1 BROOKHAVEN SCIENCE ASSOCIATES Eric Dooryh é e and Andy Broadbent, Experimental Facilities Division, NSLS-II, with acknowledgements to the staff at ACCEL

1 BROOKHAVEN SCIENCE ASSOCIATES

Eric Dooryhée and Andy Broadbent,Experimental Facilities Division, NSLS-II ,

with acknowledgements to the staff at ACCEL Instruments, and members of the BAT

Experimental Facilities Advisory Committee Meeting

April 23-24, 2009

The NSLS-II Powder Diffraction Beamline Design


Outline

• Introduction to Eric Dooryhée (XPD Group Leader)

• Scientific Mission and Requirements (Eric Dooryhée)• End Station

• Beamline Design Iteration (Andy Broadbent)• Current Optical Layout• Issues and conclusions


Eric Dooryhée

Past EmploymentJune 1st, 2009 NSLS II powder diffraction beamline2001-2008 senior scientist fellowship (Neel Institute, CNRS, FR)1996-2000 powder diffraction (ESRF BM16, now ID31)1990-1995 High energy ion and Laser Research Center (CNRS, FR)1988-1989 Post-doc powder diffraction (SRS Daresbury, UK)

Research• powder diffraction (SRS, ESRF, SOLEIL, neutrons ILL)

(in situ, line profile, direct space and Rietveld, upgrade of ESRF-BM02) • epitaxial thin films/multilayers of oxides (ferroelectric, relaxor, magnetic)• cultural heritage (chair of “SR in Art and Archaeology” + IUCr commission)


Scientific Mission

• Use the brightness of NSLS II • flux demanding - high throughput - high time resolution

• high angle resolution (structure solving, microstructure)

• beam focusing down to ~50μm (high spatial resolution)

• Use the high energy spectrum of the damping wiggler• sample environments (non-ambient, in-situ, in-operando)• high Q (PDF) on simultaneously operating side branch• access K-edge of heavy elements (contrast diffraction)


Scientific Domains

• Complex materials• Many atoms, heterogeneity, size and defects, poor scatterer

• Functional/real materials functioning: in-situ / in-operando studies• Materials change structure under synthesis/operational conditions,

e.g. catalysts, H2 storage• Towards real working devices, e.g., ultra-thin dielectric films, fuel

cell electrodes

• Nanoscale materials• Bottom up design and build of materials with directed functionality• Hierarchical materials: control structure on different length-scales


First End StationRotation stage for high energy resolution crystal analysers, 1µradian resolution 10µradian accuracy.

Standardized interface plate, supports 35kg at the sample position.

Custom Ge based strip detector with 100°coverage. 250µradian resolution on 0.5m radius.

Support table for intermediate weight sample environments (~100kg)

Robot for automated sample changing (not shown).

Courtesy of SLS and ASP


SLS (MS) 5ESRF (ID31) 9 (Ge to Si) (Hodeau et al. SPIE 1998)APS (11BM)12ALBA 13 SOLEIL (CRISTAL) 21 DIAMOND (I11) 45 (5 banks of 9)

Courtesy of Chiu Tang DIAMOND

High energy Laue curved analyzer (see Zhong, Siddons, Hastings, Kao)

Off-plane diffraction analyzer (patent 2007)

High resolution (“multi-modal”)


• many samples are inherently heterogeneous (multi-scale)• beam size should match : graininess, heterogeneity scale, sample geometry

variable focal spot size

• imaging mode, micro-diffraction (~500 to ~50μm)

• total crystallography: neither a powder nor a single crystal

High Energy Micro-Diffraction

commercially available CRL set-up of Prof. Lengeler (Aachen)


Response to Comments from EFACResponse to Comments from EFACComment Response

The EFAC is uncertain about the relationship of the BAT proposing PING to that proposing the High-Pressure, High-Energy X-ray Beamline [HiPHEX]. We recommend that these two communities engage in cooperative discussions if such discussions are not already underway.

The efforts of HiPHEX and XPD are separate, but there is excellent communication because of the presence of Lars Ehm and Johs Parise on the XPD BAT. Lars' and John's research includes scattering experiments under high pressure and they are an integral part of the high pressure community that is responsible for HiPHEX.The main issue for HiPHEX is matching the beam characteristics with highly specialized special environments making those beamlines, and the ancillary equipment, tightly coupled. In that sense, there is little overlap between the high pressure and PING beamlines, except that a high pressure component of a broader materials study making use of PING may be carried out at HiPHEX.

“…work done by Peter Siddons at the NSLS…is highly advantageous for the outcome [of the PING beamlines]… partnership of Siddons and the PING team has the possibility to leapfrog the state-of-the-art.”

We recognize this opportunity. We already have some of Peter Siddons' innovations as probable components in the beamline design (pending testing). We will work closely with Peter Siddons over the upcoming years, especially with respect to fast, efficient, high energy strip detectors, and incorporate advances into our designs where possible.

Referees comments (rather than EFAC directly). Concerns about the scientific justification for the PDF side station.

The BAT consider that the greatest growth in powder diffraction over the next 5 years will take place in the area of PDF studies of nanomaterials, making the side‐station an essential component of the suite of instruments for materials studies. Having said this, the side‐station is currently part of the mature scope for the PING project.

Although there are some doubts as to whether the PING beamlines will be “best in class,” there is widespread agreement that there is a high probability that the PING beamlines will allow the user community to achieve their important scientific objectives.

The PING lines will be best in class because of the high fluxes and small beams with focusing in the horizontal and the vertical directions and ~50 micron spot size in the 50 ‐ 80 keV range. Coupled with the proposed integration of different beamlines envisaged in the MaDiS concept, there will be nowhere in the world better for complex material diffraction experiments.


Beamline Design Iteration

• Due to extensive changes in scientific objectives ACCEL were commissioned to revise the design to concentrate on the higher energies. The changes requested use both commercial experience and unique in-house expertise, and can be made within the existing budget.

• Active involvement of all members of the BAT in developing the beamline design.

• 2nd Beamline Scientist interviews in progress.


Conceptual Beamline Layout

in use at NSLS X17 and tested at X7bDr. Z. Zhong design


Damping Wiggler Power Management• Full 7m damping wiggler length (65kW).

• Selective aperturing:• central part of the fan has higher energies, • restrict aperture to ~1mrad (H) x 0.1mrad (V),• still leaves almost 6kW!

• Concentrating on the high energies allows extreme filtering:• multistage C (5mm total) and Al (8mm total) filtering leaves just 280W, of which 21W

is absorbed in the 0.5mm Si crystal;• the cost is some loss of useful flux:

– lose 64% of flux at 50 keV, and– lose 46% of flux at 80 keV.


After filtering, the Laue mono and CRLs.


Energy (keV) Flux (ph/sec) Beam size (µm)

50 2-5 x1012 ~50 (H) x 50 (V)

80 1-2 x1012 ~50 (H) x 50 (V)

Main Beamline Performance

Vertical focusing (or collimation) with CRLs, dE/E~1x10-4, Si[311]


Beamline, Optics and Endstation Layout


Second End Station (long set-ups)

Typical experiments may include gas rigs, high-pressure, high or low temperatures....

A key requirement of the User community is to provide for fast changeover of samples and environments.


Side-Branch Beamline

Laue or Bragg single bounce mono (~4 degree deflection)

with horizontal focusing,

Vertical focusing with CRLs,

Fixed energy at 80 keV,

Energy resolution of ~4 x 10-3 allowable


Issues and Conclusions• The only high-resolution instrument in the US capable of collecting

data at high energies ( 40 keV to 100 keV) ideal for high-Q data and in situ and time resolved studies in environmental cells.

• Combining complementary analysis probes, e.g., micro-raman

• Investigation and development required on:• beam filtering and DLCM : heat load, band pass,...• deflecting side bounce monochromator (including cooling scheme)• focusing : mono and CRLs• Detector development e.g. Siddons’ work on Ge strip array

• Start work on software requirements and sample environments

• Conceptual design report due end Sept 2009.

Documents

1 BROOKHAVEN SCIENCE ASSOCIATES Eric Dooryh é e and Andy Broadbent, Experimental Facilities Division, NSLS-II, with acknowledgements to the staff at ACCEL