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Step 08 Metrology & QC

Spectroscopic Ellipsometer

J.A. Woollam Co., Inc.

: MEDIUM-HIGH ● Essential for As₂S₃ stoichiometry verification (GAP03) and SiN quality control (Flagship)

Role in QLT Fabrication

Why Ellipsometry Matters for Quantum Photonics

The ellipsometer measures polarization change of reflected light to determine thin film thickness and optical constants (refractive index n, extinction coefficient k). For QLT's quantum photonic chip, refractive index accuracy is mission-critical because the entire device operation depends on precise phase matching.

PHASE-MATCHING CONDITION FOR OPTICAL PARAMETRIC CONVERSION (OPC):

Δk = 2k_pump - k_signal - k_idler = 0

k = (2π/λ) × n_eff(λ, n_core, n_clad, geometry)

where n_eff depends on:
- n_core = f(n_SiN, n_As₂S₃)  → MUST know these precisely
- n_clad = f(n_SiO₂)           → MUST know this precisely
- waveguide geometry (width, height) → from profilometer/AFM

SENSITIVITY:
If As₂S₃ refractive index n deviates from design value of 2.43 by Δn = 0.02:
→ Phase-matching bandwidth collapses
→ OPC efficiency drops by > 10 dB
→ Quantum state generation FAILS

REQUIREMENT: Know n of As₂S₃ to ± 0.01 at 1550 nm
→ Only spectroscopic ellipsometry can provide this accuracy

Specific Measurements

MeasurementMaterialTarget nTarget ThicknessToleranceProcess Step
Refractive index @ 1550 nmAs₂S₃2.43N/A± 0.02G3 QC ● stoichiometry verification
Film thicknessAs₂S₃N/A500 nm± 5 nmG3 QC ● more accurate than profilometer
Refractive indexSiN (incoming)1.99 @ 1550 nm~800 nm± 0.01A1 Incoming QC
Refractive indexSiO₂ cladding1.45 @ 1550 nm~3.3 μm± 0.01A1 Incoming QC
Film thicknessPVDF-TrFEN/A500 nm± 50 nmB4 QC
Uniformity mappingAll filmsN/ACenter-to-edge variation < 2%N/AProduction QC
Extinction coefficient (k)As₂S₃< 0.0001 @ 1550 nmN/AMust be near zeroG3 QC ● absorption check
Dispersion curveAs₂S₃Cauchy/Sellmeier fitFull visible-NIRR² > 0.999Design validation

Critical Wavelength Coverage Issue

The J.A. Woollam Alpha-SE only covers 380–900 nm. It CANNOT directly measure refractive index at 1550 nm.
For QLT, this matters because:
- SiN and SiO₂ are well-behaved dielectrics → Cauchy extrapolation from visible to 1550 nm gives accuracy ~± 0.01 (acceptable)
- As₂S₃ has absorption features near 800–1000 nm → Cauchy extrapolation is LESS reliable → accuracy degrades to ± 0.02–0.05 (marginal for phase matching)
Options:
1. Alpha-SE + Cauchy model → Good enough for SiN/SiO₂; marginal for As₂S₃ (± 0.02)
2. M-2000 (covers to 1690 nm) → Direct measurement at 1550 nm → accuracy ± 0.001 (definitive)
3. Validate Alpha-SE accuracy by measuring first As₂S₃ films on a university M-2000, then compare Cauchy extrapolation

Ellipsometry Physics for QLT Materials

ELLIPSOMETRY PRINCIPLE:

Linearly polarized light → Sample → Elliptically polarized light

Measure: Ψ (amplitude ratio) and Δ (phase difference)

tan(Ψ) × e^(iΔ) = r_p / r_s

where r_p, r_s = Fresnel reflection coefficients for p and s polarization

From Ψ and Δ at multiple wavelengths:
→ Fit optical model (Cauchy, Sellmeier, Tauc-Lorentz, Cody-Lorentz)
→ Extract: n(λ), k(λ), thickness (t)
→ For QLT: extract n at 1550 nm with ± 0.001 accuracy (M-2000)

MODEL SELECTION FOR QLT MATERIALS:
SiN (Si₃N₄): Cauchy model (transparent in visible-NIR)
SiO₂:        Cauchy model (transparent everywhere)
As₂S₃:       Tauc-Lorentz or Cody-Lorentz model (has absorption edge near 500 nm)
PVDF-TrFE:   Cauchy model (transparent polymer)
Au:          Drude model (metallic; free electron response)
Ti:          Drude-Lorentz model (metal + interband transitions)

Technical Specifications

MeasurementMaterialTarget nTarget ThicknessToleranceProcess Step
Refractive index @ 1550 nmAs₂S₃2.43N/A± 0.02G3 QC ● stoichiometry verification
Film thicknessAs₂S₃N/A500 nm± 5 nmG3 QC ● more accurate than profilometer
Refractive indexSiN (incoming)1.99 @ 1550 nm~800 nm± 0.01A1 Incoming QC
Refractive indexSiO₂ cladding1.45 @ 1550 nm~3.3 μm± 0.01A1 Incoming QC
Film thicknessPVDF-TrFEN/A500 nm± 50 nmB4 QC
Uniformity mappingAll filmsN/ACenter-to-edge variation < 2%N/AProduction QC
Extinction coefficient (k)As₂S₃< 0.0001 @ 1550 nmN/AMust be near zeroG3 QC ● absorption check
Dispersion curveAs₂S₃Cauchy/Sellmeier fitFull visible-NIRR² > 0.999Design validation
ParameterSpecification
ManufacturerJ.A. Woollam Co., Lincoln, NE
ModelM-2000-DI (or M-2000-XI for extended range)
TechnologyRotating Compensator Ellipsometry (RCE)
Wavelength range193–1690 nm (M-2000-DI); 210–1690 nm (standard)
Direct 1550 nm measurementYES
Spectral points690+ simultaneous wavelengths
Data acquisition speed2–20 Hz (50–500 ms per measurement)
Accuracy (Ψ, Δ)± 0.020° Ψ, ± 0.040° Δ
Thickness accuracy± 0.1 nm (single-layer SiO₂ on Si)
n accuracy± 0.001 (at measured wavelengths)
Spot size~3 mm standard; 300 μm with focusing probes
Angle range45°–90° (automated angle change available)
Sample sizeUp to 200 mm wafer
Sample alignmentVacuum chuck + automated Z-align
SoftwareCompleteEASE (Cauchy, Sellmeier, Tauc-Lorentz, Cody-Lorentz, B-Spline)
InterfaceUSB or Ethernet to PC
Power100–240 VAC, < 200 W
Dimensions~50 × 50 × 35 cm (benchtop)
Weight~25 kg
Operating temperature15–30°C
Light sourceQTH (quartz tungsten halogen) lamp
ParameterSpecification
ModelAlpha-SE
Wavelength range380–900 nm (does NOT cover 1550 nm directly)
Spectral points400+ wavelengths
Acquisition speed3–30 seconds
Angles65°, 70°, 75°, 90°
Spot size~3 mm
Sample sizeUp to 200 mm
SoftwareCompleteEASE (same as M-2000)
Weight17.7 kg (39 lbs)
Power100/240 VAC, < 100 W
Can extrapolate to 1550 nm?Yes, via Cauchy/Sellmeier model fit ● accuracy ± 0.01–0.02 for SiN/SiO₂; marginal for As₂S₃
ParameterSpecification
ModelF20 (thin-film measurement system)
TechnologySpectral reflectometry (NOT ellipsometry)
Wavelength range380–1050 nm (standard) or 950–1700 nm (F20-NIR)
MeasuresFilm thickness ONLY (no refractive index)
Accuracy± 1 nm thickness
Speed1 second per measurement
Price$5,000–$10,000 (F20); $8,000–$15,000 (F40-NIR)
Delivery1–2 weeks (stock item)

Process Integration

System Installation and Daily Operation

DAILY STARTUP:

1. Power on ellipsometer (M-2000 or Alpha-SE)
2. Wait 15 min for lamp and detector stabilization
3. Launch CompleteEASE software
4. Run system calibration:
├── Straight-through (no sample): verifies beam alignment
└── Reference wafer: verifies Ψ, Δ accuracy
5. System ready for measurements

DAILY SHUTDOWN:

1. Remove sample
2. Close CompleteEASE
3. Power down (or leave in standby ● extends lamp life)

First As₂S₃ Film Characterization (Critical Measurement)

FIRST As₂S₃ CHARACTERIZATION ● DETAILED PROCEDURE:

This is the most important ellipsometer measurement for QLT.
It validates the evaporation process and establishes the As₂S₃ optical model.

STEP 1: Prepare witness samples
├── During As₂S₃ evaporation (G3), place 2 bare Si witness wafers alongside chip
├── Witness sample 1: for ellipsometry (thickness + n,k)
└── Witness sample 2: backup / for Raman spectroscopy

STEP 2: Measure witness sample
├── Place witness on ellipsometer vacuum chuck
├── Measure at 65°, 70°, 75° (multi-angle for robust fit)
├── Spectral range: full (193–1690 nm for M-2000; 380–900 nm for Alpha-SE)
└── Acquire data (< 5 seconds total)

STEP 3: Build and fit optical model
├── Layer structure: As₂S₃ / SiO₂ (native, ~2 nm) / Si
├── As₂S₃ model: Start with Tauc-Lorentz
│   ├── Initial guesses: E_g = 2.4 eV, A = 100, E_0 = 4.5 eV, C = 2.5, ε₁(∞) = 3.0
│   └── Fit all parameters + thickness
├── Check MSE < 5
├── If MSE > 10:
│   ├── Add surface roughness layer (Bruggeman EMA, 50% As₂S₃ / 50% void)
│   ├── Try Cody-Lorentz model instead
│   └── Check for crystalline As₂S₃ optical constants in database
└── Once good fit achieved: SAVE MODEL as "QLT_As2S3_v1.mod"

STEP 4: Extract critical parameters
├── n @ 1550 nm: ______ (target: 2.43 ± 0.02)
├── k @ 1550 nm: ______ (target: < 0.0001)
├── E_g (bandgap): ______ (target: ~2.4 eV = 516 nm)
├── Thickness: ______ nm (target: 500 ± 5 nm)
└── Export n(λ), k(λ) as CSV for photonic simulation

STEP 5: Validate (if using Alpha-SE)
├── Send same witness sample to university with M-2000
├── Compare Alpha-SE Cauchy extrapolation to M-2000 direct measurement at 1550 nm
├── If Δn < 0.02: Alpha-SE is sufficient for routine QC
└── If Δn > 0.02: Must upgrade to M-2000 for production

Vendor Options & Pricing

New System Pricing

SystemConfigurationPrice (2026)
Woollam M-2000-DIFull range (193–1690 nm), automated angle, CompleteEASE$100,000–$150,000
Woollam M-2000-UIStandard range (245–1690 nm), automated angle$80,000–$130,000
Woollam Alpha-SEVisible only (380–900 nm), fixed angles, CompleteEASE$35,000–$50,000
Woollam RC2Dual rotating compensator, premium accuracy$150,000–$200,000
Horiba UVISEL Plus190–2100 nm, phase-modulated ellipsometry$60,000–$120,000
Semilab SE-2000190–2500 nm, rotating analyzer$50,000–$100,000
FilMetrics F20Reflectometry, thickness only$5,000–$8,000
FilMetrics F40-NIRNIR reflectometry (950–1700 nm), thickness only$10,000–$15,000

Used/Refurbished Market

ModelUsed PriceNotes
Woollam M-2000 (older gen)$30,000–$60,000Check wavelength range; verify detector health
Woollam VASE (Variable Angle SE)$15,000–$40,000Single-wavelength scanning; slower than M-2000
Woollam Alpha-SE$15,000–$25,000Good budget option if visible range sufficient
Sopra GES5E$10,000–$20,000European manufacturer; adequate specs
J.A. Woollam IR-VASE$40,000–$80,000Infrared range; covers 1550 nm and beyond

Used market sources: CAE Online (caeonline.com), LabX (labx.com), Used-Line (used-line.com)

Vendor Contact Information

VendorContactNotes
J.A. Woollam Co.[email protected]; (402) 477-7501; Lincoln, NEIndustry standard; best software (CompleteEASE)
Horiba Scientifichoriba.com; Piscataway, NJUVISEL Plus; competitive pricing
Semilabsemilab.com; Budapest, HungarySE-2000; good value
FilMetricsfilmetrics.com; San Diego, CAThickness-only; ultra-fast delivery
CAE Onlinecaeonline.comUsed Woollam systems

Our Budget Recommendation

PHASE 1 ● IMMEDIATE (thickness QC only):

  • FilMetrics F20 (new): $7,000; lead time 1–2 weeks
  • Measures film thickness instantly; no refractive index
  • Adequate for PVDF-TrFE and SiO₂ thickness QC during initial process development

PHASE 2 ● STANDARD (visible ellipsometry + extrapolation):

  • Woollam Alpha-SE (new): $40,000; lead time 4–8 weeks
  • Measures n,k from 380–900 nm; extrapolates to 1550 nm via Cauchy/Sellmeier model
  • Sufficient for SiN/SiO₂ characterization; marginal for As₂S₃
  • CompleteEASE software is industry-standard

PHASE 3 ● PRODUCTION (direct 1550 nm measurement):

  • Woollam M-2000 (new): $120,000; lead time 8–14 weeks
  • Direct n measurement at 1550 nm ● definitive for phase-matching verification
  • Required if Alpha-SE Cauchy extrapolation for As₂S₃ proves insufficient

Budget: $7,000 (FilMetrics immediate) + $40,000 (Alpha-SE later) = $47,000

Or: $120,000 (M-2000 if budget allows ● eliminates extrapolation uncertainty)

Facility Requirements

ParameterSpecification
Footprint~50 × 50 cm (Alpha-SE); ~60 × 60 cm (M-2000)
Weight18 kg (Alpha-SE); 25 kg (M-2000)
VibrationModerate sensitivity (stable bench; no isolation table required)
Temperature15–30°C (operating); 22 ± 2°C optimal
Humidity20–60% RH (non-condensing; moisture affects optical models)
LightingCan operate in NORMAL room light (RCE technology is room-light tolerant) ✅
SoundSilent
ExhaustNone
ElectricalStandard outlet: 100–240V, < 200 W

Safety & Handling

HazardRisk LevelMitigation
QTH lamp (high-intensity white light)LOWLight is contained within optical path; no direct exposure
UV light (if DUV source on M-2000-DI)LOWEnclosed beam path; no external UV exposure
Hot lamp housingLOWDo not touch lamp housing during operation
Sample handlingLOWStandard ESD precautions for semiconductor chips
No laser hazardEllipsometers use broadband lamps, not lasers
No chemical hazardsNo chemicals, gases, or hazardous materials
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