Sample (Crystal) Growth - mini-school
Transcript of Sample (Crystal) Growth - mini-school
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data
20/10/2020
Dr. Ross Colman
Sample (Crystal) Growth
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20/10/2020
Buddhist scripture from mid 5th C BC describe crystallisation of sea salt
Crystal Growth â has been around for a while
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Outline
Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
1. Motivation for Growing Single Crystals
2. Getting Atoms Moving
3. Practical Growth Methods
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Motivation for Growing Single Crystals
Structure Solution
Polycrystalline (powder)Single Crystal
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Motivation for Growing Single Crystals
Structure Solution
Polycrystalline (powder)Single Crystal
Inte
nsi
ty
2θ (°)
Detector
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Motivation for Growing Single Crystals
Structure Solution
Polycrystalline (powder)Single Crystal
3D structural data projected onto a 1D line
Only d-spacing and intensity information is retained
3D structural data projected onto a 2D surface
Symmetry equivalence of hkl reflections can be checked to determine the Laue class
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Motivation for Growing Single Crystals
Property Measurements
Crystallographic directions
FCC â NiMagnetocrystalline anisotropy
Resistivity, Magnetoresistance
Hall-effect
Thermal expansion
Thermal conductivity
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Outline
Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
1. Motivation for Growing Single Crystals
2. Getting Atoms Moving
3. Practical Growth Methods
![Page 9: Sample (Crystal) Growth - mini-school](https://reader031.fdocuments.us/reader031/viewer/2022013009/61cde93f6dd57f6a19518309/html5/thumbnails/9.jpg)
Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Getting Atoms Moving
Solid-State Reorganisation(T < Tmelt)
Melting(T > Tmelt)
Dissolving(T > Tsolvation)
Flux (reduced the energy barrier to reorganisation)
Efusion > Esolvation
Chemical transport(T < Tvap)
Solid
Liquid Gas
Sublimation/Condensation(T > Tvap)
Recrystallisation
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Getting Atoms Moving
Heating methods
Resistive heating- Standard box and tube furnaces
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Getting Atoms Moving
Heating methods
Arc discharge
S. Fashu, M. Lototskyy, et al., Mater. Des. 186, 108295 (2020).
Resistive heating- Standard box and tube furnaces
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Getting Atoms Moving
Heating methods
Arc discharge
Resistive heating- Standard box and tube furnaces
Induction heating
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Getting Atoms Moving
Heating methods
Arc discharge
Resistive heating- Standard box and tube furnaces
Induction heating
Optical (IR) heating
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Getting Atoms Moving
Arc discharge
Resistive heating- Standard box and tube furnaces
Induction heating
Optical (IR) heating
Laser (IR) heating
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Getting Atoms Moving
Arc discharge
Resistive heating- Standard box and tube furnaces
Induction heating
Optical (IR) heating
Laser (IR) heating
Laser diode
Sample
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Outline
Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
1. Motivation for Growing Single Crystals
2. Getting Atoms Moving
3. Practical Growth Methods
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Solid State Sintering
(T < Tmelt)
Long time
Pros:Relative simplicity
Cons:Long times required
Small crystals
Crystal isolation is tricky
F. Scheibel, B. Zingsem, et al., Phys. Rev. Mater. 3, 54403 (2019).
Mn3GaC
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Recrystallising from a melt
(T > Tmelt)
Slow-cool
Pros:Relative simplicity
Cons:Limited control of nucleation
Orientation control not possible
Only works for congruently melting materials
CuMnAsJ. VolnĂ˝, D. Wagenknecht, et al., Electrical Transport Properties of Bulk Tetragonal CuMnAs, Phys. Rev. Mater. 4, 064403 (2020).
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Recrystallising from a melt: Directional solidification: Bridgeman-Stockbarge
Heating elements
Sample
Temperature gradient within the furnace
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Recrystallising from a melt: Directional solidification: Bridgeman-Stockbarge
Tem
per
atu
re
Time
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Recrystallising from a melt: Directional solidification: Bridgeman-Stockbarge
Tem
per
atu
re
Time
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Recrystallising from a melt: Directional solidification: Bridgeman-Stockbarge
Tem
per
atu
re
Time
Pros:Relative simplicity
Some control of nucleation
Large crystals possible
Cons:Orientation control not possible
Only works for congruently melting materials
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Recrystallising from a melt: Directional solidification: Bridgeman-Stockbarge
(with seed)
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Recrystallising from a melt: Directional solidification: Bridgeman-Stockbarge
(with seed)
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Recrystallising from a melt: Directional solidification: Bridgeman-Stockbarge
(with seed)Pros:Seed orientation control
Large crystals possible
Cons:Only works for congruently melting materials
Complexity is increased
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Recrystallising from a melt: Czochralskii pulling
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Recrystallising from a melt: Czochralskii pulling
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Recrystallising from a melt: Czochralskii pulling
Tri-Arc melting Resistance heater melting
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Recrystallising from a melt: Czochralskii pulling
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Recrystallising from a melt: Czochralskii pulling
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Recrystallising from a melt: Czochralskii pulling
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Recrystallising from a melt: Czochralskii pulling
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Recrystallising from a melt: Czochralskii pulling
Pros:Seed orientation control
Large (long) crystals possible
Minimised vessel contamination
Cons:Time consuming and complex
Not suitable for incongruently melting materials
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
A material is described as incongruently melting- if the solid crystallises with a different composition from the melt.
Melt
Crystallising solid
e.g. If the melt has composition
Ni50Mn28.5Ga21.5
the crystallising solid will have composition
~ Ni50.5Mn26.8Ga22.7
The ratio between melt concentration and solid concentration is known as the partition coefficient,
For Ni-Mn-Ga, these are known to be:
kNi ~ 1.04kMn ~ 0.88kGa ~ 1.09đ =
đđ đđđđ
đđđđđĄ
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
D. L. Schlagel et al. J. Alloys Compd. 312, 77 (2000).
đđ (đ) = đđ0(1 â đ)đâ1
Fraction solidified
Initial concentration
Partition coefficient
Scheil E. Z Metall 34 (1942) 70.
As the solid forming has a different composition to the melt, the composition of the melt changes during the growth.
A formula to describe the composition change was put forward by Scheil in 1942 â now known as the Scheil-Gulliver equation:
Crystalizing concentration
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
kMn = 0.88
D. L. Schlagel et al. J. Alloys Compd. 312, 77 (2000).
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
kMn = 0.88
D. L. Schlagel et al. J. Alloys Compd. 312, 77 (2000).
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
kMn = 0.88
D. L. Schlagel et al. J. Alloys Compd. 312, 77 (2000).
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Recrystallising from a melt: Directional solidification: Floating-zone
Halogen bulb, heating by IR light
Parabolic mirror
Focal point of 4x bulbs and mirrors
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Recrystallising from a melt: Directional solidification: Floating-zone
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Recrystallising from a melt: Directional solidification: Floating-zone
![Page 42: Sample (Crystal) Growth - mini-school](https://reader031.fdocuments.us/reader031/viewer/2022013009/61cde93f6dd57f6a19518309/html5/thumbnails/42.jpg)
Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Recrystallising from a melt: Directional solidification: Floating-zone
![Page 43: Sample (Crystal) Growth - mini-school](https://reader031.fdocuments.us/reader031/viewer/2022013009/61cde93f6dd57f6a19518309/html5/thumbnails/43.jpg)
Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Recrystallising from a melt: Directional solidification: Floating-zone
Pros:Orientation control possible
Suitable for incongruently melting materials
Minimal vessel contamination
Cons:Complex setup
Not possible for volatile compounds
Er2Ti2O7K. VlĂĄĹĄkovĂĄ, P. Proschek, et al., J. Cryst. Growth 546, 125784 (2020).
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Recrystallising from a melt: Directional solidification: Floating-zone
Pros:Orientation control possible
Suitable for incongruently melting materials
Cons:Complex setup
Not possible for volatile compounds
đđ (đ) = đ0 1 â (1 â đ)đ(âđđđ )
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Recrystallising from a melt: Directional solidification: Floating-zone
Pros:Orientation control possible
Suitable for incongruently melting materials
Cons:Complex setup
Not possible for volatile compounds
đđ (đ) = đ0 1 â (1 â đ)đ(âđđđ )
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Recrystallising from a melt: Directional solidification: Floating-zone
Pros:Orientation control possible
Suitable for incongruently melting materials
Cons:Complex setup
Not possible for volatile compounds
đđ (đ) = đ0 1 â (1 â đ)đ(âđđđ )
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Flux growth
(T > Tsolvation)
Flux choice:
Low melting point
Capable of dissolving chosen material
Un-reactive (towards compound)
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Flux growth
Pros:Simple
Incongruently melting materials can be prepared
Cons:Flux choice can be difficult
Nucleation is not controlled
Sample must be separated from the flux
Sample can be contaminated by flux
(T > Tsolvation)
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Hydrothermal (Flux = water) growth
Water (+ mineralising agent)
Îł-Cu3Mg(OH)6Cl2R. H. Colman, A. Sinclair, et al., Chem. Mater. 23, 1811 (2011).
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Îł-Cu3Mg(OH)6Cl2
Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Hydrothermal (Flux = water) growth
Pros:Simple
Materials that decompose before melting can be prepared
Cons:Many parameters to test:
⢠Temperature (and ramp)⢠Concentration(s)⢠Mineralising agent⢠Fill level (pressure)
R. H. Colman, A. Sinclair, et al., Chem. Mater. 23, 1811 (2011).
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Chemical transport
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Chemical transport
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Chemical transport
Transport agente.g. I2 , Cl2 , O2, S, AlCl3
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Chemical transport
![Page 55: Sample (Crystal) Growth - mini-school](https://reader031.fdocuments.us/reader031/viewer/2022013009/61cde93f6dd57f6a19518309/html5/thumbnails/55.jpg)
Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Chemical transport
![Page 56: Sample (Crystal) Growth - mini-school](https://reader031.fdocuments.us/reader031/viewer/2022013009/61cde93f6dd57f6a19518309/html5/thumbnails/56.jpg)
Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Chemical transport
![Page 57: Sample (Crystal) Growth - mini-school](https://reader031.fdocuments.us/reader031/viewer/2022013009/61cde93f6dd57f6a19518309/html5/thumbnails/57.jpg)
Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Chemical transport
![Page 58: Sample (Crystal) Growth - mini-school](https://reader031.fdocuments.us/reader031/viewer/2022013009/61cde93f6dd57f6a19518309/html5/thumbnails/58.jpg)
Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Chemical transportPros:Large, high quality crystalsCompounds can be volatile
Cons:Many parameters to test:
⢠Temperature (and gradient)⢠Concentration(s)⢠Transport agents
Slow process
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Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Getting Atoms Moving
Solid-State Reorganisation(T < Tmelt)
Melting(T > Tmelt)
Dissolving(T > Tsolvation)
Flux (reduced the energy barrier to reorganisation)
Efusion > Esolvation
Chemical transport(T < Tvap)
Solid
Liquid Gas
Sublimation/Condensation(T > Tvap)
Recrystallisation
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Conclusions
Czech-Bavarian Mini-School 2020 on Large Scale Facilities and Open Data20/10/2020
Practical Growth Methods
Solid Liquid Gas
⢠Chemical transport
⢠Condensation
⢠Melt
⢠Bridgeman-Stockbarge
⢠Czochralskii
⢠Floating zone
⢠Flux
⢠Hydrothermal
⢠Solid state reorganisation