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X- ray Diffraction (XRD) Written by Sung Yong An 1. X- 선의 발견 X- 선은 1985 년 독일의 물리학자 Roentgen(뢴트겐)에 의해서 발견되었다.X- 선의 본질은 빛(光)을 위시해서 라디오파, ã- ray등과 함께 파장이 각기 다른 전자기파에 속한다. X- 선은 뢴트겐에 의해 발견된 후 물질의 내부를 밝히는데 있어 단순한 X- 선의 투과력에 의한 10 -1 cm 정도의 해상력(resolution) 에 국한하는 'Radiography' 뿐만 아니라 원자구 조 수준의 Å(10 - 10 m) 정도의 물질의 내부구조를 밝히는데 이용될 수 있다는 소위 "X- ray diffraction(XRD)" 현상이 확립된 것은 독일의 Laue에 의한 X- 선 회절실험이 성공한 이후이며 이것은 또한 X- 선의 파동성과 결정내의 원자의 규칙적인 배열을 동시에 입증한 계기가 되기도 하였다. 한편 Laue에 의한 X- 선 회절실험결과를 같은 해 영국의 Bragg 는 훌륭하게 이를 다시 다 른 각도에서 해석하였고 Laue가 사용했던 수식보다 더욱 간단한 수식으로 회절에 필요한 조건을 Bragg's Law( )로 나타내었으며 이 X- 선 회절 현상을 이용하여 각종 물질의 결정구조를 밝히는 일에 성공하였다. 2. X- 선의 발생 및 성질 그림. 1 X- 선 발생장치 페이지 1 / 14 XRD 2001- 03- 05 http://phys.kookmin.ac.kr/~xray/xrd/xrd.html

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  • X-ray Diffraction (XRD)

    Written by Sung Yong An

    1. X-

    X- 1985 Roentgen() . X- () , -ray . X- X-

    10-1 cm (resolution) 'Radiography'

    (10-10 m) "X-ray diffraction(XRD)" Laue X- X- . Laue X- Bragg Laue

    Bragg's Law( ) X- .

    2. X-

    . 1 X -

    1 / 14XRD

    2001-03-05http://phys.kookmin.ac.kr/~xray/xrd/xrd.html

  • X- . filament . eV .

    (1)

    (2)

    (e : , m : , v : , V : ) 1 % X- . Target Material() Cr, Fe, Co, Ni, Cu, Mo, W . coulomb . X-. X- X- X-(bremsstrahlung) . . X- , X- . , X-ray X- . coulomb E x X- .

    (3)

    (4)

    (5)

    . Duane-Hunt . X- X- . 2 . X- , X- .

    2. X- X-.

    X- K, L, M . X-

    2 / 14XRD

    2001-03-05http://phys.kookmin.ac.kr/~xray/xrd/xrd.html

  • 3 .

    . 3 X- .

    , , . , X- . K X- K . , L, M , . K L X- K, M X- K . K K . , L L, L, L, M M, M, M, M, M . K K1, K2 , K1 L , K2 L . 2:1 K1, K2 . X- (6) .

    (6)

    I , V , Vk . n2.

    3. X-

    1. , . , , , , , , , , , , , thin film .

    2. .

    3 / 14XRD

    2001-03-05http://phys.kookmin.ac.kr/~xray/xrd/xrd.html

  • . , (JCPDS card) .

    3. . d () .

    4. . 50-200 .

    5. . .

    6. . 7. . 8. .

    . , BaCo3 TiO2 BaTiO3 , .

    9. . , .

    10. . , . .

    11. . .

    12. .

    4. X-

    1) X- (GENERATOR)

    (1) X-

    l X- (Sealed type) : 1KW-3KW.

    l X- (Rotating anode) : . 12KW . tube .

    (2) , , , . X- 35

    4 / 14XRD

    2001-03-05http://phys.kookmin.ac.kr/~xray/xrd/xrd.html

  • .

    2) (GONIOMETER) :

    (1) X- . . 4 X- X , . X- X- (line focus) , X- .(. 5) (sollar slit) (divergence slit) X- , (receiving slit) (scattering slit) . 1/6 , 1/4 , 1/2 , 1 , 2 , 4 1 . 0.15 mm 0.3, 0.6 mm .

    . 4 Layout of X -ray diffractometer

    F: X- A : P : R :

    D : RP : S : SS :

    5 / 14XRD

    2001-03-05http://phys.kookmin.ac.kr/~xray/xrd/xrd.html

  • . 5

    (2) (Filter) X- target X-. Cu X- 6 3 peak, Ka1(1.54056 ), Ka2(1.5443 ), Kb(1.392 ) . 100 : 50 : 20 , X- Kb peak .( . 7) K target Ka Kb . target 1-2 Cu target Ni , Mo Zr, Fe Mn, Cr V .

    . 6 Cu X-

    6 / 14XRD

    2001-03-05http://phys.kookmin.ac.kr/~xray/xrd/xrd.html

  • . 7 Primary spectrum and absorption by a b-filter.

    (3) (Monochromator) (. 8) monochromator Ka Kb , background X- X-, X- . , Cu X- Fe K X- . monochromator CuKa FeKa, FeKb background 0 .

    7 / 14XRD

    2001-03-05http://phys.kookmin.ac.kr/~xray/xrd/xrd.html

  • . 8 The diffraction beam monochromator.

    3) (Electronic circuit panel) (1) : Xe, Kr, Ar (proportional counter) . (2) X- (PHA) .

    5. X-

    1) (1) (2) , , (3) X- (4) : Cu X- , X- (Ka1=1.5406 ) . X- X- X- background . X- . CuKa Fe Co Cu Fe Co . Fe Co . , Fe Co , X- Cu .

    8 / 14XRD

    2001-03-05http://phys.kookmin.ac.kr/~xray/xrd/xrd.html

  • 2) (1) , 10 - 30 mm . . . .

    (2) . polishing .

    (3) 55 mm . 40 mm X--- plate 2 . : data . X--- . , data .

    3)

    (1) (Scan axis) /2 : X- , 2 2 : () 2 ( 0.5-3 ) X- X- . : Rocking-curve , 2 ( )

    (2) (Scan type) (Continuous scan) : . . (Step scan) :

    9 / 14XRD

    2001-03-05http://phys.kookmin.ac.kr/~xray/xrd/xrd.html

  • . , .

    (3) (Scan range) , . JCPDS Card (2=5-140 ) , peak peak (2-3 ) . Wide angle goniometer 2=3-145 .

    (4) (Scan speed) , 4-5/min . 0.25-5/min , (8/min) . background .

    (5) (Sampling interval) (Step width) . 0.05 . 0.05 1 20 data .

    (6) (Power) X- , 4-5 . . Cu 30-50 kV , background . X-ray 40 kV, 40 mA , . peak background , .

    4) X- X- X- . X- . X- , , , . X- . X- . X- (window) , . X- , . , X- . 1 , 2 . , . X- X- , . 1 2 , 1 . X- , X- power X- . X- X- . X- , X- ,

    10 / 14XRD

    2001-03-05http://phys.kookmin.ac.kr/~xray/xrd/xrd.html

  • .

    6. X-

    1) - 2

    . 9 - 2

    , . 9 X- , X- 2 . 2 2 1/2 . 2=20- 60 , 10 1 11 , 2 20 2 22 , 30

    2 60 . Bragg's law( ) .

    . 10

    (1) . 10

    11 / 14XRD

    2001-03-05http://phys.kookmin.ac.kr/~xray/xrd/xrd.html

  • . (2) Si wafer . 11 .

    . 11

    (3) , , . . . 12 (100) .

    . 12 (100)

    2) 2 (Fixed - scan)

    12 / 14XRD

    2001-03-05http://phys.kookmin.ac.kr/~xray/xrd/xrd.html

  • . 13 2

    . 13 X- X- , 2 . =2, 2=20- 60 , 2 20 60 . . 14 X- , . peak .

    . 14 2

    3) (Fixed -2 scan, Rocking-curve) . 15 X- 2 . . 16 Rocking curve . Crystal M(. 15) X- , X-ray M X- . epitaxial , Pole-figure .

    13 / 14XRD

    2001-03-05http://phys.kookmin.ac.kr/~xray/xrd/xrd.html

  • . 15

    . 16

    4) - - 2 . , . 17 X- - . , .

    . 17 -

    14 / 14XRD

    2001-03-05http://phys.kookmin.ac.kr/~xray/xrd/xrd.html


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