status update for indium cold sealing process...5.08 mm •comparing the width of indium to the...

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Status Update for Indium Cold Sealing Process Marc E. Kupfer University of Illinois at Chicago Dean R. Walters Argonne National Laboratory

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Page 1: Status Update for Indium Cold Sealing Process...5.08 mm •Comparing the width of indium to the sealing duration shows: •90% of compression will occur after 6 minutes. •Indium

Status Update for Indium

Cold Sealing Process

Marc E. Kupfer

University of Illinois at Chicago

Dean R. Walters

Argonne National Laboratory

Page 2: Status Update for Indium Cold Sealing Process...5.08 mm •Comparing the width of indium to the sealing duration shows: •90% of compression will occur after 6 minutes. •Indium

Seal Fabrication – 1 inch

Hydraulic System •Capable of 3000+ lbs pressing force •Heated platen and internal quartz

halogen heating bulbs •High vacuum (~10-7 torr) • Laser displacement sensor to

measure compression • Fabricates both 1 inch and 4 inch

samples

Fabrication process has been optimized over time to consistently make leak-tight 1 inch seals using uncoated glass parts.

Compressed 2.0mm wire

Hermetic Packaging Godparent Meeting 3 April 2013 M. E. Kupfer [email protected]

Page 3: Status Update for Indium Cold Sealing Process...5.08 mm •Comparing the width of indium to the sealing duration shows: •90% of compression will occur after 6 minutes. •Indium

Seal Fabrication – 4 and 8 inch

•4 inch and 8 inch seals are made by the use of a “spring press.” • Fabrication process uses two heavy aluminum platens compressed together

using bolts and springs. •Compression is controlled by laser measurement of the change in thickness of

the indium. • This method has the advantage of holding samples under compression for

extended periods of time. Spring press can also be placed inside an over while compressing.

4 Inch

8 Inch

Hermetic Packaging Godparent Meeting 3 April 2013 M. E. Kupfer [email protected]

Page 4: Status Update for Indium Cold Sealing Process...5.08 mm •Comparing the width of indium to the sealing duration shows: •90% of compression will occur after 6 minutes. •Indium

Seal Characterization

•Hermeticity is measured using an Alcatel helium detector. Seals are considered leak tight if the base reading is <10-10 ccm of He per second and there is no response from the gauge when the sample is hit with helium.

• The strength of the seal is measured using a lap shear test.

Hermetic Packaging Godparent Meeting 3 April 2013 M. E. Kupfer [email protected]

Page 5: Status Update for Indium Cold Sealing Process...5.08 mm •Comparing the width of indium to the sealing duration shows: •90% of compression will occur after 6 minutes. •Indium

Analysis of 1 inch Data

890

1179.25

1557.5 1891.25

0.00

1.00

2.00

3.00

4.00

5.00

6.00

700 1200 1700 2200

Wid

th o

f In

diu

m S

ea

l (m

m)

Applied Load (N)

186.9

501.1

627.0

684.9

0

100

200

300

400

500

600

700

800

700 1200 1700 2200

Sh

ea

r F

orc

e (

N)

Applied Load (N)

5.08 mm

• There is a linear correlation between the width of the indium seal and the applied load. (Temperature = 20ºC, time = 11 minutes)

• This correlation shows that in order to cause the indium gasket to flow to the entire width of the sidewall, a compression force of 2150 N (483 lbs) is needed.

• There is a general increase in force to shear failure with the increase in applied load.

• This trend suggests that the maximum strength achievable with the given fabrication procedure with uncoated glass is approximately 720 N.

Page 6: Status Update for Indium Cold Sealing Process...5.08 mm •Comparing the width of indium to the sealing duration shows: •90% of compression will occur after 6 minutes. •Indium

Analysis of 1 inch Data

60 30

11 6

1

10 sec

2.50

3.00

3.50

4.00

4.50

5.00

0 10 20 30 40 50 60 70

Ind

ium

Wid

th (

mm

)

Time (minute)

631.9 607.9

501.1

505.1

420.5

306.6

0

100

200

300

400

500

600

700

0 10 20 30 40 50 60 70

Sh

ea

r F

orc

e (

N)

Time (minute)

5.08 mm •Comparing the width of indium to

the sealing duration shows: •90% of compression will occur

after 6 minutes. • Indium will continue to flow

while under compression. • Increasing the time from 11

minutes to 60 minutes did not cause the indium to flow enough to fill the entire sidewall.

• Increasing time also did not sufficiently increase the sealing strength. A greater increase was seen when increasing applied load.

Page 7: Status Update for Indium Cold Sealing Process...5.08 mm •Comparing the width of indium to the sealing duration shows: •90% of compression will occur after 6 minutes. •Indium

Analysis of 1 inch Data

501.1

634.6 650.1 701.8

0

100

200

300

400

500

600

700

800

0 20 40 60 80 100

Sh

ea

r F

orc

e (

N)

Temperature (ºC)

20

40

60 80

0.00

1.00

2.00

3.00

4.00

5.00

6.00

0 20 40 60 80 100

Ind

ium

Wid

th (

mm

)

Temperature (ºC)

5.08 mm

• Increasing temperature of sealing had a great impact on the width of the indium. Interpolation predicts that only 50 ºC is needed to cause the indium to flow to the thickness of the sidewall in 11 minutes.

• The greatest increase in strength was between 20 ºC and 40 ºC showing that increasing the temperature by any amount will increase the strength of the seal.

• The width at 80 ºC was less than that at 60 º, however the strength is greater. This is evidence that temperature improves the bond as well as the making the indium more malleable.

Page 8: Status Update for Indium Cold Sealing Process...5.08 mm •Comparing the width of indium to the sealing duration shows: •90% of compression will occur after 6 minutes. •Indium

Analysis of 1 inch Data

0.0

100.0

200.0

300.0

400.0

500.0

600.0

700.0

800.0

2.00 3.00 4.00 5.00 6.00

Sh

ea

r F

orc

e (

N)

Indium Width (mm)

• This plot combines the data points of all tests to show the correlation between indium width and bond strength.

• Shear force appears to be asymptotic to approximately 700 N.

• It is possible this limiting nature is due to surface oxides on the indium. As the indium flows under compression, the oxide will continue to break and spread out along the bond area.

5.08 mm

Hermetic Packaging Godparent Meeting 3 April 2013 M. E. Kupfer [email protected]

Page 9: Status Update for Indium Cold Sealing Process...5.08 mm •Comparing the width of indium to the sealing duration shows: •90% of compression will occur after 6 minutes. •Indium

Inspection of Seals - SEM

Bonding Some Bonding Bonding

•Glass coated in NiCr. Sample aged 7 days at 80 ºC and then 9 days at 130 ºC. • Shear testing revealed bonding at the two outside edges of the indium, as well as

some in the middle. • Few samples were tested, however it was seen that aging NiCr samples had a great

impact on seal strength.

Hermetic Packaging Godparent Meeting 3 April 2013 M. E. Kupfer [email protected]

Page 10: Status Update for Indium Cold Sealing Process...5.08 mm •Comparing the width of indium to the sealing duration shows: •90% of compression will occur after 6 minutes. •Indium

Inspection of Seals - SEM

Bonding

No Bonding

•Glass coated in Cr. Sample aged 7 days at 80 ºC and then 9 days at 130 ºC. •Clear evidence that bonding occurs only at the outside edges of the indium. • The strength of this seal was not significantly greater than un-aged Cr samples.

Hermetic Packaging Godparent Meeting 3 April 2013 M. E. Kupfer [email protected]

Page 11: Status Update for Indium Cold Sealing Process...5.08 mm •Comparing the width of indium to the sealing duration shows: •90% of compression will occur after 6 minutes. •Indium

Leak Checking of 4 inch Seals

• Initial leak checking of 4 inch samples was difficult. Several types of spacers were used in an attempt to mitigate the deflection of the window while under vacuum.

•Most samples appeared to be leak tight at first, only to have leaks forms at the corners during testing.

• To remove the problem, the 4 mm thick window was replaced with a 16 mm thick window to reduce the deflection.

• Since making the switch, no leaks have formed in the corners. (Leaks have been found in other places.)

Hermetic Packaging Godparent Meeting 3 April 2013 M. E. Kupfer [email protected]

Page 12: Status Update for Indium Cold Sealing Process...5.08 mm •Comparing the width of indium to the sealing duration shows: •90% of compression will occur after 6 minutes. •Indium

Leak Checking of 8 inch Seals

• The same issue was occurring with the 8 inch seals. Finite element simulation of the seal shows that when the window bows downward under vacuum, the corners lift up, breaking the seal.

•16 mm thick plates were used to prevent this deflection in order to move forward with experimentation.

Hermetic Packaging Godparent Meeting 3 April 2013 M. E. Kupfer [email protected]

Page 13: Status Update for Indium Cold Sealing Process...5.08 mm •Comparing the width of indium to the sealing duration shows: •90% of compression will occur after 6 minutes. •Indium

FEA of 8 inch Seals

• Z Deflections •Blue is <0

Glass on glass, 1/8 inch corner radius

• Z Deflection on plate at inside edge of wall.

•Red is >0.

Hermetic Packaging Godparent Meeting 3 April 2013 M. E. Kupfer [email protected]

Page 14: Status Update for Indium Cold Sealing Process...5.08 mm •Comparing the width of indium to the sealing duration shows: •90% of compression will occur after 6 minutes. •Indium

Progression of 8 inch Seals

•Using the 16 mm thick windows, seals were made with large radii corners, working progressively to tight corners to match the width of the sidewalls.

• First seal made was a 14 cm diameter circle gasket. Sample was held under vacuum for 15 days, periodically being exposed to air and pumped down again.

• For the following seal, the radius was increased to 19 cm.

• This seal was held for 12 days at vacuum with periodic vacuum cycling. It remained leak tight over the entire duration.

Hermetic Packaging Godparent Meeting 3 April 2013 M. E. Kupfer [email protected]

Page 15: Status Update for Indium Cold Sealing Process...5.08 mm •Comparing the width of indium to the sealing duration shows: •90% of compression will occur after 6 minutes. •Indium

Progression of 8 inch Seals

•Most recently, a seal was made with corners that match the radius of a typical sidewall, ~6.4 mm.

•After 8 days under vacuum, the part remains entirely leak tight.

Hermetic Packaging Godparent Meeting 3 April 2013 M. E. Kupfer [email protected]

Page 16: Status Update for Indium Cold Sealing Process...5.08 mm •Comparing the width of indium to the sealing duration shows: •90% of compression will occur after 6 minutes. •Indium

Conclusions

Hermetic Packaging Godparent Meeting 3 April 2013 M. E. Kupfer [email protected]

Future Work

•Gained an understand how process parameters affect the thickness, width, and strength of the seal. Two good places to go further:

•20 ºC, 1890 N applied load, 11 minutes •50 ºC, 1180 N applied load, 11 minutes

•Consistent success making 8 inch seals using 16 mm thick glass plates.

•Complete work with NiCr coated 1 inch parts. •More work with NiCr coated 4 inch plates, moving to parts with actual

sidewalls. •Making 8 inch seals with fritted anode/sidewall and rigid internal supports

(no MCPs) •Considerations for other indium alloys.