研究目的
Investigating the nanoparticle emissions from the metal-assisted chemical etching process for silicon nanowires used in lithium ion batteries to understand and reduce potential environmental impacts.
研究成果
The MACE process for SiNWs produces significant airborne and aqueous nanoparticle emissions, with the highest airborne emissions for 140 nm SiNWs and highest aqueous emissions for 120 nm SiNWs per kWh of LIB electrodes. The study provides crucial data for environmental impact assessments and suggests that optimizing etching steps could mitigate emissions. Future work should focus on scaling up and improving sustainability.
研究不足
The study is limited to laboratory-scale experiments with specific etching parameters; it does not address large-scale industrial applications or long-term environmental impacts. The use of toxic chemicals like HF and AgNO3 poses safety concerns, and the measurements may have uncertainties due to equipment limitations (e.g., ICP-MS not used for HF-containing solutions).
1：Experimental Design and Method Selection:
The study involved synthesizing SiNWs with three different diameters (90, 120, and 140 nm) using the MACE method with varying etching parameters (AgNO3 and H2O2 concentrations). Airborne and aqueous nanoparticle emissions were measured using in-situ and ex-situ techniques, and the SiNWs were tested as anodes in LIB coin cells.
2：Sample Selection and Data Sources:
Silicon (100) wafer pieces were used as substrates, cleaned with acetone, ethanol, and deionized water. Nanoparticle emissions were collected from etching and cleaning steps.
3：List of Experimental Equipment and Materials:
Equipment included UCPC (TSI 3776), SMPS (TSI 3936), SEM (Hitachi S4800), EDS, ZetaPlus (Brookhaven Instruments Corp.), ICP-MS, XPS, and a LANHE CT2001A battery tester. Materials included AgNO3, HF, H2O2, HNO3, acetone, ethanol, carbon black, alginate binder, copper foil, lithium metal, LiPF6 electrolyte, Celgard-2320 separator.
4：Experimental Procedures and Operational Workflow:
Si wafers were cleaned, etched in HF + AgNO3 and HF + H2O2 solutions, cleaned with HNO3 to remove Ag particles, and SiNWs were collected by ultrasonication and centrifugation. Airborne particles were measured in-situ with UCPC and SMPS, and characterized with SEM/EDS. Aqueous particles were measured ex-situ with ZetaPlus, ICP-MS, SEM, and XPS. LIB coin cells were fabricated and tested electrochemically.
5：Data Analysis Methods:
Data were analyzed using statistical calculations from SMPS (e.g., geometric mean), and software tools for SEM, EDS, ICP-MS, and XPS analysis.
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Ultrafine Condensation Particle Counter
TSI 3776
TSI
Measures number concentrations and size distributions of airborne nanoparticles down to 2.5 nm in diameter.
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Scanning Mobility Particle Sizer
TSI 3936
TSI
Performs particle-size classification based on differential electrical mobility classification, used with UCPC for size distribution measurements.
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Scanning Electron Microscopy
Hitachi S4800
Hitachi
Characterizes morphologies of airborne and aqueous nanoparticles.
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Electrostatic Classifier
TSI 3080
TSI
Part of SMPS for particle-size classification.
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Energy Dispersive X-Ray Spectrometry
Used with SEM for elemental composition analysis of nanoparticles.
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Zeta Potential Analyzer
ZetaPlus
Brookhaven Instruments Corp.
Analyzes particle-size distributions in liquid suspensions using dynamic light scattering.
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Inductively Coupled Plasma Mass Spectrometry
Determines concentrations of silicon and silver nanoparticles in solutions.
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X-ray Photoelectron Spectroscopy
Determines surface chemical compositions of aqueous particles.
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Battery Tester
LANHE CT2001A
Land
Tests electrochemical performance of fabricated coin cells.
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