Characterization of deep wet etching of glass

This paper presents a characterization of wet etching of glass in HF-based solutions with a focus on etching rate, masking layers and quality of the generated surface. The first important factor that affects the deep wet etching process is the glass composition. The presence of oxides such as CaO, MgO or Al2O3 that give insoluble products after reaction with HF can generate rough surface and modify the etching rate. A second factor that influences especially the etch rate is the annealing process (560°C / 6 hours in N2 environment). For annealed glass samples an increase of the etch rate with 50-60% was achieved. Another important factor is the concentration of the HF solution. For deep wet etching of Pyrex glass in hydrofluoric acid solution, different masking layers such as Cr/Au, PECVD amorphous silicon, LPCVD polysilicon and silicon carbide are analyzed. Detailed studies show that the stress in the masking layer is a critical factor for deep wet etching of glass. A low value of compressive stress is recommended. High value of tensile stress in the masking layer (200-300 MPa) can be an important factor in the generation of the pinholes. Another factor is the surface hydrophilicity. A hydrophobic surface of the masking layer will prevent the etching solution from flowing through the deposition defects (micro/nano channels or cracks) and the generation of pinholes is reduced. The stress gradient in the masking layer can also be an important factor in generation of the notching defects on the edges. Using these considerations a special multilayer masks Cr/Au/Photoresist (AZ7220) and amorphous silicon/silicon carbide/Photoresist were fabricated for deep wet etching of a 500 μm and 1mm-thick respectively Pyrex glass wafers. In both cases the etching was performed through wafer. From our knowledge these are the best results reported in the literature. The quality of the generated surface is another important factor in the fabrication process. We notice that the roughness of generated surface can be significantly improved by adding HCl in HF solution (the optimal ratio between HF (49%) and HCl (37%) was 10/1).

[1]  M. Gijs,et al.  The introduction of powder blasting for sensor and microsystem applications , 2000 .

[2]  Shuichi Shoji,et al.  Low-temperature anodic bonding using lithium aluminosilicate-β-quartz glass ceramic , 1998 .

[3]  Yong-Kweon Kim,et al.  Micro XY-stage using silicon on a glass substrate , 2002 .

[4]  Giancarlo C. Righini,et al.  Characterization of reactive ion etching of glass and its applications in integrated optics , 1991 .

[5]  Ciprian Iliescu,et al.  Fabrication of a dielectrophoretic chip with 3D silicon electrodes , 2005 .

[6]  H. John Crabtree,et al.  Microfabricated device for DNA and RNA amplification by continuous-flow polymerase chain reaction and reverse transcription-polymerase chain reaction with cycle number selection. , 2003, Analytical chemistry.

[7]  P. J. Slikkerveer,et al.  High quality mechanical etching of brittle materials by powder blasting , 2000 .

[8]  E Obermeier,et al.  Smoothing of ultrasonically drilled holes in borosilicate glass by wet chemical etching , 1996 .

[9]  L. Roylance,et al.  A miniature integrated circuit accelerometer , 1978, 1978 IEEE International Solid-State Circuits Conference. Digest of Technical Papers.

[10]  M.-A. Grétillat,et al.  A New Fabrication Method for Borosilicate Glass Capillary Tubes with Lateral Inlets and Outlets , 1997 .

[11]  Ciprian Iliescu,et al.  Characterization of masking layers for deep wet etching of glass in an improved HF/HCl solution , 2005 .

[12]  H. Fouckhardt,et al.  Deep wet etching of fused silica glass for hollow capillary optical leaky waveguides in microfluidic devices , 2001 .

[13]  Gregory T. A. Kovacs,et al.  PECVD silicon carbide for micromachined transducers , 1997, Proceedings of International Solid State Sensors and Actuators Conference (Transducers '97).

[14]  Takayuki Fujita,et al.  Disk-shaped bulk micromachined gyroscope with vacuum sealing , 2000 .

[15]  M. Madou Fundamentals of microfabrication , 1997 .

[16]  Miko Elwenspoek,et al.  Direct integration of micromachined pipettes in a flow channel for single DNA molecule study by optical tweezers , 2001 .

[17]  Ciprian Iliescu,et al.  Optimization of an amorphous silicon mask PECVD process for deep wet etching of Pyrex glass , 2005 .

[18]  H. Gamble,et al.  Characterization of masking materials for deep glass micromachining , 2003 .

[19]  Johan Roeraade,et al.  Method for fabrication of microfluidic systems in glass , 1998 .

[20]  G. Stemme,et al.  Deep wet etching of borosilicate glass using an anodically bonded silicon substrate as mask , 1998 .

[21]  Masayoshi Esashi,et al.  Fabrication of high-density electrical feed-throughs by deep-reactive-ion etching of Pyrex glass , 2002 .

[22]  A. Evans,et al.  A new masking technology for deep glass etching and its microfluidic application , 2004 .

[23]  M. Gretillat,et al.  Micromachined injector for mass spectrometry , 1999 .

[24]  V. Fascio,et al.  In situ measurement and micromachining of glass , 1999, MHS'99. Proceedings of 1999 International Symposium on Micromechatronics and Human Science (Cat. No.99TH8478).

[25]  M. Vellekoop,et al.  Two-step Glass Wet-etching for Microfluidic Devices , 2000 .

[26]  Richard A. Mathies,et al.  Microfabrication Technology for the Production of Capillary Array Electrophoresis Chips , 1998 .

[27]  Ciprian Iliescu,et al.  Stress control in masking layers for deep wet micromachining of Pyrex glass , 2005 .