Test Results on Sealing in Options A & E Dean Walters Argonne National Laboratory Michael MinotMinoTech Engineering Inc.

D. Walters - 16 October 2 Joining and Assembly Design Configurations Assembly Process Materials Joining methods Results on Joining Status of joining Future Work

D. Walters - 16 October 3 Mechanical Configurations of the Photo-detector Option A –Borosilicate tray –Borosilicate window –Glass to glass seal –Base anode pins Option B –Borosilicate tray –Quartz window –Pre-fab Kovar edge parts –Kovar to Kovar seal –Base anode pins Option C –Kovar tray –Quartz or glass window –Pre-fab Kovar edge seal –Side pins in glass ‘header’ Option D –Ceramic tray Option E –Borosilicate base plate –Borosilicate side walls –Borosilicate window –Pass-thru anode strip lines –Frit sealing base plate to side walls

D. Walters - 16 October 4 Design configurations Option A From R. Northrop

D. Walters - 16 October 5 Design configurations –Kovar tray –Quartz or glass window –Pre-fab Kovar edge seal –Side pins in glass ‘header’ Option C From R. Northrop

D. Walters - 16 October 6 Design Configurations Option E From R. Northrop

D. Walters - 16 October 7 Design Configurations Option E From R. Northrop

D. Walters - 16 October 8 Proposed Assembly Process Option A

D. Walters - 16 October 9 Proposed Assembly Process Option E

D. Walters - 16 October 10 Materials Glass

D. Walters - 16 October 11 Materials Borosilicate – Borofloat 33 From Schott Literature

D. Walters - 16 October 12 Materials Kovar

D. Walters - 16 October 13 Materials Alumina

D. Walters - 16 October 14 Joining Methods Glass to glass joints –Frit glass joints –Laser sealing –Soldering –Anodic Bonding Glass to metal joints –Anodic Bonding –Soldering –Powdered Glass Metal to metal joints –Brazing –Soldering –Welding Electron beam welding Laser welding TIG welding

D. Walters - 16 October 15 Joining Methods First Trials on Lime Frit on Soda Glass From R. Northrop

D. Walters - 16 October 16 Joining Methods Glass Frit Sealing –Used for Glass to Glass seals –Large variety of commercial frits Ability to modify to fit various applications –Example of frit in Results Section Anodic Bonding –Voltage/Temperature Temperature lower than glass softening temperature by 200 C or less –Kovar to Glass Seals –Glass to Glass Seals From G. Wallis JAP 1969

D. Walters - 16 October 17 Laser Joining & Welding Nuclear Engineering Building 308 The 1.6 kW pulsed Nd:YAG laser Facility also contains CO 2 Laser CO 2 Laser –Vendor: Iowa Laser

D. Walters - 16 October 18 Joining Methods Soldering –UC-Davis Method D. Ferenc Talk July 2009 –ANL 50/50 Indium Tin alloy MP= 130 C

D. Walters - 16 October 19 Joining Methods E Beam Welding –Central Shops Building 363

D. Walters - 16 October 20 Joining Methods TIG Welding –APS Vacuum Shop Building 382

D. Walters - 16 October 21 Joining Methods Hydrogen and Vacuum Brazing –Central Shops Building 363

D. Walters - 16 October 22 Results First Trials on Lime Frit on Soda Glass Trial on 31 August 2009 by M. Minot Set up Conditions: Fused at 1500 F for 5 minutes Sample parts are 1.5” on long edge &.25” thick The bubbles shown here are a result of the outgassing of the frit components. It is concluded that with a better Frit glass combination will mitigate the situation In spite of lack of match between the frit & glass the parts are well adhered to each other.

D. Walters - 16 October 23 Results on Joining #1 (left) and #3 (on the right) using Vitta Frit G-1017 Glass Transfer Tape (Frit with Adhesive) This Frit is specifically designed for sealing and joining Pyrex parts, hence my application to BoroFloat (same CTE, near identical / equivalent composition). In Trials #1, the frit tape was sandwiched between two pieces of Borofloat and fired, without providing an opportunity to burn off adhesive, hence the dark (carbon) color. Trial #2 was to evaluate firing cycles to burn of adhesive. Trial #3 shows the sandwich assembled after first burning off adhesive. Good bond was achieved. Green opaque color is result of the composition of G-1017 which includes Pb- Zn-Borosilicate glass. I think the green color is from Zinc Oxides. Trial by M. Minot of MinoTech Engr

D. Walters - 16 October 24 Status of joining The G1017 samples are going to be sectioned to determine if there is evidence of bubbles in the joint. Glass will be obtained to be used as samples in testing at Minotech and ANL Materials are on order for frit trials using d410 frit from Asahi Glass (AGC) with Schott B270 glass coupons. This frit is proven hermetic based on prior application to plasma display technology. Future Work M. Minot is working on obtaining a number of candidate frits for testing in the MinoTech Engineering lab. All future trials will also include application over metallized anode strip lines to demonstrate ability to make conductive pass through. Full scale trials will also be done using extensive Incom furnace capability An agreement is being established with Brigitflex of Elgin, Illinois to use their furnace for frit trials by ANL personnel. Schott Glass has become interested in this project and they have considerable experience in glass product manufacturing and processing.