Bonding Quartz Glass at Room Temperature Tetsuya Hamaguchi, Natsuki Yamamoto, Takeshi Ooi, Kensuke Tsuchiya, Masayuki Nakao The University of Tokyo, Graduate School of Engineering 7-3-1 Hongo, Bunkyo-ku, 113-8656 Tokyo, Japan 1. Introduction The authors are developing a method for directly bonding two pieces of quartz glass at room temperature. The conventional way of bonding glass with additives, like soda glass or borosilicate glass, is anodic bonding. For bonding pure quartz glass, ways exist by softening the surface with high temperature, melting the surface with hydrogen fluoride acid (HF)[1], and using glue. Applying these methods, however, for bonding micro Total Analysis System (µ-TAS ) chips (Fig. 1), causes surface deformation or glue entering the micro grooves and destroys the micro-features on the chip surfaces. Also, optical parts that pass ultraviolet ray are made of quartz glass and gluing them together causes drops in transmissivity of the ultraviolet ray. We thus want to develop a technology to directly bond two pieces of quartz glass together. For direct bonding of metal, a known technique[2] bonds metal surfaces activated by inert gas ion beam or fast atom beam (FAB) irradiation cleaning under vacuum. We applied FAB irradiation and succeeded in bonding quartz glass. This paper reports the relations of bonding strength versus quartz glass surface roughness, FAB irradiation time, FAB source gas type and bonding pressure. 2. Test equipment and procedure Fig. 2 sketches our test equipment, with a vacuum chamber, 2 FAB guns, 2 samples fixtures, and a pressing mechanism. The FAB guns are oriented to irradiate FAB on two samples both at angles of 45 degrees. The pressing mechanism has a load cell to measure the bonding pressure. FAB FAB Vacuum pump bonding Samples hundreds of nano meter order Load cell Fig. 1 Example of µ –TAS Chip Fig. 2 Test equipment The test proceeds as follows: First the sample surfaces are cleaned with organic solvent, a mixture of H2SO4+H2O2 and then with NH4F. The cleaning process then takes the samples through boiling in a H2SO4+H2O2 mixture, and ends with pure water rinsing and drying. The two samples fixtures hold the sample to thoroughly dry them. The fixtures are then set inside the vacuum chamber which we vacuum down to 7.5 x 10-4Pa. We then fill the chamber with the source gas at a pressure of 1.3 x 10-2Pa and irradiate FAB on the sample surface. After the set irradiation time, with the FAB irradiation running, the pressing mechanism presses the two samples together to bond them. We then take the bonded sample out from the vacuum chamber and set it on the tensile test machine with the fixtures holding it in place. The load cell measures the force when the bonded surface separate to give the bonding strength value. The samples were quartz glass plates of 6 x 6mm with a thickness of 0.2mm. We prepared two types of sample with different surface roughness values of 0.17 and 3.2nmRa. We used an atomic force microscope (AFM) for measuring the surface roughness. For FAB source gas, we readied Ar gas, an inert gas commonly used for diffusion bonding, and CHF3 gas expecting some chemical reaction with quartz glass. 3. Test results and discussion 3-1. FAB irradiation time and surface roughness We expected that the sample surface roughness should strongly affect the bonding strength. Cleaning the sample surface requires FAB irradiation for its activation and we were concerned that the irradiation may degrade the surface roughness. We thus tested how the FAB irradiation time affects the surface roughness. We applied CHF3 gas FAB irradiation to the sample with an original surface roughness of 3.2nmRa, and both the CHF3 gas and Ar gas FAB irradiation to ones with 0.17nmRa. Fig. 3 shows the test results, and Fig. 4, the AFM images of the sample surface before and after 300 seconds of CHF3 gas FAB irradiation. The figures show Surface Roughness (nm Ra) 6 5 CHF3 4 3 CHF3 2 1 Ar 0 0 200 400 600 FAB irradiation time (sec) 800 Fig.3 Relation between FAB irradiation time and surface roughness 6 (nm) 4.0 0 (nm) 0 5 5 (µm) (µm) 2.0 0.0 10 6 (nm) (a) Before FAB irradiation (surface roughness = 0.17 nmRa) 4.0 0 (nm) 5 (µm) 5 10 0 (µm) 2.0 0.0 (b) After 300 seconds of FAB irradiation (surface roughness = 0.31 nmRa) Source gas: CHF3 Fig.4 Change of surface roughness with FAB irradiation that FAB irradiation degrades surface roughness. Longer irradiation worsens the surface roughness with both Ar and CHF3 gas. When neutral atoms hit the sample surface, they clean the surface by removing molecules and contamination, but at the same time, roughs the glass surface by hitting it. 3-2. Bonding strength and FAB source gas Fig. 5 shows the test results. The horizontal axis gives the surface roughness after FAB irradiation, and the vertical axis the bonding strength. Ar gas failed bonding the glass plates with both surface roughness values. CHF3 gas, on the other hand, succeeded in bonding the two pieces. A component of the CHF3 gas must have caused some chemical reaction on the quartz glass, however, the detail of this process has not been clarified. With CHF3 gas, the bonding strength maximized when the surface roughness was about 0.25nmRa. Samples with smoother surfaces had shorter FAB irradiation time. The results indicate that smoother surfaces produce larger contact area and thus stronger bonding strength, however, if the FAB irradiation time is too short for smoothness, the process loses the cleaning effect and the bonding strength drops. 3-3. Bonding strength and bonding pressure Once FAB irradiation is complete, the two samples are pushed together to make the bonding and Fig. 6 shows the bonding pressure in the horizontal axis and the bonding strength in the vertical. We compared the results with samples made of gold and quartz glass. The quartz glass samples had surface roughness of 0.31nmRa after FAB irradiation with CHF3 gas. Larger bonding pressure generated stronger bonding strength for gold. The smaller Young’s modulus of gold produced greater contact area with larger bonding pressure. In contrast, quartz glass has a large Young’s modulus and increasing the bonding pressure does not affect the contact area. The bonding strength did not increase with the bonding pressure. 16 Bonding Strength (MPa) Bonding Strength (MPa) 1 0.8 CHF3 0.6 0.4 0.2 Ar 0 0 0.2 0.4 0.6 0.8 1 1.2 14 12 Au 10 8 6 4 Quartz glass 2 0 0 Surface Roughness (nm Ra) Fig.5 Relation between surface roughness and bonding strength 2 4 Bonding Pressure (Mpa) 6 Fig.6 Relation between bonding pressure and bonding strength (CHF3, 0.31nmRa) 4. Conclusions We confirmed that we can directly bond two pieces of quartz glass at room temperature by using FAB. The following conditions are important for stronger bonding strength: - CHF3 gas is effective for the FAB source gas. - Surface roughness of 0.25nmRa after FAB irradiation produces the best results . - The bonding pressure, when it is 3MPa or less, does not affect the bonding strength. - The bonding strength will improve if we can clean the surface without affecting the surface roughness. References [1]Akihide Hibara, et al.: Nanochannels on a Fused-Silica Microchip and Liquid Properties Investigation by Time-Resolved Fluorescence Measurements, ANALYTICAL CHEMISTRY, Vol.74, pp.6170-6176, 2002. [2]Yuzo Matsuzawa, Toshihiro Itoh, and Tadatomo Suga: Room-temperture Interconnection of Electroplated Au Microbump by means of Surface Activated Bonding Method, Electronic Components and Technology Conference, pp.384-387, 2001.
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