Table 1. Comparison of Techniques for In Situ Imaging of Heterogeneous Catalysis.
Technique | Sample environment | Detection method | Characterizes | Detects reaction products? | Typical spatial resolutiona | Typical acquisition ratea | Requirements/limitations |
---|---|---|---|---|---|---|---|
STM | Vacuum | Tunneling current | Surface structure | If adsorbed on the surface | Atomic, 0.01 nm | Scan rates vary: 0.1–100 s for a 10 × 10 nm2 region | Requires clean, atomically flat surfaces |
Gas & liquid-cell TEM | Electron-transparent cell in vacuum | Electron transmission/diffraction | Particle structure and morphology | When combined with GC or EELS | Atomic to nanoscale, 0.01–10 nm, depends on liquid thickness | 8–150 frames/s for a region of 2.5 × 2.5 μm2 (low-res) to 25 × 25 nm2 (high-res) | Cells need high electron transparency; samples are subject to beam damage |
SECM | In liquid, open to air | Electrochemical current | Charge-transfer rate | Detects rate of redox reactions | Nano- to microscale 0.05–10 μm | Scan rates vary from 30 nm/s to 10 μm/s | Primarily restricted to redox reactions |
STXM | X-ray-transparent liquid cell | X-ray transmission | Distribution of elements and their oxidation states | No | Nanoscale 40–100 nm | Scan rates vary: 100 s to >1 h for a 1 × 1 μm2 region | Requires synchrotron radiation and specialized cell design |
SMF | In liquid, open to air | Fluorescence | Number of product molecules generated | If they are fluorescent | Nanoscale 10–50 nm | 10–70 frames/s for an 80 × 80 μm2 region | Requires samples and substrates with low fluorescence background |
The spatial resolutions and acquisition rates provided are based on representative examples. The resolution and either scan rate (for STM, SECM, and STXM) or frame rate (for TEM and SMF) will depend on the specific sample, reaction conditions, and instrument used.