Athena S. Sefat. mm scale Flux Method for Preparing Crystals. Main Group Compounds. Division of Materials Sciences and Engineering
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1 mm scale Flux Method for Preparing Crystals Main Group Compounds Athena S. Sefat Division of Materials Sciences and Engineering 1 Managed by UT-Battelle
2 !! Why materials synthesis? If you can make samples, then you can pursue the science that appeals to you: Magnetic materials, metals, insulators, superconductors, etc. If you know how to cook, you can create what you want. Pizza Seafood Stew 2 Managed by UT-Battelle
3 !! Definition of crystal? In a crystal, the constituent atoms are arranged in an orderly repeating pattern extending in all three spatial dimensions. Spatial extent of the ordered regions (crystallites): Crystal poly-/micro-crystalline nanocrystalline amorphous ~ mm ~ µm ~ nm < nm 3 Managed by UT-Battelle
4 !! Why single crystals?! Aesthetics gemstones Ruby Al 2 O 3 with ~ 1% Cr Diamond C Sapphire Al 2 O 3 with ~ 0.01 % Ti & Fe Emerald Be 3 Al 2 (SiO 3 ) 6 With Cr or V dopants 4 Managed by UT-Battelle
5 !! Why single crystals?! Find intrinsic properties (no grain boundaries, anisotropic)! Application in devices Silicon chips YAG-lasers Nd:Y 3 Al 5 O 12 5 Managed by UT-Battelle
6 !! What are the crystal growth techniques? 6 Managed by UT-Battelle B. R. Pamplin, Crystal Growth, Pergamonpress (1980).
7 !! What are the crystal growth techniques? Growth from gas phase precipitation from gas phase! solid! gas! xtal Chemical vapor transport need a transport agent Pulsed laser deposition need a substrate or seed Issues: Induce a phase transition homogeneous gas phase to solid + unsaturated gas Control conditions for supersaturation, usually by control of temperature gradients 7 Managed by UT-Battelle
8 !! What are the crystal growth techniques? Growth from a mixture of solids (no melting) kinetic and thermodynamic factors are important Issues: Crystals are micron size! Phase segregation, grain boundaries 8 Managed by UT-Battelle
9 !! What are the crystal growth techniques? Growth from the liquid phase! solid! liquid! solid Variations are Bridgman, Czochralski (pulling), Kyropoulos (top seeding), Verneuil (flame fusion), tri-arc, skull melting, image float-zone Issues: Induce a phase transition liquid to solid Control of temperature and gradients High melting points > 2000 C (confirmation of melting!) Reactivity of crucible Control nucleation (seed crystal) 9 Managed by UT-Battelle
10 !! What are the crystal growth techniques? Growth from solution precipitation from supersaturated solution Aqueous & organic solvents Inorganic solvent (flux, high T) Hydrothermal (high P & T) Issues: induce a phase transition homogeneous solution to solid + unsaturated solution control conditions for supersaturation concentration (evaporation of solvent), temperature (solubility or saturation is a function of temperature) reactivity of container (crucible) inclusion of solvent in crystals 10 Managed by UT-Battelle
11 !! Why solution growth? Advantages: -! Grow congruently and incongruently melting materials -! Need relatively simple equipment -! Has short growth-time scales - Need small amounts of materials Disadvantages: - Not too large a crystal (mm to cm) 11 Managed by UT-Battelle
12 e.g. Rock candy! Find the right solvent and dissolve the starting materials! Crystallize with time and temperature Important: Solvent should have reasonable solubility & Diffusivity 12 Managed by UT-Battelle
13 e.g. Rock candy! Find the right solvent and dissolve the starting materials! Crystallize with time and temperature "! Flux Growth is solution growth at high temperature "! Flux (melt; solvent) can be metals (Ni, Fe, etc.), oxides (B 2 O 3, Bi 2 O 3 ), hydroxides (KOH, NaOH), salts (BaO, PbO, PbF 2 ), eutectic binaries 13 Managed by UT-Battelle
14 e.g. Rock candy! Find the right solvent and dissolve the starting materials! Crystallize with time and temperature Key characteristics for fluxes "! Have low melting temperature "! Be easily separated from the products "! Not form stable compounds with the reactants "! Have a large difference between boiling & melting temp. 14 Managed by UT-Battelle
15 !! What are flux growth needs? glove box -! Elements - Cutting tools 15 Managed by UT-Battelle
16 !! What are flux growth needs? -! Crucibles -! Tubes (reaction under ambient conditions not possible) T max ( C) T melting ( C) borosilicate glass (Pyrex) gold silica (quartz) platinum alumina (Al 2 O 3 ) zirconia (ZrO 2 ) magnesia (MgO) tantalum Managed by UT-Battelle
17 !! What are flux growth needs? -! Crucibles -! Tubes (reaction under ambient conditions not possible) Elements Container & tube choices Alkali & alkaline-earth metals Ta, steel Al, Ga Al 2 O 3, MgO, BeO Mg MgO, Ta, graphite or steel Cu, Ag, Au graphite, MgO, Al 2 O 3, Ta Fe, Co, Ni Al 2 O 3, ZrO 2 Zn, Cd, Hg Al 2 O 3 In Al 2 O 3, Ta Rare-earth metals Ta, Mo, W, BeO Bi, Sn Al 2 O 3, SiO 2, graphite Sb SiO 2, graphite 17 Managed by UT-Battelle
18 !! What are flux growth needs? -! Arc melt - Glass sealing station 18 Managed by UT-Battelle
19 !! What are flux growth needs? -! Furnaces SiC heating elements (T max = 1500 C) MoSi 2 heating elements (T max = 1700 C) 19 Managed by UT-Battelle
20 !! What are flux growth needs? -! Centrifuges - Chemical etchers (e.g. for Al, use NaOH; for Ga or In, use HCl) - Mechanical removal tools 20 Managed by UT-Battelle
21 !! What are flux growth needs? -! Energy dispersive spectrometer -! X-ray diffractometer (powder or single crystal) 21 Managed by UT-Battelle
22 !! Where to start? #! (1) Review basic literature on flux growth Growth of single crystals from molten metal fluxes Fisk, Z. and Remeika, JP Gschneidner Jr, KA and Eyring, L. (eds) (1989) Handbook on the Physics and Chemistry of Rare Earths 12, p. 53. Elsevier, Amsterdam Paul C. Canfield 22 Managed by UT-Battelle
23 !! Where to start? #! (2) Learn about the elements e.g. reactivity, toxicity, general properties Atmosphere control may be crucial i.e. samples can t be made in air! Wikipedia descriptions La: forms a hydrated oxide with moisture in air Na: burns with a yellow flame; reacts violently with water, oxidizes in air K: oxidizes rapidly in air; very reactive with water; burns in contact with skin Ba: reacts exothermically with oxygen, & violently with water P: high reactivity; widely used in explosives, nerve agents, friction matches, fireworks As: poisonous ; frequently used for murder 23 Managed by UT-Battelle
24 !! Where to start? #! (2) Learn about the elements IE (kj/mol) metal radius (pm) T melt ( C) T boil ( C) D 20 C (g/cm 3 ) Ca Sr Ba Managed by UT-Battelle
25 !! Where to start? #! (3) Find structure data Same structure-types may give similar physical properties! e.g. Fe-based superconductor (BaFe 1.84 Co 0.16 As 2 ) has ThCr 2 Si 2 structure. Explore other Fe-based compounds with this structure: Managed by UT-Battelle
26 !! Where to start? #! (4) Find the existing phase diagrams -! Binary diagrams are a good start (may be your only option) -! Ternary, quaternary growths generally involve educated guesses. Let s review a few binary phase diagrams Ca-Ag Ba-Ag detour 26 Managed by UT-Battelle
27 27 Managed by UT-Battelle Eutectic point: - Minima in liquid region - Easily accessible liquid region
28 28 Managed by UT-Battelle Congruent reaction: Transformation from a homogeneous liquid to a homogenous solid
29 Peritectic reaction: - Melt incongruently, i.e. decompose into a mixed solid and a liquid phase liquidus-solidus line for BaAg 2, BaAg, etc. 29 Managed by UT-Battelle
30 !! Where to start? #! (5) Find a good metallic flux for crystal growth A good flux (a) has a low melting temperature, (b) has a good solubility for the elements, (c) does not enter crystal as inclusions, & (d) does not create competing phases, etc. 30 Managed by UT-Battelle
31 Review of some metallic fluxes Al! T melt = 660 C! attacks silica! spin off Al in silica tubes or use NaOH e.g. RB 4, YbAlB 4, RB 6, RBe 13, RAl 3, TiB 2, CeSi 2-x 31 Managed by UT-Battelle
32 Review of some metallic fluxes Ga! T melt = 30 C! tends to wet surfaces of grown crystal! forms compounds with rare-earths e.g. RSb, R 2 Pt 4 Ga 8 32 Managed by UT-Battelle
33 Review of some metallic fluxes In! T melt = 157 C! Proven to be a good flux for ThCr 2 Si 2 -types! T C = 3.4 K e.g. CeCu 2 Ge 2, CeNi 2 Ge 2, TyCu 2 Si 2 33 Managed by UT-Battelle
34 Review of some metallic fluxes Sn; Pb! T melt = 232 C; 327 C! form RPb 3, RSn 3 phases! T C = 3.7 K; 7.2 K e.g. YbCu 2 Si 2, TiNiSn, MnSnNi, RSb; RBiPt, RPbPt 34 Managed by UT-Battelle
35 Review of some metallic fluxes Sb! T melt = 630 C! stability of R-Sb phases e.g. RSb 2, U 3 Sb 4 Pt 3, PtSb 2 35 Managed by UT-Battelle
36 Review of some metallic fluxes Zn T melt = 420 C e.g. InSb, GaSb, InAs, Si, Ge Bi T melt = 272 C e.g. UPt 3, PtMnSb, NiMnSb, UAl 3, GaP, ZnSiP 2, CdSiP 2 Cu T melt = 1085 C e.g. RPh 4 B 4, RCu 2 Si 2, V 3 Si, RIr 2, UIr 3 36 Managed by UT-Battelle
37 !! What are some examples? (I) How to make Si? (T melt = 1412 C) Let s aim for max temperature of our furnace of ~ 1000 C Look up solvents that are low melting: Bi, Sn, Zn, Ga, Al 37 Managed by UT-Battelle
38 !! What are some examples? (1) How to make Si? (T melt = 1412 C) Let s aim for max temperature of our furnace of ~ 1000 C Look up solvents that are low melting: Bi, Sn, Zn, Ga, Al Best solvent Place Al:Si = 60:40 into Al 2 O 3 38 Managed by UT-Battelle
39 !! What are some examples? (2) How to make CeSb 2? Melts incongruently 39 Managed by UT-Battelle
40 !! What are some examples? (2) How to make CeSb 2? Melts incongruently use alumina crucible L + CeSb 2 Ce:Sb = 10:90 40 Managed by UT-Battelle
41 !! What are some examples? (3) How to make Ce 2 Sb? Melts incongruently use Ta crucible Ce:Sb = 85:15 41 Managed by UT-Battelle
42 !! What are some examples? (4) How to make CeSb? Melts congruently at 1820 C -! Melt growth technique -! Excess Ce flux -! Excess Sb flux -! a 3 rd metal flux? 42 Managed by UT-Battelle
43 !! What are some examples? (4) How to make CeSb? Melts congruently at 1820 C -! Melt growth technique -! Excess Ce flux -! Excess Sb flux -! a 3 rd metal flux? Sn is a good choice 43 Managed by UT-Battelle
44 ! Sn is a low-melting element that offered good solubility for both Sb and Ce Low T melt of Sn x Sb y Have Ce dilute in Sn e.g. Try Ce:Sb:Sn = 5:5: C 800 C 44 Managed by UT-Battelle
45 !! What are some of my research examples? Growth of BaFe 2 As 2 - Ternary phase diagram not known - Arsenic has a high vapor pressure (~600 C, 1 atm) - Look for binary phase diagrams: Ba-Fe, Fe-As, Ba-As 45 Managed by UT-Battelle
46 1 st, make FeAs 1065 C (10 hrs) 700 C (dwell 6 hrs) Ba has little solubility of Fe at T< 2000 C FeAs melts congruently at 1042 C Ba-As 46 Managed by UT-Battelle
47 2 nd, put Ba(FeAs) 5 in alumina crucible, in silica 1180 C (dwell 15 hrs) 1090 C [001] mm scale AT 2 As 2 (A = Ca, Sr, Ba; T = Cr, Mn, Fe, Co, Ni) 47 Managed by UT-Battelle Phys. Rev. Lett. 101, (2008). Physica C 469, 350 (2009).
48 BaT 2 As 2 b c a ~ 7.4 % volume collapse I4/mmm Z. Naturforsch. B 36 (1981), Managed by UT-Battelle
49 BaT 2 As 2 Cr Mn Ni Fe Co BaFe2-x Cr x As 2 BaFe 2-x Co x As 2 T C = 22 K 49 Managed by UT-Battelle Phys. Rev. Lett. 101, (2008). Phys. Rev. B 79, ; ; ; (2009). Physica C 469, 350 (2009).
50 Growth of GdMn 2 Al 10 - Ternary phase diagram not known 50 Managed by UT-Battelle
51 Try Gd:Mn:Al = 0.04: 0.08: :2:10 GdMn 2 Al 10 Al 51 Managed by UT-Battelle
52 GdMn 2 Al 10 Mn Al GdMn 2.21(4) Al 9.79(4) + Mn ~ 0.2 GdMn 2.39(2) Al 9.61(2) P4/nmm Z. Naturforsch. 53b (1998), 673. Phys. Rev. B 76 (2007), Managed by UT-Battelle
53 Growth of CeAu x Si 2 Au Ce Si [010] CeAu 4 Si 2 *T N = 9 K T c " 3.3 K I4/mmm Cmmm CeAu 2 Si 2 * T N = 4 K, 8.1 K Physica B, 378 (2006), 812 J. Magn. Mag. Mater (2004), e405. [001] 53 Managed by UT-Battelle J. Solid State Chem. 181, 282 (2008).
54 CeAu x Si 2 Grown out of Au-Si eutectic Two step growth: 1)! First melt Au and Si together at ~ 1400 C using an arc melt 2) Seal Ce and Au-Si in silica, soak & slow cool for crystal growth CeAu 4 Si 2 CeAu 2 Si 2 54 Managed by UT-Battelle
55 R = Nd Growth of RVSb 3 Sb. [100] VSb 6 R 5.4 % Pbcm Phys. Rev. B, 65 (2001), J. Magn. Mag. Mater. 320, 120 (2008). 55 Managed by UT-Battelle
56 Growth of R 2 Co 3 Zn 14 Initial melt of R:Co:Zn = 8:12:80; 6:11:83 1 mm a b R = Gd, T = Co. [001] R T Zn1, Zn2,3 J. Magn. Mag. Mater. 320, (2008), Gd 2 Co 3 Al 14 T N = 32 K R-3m Chem. Mater. 14 (2002), T mag = 6 K Y 2 Co 3 Al Managed by UT-Battelle
57 Concluding remarks: $!You can try to discover, and design that allow you to pursue the specific science that interest you. $! Although flux growth technique is less predictable than conventional crystal growth methods, the discovery of new materials may be made unexpectedly! $! Hope that you want to get in a synthesis lab and attempt crystal growth! 57 Managed by UT-Battelle
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