Willkommen

Welcome
Bienvenue

Vacuum Insulated
Glazing - Winsmart
Ernesto Claure Ramirez

Building a sustainable future

 The place I worked
Building a sustainable future

 In the department of Civil and Mechanical Engineering.

 While I worked in the labor Building Energy Materials and
Components.

1. Superinsulating materials. 2. Advanced sol-gel materials. 3. Building Integration

Building Energy Materials and Components 2

 What is about it?
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1. Introduction. What is the problem? Energy losses

2. Liquid Anodic Bonding (ALTSAB)
3. Setup
4. Problems.
a) Inhomogeneous Solder Frame.
b) Soft Soldering.
c) Anodic Bonding.
5. Experiment
a) Peel test.
b) Leak test.
6. Conclusions
7. Recommendations (Take towards a pilot facility)
8. Acknowledgments.

Building Energy Materials and Components 3

Energy losses in buildings
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Transporte; 28.00%
Industria; 33.00%

Edificios ; 39.00%

60% of heat losses

through windows

Current EU legislation:
-Facade elements ≈0.3-0.4 W/m2 K
-Glazing ≈1.2-1.7W/m2K
State-of-the-Art technologies:
-Facade elements ≈0.15 W/m2 K
-Glazing ≈0.7W/m2K
Building Energy Materials and Components 4
Current solutions on the market
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U Value [W/m2K]
Single pane 4.7

Conductivity
Double pane (air) 2.7 [mW/mK]
Air: 9.3
Argon: 6.2
Krypton: 3.3
Double pane 1.1 (0.8)
(Ar (Kr)+ low e
coating)

Triple pane
0.7
(Kr+ low e
coating)

Building Energy Materials and Components 5

Vacuum Insulated Glazing (VIG)
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Theoretical Ug≈0.3-0.5W/m2K
(P = 10-3-10-4 mbar)

Building Energy Materials and Components 6

 Gas-tight seal.
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 Highly hermetical (10-12 mbar-l/s  P=10-2mbar in 30 years.)

 Mechanically strong (P=1 bar + thermal stresses over service life.).

Spacers

Pilkinton SpaciaTM
U=1.1 W/m2K Solder
Pump-out glass
hole seal
 Bends when fully pumped.
ΔT>35oC .
 Not working at full capacity.

FLEXIBILITY
Source: pilkinton.com

Building Energy Materials and Components 7

Winsmart approach: Flexible edge seal
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 Use of a protruding metal foil.

 Glass-to-metal joint?

Half VIGs

300oC

Coin

Building Energy Materials and Components 8

Solder injection based on first experiences
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Gear system
operated by a
Bronze
DC motor.
piston

Injection tube Injector

body

Highest Al content
(failure at dilaton-solder)

Lowest Al content
(failure at glass-solder) Slag (oxides)

Molten tin

FeO/NiO + Al  Al2O3 + Fe/Ni?

Building Energy Materials and Components 9
Setup
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800V
But the current is to
300 oC high, so the voltage
will reach that
quantity in about
one minute.
P=V*i

Building Energy Materials and Components 10

 Setup
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Weight system Motor for injection

Motor for wheel

Forming gas input

Pulling
High voltage wheel.
Injector
cart.

Metallic ribbon
(dilaton -48) on
top of glass pane

Building Energy Materials and Components 11

 Building a sustainable future

4. Problems.
a) Inhomogeneous Solder Frame.
b) Soft Soldering.
c) Anodic Bonding.

Building Energy Materials and Components 12

 A). Inhomogeneous solder frame
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Too much superficial

tension

Inhomogeneous solder frame

Sucked areas

How to produce a continous

solder frame?
Overflowing must be avoided.

Overflow

Building Energy Materials and Components 13

1. Right quantitiy of tin
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Tin nedeed
Tin nedeed
[g] [g] Tin inTin
thein path [g] [g]
the path
AA 30.7330.73 33.75
34.04
BB 26.9726.97 27.86
21.58
CC 30.7330.73 32.53
48.94
DD 26.9726.97 29.45
30.59

Building Energy Materials and Components 14

2. Flatness
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 Thicker sides/corners or places where there was predominatly

overflow were lifted up by 200-1200μm.

 Compression layer sustitution, bending of bottom plate, etc.

Building Energy Materials and Components 15
3. Droplet position.
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6.5 mm

13mm 11mm 8.5mm

Building Energy Materials and Components 16

Result, completely upscaled sample.
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Overall success rate: 25%

Success rate since June: 70%

15 potentially leak-tight
upscaled samples
38perfectly
samples injected
for peel ones
test,
and 7 for leak test, which i
will present you in he
experiments.

Building Energy Materials and Components 17

B) Soft soldering
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 As you see the plots for soft soldering results, in a complete sample.

Building Energy Materials and Components 18

2. Soft soldering
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 Zero wettability experiment (show different angles)

 Explain conditions for nice soft soldering.

 Explain which conditions you have. (Dilaton, no flux, no slag, iron and
nickel oxide, atmosphere).
Building Energy Materials and Components 19
3. Anodic Bonding bubbles
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 Scattered results are surely due to bubbles and non metallic

inclusions.

Building Energy Materials and Components 20

 3. Anodic Bonding bubbles
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1. Regions without bubbles

2. Regions with porous random
distribution of size micrometer

Were there are not bubbles anymore, the strength will be higher.
Nevertheless, we do not know why and that will publish in any other
presentation

Building Energy Materials and Components 21

 Building a sustainable future

5. Experiments
a) Leak Test.
b) Peel Test.

Building Energy Materials and Components 22

Leak test
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Helium with a gun,

and detected by
Mass spectrometers

Building Energy Materials and Components 23

 Leak test
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Pressure needed: 10-3mbar.

Leak rate: 10-12mbar-l/s

Cracking (solder-dilaton
and solder-glass)

Building Energy Materials and Components 24

 Leak test
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There was epoxy between the

glass and the Dilaton

Building Energy Materials and Components 25

Peel test
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Building Energy Materials and Components 26

Peel test
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50

45

40

Average peel force (N) 35

30

25

20

15

10

0
50 100 150 200 250
Al content (ppm)
 Interesting to see that the failure is predominantly at glass interface:
1. Many deffects over large areas induce scatterring and low
strength. 2. Or we never get rid of the oxides completely.
 The higher the aluminum (150-250 ppm) the glass will fail more
easy. So maybe they have more bubbles with that composition.

Building Energy Materials and Components 27

Peel test
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Building Energy Materials and Components 28

Conclusions
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 15 samples were complete, which 8 was for peel test, and 7 for the
leak test.

 The forces of the samples with 112.5 ppm were upside 15 N (about
one half of the sample)

 The soft soldering area was really low (2-3 millimeters). To scrape
the metal before of making the sample did not work. The
atmosphere do not have enough oxygen, to have slag in the
Dilaton.

 The bubbles in the anodic bonding makes the forces to be low. The
size of the bubbles was between 10-300 microns but that is not
correctly true, and they have to be investigated.

Building Energy Materials and Components 29

Takeaways towards a pilot scale facility
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 Not trivial, it is important for further piloting and upscaling:

 1. Injection
 Flatness. (Rods in a continous production line after floating the
glass).
 Injection (better control of the surface tension and viscosity under
inert atmosphere, plus well calibrated equipment flow).

 2. Soldering
 Oxidation in leaky chamber. (Oxygen pressure control in different
spots, leak tight sealing, better control of gas flow). That will help to
optimize further the solder composition (increase the most the
aluminum content). Pumping before flushing can make the organics
fade away.

Building Energy Materials and Components 30

Takeaways towards a pilot scale facility
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 2. Soft Soldering
 No laserwelding needed if there could be machining.

 3. Bubbles AB quality:
 Solubility studies should be made to avoid this situation.
 Handeling and degassing of tin before injection (show how
metallurgists could it)
 Cleaning facilities should be there (H 2O2)

Building Energy Materials and Components 31

Acknowledgements
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 Wim Malfait

 Martin Kuckla and Robert Klemencic.

 The guy who did the drawings.

 Workshop guys.

 All the guys that have helped me (The hole team of my labor)

 Wilson.

Building Energy Materials and Components 32

Literature
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 Source of fig 1: duette.co.uk/blog/value-u-value/

 Source of fig 2. Fuente: Departamento de Energía de Estados Unidos: 2008 Buildings
Energy Data Book.
 Fig 3. Made by myself
 Fig 4. Weinläder H (2005) Vacuum Insulating Glass. 7th Vacuum Insulation Symposium.
 Fig 5. Pilklington.com
 Fig 6. Pilklington.com
 Fig 7. Made by myself.
 Fig 8, 9, 28, and 33. Malfait J. W. (2016) Optimized solder composition by
simultaneous soldering and anodic bonding. Journals of Materials Processing and
Technology 236, 176-182.
 Fig 10-19. Made by myself.
 Fig 20. Messler R.W. (2004). Joining of Materials and Structures. Elsevier. p. 396.
 Fig 21-23 made by myself.
 Fig 24. Frauenhofer.
 Fig 25. Frauenhofer.
 Fig 26-27, 29-32: Paper in proccess

Building Energy Materials and Components 33

Brushes and optimized atmosphere
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 Take pictures of brushes in action, and dissapointing results.

 Show more homogeneous soldering now (from your broken
samples) with new atmosphere.

1. It could be that thermite is not occuring

anymore.

Building Energy Materials and Components 34

 Building a sustainable future

 Show electrode configuration made (based on alumina layers

beeing formed and trapping bubbles?). Since there were still a lot of
bubbles that proofed not to be the mechanism.
 Show differences in bubbles distributions. More wettability the
tinnier the bubbles?

 Could it be close system which does not allow for permeation?

 Are the bubbles the result of degasing during/after anodic bonding?
[] Are the bubbles a result of degesing of organics (new tape),
nitrogen, hydrogen, oxygen? [].

 Under the conditions we had, there was probably a thick NiO layer
and in top of it spinel (FeONiO). Line solves this, and solves it for
whatever oxide there is.

Building Energy Materials and Components 35

Problems with strength
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 Explain the aluminum content penalty, when you do the triple interface.

 Show evidence about aluminum: The more aluminum the thicker de alumina layer formed
through the termite reaction. The less aluminum the less of this layer is formed and the more
the NiO stays. The oxide should be basically NiO because of the color and because of the
predominant formation of FeSn2. The NiO probably allows for better difussion of the solder.

 Show segregation in every bubble point, which could lead to all the scattered regions
(because of aluminum?)

Building Energy Materials and Components 36