1 BROOKHAVEN SCIENCE ASSOCIATES NSLS-II SRX Beamline Tony Lanzirotti SRX Beamline Advisory Team Chair The University of Chicago, CARS Experimental Facilities

1 BROOKHAVEN SCIENCE ASSOCIATES

NSLS-II SRX BeamlineNSLS-II SRX Beamline

Tony LanzirottiTony LanzirottiSRX Beamline Advisory Team ChairSRX Beamline Advisory Team ChairThe University of Chicago, CARS The University of Chicago, CARS

Experimental Facilities Advisory Committee MeetingExperimental Facilities Advisory Committee Meeting April 23-24, 2009April 23-24, 2009


Sub-micron Resolution X-ray (SRX)Sub-micron Resolution X-ray (SRX)spectroscopy Teamspectroscopy Team

Beamline Advisory Team Members:Beamline Advisory Team Members:Antonio Lanzirotti (Leader) -Antonio Lanzirotti (Leader) - Univ. of Chicago (microprobe design, operation and applications) Peter Eng -Peter Eng - Univ. of Chicago (beamline design/optics and instrumentation)Jeffrey Fitts -Jeffrey Fitts - BNL (environmental science applications, XAS)Keith Jones -Keith Jones - BNL (microprobe design, CMT design)Lisa Miller -Lisa Miller - BNL (life science probe design and application)Matt Newville -Matt Newville - Univ. of Chicago (XAS design, operation and applications) Paul Northrup -Paul Northrup - BNL (beamline design, management, environmental science applications)Richard Reeder -Richard Reeder - Stony Brook Univ. (microprobe applications in earth & environmental science)Mark Rivers -Mark Rivers - Univ. of Chicago (detector and control systems design) Stephen Sutton -Stephen Sutton - Univ. of Chicago (microprobe design, management and operation)Stefan Vogt -Stefan Vogt - ANL (zone plate microprobe design and operation, applications to life sciences)Gayle Woloschak -Gayle Woloschak - Northwestern Univ. (biological applications of zone plate microprobes)

NSLS-II:NSLS-II:Paul Northrup –Paul Northrup – Interim Group Leader (Hutch design, FOE component layout, accelerator group liaison)Andy Broadbent –Andy Broadbent – Beamlines Manager (budget overview, management oversight)Jürgen Thieme –Jürgen Thieme – Group Leader (July 2009)

Institute for X-Ray Physics, Georg-August-University, GöttingenLed the project of building a scanning transmission X-ray microscope at the electron storage ring BESSY II, principally for spectromicroscopy in environmental sciences.


SRX Scientific MissionSRX Scientific Mission

Workshops held by scientific communities (such as Earth, Environmental, and Life sciences, Hard Condensed Matter and Materials sciences, Chemical and Energy sciences) have all identified analytical resources that must be developed to advance our understanding complex natural and engineered systems that are heterogeneous on the micron to submicron scale.

• Higher intensity focused x-ray probes to enable the next generation of research

• Focused beam instruments with a broad, tunable and scanable range of photon energy from 2-25 keV for elemental imaging and sub-µm spectroscopy

• Versatility of focal spot size and sample geometry to accommodate varying sample needs

1 The Periodic Table of the Elements 2

H He

3 4 accessible by KB branch 5 6 7 8 9 10

Li Be accessible by ZP branch B C N O F Ne

11 12 13 14 15 16 17 18

Na Mg Al Si P S Cl Ar

19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36

K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br Kr

37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54

Rb Sr Y Zr Nb Mo Tc Ru Rh Pd Ag Cd In Sn Sb Te I Xe

55 56 72 73 74 75 76 77 78 79 80 81 82 83 84 85 86

Cs Ba * Hf Ta W Re Os Ir Pt Au Hg Tl Pb Bi Po At Rn

87 88 104 105 106 107 108 109

Fr Ra ** Rf Db Sg Bh Hs Mt

57 58 59 60 61 62 63 64 65 66 67 68 69 70 71

* La Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu

89 90 91 92 93 94 95 96 97 98 99 100 101 102 103

** Ac Th Pa U Np Pu Am Cm Bk Cf Es Fm Md No Lr

* Accessibility of absorption edges. Accessibility to fluorescence lines even larger.


Beamline Requirements and SpecificationsBeamline Requirements and Specifications

LOI Proposal: A sub-micrometer probe, insertion device sector consisting of two beamlines, each supplied by an optimized undulator with the two undulators in a canted geometry.

• Station KB: – a Kirkpatrick-Baez mirror based instrument– energy range between 4-25 keV– spatial resolution adjustable from >1000 nm down to 100 nm– instrumentation for XRF, XAS, XRD and fCMT (achromatic + long WD)– 50x > flux than current KB-microprobes in a 2000 nm spot

• Station ZP: (not in initial scope)– a zone plate based instrument– energy range between 2-15 keV– target spatial resolution of 30 nm– instrumentation for XRF, XANES and imaging– 2x > flux than current ZP-microprobes in a 200 nm spot

• Share a common sample mounting and registry system


Scientific areas where SRX will enable significant advances Scientific areas where SRX will enable significant advances

• Health Hazards of Contaminated Materials, “Bad Metals” (contaminants in agriculture and drinking water, actinides from nuclear production, industrial emissions, mechanisms of toxicity)• Processes at the Interfaces between Minerals and Micro-organisms (biogeochemistry of microbe-mineral interactions, understanding biofilm processes , CO2 sequestration)• Global Effects of Particulates and Organisms in the Atmosphere and Oceans (metals cycling, effects on climate change, modeling airborne emissions)• Evolution of Our Solar System (interplanetary dust particles, comet dust, NASA sample return)• Environmental Genomics (metal homeostatis, ionomics, metallomics, biofuels studies)• Essential Metals in Cells and Organisms and in Disease Mechanisms (nutrient acquisition, metal detoxification, microbial pathogenesis, bioremediation, diseases related to altered levels of metal ions at subcellular level)

• Metals as Therapies (understanding molecular level mechanisms of metal based therapies)• Metals in Imaging and Diagnostics (imaging of metal contrast agents, molecular imaging of “marker” proteins)• Catalysis and Chemical processes on the Single Particle Scale (coupled µXAS/µXRD of catalytic particles and interfaces to follow processes such as oxidation)• Materials Science (elemental partitioning in microelectronics, elemental diffusion into microcrystalline domains due to aging of plastics and alloys, tracking redox changes of single particle contaminants in batteries and silicon solar cells)

photon energy [keV]

norm

. ab

sorp

tion

[a.u

.]

As3+

As5+

0.5

1.0

1.5

2.0

2.5

0.0

Linear combination (LC) best fit of standard spectra [scorodite (As ) and schneiderhohnite (As )]

XANES of roaster Fe oxide

5+

3+

68% As5+

32% As3+

Model CompoundLC Fit

1st Derivative of XANES Spectrum

500

0.0

-500

11.85 11.90 11.95

Walker et al., Can. Miner., (2006)

Twining et al., Anal. Chem. 75, 3806 (2003)

Light, epi, and SXRF (ZP) maps of a centric diatom

µ-XRF, -XRD, and –XANES of As bearing minerals in Au-tailings


SRX Project Beamline MilestonesSRX Project Beamline Milestones

SRX BAT Meeting and MOU Signing 10/30/08SRX BAT Meeting and MOU Signing 10/30/08• First SRX BAT meeting and MOU First SRX BAT meeting and MOU signing October 30, 2008.signing October 30, 2008.• Many design aspects since then Many design aspects since then adjusted to incorporate BAT adjusted to incorporate BAT recommendations already (Northrup, recommendations already (Northrup, Broadbent).Broadbent).• SRX Group Leader hired by NSLS-SRX Group Leader hired by NSLS-II project July 2009.II project July 2009.

• April 1, 2008 – SREEL BAT submits LOI to NSLS-II project.April 1, 2008 – SREEL BAT submits LOI to NSLS-II project.• LOI reviewed by EFAC at May 5-7, 2008 meeting (one of 11 LOIs). EFAC report LOI reviewed by EFAC at May 5-7, 2008 meeting (one of 11 LOIs). EFAC report received June 2008.received June 2008.• Microprobe spectroscopy beamline selected as one of the six beamlines to be built Microprobe spectroscopy beamline selected as one of the six beamlines to be built within the project scope September 2, 2008. Renamed SRX.within the project scope September 2, 2008. Renamed SRX.


Response to Comments from EFACResponse to Comments from EFACComment Response

The EFAC felt the case for the zone plate nanoprobe was notstrong. EFAC therefore supports the KB branch more strongly than the ZP one. Published KB designs can already reach 30nm.

KB branch will be constructed as part of initial project scope, optimized for 4.65-23.3 keV. ZP later (mature scope).

No coincident microscopy is planned: with 50-nm probes, visible-light microscopy cannot be used to identify the location of the chemical signatures in thin sections or on surfaces.

BAT has requested adjacent microscopy laboratory facility with integrated registry system for off-line characterization and targeting. On-line sub-micron XRD and phase contrast techniques will help. Other microscopies being evaluated.

EFAC felt that it might not be good policy for a centrally operated facility such as NSLS-2 to build beamlines catering to special interest groups such as earth, environmental and life scientists.

As a project beamline access to all users will be through the NSLS-II GU program and be merit based & peer reviewed. The BAT will consider if the NSLS-II PU proposals may be an avenue of enhancing support for key science groups.

“The EFAC was impressed with the presentation of a beamline plan to build a pair of undulator beamlines for the earth, environmental and life sciences. The design was one of the most detailed presented with full, realistic estimates of the sizes and apertures of all the optics (i.e. mirrors) needed to achieve the small spot sizes required.”

Thank You!


Beamline OverviewBeamline Overview

• Canted geometry consists of an undulator optimized for lower energy (ZP) in the upstream position and one optimized for higher energy (KB) in the downstream position.

• The total cant shown is 2 mrad. This is minimum acceptable, provides sufficient space to place separate apertures around each beam before they exit the shield wall and adequate separation in the end stations.

not in initial scope

100nm

30nmOnly one undulator

is in initial scope


SRX-KB Conceptual DesignSRX-KB Conceptual Design• Canted, on a short (low beta) straightCanted, on a short (low beta) straight• 4.65–23.3 keV incident photon energy 4.65–23.3 keV incident photon energy • Suitable harmonic rejection Suitable harmonic rejection • Continuously variable energy range over the energy range Continuously variable energy range over the energy range specified with no gaps specified with no gaps • No scientifically “important” edges (e.g. U L3) caught badly No scientifically “important” edges (e.g. U L3) caught badly in a transition between harmonicsin a transition between harmonics

RemovableRemovableAssume Windowless Ops.Assume Windowless Ops.

w/ differential pumpw/ differential pump

Phosphors, filters and imaging devicesPhosphors, filters and imaging devices

Cryogenically cooled Cryogenically cooled Horizontally diffractingHorizontally diffracting

Rh and bare Si stripesRh and bare Si stripes280 mm, 2.5 mrad inc. angle280 mm, 2.5 mrad inc. angle

w/ benderw/ bender

BPM and feedback to stabilize SHSBPM and feedback to stabilize SHS by controlling the HFM pitchby controlling the HFM pitch

100 mm H-KB, 280 mm V-KB100 mm H-KB, 280 mm V-KB< 0.2 µrad RMS (requires effort)< 0.2 µrad RMS (requires effort)

e-


SRX Conceptual DesignSRX Conceptual Design

SRX-KBSRX-KBhutchhutch

SRX-ZPSRX-ZPhutchhutch

FOEFOE

FOEFOE

ZP mirrorZP mirrorpairpair

KB & ZP DCM’sKB & ZP DCM’sKB HFMKB HFMPhotonPhoton

ShuttersShutters

Shielded Beampipe

Shielded Beampipe

downstream


SRX Conceptual DesignSRX Conceptual Design

2 mrad canting angle

KB

ZP

downstream


Vertical Optical Layout of the KB BranchVertical Optical Layout of the KB Branch

Small KBMirrorVertical(SKBV)

mmOAmrad

mL

4.15280.0

radRMSDeMag

keVE

E

Rh

c

20.0208

12

Focal Point@ 56.5m

mradmfwh

nmfwhm

V

V

5.2

70

.

Source

rad

mS

m

rad

mS

m

H

cohH

H

V

cohV

V

6.19

68

29

2.5

6.7

2.3

,

,

FrontEndAperture(FEFM+FEHA)

Horizontal FocusingMirror (HFM)

Vertical optics layout for the KB beamline showing a single 280 mm long vertical focusing mirror at 56.23 m

Calculations by Peter Eng (SRX BAT)


Horizontal Optical Layout of the KB BranchHorizontal Optical Layout of the KB Branch

Horizontal optics layout and scatter plots for the KB beamline with a secondary horizontal source at 53.6 m, produced by a horizontal focusing mirror at 34.8 m. Working distance ~ 30 mm.

Source Secondary Horizontal Source and Aperture (SHSA)

mFWHMH

37)3(

Horizontal Focusing Mirror (HFM)

mmOA

mrad

mL

0.3

5.2

2.1

radRMS

DeMag

E 4.0

85.1

keVE

keVESic

Rhc

14

24

Small KB Mirror Horizontal (SKBH)

mOA

mrad

mmL

500

5

100

radRMS

DeMag

keVE

E

Rhc

2.0

35

12

mradmfwh

nmfwhm

H

H

0.3

711099

Focal Point @ 56.5m

.

Secondary Source

SHSA = Open

2.7 μm

SHSA = 2.7 μm

2.7 μm

SHSA = 2.7 μm SHSA = Open SHSA = 2.7 μm

Horizontal [μm] Horizontal [μm]

Ver

tica

l [μ

m]

7% Transmitted

71 nm x 71 nm fwhm(H x V)

95% Transmitted

1099 nm x 70 nm fwhm(H x V)

rad

mS

m

rad

mS

m

H

cohH

H

V

cohV

V

6.19

68

29

2.5

6.7

2.3

,

,

Front End Aperture (FEFM + FEHA)

Calculations by Peter Eng (SRX BAT)


Selected SRX BAT RecommendationsSelected SRX BAT Recommendations

Items Status

Detailed interaction with BAT for individual components (use our expertise).

In progress, A. Broadbent and P. Northrup have had frequent meetings with BAT members on design

Pursue discussions with User community to prioritize research projects and allow them to open discussions with other funding agencies.

User workshop being planned by BAT for late 2009

Optical Design:• We envision the need to maintain sample/beam stability on the

sample at a 10 nm level. • Consider suggestions for BPMs – current plans may be inadequate

given likely stability requirements• Vigorous evaluation of beamline stability required.• BAT member collaborations with ASP on their microprobe design

shows significant potential similarities in design which can provide lessons learned.

• Commission an optical study from IDT (optical performance, thermal evaluation, stability requirements)

• Specification for energy stability and reproducibility recommended to be 0.1 eV

In progress:• P. Siddons and P. Yoon

developing BMP systems• Broadbent evaluating BPM

requirements and ASP layout• Optical Study commissioned from

IDT for summer 2009


Selected SRX BAT RecommendationsSelected SRX BAT RecommendationsItems Status

Sample Environments:Environmentally controlled hutches to reduce thermal instability, development and utilization of an active registry system for KB/ZP sample interchangeability (i.e. active laser interferometer ), specialized enclosed sample environment will be needed, cryo cooling, etc.

• To be evaluated.• XRadia chambers a potential starting design.

Beamline Controls: EPICS, but evaluate new User interfaces and hardware standards (eg. Fieldbus, Java IOC).

To be evaluated. Bob Dalesio (Controls Group Leader) will act as lead on this effort in collaboration with BAT.

IVU Recommendations:• 4 mrad canting angle should be pursued if possible (2 mrad is

absolute minimum)• Evaluate suitable devices to achieve 4.65–23.3 keV incident photon

energy, suitable harmonic rejection, continuously variable energy range over the energy range specified with no gaps.

• Evaluate of the feasibility of continuous scanning of the undulator gap with optical/interferometry feedback from the monochromator for spectroscopy

• Canting angles being evaluated by accelerator group.• P. Northrup and O. Tchoubar have evaluated IVU options and presented to BAT, candidate device selected (discussion follows).• IVU Feedback mechanisms to be evaluated.

Monochromator Design: consider the potential utility of a horizontally diffracting cryo-cooled DCM for SRX-KB (discussion follows).

Has been specified for evaluation as part of IDT optical study

* BAT Meeting summary contains many additional suggestions * BAT Meeting summary contains many additional suggestions and recommendations.and recommendations.


NSLS-II Accelerator RestrictionsNSLS-II Accelerator Restrictions

• The device length, for a given minimum gap, is defined by the beta function for the straight. Minimum allowable gap of 5.0 mm.

• IVU must fit in half-straight with room for canting magnets. • This means that 0.5m needs to be removed, then space divided in half,

as two devices are fitted to the straight.


Evaluation suggests a 1.5 m long, 21 mm period device with a minimum magnet gap of 5.5 mm will provide excellent performance at the lowest specified energies at the 3rd harmonic energy for 3.0 GeV beam < 4.65 keV. This will also provide at the highest operational energy range (23.3 keV Rh K edge practical limit).


Potential SRX Monochromator DesignPotential SRX Monochromator Design

Australian Synchrotron’s X-Ray Fluorescence Microprobe Australian Synchrotron’s X-Ray Fluorescence Microprobe horizontally diffracting monochromator:horizontally diffracting monochromator:

• No gravity effect, eliminating distortions such as crystal cage twist and sag and unwanted angular rotations of the second crystal.• Eliminates need for longitudinal second crystal translation stage • A properly designed horizontal DCM can be mechanically more stable particularly as energy is changed.• Horizontal deflection can increase separation between the KB and ZP branches.• Horizontal diffraction will enable the beam defining aperture to filter out any horizontal vibration and slope errors.• Space for incorporating interchangeable lattice cuts, including Si(311) DCM and DMM as potential upgrades.• Potential performance benefits of utilizing dread-lock vs. braided copper cooling designs.

Potential complications to evaluate:Potential complications to evaluate:• Intensity loss of intensity due to polarization losses • Potential beam divergence effects compared to vertical geometry

ASP Microprobe DCM


Overall Project Beamline BudgetOverall Project Beamline Budget

• SRX Cost Estimate is $10,707,772• The costs were adapted from XAS• XAS SRX swap is feasible with $1.9M, mainly from high-heatload optics, redirected for ID development and purchase (which XAS didn’t incur)• Detailed cost re-analysis is part of planned FY09 design efforts (SRX Group Leader)• Only the KB branch of SRX is included in baseline, but space and design accommodations are made for development of ZP branch


Conceptual Design Report due September 2009Conceptual Design Report due September 2009

• Next BAT meeting June/July 2009• Group Leader on hand• IDT optical report will be in hand summer 2009• NSLS-II and SRX front end design refined• Undulator specs refined and incorporated into SRX

design• Cost estimate and schedule updated• Beamline scientist hired• User Workshop by end of 2009

Documents

1 BROOKHAVEN SCIENCE ASSOCIATES NSLS-II SRX Beamline Tony Lanzirotti SRX Beamline Advisory Team Chair The University of Chicago, CARS Experimental Facilities