Technology Development Lance Cooley TD / SRF Development Dept. / - - PowerPoint PPT Presentation

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Technology Development Lance Cooley TD / SRF Development Dept. / - - PowerPoint PPT Presentation

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Technology Development Lance Cooley TD / SRF Development Dept. / SRF Materials Group Leader f Goals for SRF Materials R&D Goals for SRF Materials R&D Fermilab Our job is to figure out Feb09 vs Nov08 how to advance the Target

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Technology Development

Lance Cooley

TD / SRF Development Dept. / SRF Materials Group Leader

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Fermilab 2

Goals for SRF Materials R&D Goals for SRF Materials R&D

  • Our job is to figure out

how to advance the state of the art.

  • Goal: Advance the state
  • f the art toward the

2012 ILC goal (90% yield at 35 MV/m)

– This goal also satisfies performance goals for Project X.

  • Goal: Can we define

and approach even higher limits?

Feb09 vs Nov08

Target ILC yield in 2012 Target ILC yield in 2009 25 MV/m

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Fermilab 3

Baseline fabrication sequence Baseline fabrication sequence

Geometry difficult Clean weld Cavity shape Ductility, flatness Make sheets Uniform props Clean, high KTh EAcc∝RRR1/2

Why?

End pcs weld Dumbell weld

(from outside)

Iris weld

(from inside)

Form ½ cells Deliver Rx and level Roll Forging Melt Nb

Step

RGA, qualification EBW + tooling RGA, qualification EBW + tooling RGA, qualification EBW + tooling Tune Die + press ECS, RRR, Microscopy, mechanical meas. Flatness spec Elongation spec High-vac Oven, Proprietary Grain size spec, surface finish spec Mill, Oven Proprietary Grain size spec Forge RRR ~ 300 E-beam melt

ASTM Spec, QA/QC Tool / facility At niobium vendor At cavity vendor

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Fermilab 4

Baseline processing sequence Baseline processing sequence

RGA High-Vac Oven

Hydrogen

800 °C bake Temperature BCP tool + Acid

Better heat xfer

Outer etch

( It works ) Dust

  • Chem. Residue

Smooth surface Shape changes

  • Chem. Residue
  • Fab. damage

Why?

Low-T oven 120 °C bake HPR + UPW, class 10 Rinse Tmap, Opt Inspx VTS

  • Vert. test

Vac, Class 10 Assemble US + UPW + alcohol? Wash Raman, T, V(I) EP tool + Acid Fine EP Tuning machine Re-tune US + UPW Wash Raman, T, V(I) EP tool + Acid Bulk EP

Ultrasonic tank (US) + ultra-pure water (UPW)

Degrease

  • Opt. Inspx, Dim.

Receipt

Diagnoses, QA Tool / Facility Step

FE

Quench

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Fermilab 5

Issues lurk at every step because the art is based on Issues lurk at every step because the art is based on recipes and not on understanding recipes and not on understanding

  • Raw material

– Niobium is not “sheet metal” – Each batch is different! – Grain texture affects later forming and chemistry – Alternate: Ingot slices (Lg gr)

  • Forming

– Shear is required to maintain thickness – shear bands promote dislocation etch pitting – Keeping ductility imposes restrictions on raw material

  • Welding

– Pits! Many mechanisms are plausible – Tooling, vacuum artifacts – Vendor experience varies – Remove forming history? – Alternate: hydroforming

  • Tuning: Heat treatments soften

metal, promote detuning

  • Chemistry

– Acids are dangerous – Acid reactions are very sensitive to process params, mat’l history – EP does not obey “classic” science; high flow is used – Cavity surface is complex – how to model and control? – Alternate: Non-HF process

  • HPR:

– Ablative – What is being removed? Damaged? – Assembly experience varies

  • Diagnoses:

– Can’t touch RF surface! – Repair in situ?

  • ALD, etc.: New! What’s the payoff?
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Fermilab 6

Optical inspection – Optical inspection – key breakthrough! ey breakthrough!

Hayano group, Kyoto Image enhanced by FSU

  • D. Sergatskov, C. Ginsburg FNAL

Thermometry locates hot spots

Hot spots correlate with location of defects (pits)

Seeing the microstructure provides the feedback needed to drive the materials science! Seeing the microstructure provides the feedback needed to drive the materials science!

WELD

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Fermilab 7

Management to address issues Management to address issues

  • FNAL cannot do everything – therefore we coordinate

a comprehensive array of ~30 partners from academia, labs, and industry (next slide)

– Many will be supported with ARRA funds – Primary reporting is via SRF Materials Workshop

  • FNAL is organizer
  • HEP, JLab, Cornell, FSU, MSU also on program committee
  • FNAL maintains QA/QC to support fab and processing
  • FNAL conducts some basic work and processing R&D
  • FNAL performs activities not easily done by partners

– Pre-weld, coupon, and cavity acid work – HPR, assemble, and test – Diagnostics, including T-mapping, optical inspx., and ECS

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Fermilab 8

U.S. Materials R&D Community U.S. Materials R&D Community

Surface Science

FSU U Chicago IIT Maryland ANL-APS William & Mary Virginia Tech

Materials Science

Florida State Michigan State Northwestern UIC

Processing Science

FNAL JLab Cornell ANL Ohio State Northeastern Nevada-Reno Texas A&M Black Labs Interlaken VCU

  • Penn. State

ABLE EP Cabot Faraday Inc

Niobium vendors

ATI Wah Chang HC Starck (Foreign vendors)

Cavity vendors

AES Niowave (+Roark) PAVAC Sciaky (Foreign vendors)

Mgmt.

FNAL JLab Cornell

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Fermilab 9

Ties with international materials community Ties with international materials community

  • Participate on organizing and program committees for

SRF Workshop, TTC, Thin Film SRF Workshop

  • Integration with S0 and GDE periodic meetings
  • Broader interaction with large conferences and

journals

– ASC 2008 special session – ICMC 2009 plenary

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Fermilab 10 10

Shepherding the Materials Community Shepherding the Materials Community

  • Labs’ role:

– Steer the agenda, define issues – Get samples to academics = coupons and pieces cut from cavities – Zero in on real defects = ECS, optical inspection, T-map – Develop processing = do work, modify based on understanding – Facilitate ideas = get 1-cell cavities to SBIRs, labs, academics – Drive vendor development = buy cavities, transfer processes – Test cavities from vendors and give feedback

  • Academics’ role:

– Provide understanding based on materials, physics, and chemistry – Provide reality checks, define limits, describe mechanisms

  • Industry role:

– Define the fabrication and processing realities – Engage in dialogues with academics and labs – Deliver cavities – Generate new ideas (SBIR)

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Fermilab 11 11

Means to fill the lab role Means to fill the lab role

  • Routes to understanding require

control over all steps

  • We have our own Nb supply and

conduct QA

– Also supports procurements – ~1 ton eddy-current scanned by end of FY09 – RRR and other diagnoses – SEM, Instron, CryoInstron (MSU)

  • Coupons and single-cell forming

& welding done by us

– We do the weld prep and etch – We presently rent Sciaky EBW – We plan to buy and support an e-beam welder – ARRA

  • 1-cell inventory for R&D / SBIR

(16 3.9GHz + 18 1.3GHz)

  • Dedicated single-cell chemical

processing in IB4 – op. mid FY10

– TD investment to support SRF – ANL facility busy with 9-cell production – We need to vary parameters and try new ideas, too

  • Dedicated lab area
  • Dedicated HPR and assembly –
  • p. end FY09
  • Dedicated single-cell test @ A0

– Now op.; set up by 3.9GHz SRF – IB1 VTS busy with 9-cell

  • Tumbling machine – op. June 09

– Enables non-HF cavity R&D

  • Diagnoses – plan for dedicated
  • ptical inspection
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Fermilab 12 12

New coupon tools New coupon tools

New coupon EP tool New coupon EP tool New witness sample fixture New witness sample fixture

Sample Same elliptical shape as 1.3 GHz cavity Fixture goes in-line with standard EP tool

Ready for draft and build In operation

Heat exchanger for temperature control, pH monitoring, pumped acid

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Fermilab 13 13

Single-cell R&D FY09-FY12 Single-cell R&D FY09-FY12

  • Approx. 50 cavities, 90

processes, and 125 tests

– See A. Rowe breakout talk

  • Vendor qualification

– Niowave-Roark, Accel and AES – 6 cavities from each – Other N. America

  • Tool / facility qualification

– ANL facility – Single-cell VTS – Tumbling machine at FNAL – EP industrialization at ABLE – Optical inspection benchmark – NR-4

  • Processing R&D

– 2 ECS defect cavities – 6 cavities planned – study material variations… – …then carbon removal – 6 cavities - EP science

  • Alternate

– 2 cavities - Large grain and single crystal cavities – 6 cavities - Non-HF processing, tumbling, CMP – Planned hydroforming

  • New ideas

– 4+ cavities - ALD cap – ALD multilayer, Nb/Cu – MgB2 cavities – SBIR

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Fermilab 14 14

Single-cell chemistry area (op. late FY10) Single-cell chemistry area (op. late FY10)

Acid storage Acid storage EP Cabinet EP Cabinet Scrubber & Neutralizer Scrubber & Neutralizer

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EP tool development EP tool development

Prototype Prototype

Generation 2 EP tool Generation 2 EP tool

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Single-cell clean room and HPR (op. FY10) Single-cell clean room and HPR (op. FY10)

Class 10 clean room Class 10 clean room

Certification and training 5/20/09

HPR Pump Location

  • f

HPR “Shower Stall” Dessicator for HPR mists

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Tumbling and non-HF processing Tumbling and non-HF processing

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Fermilab 18 18

Capabilities Capabilities

  • ~100 coupon samples per year – should saturate

academics

  • ~30 single-cell acid processes per year late FY2010

– Limited by staffing, facility is capable of 50 or more – Supplying “qualified” 1-cells requires ANL-FNAL at present

  • ~50 HPR 1-cell processes per year starting FY2010

– Excess capacity expected to support 9-cell work

  • ~30 vertical tests per year, staff shared with AD
  • EP team, Diagnosis team, QA team, Alternates all

meet present needs; ~2 postdocs to be added

  • See A. Rowe talk for more details
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Coupon EP1-1

210 total µm removed

RF side

Example: Rapid information return from academics Example: Rapid information return from academics (Here: Does pit morphology (Here: Does pit morphology indicate how it formed?) indicate how it formed?)

Blue-to-orange depth 60 µm Is there a “moat”?

100 µm FNAL Keyence 3D microscopy

Pit 1

~ 3 inches Pit Row via stitching anaglyph @ FSU (Lee, Sung) Pit Row via stitching anaglyph @ FSU (Lee, Sung)

Carbon ??

250 µm Carbon ??

Cross-section of Pit 1 cut and polished @ FSU (ZH Sung, PJ Lee) Then SEM with Orientation Imaging Microscopy Cross-section of Pit 1 cut and polished @ FSU (ZH Sung, PJ Lee) Then SEM with Orientation Imaging Microscopy

1 grain

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Example: coordination of co Example: coordination of complementary measurements mplementary measurements validates observations validates observations

Pit in TE1AES004

µm 10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190 200 210 220 230 240 250 260 270 280 290 300

Profilometer 5 x 5 mm, 0.3 mm ∆z FNAL Silicone molding was used to make a replica of this pit Silicone molding was used to make a replica of this pit Replica shows a raised feature in the center seen both by profilometer and Keyence 3D microscopy Replica shows a raised feature in the center seen both by profilometer and Keyence 3D microscopy FNAL Keyence 3D microcopy 300 µm x 300 µm x 15 µm Keyence 200 µm 15 µm

µm

  • 60
  • 50
  • 40
  • 30
  • 20
  • 10

10 20 30 0.5 1 1.5 2 2.5 3 3.5 4 4.5 5 mm Length = 5.02 mm Pt = 108 µm Scale = 108 µm

Profilometer 200 µm 15 µm

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Example: Understanding comes Example: Understanding comes at high levels of detail at high levels of detail (Here: understanding the impact (Here: understanding the impact of raw material variability)

  • f raw material variability)
  • Prof. Tom Bieler, MSU

Blue is good, Red is ok, Green is bad SEM with Orientation Imaging Abrupt changes in color may be bad

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Example: Synergistic studie Example: Synergistic studies determine basic SRF limits s determine basic SRF limits (Here: possible explanation why lo (Here: possible explanation why low-T baking improves cavities) w-T baking improves cavities)

  • IIT: magnetic scattering

(never considered before)

– Proslier et al., APL 92, 212505 (2008)

  • Oxygen defects are magnetic

(Cava et al., 1991)

  • Chicago: Nb2O5 formed after

etching is defected

  • Thus mild baking…

– Thickens the sub-oxides and reduces scattering – Heals defects

  • Then: Capping by ALD + bake

improves Nb

– Proslier et al., APL 93, 192504 (2008) superconductor point-contact junction X-ray photoelectron spectroscopy

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Example: Materia Example: Materials community s community synergism produces collective synergism produces collective effort greater than individual effort greater than individual parts (Here: Hydroforming) parts (Here: Hydroforming)

  • Main issue: raw material

(fine-grained annealed tubes)

  • No single vendor could take

this on – big problem!!

  • New advances at Wah Chang,

Texas A&M, and Nevada Reno make significant headway

– Not competition; all ideas fit together and address main issues

  • National effort now being
  • rganized, will initially use 3-

cell DESY tool and then transfer to American Hydroforming for full 9-cell

Fine-grained tube produced by Wah Chang for Black Labs Single Crystal tube produced by Nevada-Reno

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Response to issues i Response to issues is broad and enthusia broad and enthusiastic stic

  • Raw material & Forming

– Texture & forming: MSU, BL, TAMU – Impact of forging history: MSU, FSU, NWU, UC – Alternate: MSU, Niowave, FSU – Ductility: BL, MSU, TAMU, WahChang – FNAL spec – QA: ECS 1-cell – Standards: OrSU, FSU

  • Welding

– Pits: FSU, MSU, IIT, NWU, UC, vendors – coupons & 1-cells – Tooling, vacuum, experience: vendor round-robin – Annealing etc: multi-vendor 1- cells, also FNAL coupons – Hydroforming: MSU, UNR, BL TAMU, WahChang, DESY, Interlaken, Amer. Hydroforming,

  • Chemistry

– EP science: FNAL group, NWU Ph.D. thesis, ABLE EP – Non-HF EP: FNAL, Faraday Inc, – Non-HF process: FNAL tumbler + Cabot, Northeastern

  • HPR

– Plasma clean: Dzubya M.S. – Identify Field emitters: ORNL

  • Diagnoses / Repairs:

– Augmented Opt. probe: IIT Joint faculty, U Maryland – Remelting

  • ALD, etc.: 6 1-cells planned

Univ SRF $$ SBIR SBIR SBIR ARRA ARRA SBIR SBIR

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Conclusions Conclusions

  • A synergistic, coordinated, and broad community has

been mobilized and are producing exciting science

– SRF University $$ will greatly accelerate the development of materials-based understanding

  • It has been kept alive with small seeds and the investigators’
  • ther resources; previous main grants have lapsed

– FNAL will continue to shepherd; workshop pace will double

  • We are converting from processes based on recipes

to processes based on understanding!

  • Progress on basic SRF themes continues as well.
  • FNAL SRF Materials Group – internal R&D topics

– Non-HF, Hydroforming (coord), EP science, coupons, laser remelting, diagnostic R&D, EP processing, HPR, Vert. test.