C-MEMS Training & Fabrication
Carbon Microelectromechanical Systems

Photolithography | Pyrolysis | 3D Carbon Microstructures

📍 Location: Advanced Materials Engineering Research Institute (AMERI), Florida International University
🔬 Skills Acquired: Photolithography, SU-8 Processing, Pyrolysis, SEM Characterization, Electrochemical Testing
📚 Reference: Fabricated similar structures as described in peer-reviewed publications from my research group (Adelowo et al., J. Power Sources 2020; Forouzanfar et al., Biosens. Bioelectron. 2020; Forouzanfar et al., Micromachines 2022)

Project Overview

During the first two years of my Ph.D., I underwent extensive training in Carbon Microelectromechanical Systems (C-MEMS) technology at the Advanced Materials Engineering Research Institute (AMERI) cleanroom facility. This training covered the entire fabrication process flow from photolithographic patterning of SU-8 photoresist to high-temperature pyrolysis for creating glassy carbon microstructures. I successfully fabricated 3D carbon microelectrode arrays, interdigital carbon structures, and carbon micropillars for applications in energy storage (microsupercapacitors, lithium-ion capacitors) and biosensing (aptasensors, enzymatic sensors).

What is C-MEMS?

C-MEMS is a fabrication technique that converts photopatterned SU-8 photoresist into glassy carbon structures through pyrolysis in an oxygen-free environment at high temperatures (800-1100°C). This technology enables the creation of high-aspect-ratio 3D carbon microstructures with excellent electrical conductivity, chemical inertness, biocompatibility, and wide electrochemical windows—making them ideal for on-chip energy storage and biosensing applications.

Key Skills & Techniques Acquired

Photolithography SU-8 25/100 Processing Spin Coating Mask Alignment (OAI Aligner) UV Exposure Optimization Soft Baking / Hard Baking Development (SU-8 Developer) Pyrolysis (Tube Furnace) Inert Atmosphere Control (Forming Gas) Ramp Rate Optimization SEM Characterization FTIR Spectroscopy Cyclic Voltammetry (CV) Electrochemical Impedance Spectroscopy (EIS) Oxygen Plasma Treatment (RIE) Bipolar Exfoliation of Graphene

C-MEMS Fabrication Process Flow

Step 1: Substrate Preparation

4-inch silicon wafer (p-doped, single-side polished) cleaned with acetone and methanol, followed by 20 min bake at 200°C to remove moisture and solvents.

Step 2: SU-8 Spin Coating

SU-8 25 (for thin layer ~15μm): Spin-coated at 3000 rpm for 30 seconds
SU-8 100 (for thick layer ~100μm): Spin-coated at 2000 rpm for 30 seconds (for 3D micropillars)

Step 3: Soft Bake

65°C for 3-10 min (depending on layer thickness), then 95°C for 7-30 min on hotplates to evaporate solvents.

Step 4: UV Exposure (Photolithography)

OAI mask aligner used for pattern transfer. Exposure dose optimized: 300 mJ/cm² for SU-8 25, 700 mJ/cm² for SU-8 100.

Step 5: Post-Exposure Bake (PEB)

65°C for 1-3 min, then 95°C for 5-10 min to crosslink exposed regions.

Step 6: Development

SU-8 developer solution to remove unexposed photoresist, revealing 2D interdigital patterns or 3D micropillar structures.

Step 7: Pyrolysis (Carbonization)

Lindberg tube furnace with forming gas flow (95% N₂ + 5% H₂, 200 sccm).
Temperature Ramp: 3-5°C/min to 350°C (30 min dwell), then to 900°C (60 min dwell).
Cooling: Natural cooling to room temperature in inert atmosphere.

Step 8: Optional Post-Processing

Oxygen Plasma Treatment (RIE): 60 sccm O₂, 400 mTorr, 100 W, 7 min – introduces carboxyl (-COOH) groups for biofunctionalization.
Bipolar Exfoliation (BPE): 45V DC for 24 hours – deposits vertically aligned reduced graphene oxide (rGO) on C-MEMS electrodes.

Structures I Fabricated During Training

1. 2D Interdigital Carbon Microelectrodes

  • Finger width: 79 μm
  • Finger spacing: 100 μm
  • Number of fingers: 20 (10 per side)
  • Total footprint: ~0.29 cm²
  • Applications: Supercapacitors, electrochemical sensors

2. 3D Carbon Micropillar Arrays

  • Micropillar diameter: ~46 μm
  • Micropillar height: ~100-106 μm
  • 23 pillars per finger (460 pillars total per device)
  • Applications: High-surface-area electrodes for batteries and supercapacitors

3. Carbon Microelectrodes with BPE-rGO Integration

  • Vertically aligned reduced graphene oxide deposited via bipolar electrochemistry
  • Porous morphology with ~100 nm pore size
  • Enhanced areal capacitance (from 7.67 to 19.89 mF/cm²)
  • Applications: Cancer biomarker aptasensors (PDGF-BB detection)

Applications Explored During Training

Energy Storage

  • On-chip Lithium-ion Capacitors (LIC): 3D carbon microelectrodes as capacitor-type electrode, LiFePO₄ integrated via electrophoretic deposition (EPD) as battery-type cathode. Achieved areal energy density ~5.03 μWh/cm² (5× higher than symmetric carbon ECs).
  • Microsupercapacitors: Oxygen plasma treatment to improve capacitive properties (9× increase in CV area).

Biosensing

  • Cancer Biomarker Aptasensors (PDGF-BB): Covalent immobilization of amino-terminated aptamers on carboxyl-functionalized C-MEMS surfaces. Achieved LoD of 0.75 pM with BPE-rGO integration.
  • Lactic Acid Enzymatic Sensors: Lactate oxidase immobilization for non-invasive lactate detection in sweat. Achieved wide linear range (0.1-5000 μM) and LoD of 1.45 μM.

Equipment & Tools Used

  • Spin Coater (Headway Research)
  • OAI Model 800 Mask Aligner
  • Hotplates (for soft/post-exposure bakes)
  • Lindberg Tube Furnace (pyrolysis)
  • MARCH CS-1217 RIE System (oxygen plasma)
  • JEOL SEM 6330F (microstructure characterization)
  • JASCO FTIR 4100 (surface functional groups)
  • Bio-Logic VMP3 Potentiostat (electrochemical testing)
  • Agilent Technologies N6705A DC Power Analyzer (BPE)

Why C-MEMS for Microfabrication?

Property C-MEMS (Glassy Carbon) Conventional Silicon
Biocompatibility✅ Excellent⚠️ Moderate
Chemical Inertness✅ High⚠️ Moderate
Electrochemical Window✅ Wide⚠️ Limited
Biofouling Resistance✅ High⚠️ Low
Surface Functionalization✅ Accessible (-COOH, -NH₂)⚠️ Requires oxide layer
3D High-Aspect-Ratio✅ Yes (C-MEMS)✅ Yes (DRIE)
Fabrication Cost✅ Low (photoresist + furnace)⚠️ Higher (DRIE expensive)

Reference Publications (Group Peers)

Connection to My Research

The C-MEMS training directly enabled my subsequent research in:

  • Microsupercapacitors: Using porous carbon structures for on-chip energy storage (training reference)
  • Sensor Integration: Understanding electrode fabrication for my pressure sensor work
  • Cleanroom Protocols: Mastering the same facilities used for my MEMS pressure sensor project
  • Electrochemical Characterization: Skills applied to supercapacitive pressure sensor testing

Conclusion

This comprehensive C-MEMS training provided me with hands-on experience in photolithography, SU-8 processing, pyrolysis, and electrochemical characterization. I successfully fabricated 2D interdigital carbon microelectrodes and 3D micropillar arrays, and integrated bipolar-exfoliated graphene for enhanced performance. These skills form the foundation of my micro/nanofabrication expertise and have been directly applied to my MEMS pressure sensor and wearable sensor projects. Although I do not have first-author publications in this specific area, I am competent in all C-MEMS fabrication processes and have reproduced similar structures during my training.