electrons can be detached very easily.
Energy of X-ray quants ∞ Pulse height of voltage produced in PMT
Analyzer Crystals : Resolution
SiO2 (Matrix Correction)
-
-
-
-
-
-
-
-
-
0.5 g0.6 g0.7 g0.8 g0.9 g1.0 g1.1 g1.2 g1.3 g1.4 g
MgO
Na2O
K2O
TiO2
MnO
P2O5
-
-
-
-
-
-
-
-
0.5 g 0.6 g 0.7 g 0.8 g 0.9 g 1.0 g 1.1 g 1.2 g 1.3 g 1.4 g
SiO2
Al2O3
Fe2O3
CaO
ZrO2
XRF (-)
XRF ( )
19.
-
-
-
- certification
-
- ?
- ?