ANSI ASC OP Task Force 6: IR Materials Standards and SPIE IR - - PowerPoint PPT Presentation

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ANSI ASC OP Task Force 6: IR Materials Standards and SPIE IR - - PowerPoint PPT Presentation

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1 ANSI ASC OP Task Force 6: IR Materials Standards and SPIE IR Materials Standards Working Group Wednesday, April 22, 2015 Baltimore Hilton Hotel 08:00 10:00 EDT 401 West Pratt St. Baltimore, MD 21201 SPIE DSS Calloway A Room

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ANSI ASC OP – Task Force 6: IR Materials Standards and SPIE IR Materials Standards Working Group

Wednesday, April 22, 2015 08:00 – 10:00 EDT SPIE DSS Baltimore Hilton Hotel 401 West Pratt St. Baltimore, MD 21201 Calloway A Room

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1. Welcome, Introductions, and appointment of note taker – A. Phenis 2. Appointment of note taker – A. Phenis 3. Adoption of agenda – A. Phenis 4. Approval of previous meeting minutes – A. Phenis 5. Reports

1. Pilot study status update – A. Phenis 2. Submitted projects update (OEOSC) – D. Aikens 3. Refractometer measurements update (NIST) – J. Burnett 4. Other reports and updates – Project Leaders

6. Group Discussion Topics – A. Phenis 7. Time and Place for next meeting - suggestions

1. Teleconference 2. SPIE Annual Meeting, San Diego, CA August 9th – 13th, 2015 3. SPIE DSS, Baltimore, MD April 18th – 22nd, 2016

8. Adjourn – A. Phenis

Draft Agenda

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Welcome

  • ASC OP/TF6 (OEOSC)
  • Write the materials standards standards
  • Coordinate with other TF developing supporting standards
  • IRMSWG (SPIE)
  • Advise TF6 regarding instrumentation and measurement methods
  • Meetings will consist of status reports, technical evaluations, recommendation
  • Work the details of the measurements
  • Test plans
  • Instrument development /upgrades
  • Sampling protocols
  • Sample specs and procurement
  • Identify funding sources
  • All documents from this meeting will be posted to:
  • http://www.optstd.org/op1%202015meetings.htm

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Approval of previous meeting minutes

  • Previous meeting minutes can be found at
  • http://www.optstd.org/OP1%20Meeting%20Docu

ments/2014/TF6/140505%20Draft%20Minutes% 20ASC%20OP%20TF6%20IR%20Materials%20 v1.pdf

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SLIDE 5

Reports

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Pilot study status update

  • A. Phenis – Cymer, an ASML Company

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Study Status

  • NIST has started testing with Germanium
  • Testing has been prioritized by the results from a survey

done by Gary Wiese (April 2013)

  • The testing order/priority can change based on what is available

at NIST.

  • NIST will start at the highest priority and move down the list

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Pilot Study Material Status

Measurement Priority Material Supplier Status 1 Germanium Photonic Sense GmbH Samples delivered, Measurements underway 2 ZnSe II-VI NA 3 Multispectral ZnS (Cleartran) DOW NA 4 Silicon Lattice Materials NA 4 Silicon Novotech NA 5 CaF2 Fairfield Crystal NA 5 CaF2 Hellma Materials GmbH Expected delivery May 2015 6 BaF2 Fairfield Crystal NA 6 BaF2 Hellma Materials GmbH Expected delivery May 2015 6 BaF2 ISP Samples delivered 7 IRG26 (As2Se3) Schott Delayed due to factory fire, Expected deliver TBD 8 GASIR1 Umicore Expected delivery June 2015 9 BD2 glass (Ge28Sb12Se60) Lightpath Technologies NA

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Submitted projects update

  • D. Aikens – OEOSC and Savvy Optics, LLC

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Spectral Bands – OP1.007

  • Draft standard OP1.007 submitted for review
  • Ballot complete; 7 votes received, one page of comments
  • Draft has been revised to accommodate comments
  • Added table for reference wavelengths by band for measurements
  • Modified ranges based on input
  • Ballot has been submitted to entire ASC OP for adoption as an

American National Standard

  • Ballot is due by June 19, 2015
  • If approved by 20 ballots, it will be submitted to ANSI for publication

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Sampling protocol– OP1.008

  • Project initiation approved by ANSI
  • Draft standard OP1.008 submitted for review
  • No comments received
  • TF6 ballot has begun
  • Ballots due by July 19, 2015
  • Will revise draft to accommodate comments
  • Presuming it does not need to be reballoted, can then be submitted to

ASC OP for adoption as an American National Standard

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Measurement Methods

  • Bubbles/Inclusions
  • Chinese resubmitted proposal for an ISO standard on IR impurities based on bright field inspection
  • Straie
  • Chinese resubmitted proposal for an ISO standard on straie based on a shadowgram
  • Homogeneity
  • Chinese resubmitted proposal for an ISO standard on homogeneity based on interferometry
  • All three have been approved as New Work Items; US experts are Eric Stover,

Leonard Hanssen and Adam Phenis

  • Others are welcome to join; see Leonard for more information
  • We should be able to influence the development of these standards to be

acceptable to us

  • Leonard Hanssen, head of the US delegation, will continue to manage these

activities

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Measurement Methods (continued)

  • Refractive Index
  • Plan to use ISO 17328 as starting point, but publish our own

American National Standard version

  • NIST to draft document based on NIST measurement method
  • Waiting for NIST draft
  • dn/dT
  • can be incorporated into RI measurement standard
  • Absorption/Transmission
  • Plan to use ISO 15368; need to revise and update
  • Leonard and Dave will work at the ISO level to start a project for

revision

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SLIDE 14

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Other Standards

  • Material properties specification and grades
  • Currently monitoring work in TF1 for a new standard for raw optical glass
  • New standard includes grades for index, homogeneity, straie, bubbles,

inclusions, etc.

  • May be able to use the same grades for IR materials
  • Material properties library for design codes
  • Schema developed by ORA in coordination with Zemax and Lambda
  • Other code houses have not responded
  • Waiting for sample data from the pilot campaign to try it out
  • Can publish the schema as American National Standard once the

schema is confirmed

  • Can’t really offer it to ISO due to conflicting standards
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Refractometer measurement update

  • J. Burnett – NIST

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Other reports and updates

Project Leaders

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Group Discussion Topics

  • A. Phenis – Cymer, an ASML Company

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NIST IR Materials Pilot Study - Update

John Burnett, Leonard Hanssen, and Simon Kaplan

National Institute of Standards and Technology Physical Measurement Laboratory john.burnett@nist.gov

SPIE DSS 2015 – IRMSWG Meeting – 22 April 2015

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Outline

  • 1. NIST Refractometry System
  • 2. NIST Commitment to IR Materials Index Pilot Study
  • 3. Index Measurement Issues
  • 4. IR Refractometry Capability
  • 5. Measurement Schedule
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NIST Refractometry System

SPIE DSS 2015 – IRMSWG Meeting – 22 April 2015

19 NIST Refractrometry Facility located at NIST AML 217/F117 goniometer entrance/collimation box exit/collimation box (rotates) detector purged sample chamber sample prism temp control system entrance slit exit slit

  • All reflective optics + purge housing + sources/detectors ⇒ operates VUV (120 mm) through near-IR.
  • Temperature range - operates normally near room T (15 - 25 °C).
  • Specs.:
  • FL=0.5 m, F/# = 10.
  • Goniometer - calibrated angle encoder scale: absolute angle uncertainty ≤ 0.2 arc-sec.
  • Feedback temperature control of sample to ≤ 5 mK, purge gas to to ≤ 10 mK.

⇒ Absolute index uncertainty ≤ 5 × 10-7 routinely attained in visible and UV. dn/dT in range T (15 - 25 °C).

  • Delivering index results with above uncertainty in UV/vis to the semiconductor lithography industry.

⇒ For lens design and lens material quality control, needs absolute sub-ppm index measurements. NIST focus has been highest-accuracy index in vis/UV. Laborious process, at least 1 week/sample. 1) Developing index database for values for important optical materials. 2) Accuracy allows investigation of index variations between nominally the same materials.

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NIST Commitment to IR Mat’ls Index Pilot Study

SPIE DSS 2015 – IRMSWG Meeting – 22 April 2015

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In response to request, NIST (with director’s blessing) committed in 2013 to participate in IR Materials Index Pilot Study with a direction of substantial resources to make most accurate index measurements of key IR materials.

  • Upgraded sub-ppm-accuracy UV-vis Min-Dev refractometry facility for λ ~14 µm.
  • Goal - Maintain UV-vis capability while achieving highest possible IR accuracy.
  • Completed and tested in Jan 2015.
  • Worked with Gary Wiese (Lockheed) to develop optimal specs. for key materials:

Ge (single X’tal), ZnSe, ZnS, Si (single X’tal), CaF2, BaF2 (poly), GASIR1 (Umicore glass), IRG26 (As2Se3) (glass), BD2 (glass), GaAs (single X’tal), Spinel, AMTIR5 (As-Se), IR Fused Silica, LiF, MgF2.

  • Materials received (multiple samples from different boule locations):

Ge prisms: 15 (Photonic Sense (Reynard Corp) (Apex Ang. 15° nom) 1/25/15. BaF2 (poly): 2 (ISP Optics Corp.) (Apex Ang. 15° nom) + 6 plates. 3/11/15.

  • Jan. – March, NIST complete other commitments. Started on Ge in April.
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IR Mat’ls Index Pilot Study – Uncertainty

SPIE DSS 2015 – IRMSWG Meeting – 22 April 2015

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Estimated Uncertainty

  • For each material, investigated estimated uncertainty vs. sample specs.
  • prism geometry (apex angle), surface figure (Zernike coefficients).
  • For example, as λ gets longer
  • Uncertainty due to diffraction width increases
  • Uncertainty due to figure error decreases.
  • Developed optimal specs. for each material
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Index Measurement Issues

SPIE DSS 2015 – IRMSWG Meeting – 22 April 2015

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High-Accuracy Index Measurements: Determine index from minimum-deviation-

  • angle. Actually, requires numerous measurements w/ numerous sources of error.

At Minimum Deviation Angle Dev Angle

Goniometer w/ calibrated encoder Alignment issues (∆θ ≤ 0.2 arc-sec)

Prism Surface Flatness

Zygo Interferometer (Wavefront RMS λ/40)

Prism Apex Angle

Auto collimator + encoder (∆θ ≤ 0.2 arc-sec)

Temp Control – dn/dT

TWP and MPGa calibration (∆T ≤ 5 milli K)

λ Calibrations

Spectral calibration lamps (∆λ ≤ 0.01-0.1 nm)

Material Absorb.

Transmission spectrometer (A10 ≤ 0.01/cm)

Index Homogeneity

n variation on ingot ⇒ n variation on sample Vis/UV interferometer (∆n ≤ 1 x 10-7)

Stress Birefringence

grown-in or external (stress-optic coeff. - πijkl) Polarimeter (1 nm/cm [∆n ≤ 1 x 10-7])

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Temperature Control

Sample- and gas-temperature control by PID feedback control loop.

  • PRT thermometers calibrated at triple-point water and melting-point of Ga.
  • PID control loop using mixing of hot and cold baths.
  • Controls absolute temperature < 5 mK (<2 mK RMS).

SPIE DSS 2015 – IRMSWG Meeting – 22 April 2015

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prism sample Heat bath (<set point) Pre-cool heat bath Heat bath (>set point) PID Control System proportional valve PRT thermometers mixed just before sample feedback loop

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Temperature Control

Ge prism sample mounted in temperature-control stage.

SPIE DSS 2015 – IRMSWG Meeting – 22 April 2015

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Temp control water jackets PRT holders tilt-alignment motors calibrated strain mounting input water hoses

  • utput water hoses

Ge prism (15° apex angle) PRT holder

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IR Refractometry System

λ range to IR – λ=0.12-14 µm (T=15-25 °C)

(Consistent w/ ISO/TC 172/SC 3 N223 Test Method for IR Index)

  • All reflective optics from source to detector.
  • Blackbody source (1200 °C), 1 m FL monochromator - Resolution at λ =5 µm ~ 0.1 nm.
  • IR detector (Liquid N2 cooled MCT), lock-in detection.
  • Index accuracy ~1 × 10-5 for λ = 1 µm - 14 µ m – now being verified (dep. on material, prism specs.)

McPherson Model 2061 1 m FL Monochromator (λ=185 nm – 20 µm) (Res=0.01=0.2 nm) Spectral Line Sources (120 nm – 2.5 µm) Autocollimator for alignment and apex angle measurements material prism entrance slit exit slit IR detector: L-N2 cooled MCT w/ lock-in detection θ/2θ stacked goniometers Res: 0.2 arc-sec

Minimum Deviation Refractometer Layout (FL=0.5 m, F/#=10, temp control: 2 mK rms)

vertically-stacked parabolic mirrors entrance slits exit slit blackbody source 1200 °C chopper

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SPIE DSS 2015 – IRMSWG Meeting – 22 April 2015

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NIST Refractometry System – Source Side

Blackbody source 1200 °C collection mirror chopper turning mirror entrance slit 1-m FL grating monochromator spectral sources UV-vis- near IR exit slit input parabolic mirror Refractometer entrance slit

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SLIDE 27

SPIE DSS 2015 – IRMSWG Meeting – 22 April 2015

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NIST Refractometry System – Refractometer Side

autocollimator for apex-angle measurements input parabolic mirror entrance slit nested goniometers/ encoders exit slit purged sample chamber MCT detector Temp-controlled gas lines and Temp sensors lines entrance collimating optics exit focusing

  • ptics
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SLIDE 28

SPIE DSS 2015 – IRMSWG Meeting – 22 April 2015

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NIST Refractometry System – Sample Chamber

purged sample chamber - open Temp control water tubes and Temp sensor lines Sample Temp control water jackets PRT prism Temp sensors entrance

  • ptics

exit

  • ptics

prism sample PRT gas Temp sensor

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Measurement Schedule - Ge

  • Goal: for each material, measure samples from various locations in the

ingot to assess growth-position dependence.

  • IR Sampling protocol of September 2014 – For Ge:

SPIE DSS 2015 – IRMSWG Meeting – 22 April 2015

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  • For Ge, 15 samples, 5 per layer.
  • Due to priorities for now, for Ge, 6 samples is reasonable.

Will measure the center sample and 1 edge sample from each layer.

  • Have started with center layer, center sample.

The first sample takes longest because finding parameters and optimizing trade-off, such as resolution and S/N at each λ.

  • After this, each sample takes about 1 week.
  • Expect to complete Ge in early July.
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Measurement Schedule – Other Materials

  • After we complete Ge, we will measure the next material that this group

decides is next highest in priority, if this materials has been delivered.

  • Priority List 2014

SPIE DSS 2015 – IRMSWG Meeting – 22 April 2015

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  • The 2nd sample received is BaF2 poly.
  • Will measure this next unless one higher on the list is delivered.

Priority Material 1 Germanium 2 ZnSe 3 ZnS 4 Silicon 5 CaF2 6 BaF2 7 GASIR 1 8 IRG26 9 BD2

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Measurement Schedule – Other Materials

  • As measurements are completed, the turn around will become somewhat faster

– but probably not by much!

  • NIST facilities set up for high-absolute-accuracy, NOT high-throughput.
  • Expect no faster than 1 sample/week ⇒ 1 material/2 months.

⇒ Multi-year project.

  • We expect that at least for some materials, NIST will establish generic values

and ranges.

  • Other methods (e.g., prism coupling techniques), faster/commercial apparatus.
  • Not as accurate as Min-Dev method, but good at relative measurements.
  • Hoped that good correlations will be found between sample differences

found at NIST by the Min-Dev method and by commercial methods.

  • Ideally NIST could measure just one or a few samples for a new material,

and sample/batch variations determined by faster commercial methods.

  • NIST intends to publish data from the important materials.
  • Set up NIST materials index database (UV-vis-IR), w/ dn/dTs near 20 °C.
  • Longer term: increase T range – cryogenic → >> RT.

SPIE DSS 2015 – IRMSWG Meeting – 22 April 2015

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Time and place for next meeting - suggestions

  • 1. Teleconference
  • 2. SPIE Annual Meeting, San

Diego, CA

  • 1. August 9th – 13th, 2015
  • 3. SPIE DSS, Baltimore, MD
  • 1. April 18th – 22nd, 2016

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Adjourn

All meeting documents will be posted to: http://www.optstd.org/op1%202015meetings.htm

Thank you for coming to this meeting and we look forward to seeing you in future meetings.

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