crystal quality measurement by ebsd - home | jefferson lab · 2016-03-15 · ced-047 ced-046...
TRANSCRIPT
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Crystal Quality Measurement
on Niobium Materials
Xin Zhao, L. Phillips, C. Reece, Jefferson Lab
Qiguang Yang, D.A. Temple, Norfolk State University
M. Krishnan, C. James, Alameda Applied Science Corporation (AASC)
1
X.Zhao et al, Talk on 5th SRF Thin Film Workshop, JLab. 2012
The work at AASC was supported by DOE Grant # DE-FG02-08ER85162. This research is also funded by
Jefferson Science Associates, LLC under U.S. DOE Contract No. DE-AC05-06OR23177. The U.S. Government
retains a non-exclusive, paid-up, irrevocable, world-wide license to publish or reproduce this manuscript for U.S.
Government purposes.
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Crystal Quality – a definition based on crystallography
• Ref. “Elements of X-ray Diffraction”, B.D. Cullity. 2nd edition, page 260. 2
X.Zhao et al, Talk on 5th SRF Thin Film Workshop, JLab. 2012
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Outline • Crystal Quality Measurement by EBSD
– “Image Quality” and “Misorientation Angles”
as figure-of-merits
– Surveying AASC Nb Films
– Surveying bulk Nb and MgB2 Epitaxy film
• Crystal Quality Measurement by XRD
– Introduction of Pole Figure and Reciprocal
Space Mapping (RSM) techniques
– RSM Experimental Data on film and bulk Nb
• Summary
• Acknowledge
• Questions X.Zhao et al, Talk on 5th SRF Thin Film Workshop, JLab. 2012
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Crystal Quality Measurement
by EBSD
Image Quality and Misorientation Angles
as Figure-of-Merits
4
X.Zhao et al, Talk on 5th SRF Thin Film Workshop, JLab. 2012
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Misorientation Angles - as a caliber of crystal quality
• Misorientation Angles of a survey area could be measured by XRD (Rocking Curve, RSM), or by EBSD
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X.Zhao et al, Talk on 5th SRF Thin Film Workshop, JLab. 2012
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EBSD Image Quality (I.Q.) parameter - as a caliber of crystal quality
• Ref. “EBSD Indexing Tutorial”, Lecture Handout from EDAX/TSL company.
Recrystallized grain Deformed grain
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X.Zhao et al, Talk on 5th SRF Thin Film Workshop, JLab. 2012
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Nb Thin Film Samples
Sample CED-47 CED-46 CED-38
Thickness ~60 nm ~120 nm ~800 nm
RRR 46 62 136
Tc (K) 8.95 9.14 9.20
• The samples were coated by cathodic-arc deposition at
AASC(CEDTM)
• Substrates are magnesium-oxide crystal, with MgO(100) in-plane
• Before coating, the substrates were annealed at 7000C; The
substrate temperate was set at “5000C” during Nb thin film
deposition. Note as, “7000C/5000C”
• The films are single crystals with epitaxial relationship,
Nb(100)//MgO(100) 7
X.Zhao et al, Talk on 5th SRF Thin Film Workshop, JLab. 2012
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EBSD Measurement (I)
Sample CED-47 CED-46 CED-38
Avg. C.I. 0.67 0.72 0.90
Avg. I.Q. 1121 1003 2101
Avg. Miso. Angle 0.18’ 0.20’ 0.15’
CED-047 CED-046 CED-038
EBSD Survey Area: 250X250 um, Step10 um. The bottom pic. are Inverse Pole Figures.
IPF grayscale are rendered by the same I.Q. value: [min,max] = [500, 2100]
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Sample CED-47 CED-38
Avg. I.Q. 1121 2101
Avg. Miso. Angle 0.18’ 0.15’
RRR 46 136
Crystal quality progressively evolves
on film thickness
CED-38
CED-47 EBSD I.P.F.
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Misorientation Angle [degrees]
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Misorientation Angle [degrees]
EBSD Measurement (II)
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Misorientation Angle [degrees]
CED-046 CED-038
Sample CED-47 CED-46 CED-38
Avg. Miso. Angle 0.18’ 0.20’ 0.15’
CED-047
• Average misorientation angles have small
change , if compared by Image Quality (I.Q.)
index.
• Higher RRR sample has a slightly smaller Avg.
Miso. Angle (0.15’) 10
X.Zhao et al, Talk on 5th SRF Thin Film Workshop, JLab. 2012
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Comparison to BCP Nb bulk samples
Mean values of the local average misorientation
distributions, obtained from the EBSD data on
each grain for all the samples (black circles) and
average density of pits measured on each grain
for six samples (red squares). Samples with
more than one grain have multiple points in the
plot, corresponding to the different
misorientation angle distributions for each grain.
Sample CED-47 CED-46 CED-38
Avg. Miso. Angle 0.18’ 0.20’ 0.15’
EBSD survey of 12 bulk Nb samples (BCP’ed and cut from a SRF cavity)
Smallest Avg. Miso. Angle is ~0.150 I.P.F.
and Legend
Citation from: Xin Zhao, G. Ciovati, and T. R. Bieler, Phys.
Rev. ST Accel. Beams 13 (12), 124701 (2010).,
“Characterization of etch pits found on a large-grain bulk
niobium superconducting radio-frequency resonant cavity”
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Comparison to a MgB2 Epitaxial Film
– from Temple .U. (Prof. Xi’s group) EBSD Inverse Pole Figure
Average CI is 0.56 (0.086…0.743), Avg IQ=997,
Grayscale: [0.1, 0.743]; Avg Misorientation: 0.280
Sample: “1109C”, MgB2/C-plane sapphire
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Comparison Chart
• EBSD Survey Area 200X200um.
X.Zhao et al, Talk on 5th SRF Thin Film Workshop, JLab. 2012
13
Sample
MgB2 CVD
Epitaxy
Film
Bulk Nb Nb Film
(CED-38)
Avg. Miso. Angle 0.280 0.150 0.150
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Crystal Quality
Measurement by XRD
Introduction of Pole Figure and
Reciprocal Space Mapping (RSM)
techniques
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Outline • Crystal Quality Measurement by EBSD
• Crystal Quality Measurement by XRD
– Introduction of Pole Figure and Reciprocal
Space Mapping (RSM) techniques
– RSM Experimental Data
• Probing a Nb Film
• Probing a Single Crystal Bulk Nb
• Probing a Polycrystalline Bulk Nb
• Summary
• Acknowledge
• Questions
X.Zhao et al, Talk on 5th SRF Thin Film Workshop, JLab. 2012
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Real Lattice vs. Reciprocal Lattice
http://leung.uwaterloo.ca/CHEM/750/L
ectures%202007/SSNT-3-
Surface%20Structure%20II.htm
R space is also known as momentum space or k-space
Lattice Transformation: XRD Diffraction and Reciprocal Lattice
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Source:
http://aluminium.matter.org.uk/c
ontent/html/eng/0210-0010-
swf.htm
Pole Figure – exploring the Texture of crystallites
Equatorial Plane is viewed from
top to form stereographic
projection (Pole Figures)
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XRD Pole Figure Experimental Setup
and Standard Nb (110) Pole Figure • Nb (110) Pole Figure
(011)(101)
(101) (011)
109.480
70.520
Nb
600
900
(110) φ
ψ(110)
Crystal Plane ψ (0) φ (0)
(110) 0 0
(011) 60 54.74
(101) 60 125.26
(1,0,-1) 60 234.74
(0,1,-1) 60 305.26
(1,-1,0) 90 180
(-1,1,0) 90 0
1
•Fixed 2θ of a {hkl} crystal plane. (Bragg Law 2d{hkl}*sin(θ)=λ)
•Rotated around Normal Direction (Azimuthal φ, from 0-3600 )
•Titled off-angle from Normal Direction (ψ, 0-900)
Experimental Steps:
P.F. is to visualize Reciprocal Lattice Space
One Crystal Plane in real lattice space is a Pole in
reciprocal space 18
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Reciprocal Space Mapping (RSM)
Ref. Ni et al “X-ray reciprocal space mapping studies of strain relaxation
in thin SiGe layers”, J. Crystal Growth 227-228 (2001), 756-760.
RSM is a well established XRD technique.
RSM Experimental Results
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Reciprocal Space Mapping
- XRD Experimental Setup WORK STAGES:
1. Set ω0, 2θhkl
2. Run θ/2θ mode scan,
3. Slightly change ω0 . Set ω1,2θhkl
4. Run θ/2θ mode scan
n. …Plot diff(ω) vs. diff(θ)
Use Detector(1)
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X.Zhao et al, Talk on 5th SRF Thin Film Workshop, JLab. 2012
2dhkl sin(θhkl) = λcu
ΔdNb(110)=-1.871*ΔθNb(110)
For ΔθNb(110) = 0.10
Δd/dNb(110) *100% =8%
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XRD Bragg-Brentano Scan
Time/Step 0.20 sec; Step size: 0.030 21
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XRD RSM Experimental Data
Samples:
A High RRR Nb Film
CMP’ed Bulk Nb Coupons
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Outline • Crystal Quality Measurement by EBSD
• Crystal Quality Measurement by XRD
– RSM Experimental Data
I. Probing a Nb Film
II. Probing a Single Crystal Bulk Nb
III. Probing a Polycrystalline Bulk Nb
• Summary
• Acknowledge
• Questions
X.Zhao et al, Talk on 5th SRF Thin Film Workshop, JLab. 2012
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RSM Data I. Survey a Nb Film
• AASC Nb Thin Films “CED-34”, on MgO
crystal substrate. MgO(100) in-plane.
• Thickness: ~ 1.6 um (3000 arc-pulse)
• Epitaxial Relationship (“Op” - type),
Nb(100)//MgO(100), Nb[100]//MgO[110]
• RRR = 277, Tc=9.21-9.25K
• Pre-coating Substrate Heat-Treatment
T=7000C
• Substrate temperature in coating T=5000C 24
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Preparation Before RSM Through Pole Figure Simulation and k-space Analysis,
Select Pole (231) for RMS
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[Cont.] I.Probing Different Film Thickness
by Varying X-ray Incident Angle
• High Incident Angle (ω = 60.90):
– Probing Depth (if for a bulk Nb, 3645 nm): entire film (1.6 um)
• Low Incident Angle:(ω = 3.090):
– Probing Depth: 430 nm
• Definition of penetration depth
t = sina/m
With a the incident angle and m = 1259 is the absorption coefficient of Nb at 0.154 nm.
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RSM Probing Film’s Top-layer
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RSM Probing Entire Film
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#1. High Incident Angle
RSM probes entire film
thickness (1.6 um)
(Probing Depth 3.6um if
bulk Nb)
Δω = ~ 0.60
Δ θ = ~ 0.20
#2. Low Incident Angle
RSM probes film top-layer
(Probing Depth 430nm )
Δω = ~ 0.10
Δ θ = ~ 0.10
168
4085
Sample: CED-34
RSM Survey
on Plane/Pole (231)
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Crystal Quality Evolution of Epitaxy Growth
RSM of Top-layer
RSM probing
interface?
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RSM Data II. Survey a Nb Single
Crystal Bulk Material
• A Single Crystal Bulk Nb Coupon Sample
• Chemical-Mechanical Polished (CMP’ed)
by ATI Wah ChangTM, then Buffered
Chemical Polished (BCP’ed) ~2micron.
Mirror Finished (Rq ~40nm)
• Orientation: Nb(110) in-plane.
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Pole Figure of the Single Crystal Nb • Nb {110}
Pole Figure
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-0.4 -0.3 -0.2 -0.1 -0.0 0.1 0.2 0.3 0.4Omega/2Theta
-0.4
-0.3
-0.2
-0.1
-0.0
0.1
0.2
0.3
0.4
Omega
0 Omega 20.530102Theta 38.55100
Phi 0.00Psi -8.12
X 0.00Y 0.00Z 5.039
Reciprocal Batch_1_0.xrdml
1.5
2.4
4.0
6.6
10.8
17.7
29.1
47.9
78.7
129.3
212.5
349.3
574.0
943.4
1550.3
2547.9
4187.2
6881.2
11308.7
18584.8
30542.4
RSM Probing a Bulk Nb from
top to 4 um deep layer
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-0.4 -0.2 0.0 0.2 0.4Omega/2Theta
-0.5
-0.4
-0.3
-0.2
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-0.0
0.1
0.2
0.3
0.4
0.5Omega
0 Omega 19.275502Theta 38.55100
Phi 69.34Psi 83.02
X 0.00Y 0.00Z 4.686
Reciprocal Space Mapping (110).xrdml
1.2
1.7
2.3
3.2
4.4
6.0
8.2
11.2
15.4
21.1
28.9
39.6
54.3
74.4
102.0
139.8
191.7
262.8
360.2
493.7
676.8
RSM Probing a Bulk Nb Top-layer
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Sample: CMP’ed Nb
Single Crystal Bulk
Material
Probing Top&Deep Layer
(High Incident Angle, ~200)
Δω = ~ 0.10
Δ θ = ~ 0.10
-0.4 -0.2 0.0 0.2 0.4Omega/2Theta
-0.5
-0.4
-0.3
-0.2
-0.1
-0.0
0.1
0.2
0.3
0.4
0.5Omega
0 Omega 19.275502Theta 38.55100
Phi 69.34Psi 83.02
X 0.00Y 0.00Z 4.686
Reciprocal Space Mapping (110).xrdml
1.2
1.7
2.3
3.2
4.4
6.0
8.2
11.2
15.4
21.1
28.9
39.6
54.3
74.4
102.0
139.8
191.7
262.8
360.2
493.7
676.8
RSM Survey
on Plane/Pole {110}
Probing Top-Layer only
(Low Incident Angle, ~80)
Δω = ~ 0.60
Δ θ = ~ 0.20
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Crystal Quality Evolution of
a Bulk Nb sample
RSM of Top-layer
RSM of bulk
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RSM Data III. Survey a Nb
Polycrystalline Bulk Material
• A Fine-grain Polycrystal Nb
• Grain size ~50 microns
• CMP’ed , then BCP’ed ~2micron.
• No preferred Orientations
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Nb {110} Pole Figure Sample:
CMP+2 um BCP’ed
Nb Fine-grain polycrystal Bulk Material
X.Zhao et al, Talk on 5th SRF Thin Film Workshop, JLab. 2012
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Probing Top&Deep Layer
(High Incident Angle
Omega 19.270 )
Probing Top Layer only
( Low Incident Angle
Omega 1.50 )
Sample:
CMP+2 um BCP’ed
Nb Fine-grain polycrystal Bulk Material
X.Zhao et al, Talk on 5th SRF Thin Film Workshop, JLab. 2012
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Summary
• 1. Crystal quality of epitaxy film progressively
evolves on Growth Thickness (Verified by EBSD
and XRD-RSM).
• 2. Reciprocal Space Mapping (RSM) is an non-
destructive technique to probe crystal quality of
film or bulk Nb, via 2-D mapping of crystal mis-
orientation angle (ω) & crystal plane distance
(dhkl)
• Besides ω, RSM discerns dhkl
• 4. Top-layer and deep-layer Nb film/bulk have
obvious crystal quality difference.
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Implication to Structure Zone Model - microstructure evolution along thickness
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Grayscale mask renders Anders’ SZM to visualize crystal
quality
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“Top-down” vs “Bottom-up”
- Crystal Etching vs Growth
- Bulk vs Film
X.Zhao et al, Talk on 5th SRF Thin Film Workshop, JLab. 2012
42
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Acknowledge
• Colleagues of Jefferson Lab, who provided
the samples, enlightening advices and
critical thoughts: Hui Tian, Anna-Marie,
Josh ……
• Collaborators from FSU, Zuhawn et al
• Collaborators from NCSU, Fred, et al
• Collaborators from WM
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Questions to You 1. Why crystal quality progressively evolves on
growth thickness (for Epitaxy Energetic
Condensation Film) ? strain/stress relaxation,
“Subplantation” outward growth…?
2. Will crystal quality of Fiber-Columnar Film also
evolves along growth thickness?
3. What is the optimal thickness for Fiber Growth
Film?
4. Besides Crystal Quality, Is a way to measure
“Grain Boundary Quality”?
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Appendix
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Energetic Condensation – Deposition of
“Hyperthermal Ions”
SRIM simulation shows penetration depth: 0 - 0.2nm 46
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Three-dimensional epitaxy
relationship of Nb/MgO(100)*
• Illustration of three types
Nb/MgO(100) epitaxial relationship,
as proposed by Hutchinson et al *.
Orientation: Op
Top
View
F O
Cross-section View1. *E. Hutchinson and K. H. Olsen, “Substrate Condensate Chemical Interaction and the Vapor Deposition of
Epitaxial Nb Films”, J. Appl. Phys. 38, 4933 (1967).
2. J. E. Mattson, Eric E. Fullerton, C. H. Sowers, and S. D. Bader, “Epitaxial growth of body-centered-cubic
transition metal films and superlattices onto MgO (111), (011), and (001) substrates”, J. Vac. Sci. Technol.
A 13, 276 (1995).
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