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Deposition of Mesoporous Silicon Dioxide Films Using Microwave PECVD.

Marcel Laux1, Ralf Dreher1, Rudolf Emmerich1

  • 1Fraunhofer Institute for Chemical Technology, Joseph-von-Fraunhofer-Straße 7, 76327 Pfinztal, Germany.

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Summary

Mesoporous silica films enhance polymer-metal adhesion through nanoscale form-locking. Process parameter optimization using Design of Experiments improves film morphology and adhesion performance.

Keywords:
PECVDSiO2adhesion layerhexamethyldisiloxaneinjection moldingmesoporousmicrowavepolymer–metalsilicasilicon dioxide

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Area of Science:

  • Materials Science
  • Surface Science
  • Chemical Engineering

Background:

  • Mesoporous silica films serve as effective adhesion-promoting interlayers for polymer-metal interfaces.
  • Fabrication via microwave plasma-enhanced chemical vapor deposition (MPECVD) with hexamethyldisiloxane (HMDSO) and oxygen enables nanoscale form-locking.
  • Adhesion strength is critically dependent on the deposited film's morphology.

Purpose of the Study:

  • To investigate the growth behavior of mesoporous silica films.
  • To understand the underlying deposition mechanisms for improved process stability.
  • To establish a correlation between film morphology and adhesion performance.

Main Methods:

  • Systematic variation of seven process parameters (coating time, distance, pressure, temperature, flow rate, pulse duration, pause-to-pulse ratio) within a Design of Experiments (DOE) framework.
  • Characterization of film morphology (free surface area, mean agglomerate diameter, film thickness) using digital image analysis, white light interferometry, and atomic force microscopy (AFM).
  • Overmolding via injection molding followed by mechanical testing to evaluate adhesion performance.

Main Results:

  • Mesoporous silica films exhibited diverse morphologies, from quasi-dense to dust-like structures.
  • Key morphological parameters varied significantly: free surface area (15-55%), mean agglomerate diameter (17-126 nm), and film thickness (35-1600 nm).
  • A statistically accurate growth model was derived, correlating process parameters with film morphology.

Conclusions:

  • The study successfully established a direct correlation between mesoporous silica film morphology and their performance as adhesion-promoting interlayers.
  • The developed growth model provides a pathway for optimizing MPECVD processes for enhanced polymer-metal adhesion.
  • Understanding and controlling film morphology is crucial for achieving high-strength polymer-metal interfaces.