Aula DRX

Difração de Raios-X
Caracterização de Materiais
Conrado Ramos Moreira Afonso

Departamento de Engenharia de Materiais (DEMa)
Centro de Ciências Exatas e de Tecnologia (CCT)
Universidade Federal de São Carlos (UFSCar)
*e-
*e-mail: conrado@ufscar.br
Programa Disciplina
Data Horá
Horário Local Descriç
Descrição Obs
11/03/11 14:00 – 17:40h 173/AT7 1 – Aula Introdutória Nascente
19/03/11 14:00 – 17:40h 173/AT7 2 – Aula nº 2 Ademar
25/03/11 14:00 – 17:40h 173/AT7 3 – Aula nº 3: Análise Térmica de Conrado/
Metais / Polímeros Ademar
15/04/11 14:00 – 17:40h 163/AT7 6 – Aula nº 6 Conrado

22/04/11 14:00 – 17:40h 163/AT7 Não haverá Aula Feriado
29/04/11 14:00 – 17:40h 163/AT7 7 – Aula nº 7: Difração de Raios-X Nascente/
(DRX) Conrado
20/05/11 14:00 – 17:40h 163/AT7 10 – Aula nº 10 Nascente
Programa Disciplina
Data Horá
Horário Local Descriç
Descrição Obs
20/05/11 14:00 – 17:40h 163/AT7 10 – Aula nº 10 Nascente
27/05/11 14:00 – 17:40h 163/AT7 11 – Aula nº 11: Microscopia de Nascente/
Força Atômica (AFM) Conrado
03/06/11 14:00 – 17:40h 163/AT7 1ª Avaliação Semestral P2
10/06/11 14:00 – 17:40h 163/AT7 Apresentação Seminário S1
17/06/11 14:00 – 17:40h 163/AT7 Apresentação Seminário S1
24/06/11 14:00 – 17:40h 163/AT7 2ª Avaliação Semestral (Sub) P3
Estudos de Casos de DRX

XRD patterns of La2-xCaxCuO4 perovskites; x- orthorhombic La2CuO4
x
x
x xx
Intensity (a.u.)
x x
x xx xx
x=0 x xxx
x=0.05
orthorhombic La2CuO4
x=0.10
x=0.15
tetragonal La2CuO4
x=0.20
0 10 20 30 40 50 60 70 80
2θ
P. Nascente et al. / to be submited to publication
REFINAMENTO DE RIETVELD DE AMOSTRAS DE BaTiO3
Padrão de DRX nas diferentes temperaturas de calcinação; (a) 1150°C; (b) 1000°C; (c) 900°C (d) 800°C (e)700°C. Os
símbolos * e # mostram os picos referentes ao carbonato de bário e ao dióxido de titânio, respectivamente.
Jorge Correa de Araú

Araújo et al. / X Enc Modelagem Computacional

EBSD and Micro-
Micro-XRD Study of CP-
CP-Ti
Grain orientationmapsrepresentedintermsoftheEulerangle y for the CPTi sample:(a) portion of the EBSD map with the region of
interest highlighted by the dashed box,(b) equivalent micro-XRD map of the region highlighted in the EBSD map.
Lynch et al., Nucl Instr Meth Phys Res A, 2010

EBSD and Micro-
Micro-XRD Study of CP-
CP-Ti
The {0002} and {10-10} pole figures for the micro-XRD (a) and (c), and EBSD data.

EBSD and Micro-
Micro-XRD Study
of CP-
CP-Ti
Euler angle distributions across Grain A

based on the EBSD and micro-XRD
measurements.

Estudos de Casos de DSC
Texture changes during annealing of electroplated Copper
XRD patterns for (a) polycrystalline copper of PCB substrate and (b) standard
polycrystalline copper powders (JCPDS 40-0836).
W.Q. Zhang et al. / Microelectronic Engineering 87 (2010) 2488–
2488–2494

XRD profiles at different stages of self-annealing, and

dependence of FWHM and NPI of (b) (2 2 0) and (c) (3 1 1)
peaks on time. ‘‘An” refers to electroplated copper
foils annealed at 120 C for 4 h immediately after deposition,
and ‘‘An*” refers to the foils annealed at 120 C for 4 h after
96 days storage at room temperature after deposition.

2488–2494
(a) EBSD orientation maps of electroplated copper foils annealed for 4 h at 120oC after
storage at room temperature for 96 days. (b) The orientation color key.
2488–2494

Microstructure–
Microstructure–property relationship in textured ZnO
SEM micrograph of the cross-section of R sample after sintering at 1100 C for 2 h. XRD
patterns of (a) 10T, (b) 0T and (c) R samples after sintering at 1100 C for 2 h.
I. Ozgur Ozer a, Ender Suvaci,
Suvaci, Slavko Bernik,
Bernik, Acta Materialia 58 (2010) 4126–
4126–4136
Microstructure–
SEM micrographs of (a) x- and (b) y-directions of 10T sample. Inner micrograph
at (b) shows Bi2O3-rich phase at a grain boundary at higher magnification.
4126–4136

Microstructure–
EBSD inverse pole figure maps of (a) R and 10T sample taken from (b) x-, (c) y- and (d) z-
directions. (e) Stereographic triangle
4126–4136
Strain tomography of polycrystalline zirconia dental
prostheses by synchrotron XRD
A.M. Korsunsky et al. / Acta Materialia 59 (2011) 2501–

2501–2513

The pattern of Debye–Scherrer rings recorded from the dental bridge under a 300 N nominal applied load. (b) The equivalent line profile
(intensity vs. scattering angle 2h) under a 300 N nominal applied load. The pattern was extracted from the diffraction pattern by “caking” over a 10
“slice” illustrated in (a).
2501–2513
The simulated bending (and tension) strain contour plot from the chosen section of the dental bridge
under a 300 N nominal applied load. (b) The result of strain tomography reconstruction of the bending
strain distribution within the same cross-section under a 300 N nominal applied load.
2501–2513

IMAGING BIOFILM IN POROUS MEDIA USING X-
X-RAY COMPUTED
MICROTOMOGRAPHY
Three-dimensional surface reconstructions of the polyamide bead at time t = 0 using BaSO4 as the contrast agent and
the biofilm (soft blue-green) and the polyamide bead (dark) at time t = 10 days.
DSC curves of water quenched Ti–24Nb–4Zr–7.5Sn alloy
In situ optical microstructure observation of

Ti–24Nb–4Zr–7.5Sn alloy WQ to (a) 20 and (b) −80 ◦C.
Y.L. Hao et al. / Materials Science and Engineering A 441 (2006) 112–
112–118

DSC curves of water quenched Ti–24Nb–4Zr–7.5Sn alloy
Y.L. Hao et al. / Materials Science and Engineering A 441 (2006) 112–
112–118
Estudos de Casos de DTA/TG
DTA and TG curves of Ti–6Al–2Sn–4Zr–2Mo nitrided at 950 °C for 5 h
A. Zhecheva et al. / Surface & Coatings Technology 201 (2006) 2467–2474

X-ray diffraction patterns of Ti–6Al–2Sn–4Zr–2Mo nitrided at 950 °C for 5 h

SEM micrograph of Ti–6Al–2Sn–4Zr–2Mo nitrided at 950 °C for 5 h

DSC curves of Ni50Ti47Ta3, Ni50Ti45Ta5, and Ni49Ti46Ta5 alloys
In situ optical microstructure observation of

Ti–24Nb–4Zr–7.5Sn alloy WQ to (a) 20 and (b) −80 ◦C.
C.W. Gong et al. / Materials Chemistry and Physics 96 (2006) 183–187

DSC traces obtained from Ti34Zr31Cu10Ni8Be17 ribbon
Y.C. Kim et al. /Materials Science and Engineering A 375–377 (2004) 749–753

XRD traces obtained from Ti34Zr31Cu10Ni8Be17 ribbon
Y.C. Kim et al. /Materials Science and Engineering A 375–377 (2004) 749–753
DSC of martensitic (a) and reverse (b) transformation in ribbon aged at 450◦C
J. MORGIEL et. at., JOURNAL OF MATERIALS SCIENCE 37 (2002) 5319 – 5325

DSC of martensitic (a) and reverse (b) transformation in ribbon aged at 450◦C
J. MORGIEL et. at., JOURNAL OF MATERIALS SCIENCE 37 (2002) 5319 – 5325

Ti-25Ni-25Cu
ribbon in situ
heating of the
ribbon first
aged at
450◦C/2 min.
and next
cooled to R.T.
Estudos de Casos de DTA

DTA curve for the dissolution of the sigma phase in Steel
K. H. Lo • C. H. Shek • W. W. Zhang, J Mater Sci (2010) 45:1790–1795

Estudos de Casos de DTA
C. Menapace et al., Nanostructured M300 maraging steel

Nanostructured Sintered M300 maraging steel
C. Menapace et al., Nanostructured M300 maraging steel, J Therm Anal Calorim (2010) 101:815–821
DSC scans for selected Fe–Cr–Nb–B alloys
J. Cheney, K. Vecchio / Materials Science and Engineering A 492 (2008) 230–235
Estudos de Casos de DSC/DTA

DTA scans for selected Fe–Cr–Nb–B alloys
J. Cheney, K. Vecchio / Materials Science and Engineering A 492 (2008) 230–235

XRD patterns of the as-milled powders FeCrMnN alloys
R. Amini et al. / Journal of Alloys and Compounds 480 (2009) 617–624

SEM micrographs of the as-milled powders FeCrMnN alloys / DSC

XRD patterns of annealed powders FeCrMnN alloys

OM and SEM images of annealed powders FeCrMnN alloys
P. Bassani, E. Gariboldi, and A. Tuissi, J. Therm. Anal. Cal., 80, 2005

Application of EBSD to Q&P Steels (Austenita Retida)
Grant Thomas, Microsc. Microanal. Page 1 of 6, 2011
Amorphous Iron Based Alloys

Viscosity (Poise)
1020 1012 107 104
Melted
Metal or
Alloy
Tm
Coarse Grains
- Refined Grains
> dT - Globular
dt - Dendrites
Metaestable
Tg Phases
Amorphous
Structure
Solidification x
Undercooling 1800%
Parameters related with GFA

CS Liga Fe83Zr3.5Nb3.5B9Cu1 (%at)
Pó “Overspray”
Overspray” Depó
Depósito
3000
2500 α -Fe Fe3Zr
Posição-2
2000 <5µm
Fe2Nb Fe2B
1500
5-20µm
Intensidade (cps)
1000
20-30µm
500
30-53µm
0
Posição-4
6000
5000 Fe-α
4000 180-250µm
3000
2000 Posição-0
1000
0 0
40 50 60 70 80 90 100 30 40 50 60 70 80 90 100 110
2θ (graus) 2 θ (graus)
DRX do Pó e do Depósito em Diferentes Posições em Relação ao Centro

CS Liga Fe83Zr3.5Nb3.5B9Cu1 (%at)
12 12
10 11
TC α --> γ
10
Fe = 770ºC TFe = 921ºC
8 9
P-1 = 748ºC TP-1 = 925ºC Fita
6 P-4 = 750ºC TP-4 = 937ºC 8
7 Amorfa
DSC (µV)
DSC (µ V)
4 6
2 5
Ferro Eletrolítico 4
0 3
-2 Depósito P-1 2 Pó "Overspray"
1
-4 Depósito P-4 0
-6 -1 Depósito
-2
500 550 600 650 700 750 800 850 900 950 1000 300 400 500 600 700 800 900
Temperatura (ºC) Temperatura (ºC)
DSC em Diferentes Posições do
Depósito e Fe Eletrolítico para DSC para a Fita Amorfa obtida por
Comparação das Temperaturas de “Melt-Spinning”, Pó “ Overspray”
Curie (Tc) e Transformação α → γ e o Depósito

CS Liga Fe63Nb10Al4Si3B20 (%at)
Pó “Overspray”
Overspray” Depó
Depósito
Fe-α
α α FeFe
Fe-α 23B6B
23 6
FeB
FeB FeNbB
FeNbB
α-Fe Fe23B6
150-180 µm
150-180 µm FeB FeNbB
Intensidade (u.a.)
Intensidade (u.a.)
45-75 µm
20mm
45-75 µm
5-20 µm
5-20 µm 1mm
Fita
Fita
Amorfa
Amorfa
20 25 30 35 40 45 50 55 60 65 70 75 80 85 90
2θ
θ2θ
(graus)
θ (graus) 2 θ (graus)
DRX do Depósito e do Pó “Overspray” em Diferentes Faixas Tamanhos
CS Liga Fe72Nb4Si10B14 (%at)
Pó “Overspray”
Overspray” Depó
Depósito
Fe-α Fe23B6 Fe-α Fe23B6
> 425 µm Fe2Nb Fe2B
e = 20 mm
250-425 µm
Intensidade (u.a.)
Intensidade (u.a.)
150-180 µm
75-106 µm
30-45 µm e = 1 mm
20-30 µm
e = 0,5 mm
5-20 µm
Fita Amorfa
Fita Amorfa
40 50 60 70 80 90 100 40 50 60 70 80 90 100
2 θ (graus) 2 θ (graus)
DRX do Depósito e do Pó “Overspray” em Diferentes Faixas Tamanhos

CS Liga Fe63Nb10Al4Si3B20 (%at)
Fe63Nb10Al4Si3B20 Fe72Si9,6Nb4B14,4
12
10 10
8 e = 20mm
5 e = 20 mm
6
e = 1mm %FA = 68% e = 1 mm %FA = 25%
DSC (µV)
DSC (µV)
4 0
e = 0,5 mm %FA = 100%
2
Fita Amorfa %FA = 100% -5
0 Fita Amorfa %FA = 100%
-2 -10
-4
-6 -15
-8
400 500 600 700 800 900 1000 -20
400 500 600 700 800 900 1000
Temperatura (ºC)
Temperatura (ºC)
DSC para a Fita Amorfa obtida por “Melt-Spinning” e para o Depósito

Fe63Nb10Al4Si3B20 Fe72Si9,6Nb4B14,4
100 100
90
90
% Fase Amorfa
% Fase Amorfa
80
80
70
60 70
50 60
40
50
30
MS 0 0 5 5 6 0 0 0 -- 0 0 5 5 6 0 0 5 5
5-2 20-3 30-4 45-7 75-10 06-15 50-18 >18 MS 5-2 20-3 30-4 45-7 75-10 06-15 80-25 50-42 >42
1 1 1 1 2
Fita MS / Faixa Granulométrica do Pó (µm) Fita MS / Faixa Granulométrica do Pó (µm)
DSC do Pó “Overspray” em Diferentes Faixas Granulométricas

e Gráfico da % de Fase Amorfa pela Faixa de Tamanho do Pó.

Fe83Zr3,5Nb3,5B9C Fe63Nb10Al4Si3B20 Fe72Si9,6Nb4B14,4
u1
MEV do Pó em Diferentes Faixas Granulométricas – Superfície

Fe83Zr3,5Nb3,5B9Cu Fe63Nb10Al4Si3B20 Fe72Si9,6Nb4B14,4
1
Fe2Nb
α-Fe
MEV do Pó em Diferentes Faixas Granulométricas – Seção Transversal

Fe83Zr3,5Nb3,5B9Cu Fe63Nb10Al4Si3B20 Fe72Si9,6Nb4B14,4
1 Base e = 1mm e = 1mm
Fe23B6
Fe23B6
Topo e = 20mm e = 0,5mm
Fe2Nb
Fe2B
MEV - BSE em Diferentes Posições em Relação ao Centro do Depósito

3 – Experimental Procedure
Melt-
Melt-Spinning Process
Advantages:
High Cooling Rates (106 K/s);
Low Quantities of Material (20 g) ;
Induction Coils
Crucible
Al2O3 Crucible
Copper
Wheel Liquid Metal Solidified Ribbon
or Alloy
θ
Melt-Spun Wheel
Ribbon Surface
Schematic Illustration of Melt-Spinning Process for

obtaining of Amorphous Ribbons.
In-Situ Crystallization –
Synchrotron Radiation
60
6 Heating Rate ~ 100 K/s Tv = TP4
Acquisition Time ~ 30 s 50
4
Tiv =
2 TP3 40
DSC (µV)
Time (min)
0 Tiii =
TP2 30
-2
20
-4
-6
Ti = 10
RT Tii =
TP1
-8 0
400 500 600 700 800 900 1000
Temperature (ºC)
DSC
10
6 Fe68Nb5Al4Si3B20
4
DSC (µ V) 2
-2
-4
-6
Fe63Nb10Al4Si3B20
-8
-10
400 500 600 700 800 900 1000
Temperature (ºC)
DSC analysis of melt-spun ribbons in as-quenched state and annealed state
for Fe73-xNbxAl4Si3B20 (x=5,10), respectively.
Difração de Raios-X (DRX)
Convencional Sincrotron In-

In-Situ
a b α-Fe FeNbB
Fe-α
FeNb Fe2B
FeB ? Unknown
NanocrystalLine
530ºC / 1h
Intensity (a.u.)
?
v ? ? ? ? ?? ? ??
iv
? ??
As-Quenched
iii
ii
i
25 30 35 40 45 50 55 60 65 70 75 80 85 90 30 40 50 60 70 80 90 100
2 θ (degrees) 2 θ (degrees)
Crystallization through XRD with Cu-Kα α (λ
λ = 1.54 nm) and Synchrotron
Radiation (λ λ = 1.77 nm) analysis of Fe68Nb5Al4Si3B20 alloy.
Difração de Raios-X (DRX)
Convencional Sincrotron In-

In-Situ
α-Fe Fe23B6 α-Fe FeNbB
a FeB FeNbB b FeB
850ºC iv
Intensity (a.u.)
iii
740ºC
680ºC ii
595ºC
As-Quenched i
25 30 35 40 45 50 55 60 65 70 75 80 20 25 30 35 40 45 50 55 60 65 70 75 80
Crystallization through XRD with Cu-Kα α (λ

λ = 1.54 nm) and Synchrotron
Radiation (λ λ = 1.77 nm) analysis of Fe63Nb10Al4Si3B20 alloy.
Microscopia Eletrônica
de Transmissão (TEM)
TEM analysis of melt-spun ribbons in as-quenched and annealed state

for Fe68Nb5Al4Si3B20 alloy.
Microscopia Eletrônica
de Transmissão (TEM)

Propriedades Magné
Magnéticas Moles
1,50
1,25
1,00
500ºC / 5'
Magnetic Indution, B (T)
0,75 As-Quenched
0,50
0,25
0,00
-0,25
-0,50
-0,75
-1,00
-1,25
-1,50
-6000 -4000 -2000 0 2000 4000 6000
Magnetic Field, H (A/m)
Propriedades Magné
Magnéticas Moles
0,8
0,6
Magnetic Induction, B (T)

590ºC / 10 min
0,4 As-Quenched
0,2
0,0
-0,2
-0,4
-0,6
-0,8
-3000 -2000 -1000 0 1000 2000 3000

Magnetic Field, H (A/m)

Propriedades Magné
Magnéticas Moles
Soft Magnetic Properties
Alloy (Condition) Bs (T) Hc (A/m) Br/Bs Pt (W/m3) µmáx
Fe68Nb5Al4Si3B20 (Amorphous) 1.19 45.0 0.25 42.0 13,300
Fe68Nb5Al4Si3B20 (500ºC / 5’) 1.38 18.0 0.26 14.0 25,200
Fe63Nb10Al4Si3B20 (Amorphous) 0.58 11.0 0.15 16.0 6,000
Fe63Nb10Al4Si3B20 (590ºC / 10’) 0.77 7.0 0.40 8.2 11,000
Magnetic properties Bs (T), Hc (A/m), Br/Bs, Pt (W/m3) and µmáx of

melt-spun ribbons in as-quenched state and annealed state
for Fe73-xNbxAl4Si3B20 (x=5,10), respectively.
In-Situ Aging Ti-Nb Alloys
Arc Furnace Melting
The Ti-Nb (25 and 30wt%Nb) alloys was prepared from high purity Ti
sheets (99.84%) and Nb pieces (99.99%) according to nominal
composition in an arc-melting furnace under vacuum and inert argon
atmosphere.
Observation
Vacuum Window
Sensor Pole
Vacuum
Pump
Water
Exit
Pole Water
Crucible Entrance
Water Water
Exit Entrance
Experimental Procedure
Water Quenching ≠ Cooling Rates
Schematic illustration of experimental apparatus for water

quenching of Ti-Nb cylindrical sample through different
cooling rates (~ Jominy Test)
Experimental Procedure
In-Situ Aging XRD through Synchrotron Radiation
Solution
Aging
Temperature
1000ºC
600ºC / 2 h
Aging
400ºC / 2 h FH
WQ
AC
FH
Troom 25ºC
Time
Schematic diagram of experimental steps for sample solution
heat treatment and in-situ aging at 400ºC and 600ºC/2 h using
synchrotron radiation for Ti-Nb alloys (WQ: water quenching;
FH: furnace heating at 50ºC/min; AC: air cooling).
Results
Chemical Composition
Nominal Measured wt%

Composition Nb content
Ti-25Nb 24.49 ± 0.30
Ti-30Nb 30.90 ± 0.33
Chemical composition of alloys was measured by X-ray

Fluorescence Spectrometry (Rigaku RIX 3100)
Results Thermal Profiles
1200
1000
Region I
Temperature (ºC) Region II
800 Region III
Region IV
600 Region V
Region VI
400
200
800 1000 1200 1400 1600 1800 2000 2200

Time (s)
Thermal profiles of each thermocouple positioned
along the cylindrical sample of Ti-25Nb alloy.
Ti-25Nb X-Ray Diffraction (XRD)
α" β α
Intensity (a.u.)
VI
IV
I
30 35 40 45 50 55 60 65 70 75 80 85 90
2 θ (degrees)
XRD patterns obtained through Cu-Kα α radiation of solution treated and
WQ through different cooling rates (I to VI) for Ti-25Nb alloy.
Ti-30Nb X-Ray Diffraction (XRD)
VI
V
Intensity (a.u.)
α"
IV
β
I
70 75 80 85
VI
IV
I
30 35 40 45 50 55 60 65 70 75 80 85 90
2 θ (degrees)
XRD patterns obtained through Cu-Kα α radiation of solution treated and
WQ through different cooling rates (I to VI) for Ti-30Nb alloy.
Ti-25Nb Scanning Electron Microscope
SEM (SE sign)
SEM micrographs of Ti-25Nb alloy quenched under a) slowest

and b) highest cooling rate showing α phase at grain boundaries,
α” martensite from GB of β grains and completely α” martensite
structure, respectively.
Ti-30Nb Scanning Electron Microscope
SEM (SE sign)
SEM micrographs of Ti-30Nb alloy quenched under c) slowest

and d) highest cooling rate showing α phase at GB and β
grains and a mixture of α” martensite and β phase.
Ti-25Nb In-Situ XRD Aging
α β α"
Intensity (a.u.)
600ºC / 2 h
Ti-25Nb
400ºC / 2 h
Troom
30 35 40 45 50 55 60 65 70 75 80 85 90
2 θ (degrees)
XRD patterns obtained through synchrotron radiation of WQ samples
aged in-situ at Troom, 400ºC/2 h and 600°°C/2 h for Ti-25Nb alloy.
α β
Intensity (a.u.)
α" ω
600ºC / 2 h
Ti-30Nb
400ºC / 2 h
Tamb
30 35 40 45 50 55 60 65 70 75 80 85 90
2 θ (degrees)
XRD patterns obtained through synchrotron radiation of WQ samples
aged in-situ at Troom, 400ºC/2 h and 600°°C/2 h for Ti-30Nb alloy.
600ºC / 2 h
Intensity (a.u.)
DETAIL 400ºC / 2 h Ti-30Nb
TROOM
30 40 50 60 70 80 90
2 θ (degrees)
XRD patterns in detail obtained through synchrotron radiation of
solution treated and water quenched samples aged in-situ at
room temperature, 400ºC/2 h and 600°°C/2 h for Ti-30Nb alloy.
CCT Diagrams
Ti-25Nb Ti-30Nb
Schematic CCT diagrams for a) Ti-25Nb and b) Ti-30Nb alloys
with the preview of phases formed (αα, β , α” e ω) according to
cooling rate and/or heat treatment (aging) imposed.
Conventional TEM (Low Mag.)
50 nm ω
TEM analysis of a) Ti-25Nb and b) Ti-30Nb water quenched alloys

showing bright field (BF) images with metastable ω phase, α”
martensite and β matrix together with respective SAPD for each phase.
Results Mechanical Properties
Elastic Modulus (GPa)

Alloy
Cooling Condition (Rate – K/s)
Composition
Furnace (0.05 K/s) Air Cooled (4 K/s) Quenched (160 K/s)
Ti-25Nb 87 ± 2 85 ± 2 77 ± 1
Ti-30Nb 95 ± 3 82 ± 1 89 ± 2
Results / Region I II III IV V VI

Alloys
Cooling Rate (K/s) 4.4 5.8 7.8 11.0 33.6 167.7
Microhardness (HV) 221 ± 5 225 ± 9 226 ± 9 241 ± 5 237 ± 7 238 ± 4
Ti-25Nb Phases Formed α, α”, β α, α”, β α, α”, β α, α”, β α”, β α”, β
Microhardness (HV) 218 ± 4 223 ± 5 225 ± 3 274 ± 5 286 ± 6 285 ± 3

Ti-30Nb Phases Formed β β β β, ω α”, β, ω α”, β, ω
Results and Discussion

X-Ray diffraction (XRD)
β β α
400oC 700oC
Intensity (a.u.)
300oC
600oC
200oC
Solubilized 8 2 ,2 8 2 ,4 8 2 ,6 8 2 ,8 500ºC
30 35 40 45 50 55 60 65 70 75 80 85 90 30 35 40 45 50 55 60 65 70 75 80 85 90
2θ (degrees) 2θ (degrees)
Ti-
Ti-35Nb-
35Nb-5Ta-
5Ta-7Zr
X-ray diffraction patterns obtained through Cu-Kα α (λ
λ = 1.54 Å) radiation of
solution treated and water quenched samples and aged at 200, 300 and
400, 500, 600 and 700°°C /4 h for Ti-35Nb-Ta-Zr alloy.
Phase Separation Ti-35Nb-5Ta-7Zr
SEM Optical Microscopy

a b
50 µm 25 µm
400ºC / 4h 700ºC / 4h
Aging up to 400ºC did not show α phase in the GB, but aging at greater
T = 700ºC / 4h presented intense grain boundary α precipitation (b),
which agrees with the fact that grain boundary act as α nucleation site.

Mechanical Property
350
Vickers hardness (HV)
325 Alloy 1
FERRANDINI et al.
300
Aging response of the
Ti-
Ti-35Nb-
35Nb-7Zr-
7Zr-5Ta and
275 Ti-
Ti-35Nb-
35Nb-7Ta alloys. J. of
Alloy 2
Alloys and Compounds,
250 v. 433, p. 207-
207-210, 2007.
225
200 300 400 500 600 700
o
Temperature ( C)
The maximum Vickers hardness (HV) for both alloys were obtained to
samples aged at 400ºC / 4h and the values are 336±
±9 and 317±
±13 HV
for alloys 1 and 2, respectively.
Synchrotron X-Ray diffraction (XRD)
β β'
Intensity (a.u.)
β
400ºC / 4 h
400ºC / 4 h
30 35 40 45 50 55 60 65 70 75 80 85 90 37,50 37,75 38,00 38,25 38,50 38,75 39,00

-X ray diffraction patterns obtained through synchrotron radiation

(λ
λ = 1.54 Å) of solution treated and water quenched samples aged at
400ºC/4 h for Ti- 35Nb - Ta- Zr alloy.

TEM Analysis
100 nm 20 nm
TEM bright field (BF) micrographs of Ti-35Nb-7Zr -5Ta alloy showing (a) grain
boundary (GB) and the absence of α phase and (b) microstructure at [111]β β
zone axis after homogenization followed by water quenching and annealing at
400ºC for 4 h, revealing contrast between β (dark) and β’ (bright) phases.
Alloy 1: Ti-
Ti-35Nb-
35Nb-5Ta-
5Ta-7Zr – Aged at 400º
400ºC / 4 h
Region Ti (wt%) Nb (wt%) Ta (wt%) Zr (wt%)

Bright - β 50.4 32.6 7.1 10.0
Dark - β’ 51.3 35.4 5.8 7.4
GB α 53.8 30.6 6.5 9.1
XEDS nanosized (3 nm) probe analysis of different

phase separation regions and grain boundary
showing chemical compositions (wt%).

HRTEM Analysis
[111] β
β β’
a β = 2.98 Å d110 β ' = 2.11 Å

a β’ = 3.28 Å d110 β = 2.32 Å
HRTEM image of Ti-35Nb-5Ta-7Zr alloy showing image and Fourier

space map of this regions at the [111]β zone axis. The Fourier space
map reveals the splitting of (110) reflections (white arrows).
FFT JEMS Simulation

(011)
(110)
(101)
β β’
d110 β ' = 2.11 Å

[111] β d110 β = 2.32 Å
Ti-bcc Ti-bct (β’)
(β) a = 3.0 Å
a = 3.3 Å c = 3.3 Å
FFT of HRTEM micrograph showing double spots indicating phase
separation of β and β’ phases and JEMS simulation of β and β’.
Geometric Phase Analysis (GPA)
Dislocations
GPA combined with HRTEM showing GPA showing localized strain map
variations of strain localized in (green= stretched, blue= compressed)
between domains of β and β’ phases associated with FFT spots (β
(β and β’)
e (%) Geometric Phase Analysis (GPA)

2 [111] β
0 (101)
-2
-4
-6 Strain Dislocations
-12 (%)
-8
-10
-12
-14
-16
0 2,5 5,0 7,5 10
Distance (nm)
Profile of Strain variation (%) or GPA showing localized strain map
distortion of lattice parameter in (1 0 1) (green= stretched, blue= compressed)
direction with Distance (nm) associated with FFT spots (β
(β and β’)
Geometric Phase Analysis (GPA)
Dislocation
(1 0 1)
( 1 1 0)
(0 1 1)
[111] β Strain Field

GPA combined with HRTEM showing GPA showing localized strain map
localized strain map around a around a dislocation generated to
dislocation.
dislocation. accommodate accumulated strain.

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