10 /16/2014 Soon Ho Kwon Computational Materials Science lab. KAIST MS213 Crystallography and Diffraction.

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10 /16/2014 Soon Ho Kwon Computational Materials Science lab. KAIST MS213 Crystallography and Diffraction

X-ray X-Rays are part of the spectrum of electromagnetic radiation occupying the region between the ultraviolet and gamma rays. The wavelengths of X-radiation commonly used for x-ray diffraction lie between 0.7 and 2.3 Å. Cu Kα is 1.54Å.

X-ray A high voltage power source is connected across cathode and anode to accelerate the electrons. The X-ray spectrum depends on the anode material and the accelerating voltage.

X-ray Continuous X-rayCharacteristic X-ray

X-ray

Filter for characteristic X-ray

Bragg’s law nλ=2dsinθ : Bragg’s Law CB+BD=dsinθ + dsinθ = 2dsinθ

Interference of Waves

Basic Features of Typical XRD Experiment

Detection of Diffracted X-rays

A Modern Automated X-ray Diffractometer

 General mode  Angle of X-ray and sample = θ Angle of X-ray and detector = 2 θ diffraction only planes parallel to sample surface  Preferred orientation θ/2θ scan (coupled mode)

 Angle of X-ray and sample = α fixed (constant, 2~3 o ), Angle of X-ray and detector = 2 θ increase the X-ray dose rate in sample surface protect the detector from strong peak from substrate  No preferred orientation θ fixed, 2θ scan (glancing XRD)

 Angle of X-ray and sample = θ Angle of X-ray and detector = 2θ fixed Orientation of sample  Crystallinity is better as FWHM(full width at half maximum) is smaller. 2θ fixed, θ scan (rocking curve) Cu Kα Cu Kα + Cu Kβ

 Fundamentally, similar method to θ/2θ mode  Angle of X-ray and sample = θ Angle of X-ray and detector = θ Applicable for powder, liquid sample θ/θ scan

D-spacings and lattice parameters

JCPDF card

XRD Pattern of NaCl Powder

Nondestructive method Easily getting lattice parameter Determination of small crystallite size Easy to operate Qualitative analysis Quantitative analysis Phase, crystallinity, preferred orientation Merits of XRD measurement

일정실험 / 실습 내용장소구분 1 주 (9 월 4 일 ) 실습 소개 및 조 편성 응용공학동 (W1) 2427 호 단체 2 주 (9 월 11 일 ) 결정구조 모형 (BCC, FCC) 응용공학동 (W1) 2427 호 단체 3 주 (9 월 18 일 ) 결정구조 모형 (HCP, Diamond Cubic) 응용공학동 (W1) 2427 호 단체 4 주 (9 월 25 일 ) 결정구조의 이해 및 회절 응용공학동 (W1) 2427 호 단체 5 주 (10 월 2 일 ) 결정구조의 이해 및 회절 응용공학동 (W1) 2427 호 단체 6 주 (10 월 9 일 ) 한글날 7 주 (10 월 16 일 ) 예비 응용공학동 (W1) 2427 호 단체 8 주 (10 월 23 일 ) 중 간 고 사중 간 고 사 응용공학동 (W1) 2427 호 9 주 (10 월 30 일 ) TEM 의 소개 및 실습 KARA 조별 (A) 10 주 (11 월 6 일 ) TEM 의 소개 및 실습 KARA 조별 (B) 11 주 (11 월 13 일 ) X-ray diffractometer 의 소개 응용공학동 (W1) 2427 호 단체 12 주 (11 월 20 일 ) X- 선 회절 분석 KARA 조별 (A) 13 주 (11 월 27 일 ) X- 선 회절 분석 KARA 조별 (B) 14 주 (12 월 4 일 ) 고분해능 / Pole-figure X- 선 회절 분석 응용공학동 (W1) 2427 호 단체 15 주 (12 월 11 일 ) 예비 응용공학동 (W1) 2427 호 단체 16 주 (12 월 18 일 ) 기말고사 응용공학동 (W1) 2427 호 Schedule