Status of the crystallography beamlines at Elettra 2 Andrea Lausi - - PowerPoint PPT Presentation

• A. Lausi

Status of the crystallography beamlines at Elettra

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

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Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

Photon sources at Elettra

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Peak Brilliance (Photons/s/mm

2/mrad 2 /0.1%bw)

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Photon Energy (eV)

0.1 1 10 100 1000

Wavelength(nm)

U5.6 1 3 5 U12.5 FEU W14.0 SCW Short W15.0 Short U5.6 1 3 5 Bending Magnet EUFELE 100 nm 40 nm 10 nm Elettra E=2 GeV I=400 mA FERMI

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

1995-2006:

XRD beamline

macromolecules but also material science, high pressure, fibers, inorganic crystals...

Diffraction at ELETTRA

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Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

HRD(1) diffraction beamline (1995 version)

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source slits monochromator refocussing mirror sample stage filter

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

XRD1: present and future

General purpose X-ray beamline with a extended spectrum(4-21 keV) from a wiggler source, shared with the SAXS BL. The BL hosts PX and material science experiments, in collaboration with CNR.

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

• Top-up mode introduced serious thermal load problem affecting the BL
• monochromator. Three water direct-cooled crystals already substituted

in the last three years. This was reflected in a reduced (total) flux and enlarged spot size, causing problems both with users and industry (long exposure time, and beam divergence in particular).

XRD1: present and future

A closed loop cryogenic system (liquid nitrogen) from Bruker has been purchased and is expected to be tested by the early 2015.

XRD1 is expected to be up and running at full capacity at the beginning of 2015.

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

Structural biology lab

Molecular biology Large scale protein expression Protein purification Protein characterisation Biophysical analysis Biochemical analysis Crystallisation

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

Recombinant proteins are fundamental “reagents” for basic and applied

• bioresearch. Obtaining pure and folded proteins is usually a bottleneck in biological

studies.

The PROTEO protein factory

Construct Design

Multiple Cloning

Test Expression Purification

SCALE UP

Thanks to an INTERREG grant we have established a biotechnological platform that provides a specialized support to express and purify recombinant proteins for functional and structural studies. We implemented a multistep process to go from gene to protein with high efficiency using multiparallel protocols in bacteria, insect and mammalian cell expression systems

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

Tecan liquid handler robotic platform for High Troughput cloning & small scale purification 2 Sartorius Certomat BS-1 orbital shakers to grow bacterial cells 5 Sartorius fermentors for controlled expression in prokaryotic and eukaryotic cells, including 2 Biostat B (2L), 2 Biostat C (10L) and one Cultibag 20/50 RM (50 L). 4 Akta FPLC with column fleet for chromatographic protein purification Suite of centrifuges (Beckmann Allegra 22R, Allegra 64R, Avanti J-26XP) with rotor fleet Spectrophotometers & gel imaging system (ImageQuant)

Expression & purification facilities

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

Molecular biology lab

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

Bacterial protein expression

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

Liquid handler Tecan EVO Freedom 150 for re-formatting commercial crystallization screens and setting up crystallisation plates TTP Labtech Mosquito nanoliter crystallization robot to set up 50-100nL crystallization drops Explora Nova Xtal Focus system for automatic crystal imaging and remote monitoring of crystallization experiments The facility has been designed to be open for external users. Users will be able to bring/send purified protein samples, set up a variety of commercial crystallization screens, and monitor the results of the experiments in remote, through a web- based system.

The crystallization suite

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

Crystallization lab

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

2009 - Present: MCX new XRD1 currently in construction: XRD2 cluster

BM 7.1

• Beamline designed for non

single crystal diffraction experiments

• Open to users since 2009

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

Before MCX: “Powder Diffraction Facilities at ELETTRA”

• Powder in capillary on XRD1 area detector

(Si powder @ ~18 keV)

• Fit2D to integrate rings
• Resolution limited by spatial response of

detector and by sample dimensions

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Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

Diffraction analyses

 Phase identifications  Texture analysis  Phase transitions  Crystal structure determination  Crystal structure refinements  Quantitative phase analysis (and crystallinity determination)  Microstructural analyses (crystallite sizes - microstrain)  Residual stress analysis

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Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

Design Guidelines

• High-flux tuneable source with a wide spectral range,

(6-12 keV)

• Possibility to extend the
• Flexible optics

– line focus (10 x 1 mm2) – point focus (1 x 1 mm2 and below)

• Accommodate large volume samples
• Use of different detectors
• Sample temperature control
• User-friendly software

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Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

1010 1011 1012 1013 Photons/s/0.1%bw (/2 mrad horiz /0.27 mrad vert.) 103

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Photon Energy (eV) 1010 1011 1012 1013 Photons/s

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10 l (Å) ELETTRA operated at 2.4 GeV, 200 mA bending magnet spectral flux Flux at the sample (Air environment) Flux at the sample (He environment)

MCX optical design : source

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Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

1010 1011 1012 1013 Photons/s/0.1%bw (/2 mrad horiz /0.27 mrad vert.) 103

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Photon Energy (eV) 1010 1011 1012 1013 Photons/s

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10 l (Å) ELETTRA operated at 2.4 GeV, 200 mA bending magnet spectral flux Flux at the sample (Air environment) Flux at the sample (He environment)

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MCX optical design : source

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

• High-transmission Filter-

window assembly

• Collimating Pre-mirror
• Wide range

monochromator with II crystal bender for dynamical sagittal focusing

• Bendable focusing mirror

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MCX optical design : outline

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

Sagittal Focussing

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Grazing incidence reflection optics:

• geometrical loss
• small acceptances
• difficult to manufacture
• expensive

bent II crystal

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

long 2nd crystal movement capability allow for the wide energy range

The Elettra Hard X-ray Monochromator

• E. Busetto, I. Cudin, G. Fava
• R. Borghes, G. Cautero

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Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

The Elettra Hard X-ray Monochromator

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Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

Anrea Lausi The CX project…

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Front-end Hutch

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

First mirror

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Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

0.5 µrad slope error measured on the Elettra Long Trace Profilometer First mirror

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Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

0.65 µrad slope error

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Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

From the Optical to the Experimental Hutch

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Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

Experimental Station

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Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

Experimental Station

• 4 circle diffractometer

(0.0001° precision in 2θ)

• XYZ translation stage
• Recieving slits
• Analyzer crystal / scintillator

detection system

• Hot air blower (up to 1273K)
• Cryo stream (down to 100K)
• Laser sensor for accurate

sample positioning

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Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

General User Interface

Control system based on pyton General command interface for:

• driving motors
• theta-2theta scan
• multiple theta-2theta scans
• single or two motor scan
• multiple scans
• monochromator functions
• calibration functions
• warnings management...
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Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

Experimental Station

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Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

Experimental Station

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Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

Instrumental profile (capillary)

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Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

Instrumental profile (flat plate)

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Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

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Instrumental profile (capillary)

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

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In Situ Reaction Furnace

• Designed as a stand alone

equipment to be used on mcx beamline.

• Maximum temperatures reached in

current setup 1000 C.

• Ideal for powder samples
• Diffraction data recorded on a

translating Imaging plate.

• Remote controlled

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

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Furnace Design

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

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Furnace Design

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

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Detection system

• Images recorded on

translating imaging plate

• Translation controlled by

Labview program

• Measurements in

contiunuous and discrete mode

• Data integration using fit2d

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

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Capillary holder

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

Experimental Station

• Phase identification
• Residual stress
• Micro-structural analysis
• Structure determination
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Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

The SCW beamlines cluster

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Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

• Crytical photon energy 13.4 keV
• Total radiated power

6.85 kW

• Maximum field:

3.5 T

• Poles

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• Pole gap

16.5 mm

• Period length

64 mm The multipole superconducting wiggler, constructed by Budker Institute of Novosibirsk, was designed to produce a high flux and brilliance source in the 10-25 keV range. Currently refurbished at Novosibirsk with new cryostat allowing to limit the liquid helium (LHe) consumption to a maximum of 2 refills per year

Multipole Superconducting Wiggler

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

The new SCW compared to the permanent magnet wiggler of the existing Diffraction beamline (xrd1)

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Brilliance (photons/s/0.1%BW/mm

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Photon energy (eV) E=2.4GeV; I=100mA

SCW W 14.0

A factor 14 higher brilliance at 25 keV !!

Multipole Superconducting Wiggler

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

25 keV High Pressure branch-line

Super conducting wiggler Si111 17.2 m Toroidal Mirror 33 m Experiment 44.8 m Mask Filters

Acceptance 500*120 μrad2 Flux in 80*80 μm2 aperture at sample:

1011 ph/s @ 2.4 GeV, 100mA

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

XRD2 – general layout

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

 XRD2 and Xpress have been designed in collaboration with the Indian

Institute of Science (Bangalore)

 The source can host a third fixed energy beamline (Pharma?).  Most optical components already characterized and installed. Orders

have been placed for >95% of the necessary items and we expect to have all the items vacuum-related, controls and plants in house and installed for September 2014 (commissioning till February 2015).

 Will present all the features of a high throughput MAD BL (including

sample changer, SPINE compatible), with remote data collection capability.

Xpress is expected to be up and running in Spring 2015. XRD2 is expected to be up and running in Summer 2015.

XRD2: status and perspective

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

SCW Front-end mask

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

Beam splitter

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

Flux at the sample: 3.3 E13 ph/s/0.1%BW (2GeV, 100mA) Sizes of the focal spot: 330μm X 90μm, 2.3mrad X 0.3mrad [FWHM] Estimated fluxes at the sample (taking account of filters, efficiency of the monochromator, reflectivity of the mirrors and different sample sizes):

Flux @2GeV, 310 mA Flux @2.4GeV, 140 mA Square size 1 x 1013 7 x 1012 200µm X 200µm 9 x 1011 6 x 1011 50µm X 50µm 2.5 x 1010 2 x 1010 10µm X 10µm

XRD2: flux at focus

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

Flux @2GeV, 310 mA0 Flux @2.4GeV, 140 mA Square size 1 x 1013 7 x 1012 200µm X 200µm 9 x 1011 6 x 1011 50µm X 50µm 2.5 x 1010 2 x 1010 10µm X 10µm

BL spot size flux (ph/s) BM14 300 x 750 4,50E+011 ESRF - Id14-1 50x200 1,00E+011 ESRF – Id14-2 100x100 1,00E+011 ESRF – Id14-4 90x250 5,00E+012 ESRF – ID23-2 10x10 4,00E+011 ESRF – ID29 30x50 1,00E+013 ALBA - XALOC 6x50 2,00E+012 BESSY - 14.1 50x50 1,60E+011 SLSPSI - X06DA 90x70 4,00E+011 SLSPSI - X10SA 50x10 2,00E+012 DIAMOND - I24 80x80 1,00E+012

Set against the existing MX beamlines in Europe, XRD2 compare favourably with most non-microfocus beamlines, such as ESRF BM14/ID14-1/ID14-2, Bessy 14.1, SLS X06DA, Diamond I24.

XRD2: status and perspective

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

XRD2 status

Andrea Lausi – 20-21 April 2015 7° ILSF Users’ Meeting – Qazvin

XRD2 status

THANK YOU FOR YOUR ATTENTION