Types of Diamond-Anvil Cells and how to work with them. Ronald MILETICH
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1 and how to work with them Ronald MILETICH Institut für Mineralogie und Kristallographie Universität Wien ECM-27 high-p workshop methods of high-p single crystal x-ray diffraction Introduction Outline 1
2 Introduction Outline Introduction Outline 2
3 Introduction Outline Introduction Outline How to Work with Them 3
4 Introduction Outline How to Work with them Introduction Outline How to Work with Them 4
5 part 1 High-Pressure Techniques Percy 2012: W. modern Bridgman, large-volume Nobel Prize presses the pioneer era in high-pressure research 5
6 Opposed Anvil Assembly (1/3) backing plate diamond anvil gasket diamond anvil backing plate Opposed Anvil Assembly (2/3) upper anvil gasket pressure chamber lower anvil 6
7 Opposed Anvil Assembly (3/3) polycrystalline sample oriented single crystal sample Opposed Anvil Assembly (3/3) polycrystalline sample oriented single crystal sample hydrostatic pressure transmitting medium 7
8 Mechanical Pressure Generation (1/3) Reduction of the volume of the pressure chamber by successive mechanical deformation of the gasket Mechanical Pressure Generation (2/3) Reduction of the volume of the pressure chamber by successive mechanical deformation of the gasket 8
9 Mechanical Pressure Generation (3/3) Reduction of the volume of the pressure chamber by successive mechanical deformation of the gasket Specifications of Anvils Cut, Geometry, and Dimensions 9
10 Specifications of Anvils (1/6) Cut, Geometry, and Dimensions C... culet-face diameter T... table-face diameter X... girdle diameter H... height between C face and T face Specifications of Anvils (2/6) Cut, Geometry, and Dimensions C... culet-face diameter B... bevel-face diameter bc.. bevel angle 10
11 Specifications of Anvils (3/6) Cut, Geometry, and Dimensions triple bevel (Scimed GmbH) Specifications of Anvils (4/6) Cut, Geometry, and Dimensions Almax-Boehler design 11
12 Specifications of Anvils (6/6) Cut, Geometry, and Dimensions Typical weight: ct Material: type Ia, Ib (IIa, IIb) C maximum P * 0.60 mm 15 (25) GPa 0.45 mm 40 (50) GPa 0.30 mm 80 (100) GPa 0.20 mm 150 (200) GPa *X=3.0mm, H=1.4mm Sample Environment and Pressure Calibration 12
13 Sample Environment and Pressure Calibration (1/7) Sample Environment and Pressure Calibration (1/7) 13
14 Sample Environment and Pressure Calibration (2/7) Sample Environment and Pressure Calibration (3/7) LiAlSi 2 O 6 and SiO 2 (quartz) crystals 14
15 Sample Environment and Pressure Calibration (4/7) BaTiSi 3 O 9 crystal and ruby spheres Sample Environment and Pressure Calibration (5/7) Optical pressure sensor: Laser-induced luminescence, e.g. R 1,R 2 spectral lines in ruby 15
16 Sample Environment and Pressure Calibration (5/7) Optical pressure sensor: Laser-induced luminescence, e.g. R 1,R 2 spectral lines in ruby R 2 R 1 0 = nm/gpa Sample Environment and Pressure Calibration (6/7) Unit-cell dimensions of internal diffraction standards (Quartz, NaCl, Au, Pt, W, Ne,...) sample crystal quartz 16
17 Sample Environment and Pressure Calibration (6/7) Unit-cell dimensions of internal diffraction standards (Quartz, NaCl, Au, Pt, W, Ne,...) sample crystal quartz EoS: 0 = GPa = 5.99 (Angel et al., 1997) Sample Environment and Pressure Calibration (7/7) Unit-cell dimensions of internal diffraction standards (Quartz, NaCl, Au, Pt, W, Ne,...) 0.03 Unit cell volume, A K 1250 K 2100 K V-V fit, A 3 /at Pressure, GPa Pressure, GPa 17
18 Part 2 Various Types of Goniometers 18
19 Access in reciprocal space (1/8) Geometric interpretation of the Bragg equation Access in reciprocal space (1/6) Geometric interpretation of the Bragg equation Simple trigonometry: /d hkl sin = = = 2d 2 d hkl * 2 19
20 Access in reciprocal space (2/6) Geometric interpretation of the Bragg equation Access in reciprocal space (3/6) Restrictions determined by DAC opening angle 20
21 Access in reciprocal space (4/6) Restrictions determined by DAC opening angle Access in reciprocal space (5/6) Restrictions determined by DAC opening angle toroidal shape of accessible part of the reciprocal space 21
22 Access in reciprocal space (6/6) Restrictions determined by DAC opening angle accessible reciprocal space depends on opening angle Access in reciprocal space (6/6) Restrictions determined by DAC opening angle accessible reciprocal space depends on opening angle 22
23 Limitations in reciprocal space (1/5) reconstructed reciprocal space of BaTiSi 3 O 9 O* hk0 reciprocal lattice plane O* a 2 * a 1 * Limitations in reciprocal space (2/5) reconstructed reciprocal space of BaTiSi 3 O 9 hk0 reciprocal lattice plane O* hk2 reciprocal lattice plane 23
24 Limitations in reciprocal space (3/5) reconstructed reciprocal space of BaTiSi 3 O 9 hk0 reciprocal lattice plane O* hk4 reciprocal lattice plane Limitations in reciprocal space (4/5) reconstructed reciprocal space of BaTiSi 3 O c* O* a 2 * 0kl reciprocal lattice plane 24
25 Limitations in reciprocal space (5/5) reconstructed reciprocal space of BaTiSi 3 O c* O* d 110 * hhl reciprocal lattice plane Various Diffraction Features from DAC Components (1/4) c* O* a 2 * diffraction from the sample 25
26 Various Diffraction Features from DAC Components (1/4) diffraction from the metal gasket Various Diffraction Features from DAC Components (1/4) diffraction from the diamonds 26
27 Various Diffraction Features from DAC Components (2/4) diffraction from the backing plates (Be) Various Diffraction Features from DAC Components (2/4) Weak sample signal 27
28 single IP image MAR345, =0.08 DAC with Be seats 1800 s exposure time Various Diffraction Features from DAC Components (2/4) Decagonal QC Edagawa phase (Al 70 Co 12 Ni 18 ) at 10.7 GPa Krauss, Miletich & Steurer, 2003 single IP image MAR345, =0.08 ESRF, SNBL: DAC with diamond seats reconstruction from 116 IP images total 9.28 (58h) Various Diffraction Features from DAC Components (3/4) Edagawa phase (Al 70 Co 12 Ni 18 ) at 10.7 GPa reciprocal 0kl plane reciprocal h0l plane 28
29 single IP image MAR345, =0.08 ESRF, SNBL: DAC with diamond seats reconstruction from 116 IP images total 9.28 (58h) Various Diffraction Features from DAC Components (4/4) Edagawa phase (Al 70 Co 12 Ni 18 ) at 10.7 GPa reciprocal h 1 / 2 l plane reciprocal h1l plane Crystal Orientation hk O* hk4 29
30 Crystal Orientation (1/3) c b Crystal Orientation (2/3) c a Preparation of oriented sections c (010) a 30
31 ...directions of highest resolution occur parallel to the culet-face plane... Crystal Orientation (2/3) c a Preparation of oriented sections c (010) a achieving equivalent resolution in all three dimensions Crystal Orientation (3/3) c c b a 2-crystals mount 31
32 achieving equivalent resolution in all three dimensions Crystal Orientation (3/3) 2-crystals mount Part 3 32
33 Demands on DACs for sxrd Demands on DACs for sxrd - large opening angle - low background contribution from DAC components (diamond, Be, gasket) - small dimensions for low absorption 33
34 Demands on DACs for sxrd - large opening angle - low background contribution from DAC components (diamond, Be, gasket) - small dimensions for low absorption - adjustable anvils (hemisphere, xy stage) - independent pressure-generating mechanisms - small weight for diffractometry - small height for microspectroscopy - cylindrical shape for use in gas-loading autoclaves - implementation of cooling system for HPHT operation 50 years history 34
35 50 years history The first DAC (1958, Nat.Bur. Standards) 50 years history triangular Merill-Bassett DAC 35
36 50 years history triangular Merill-Bassett DAC 50 years history triangular Merill-Bassett DAC 36
37 50 years history DXR-6 DAC (Diacell Ltd.) 50 years history DXR-6 DAC (Diacell Ltd.) 37
38 50 years history ETH-type DAC (BGI-type DAC) 50 years history ETH-type DAC (BGI-type DAC) 38
39 50 years history ETH-type DAC (BGI-type DAC) 50 years history ETH-type DAC (BGI-type DAC) 39
40 50 years history plate DAC (Almax Industries) 50 years history plate DAC (Almax Industries) 40
41 The new HDHPHT-DAC Heidelberg High-Pressure High-Temperature Pippinger et al. (2011) Rev.Sci.Instrum. 82, The new HDHPHT-DAC new solution guiding pins dog clutch guidance 41
42 The new HDHPHT-DAC (1/13) radial optical access The new HDHPHT-DAC mechanism I: gas-pressure inflated membrane mechanism II: conventional mechanical bolts inflatable membrane dual-mode device for independent pressure generation 42
43 The new HDHPHT-DAC grey: counter-bearing bolts green: screws for P change The new HDHPHT-DAC module 1 module 2 43
44 The new HDHPHT-DAC ESRF, Beamline ID09a, experiment HS4323 The new HDHPHT-DAC How to Work with DACs? 44
45 Cr 3+ :Al 2 O 3 (ruby) P reference CaCO 3 -III sample crystal argon pressure medium (s,l) Thank you. ECM-27 high-p workshop methods of high-p single crystal x-ray diffraction
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