HIGH Z DOPING OF GLASS SHELLS Presented by Martin
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• First glass shell from SiGDP
1999
2001
2003
2005
Year
2007
2009
•Optimum pyrolysis temperature needs to be found that results in maximum density (i.e. highest shell strength and lowest permeability)
SEM/EDXS Analysis of SiGe shells reveal changes in surface texture at high temperatures
Initial test indicates rotation system improves wrinkles and dimples but….
nm2 nm2
1.0E+5 1.0E+4 1.0E+3
- CH NIF curve
-Shell conversion without rotation
1.0E+00 1.0E-01 1.0E-02 1.0E-03
1
10
100
1000
Mode number
•Bull’s-eye fringe pattern and spheremapper/wallmapper plots show the high quality of a 1130 x 12.0µm glass shell made from SiGe-GDP
XRFer composition:
d(Silicon)
= 0.84 g/cc
d(Germanium) = 0.43 g/cc
d(Oxygen) = 1.16 g/cc
Air conversion conditions are still being fine tuned
Phase separation?
- OD 200-2200mm - Wall 3.0-35mm
• Enables filling with high Z gases (Ar, Kr, Xe)
- allows for mix experiments
• Allows for experiments requiring a dopant placed inside the glass
1.0E-1
1.0E-2 1
10
100
1000
Mode number
• With rotation
The state-of-the-art for glass shell production continues to move forward
Progress
• First SiGeO2 shells
SiGe GDP SiGeO2 (T1)
•5% Si •1% Ge •Remainder CHO
•28% Si •6% Ge •66% O
Temperature (T) T1<T2<T3
SiGeO2 (T2)
•28% Si •6% Ge •66% O
SiGeO2 (T3)
•28% Si •6% Ge •66% O
- currently homogeneously distributed throughout - specific location within the wall in the future?
Ge doped glass is made using the SiGDP to glass process
•The thinner the glass wall, generally the worse the dimpling problem.
The conversion oven used for this process has been modified to enable rotation capability
Element Weight% Atomic%
OK
57.6
75.2
Si K
27.6
20.5
Ge L
14.8
4.3
Element Weight% Atomic%
OK
55.2
74.3
Si K
26.4
20.2
Ge L
18.4
5.5
SEM/EDXS of lower temperature shard
SEM/EDXS of higher temperature shard
Metal rod with ceramic rings
•Magnetically coupled rotation of rod inside of PARR Model NJ45551 oven fitted with ceramic rings containing cavities for glass shells. Rotation prevents dimples caused by shells sitting stationary in place.
thickness, microns
nm2
1.0E+05 1.0E+04
- CH NIF curve
1.0E+03
1.0E+02 1.0E+01
- SiGe shell
11.5 11.4 11.3 11.2 11.1
0
Total ∆ wall =0.04 µm
90
180
270
360
shaft angle, deg
HIGH Z DOPING OF GLASS SHELLS
Presented by Martin Hoppe Brian Vermillion
18th Target Fabrication Specialist Meeting Lake Tahoe
May 11-15, 2008
Work supported by the U.S. Department of Energy under Contract DE-AC52-06NA27279
First successfully doped glass shell as determined by XRF is ~6 at% germanium
X-ray counts
XRF spectrum of SiGe shell
Ge Si
Ge Mo (x-ray tube)
;2
1.0E+1
1.0E+0
1.0E-1
1.0E-2 1
10
100
1000
Mode number
• Without rotation
1.0E+5 1.0E+4 1.0E+3
- CH NIF curve
-Shell conversion with rotation
1.0E+2
1.0E+1
1.0E+0
22 3.4x106
Si glass 1.47+/-0.2 2.20+/- 0.01
67 6.0x106
*SiGeO2 is ~6%Ge; 28% Si and has been pyrolyzed in air, although densification process has not yet been optimized.
IFT\P2008-034
Doped “Hoppe” glass shells enable experiments not possible with drop-tower glass shells
• Highly uniform glass shells - <0.1mm Dwall • Wide range of aspect ratios
PAMS
Si-GDP/PAMS
Si-GDP
SiO2
1
2
3
2
Si-doped GDP
Pyrolyze in N2
Sinter in air
1
2
(SiGe)-GDP 3
(SiGe)O 2
(SiGe)-doped GDP
Pyrolyze in N2
Sinter in air
Surface finish and thickness uniformity of Ge doped glass shells can be superb
• Tailored DD HL
• Low residual gases (~0.1 atm) and add inert gases such as Ar, Kr and/or Xe
• OD increased from 1.4mm to 2.2mm and maximum wall thickness increased to 35mm
Properties of 6% Ge doped glass similar to pure Si glass
Index of refraction Density (g/cc)
He Time constant t (min)
Young’s modulus (psi)
*SiGe glass 1.48+/- 0.2 2.44+/- 0.01
1.0E+5 1.0E+4 1.0E+3
- CH NIF curve
-900x4mm shell
nm2
1.0E+2
1.0E+1
1.0E+0
1.0E-1
1.0E-2 1
10
100 1000
Mode number
•Shells are stationary for days at high temperature in the conversion oven which often results in dimple formation at contact spots.
Note: Expected density of a 6% Ge doped glass is 2.48g/cc (ignoring lattice expansion caused by replacing Si with Ge).
Wrinkles and dimples reduce the yield of thin wall (<5mm) shells during the conversion process
1999
2001
2003
2005
Year
2007
2009
•Optimum pyrolysis temperature needs to be found that results in maximum density (i.e. highest shell strength and lowest permeability)
SEM/EDXS Analysis of SiGe shells reveal changes in surface texture at high temperatures
Initial test indicates rotation system improves wrinkles and dimples but….
nm2 nm2
1.0E+5 1.0E+4 1.0E+3
- CH NIF curve
-Shell conversion without rotation
1.0E+00 1.0E-01 1.0E-02 1.0E-03
1
10
100
1000
Mode number
•Bull’s-eye fringe pattern and spheremapper/wallmapper plots show the high quality of a 1130 x 12.0µm glass shell made from SiGe-GDP
XRFer composition:
d(Silicon)
= 0.84 g/cc
d(Germanium) = 0.43 g/cc
d(Oxygen) = 1.16 g/cc
Air conversion conditions are still being fine tuned
Phase separation?
- OD 200-2200mm - Wall 3.0-35mm
• Enables filling with high Z gases (Ar, Kr, Xe)
- allows for mix experiments
• Allows for experiments requiring a dopant placed inside the glass
1.0E-1
1.0E-2 1
10
100
1000
Mode number
• With rotation
The state-of-the-art for glass shell production continues to move forward
Progress
• First SiGeO2 shells
SiGe GDP SiGeO2 (T1)
•5% Si •1% Ge •Remainder CHO
•28% Si •6% Ge •66% O
Temperature (T) T1<T2<T3
SiGeO2 (T2)
•28% Si •6% Ge •66% O
SiGeO2 (T3)
•28% Si •6% Ge •66% O
- currently homogeneously distributed throughout - specific location within the wall in the future?
Ge doped glass is made using the SiGDP to glass process
•The thinner the glass wall, generally the worse the dimpling problem.
The conversion oven used for this process has been modified to enable rotation capability
Element Weight% Atomic%
OK
57.6
75.2
Si K
27.6
20.5
Ge L
14.8
4.3
Element Weight% Atomic%
OK
55.2
74.3
Si K
26.4
20.2
Ge L
18.4
5.5
SEM/EDXS of lower temperature shard
SEM/EDXS of higher temperature shard
Metal rod with ceramic rings
•Magnetically coupled rotation of rod inside of PARR Model NJ45551 oven fitted with ceramic rings containing cavities for glass shells. Rotation prevents dimples caused by shells sitting stationary in place.
thickness, microns
nm2
1.0E+05 1.0E+04
- CH NIF curve
1.0E+03
1.0E+02 1.0E+01
- SiGe shell
11.5 11.4 11.3 11.2 11.1
0
Total ∆ wall =0.04 µm
90
180
270
360
shaft angle, deg
HIGH Z DOPING OF GLASS SHELLS
Presented by Martin Hoppe Brian Vermillion
18th Target Fabrication Specialist Meeting Lake Tahoe
May 11-15, 2008
Work supported by the U.S. Department of Energy under Contract DE-AC52-06NA27279
First successfully doped glass shell as determined by XRF is ~6 at% germanium
X-ray counts
XRF spectrum of SiGe shell
Ge Si
Ge Mo (x-ray tube)
;2
1.0E+1
1.0E+0
1.0E-1
1.0E-2 1
10
100
1000
Mode number
• Without rotation
1.0E+5 1.0E+4 1.0E+3
- CH NIF curve
-Shell conversion with rotation
1.0E+2
1.0E+1
1.0E+0
22 3.4x106
Si glass 1.47+/-0.2 2.20+/- 0.01
67 6.0x106
*SiGeO2 is ~6%Ge; 28% Si and has been pyrolyzed in air, although densification process has not yet been optimized.
IFT\P2008-034
Doped “Hoppe” glass shells enable experiments not possible with drop-tower glass shells
• Highly uniform glass shells - <0.1mm Dwall • Wide range of aspect ratios
PAMS
Si-GDP/PAMS
Si-GDP
SiO2
1
2
3
2
Si-doped GDP
Pyrolyze in N2
Sinter in air
1
2
(SiGe)-GDP 3
(SiGe)O 2
(SiGe)-doped GDP
Pyrolyze in N2
Sinter in air
Surface finish and thickness uniformity of Ge doped glass shells can be superb
• Tailored DD HL
• Low residual gases (~0.1 atm) and add inert gases such as Ar, Kr and/or Xe
• OD increased from 1.4mm to 2.2mm and maximum wall thickness increased to 35mm
Properties of 6% Ge doped glass similar to pure Si glass
Index of refraction Density (g/cc)
He Time constant t (min)
Young’s modulus (psi)
*SiGe glass 1.48+/- 0.2 2.44+/- 0.01
1.0E+5 1.0E+4 1.0E+3
- CH NIF curve
-900x4mm shell
nm2
1.0E+2
1.0E+1
1.0E+0
1.0E-1
1.0E-2 1
10
100 1000
Mode number
•Shells are stationary for days at high temperature in the conversion oven which often results in dimple formation at contact spots.
Note: Expected density of a 6% Ge doped glass is 2.48g/cc (ignoring lattice expansion caused by replacing Si with Ge).
Wrinkles and dimples reduce the yield of thin wall (<5mm) shells during the conversion process