dispensable getter materials for lifetime insurance in...
TRANSCRIPT
Dispensable Getter Materials for lifetime insurance in Organic Electronics
Paolo Vacca,
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Paolo Vacca,
Roberto Giannantonio, Antonio Bonucci, Stefano Zilio, Stefano Tominetti
SAES Getters
"ORGANIC ELECTRONICS : principles, devices and applications“Politecnico di Milano – November 18, 2011
Outline
� Overview of the SAES Group
� Organic device degradation
� Encapsulation lay-out
� A new family of Dispensable Getter Materials
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� A new family of Dispensable Getter Materials
� Conclusions
2 SAES Getters S.p.A.
Overview of the SAES Group
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1947 SAES, Società Apparecchi Elettrici e Scientifici based in Milan (Italy), becomes operative through investments by families della Porta and Canale.
3 SAES Getters S.p.A.
Overview of the SAES GroupSAES core business
The SAES® Getters Group develops technologies and products addressing a variety of scientific and industrial applications needing:
� high vacuum� pure metals evaporation� ultra-high pure gases
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A Customer-focused approach
Nearly 3,000 active customers in 5 continents, spanning from universities and research centers to business start-ups and blue chip companies
High flexibility in product development, fine-tuning and manufacturing, to foster emerging and forefront application technologies
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blue chip companies technologies
70 years of expertise in partnering with customers for the engineering of fully customized solutions
Technical service network and CRM structure supporting customers’ innovation24 hours a day
5 SAES Getters S.p.A.
Corporate Headquarters
� Management of the Group
� Corporate R&I laboratories
� Corporate functions
Milan-area Headquarters
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� Corporate functions
� Technical support
6 SAES Getters S.p.A.
Global Presence
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Research & Innovation
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� About 12% of net consolidated sales allocated to R&I activities every year
� State-of-the-art corporate laboratories covering a surface of over 3,300sq. m.
� Nearly 80 people committed to investigating problems, developingproposals and testing solutions
8 SAES Getters S.p.A.
Outline
� Overview of the SAES Group
� Organic device degradation
� Encapsulation lay-out
� A new family of Dispensable Getter Materials
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� A new family of Dispensable Getter Materials
� Conclusions
9 SAES Getters S.p.A.
0,8
1,0 450
482
Intensity [a.u.]
12V
420
OLED OLED degradation
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350 400 450 500 550 600 650
0,0
0,2
0,4
0,6
wavelength [nm]
Intensity [a.u.]
12V 11V 9V
PhD Thesis “TECHNOLOGY AND ELECTRO-OPTICAL CHARACTERIZATION ON ORGANIC SEMICONDUCTOR DEVICES” P. Vacca
10 SAES Getters S.p.A.
Organic Electronic Devices degradation phenomena
H2O, O2contamination
Extrinsic
External contamination
Intrinsic
Inter-diffusion
Material changes
Material blending
EvolutionEvolution
MechanismMechanism
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During shelf life During operation During operation
Dark spots Pixel shrinkage
Dark spots Short circuits
Luminance decrease
Anisotropic Anisotropic Isotropic
EvolutionEvolution
DefectsDefects
UniformityUniformity
11 SAES Getters S.p.A.
Organic Electronic Devices degradation phenomena
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In order to limit dark spot area growth and pixel shrinkage below values significantly affecting the display uniformity: maximum H2O pressure inside OLEDs ~ 1.1x10-4 Torr or ~ 0.1 ppm
12 SAES Getters S.p.A.
Outline
� Overview of the SAES Group
� Organic device degradation
� Encapsulation lay-out
� A new family of Dispensable Getter Materials
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� A new family of Dispensable Getter Materials
� Conclusions
13 SAES Getters S.p.A.
Permeation fronts in inefficient encapsulation package
glass sheet
Barrier sealant
d� Interfaces
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glass substrate
anode
cathode
dInterfaces
� Barrier bulk
� Organic EL layers
14 SAES Getters S.p.A.
Barrier properties of some coatings
10-2
100
102
sensitive food products
oxy
gen
tra
nsm
issi
on
rat
e (c
m3 /m
2 d)
LCD LED
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10-6 10-4 10-2 100 10210-6
10-4
10-2
OLED displays, organic solar cells
oxy
gen
tra
nsm
issi
on
rat
e
Water vapour transmission rate (g/m2 d)
15 SAES Getters S.p.A.
Encapsulation package optimization (1): lay-out
glass sheet
2. Barrier sealant : SAES active barrier
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glass substrate
anode
cathode
1. Patterned Organic EL layers
l
16 SAES Getters S.p.A.
Encapsulation lay-out
Barrier sealantIncreased lag time can be achieved by increasing l (1-2mm) and
Organic ELPatterned layer to reduce the penetration front
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Increased lag time can be achieved by increasing l (1-2mm) andby decreasing h (up to 5-10 µm scale)
h
17 SAES Getters S.p.A.
Encapsulation package optimization (1): improved interfaces
� filler size
� filler surf.-mod.
Drop surface
tension
- fVS ; + fLV� non-wetting
Increasing
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� filler surf.-mod.
� matrix polarity
� filler content
� viscosity
Drop surface
tension
Substrate surface energy
+ fVS ; - fLV� good wettability
Increasingpaste polarity
18 SAES Getters S.p.A.
Dispensing quality depends on viscosity which is affected by:
o molecular weight of organic matrixo nature and amount of filler contento nature and amount of scavenger contento filler and scavenger particle size distributiono scavenger surface modification
Viscosity modulation
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Particle size distribution effect
Surface modification effect
19 SAES Getters S.p.A.
Jet dispensing
Jetting fluid dispensing technology is gaining popularity in the manufacture of Flat Panel Displays (FPD) due to increased throughput, improved yields, and simpler setup.
o jets in tight spaces as small as 175 µmo small fillet sizes as small as 300 µmo dot diameter as small as 200 µm
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o dot diameter as small as 200 µmo shot volumes as small as 1.0 nanoliters
o jet stream size as small as 50 µm
o jets fluids from 1 to 250,000 mPa
20 SAES Getters S.p.A.
Jet dispensing
Shear rate related to the
The key element of a jet dispensing system is a valve that meters and ejects fluid droplets: gas pressure retracts an internal spring-driven plunger, allowing a precise amount of fluid from the reservoir to enter the chamber under pressure. The spring-driven plunger then returns to its seat, ejecting the fluid as a droplet though the nozzle.
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� Shear rate related to the ejecting process: 102-104 s-1
With non-Newtonian fluids like dispensable scavengers, viscosity decreases with increasing shear rate.
The paste must have the ability to restructure and recover its viscosity as soon as it reaches the substrate (thixotropy).
21 SAES Getters S.p.A.
Thixotropy for improving scavengers processability
1,0E+03
1,0E+04
shear stress (Pa
)
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1,0E+00
1,0E+01
1,0E+02
1,0E-03 1,0E-02 1,0E-01 1,0E+00 1,0E+01 1,0E+02 1,0E+03 1,0E+04
shear stress (Pa
)
shear rate (s-1)
thixotropic
22 SAES Getters S.p.A.
Molecular weight impact on jet dispensing
� Drop break-up is strongly related to the polymer molecular weight.
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Molecular weight much too high
23 SAES Getters S.p.A.
ODF process for optimized encapsulation
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ODF process for optimized encapsulation
Process step:• Coated glass is placed on the substrate mask into the chamber• Cover glass is held by the clamp device (chuck) on the cover of the UV-press• The system is evacuated to the process-pressure value (10-2 mbar)• The two glasses are put in contact• System pressure is equalized to the atmospheric pressure• The UV-lamp irradiate the sample
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• The UV-lamp irradiate the sample• The encapsulated sample can be removed
25 SAES Getters S.p.A.
Outline
� Overview of the SAES Group
� Organic device degradation
� Encapsulation lay-out
� A new family of Dispensable Getter Materials
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� A new family of Dispensable Getter Materials
� Conclusions
26 SAES Getters S.p.A.
The concept of Lag time
Slope = WVTR
Typical permeation curveof a sealed system
Moisture concentration
w e support your innovationBreakthrough time
Lag time
Moisture concentration increases rapidly, even with a “good” WVTR.
Therefore, a desiccant is needed.
27 SAES Getters S.p.A.
Getter technologiesdefinition of getter
� Gases can be captured through GETTER materials
� Capture = adsorption, dissolution, chemical reaction
� Specific feature of a GETTER material: capture kinetics is very fast, at the
given operating temperature, even if the gaseous species are highly rarefied
(highly diluted)
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� capture is either irreversible
G + g G�g×
� or reversible
G + g G�g
28 SAES Getters S.p.A.
Getter integration in OLED devices: modeling
Once moisture sources are identified, moisture distribution within a device depends on geometry and placement of the desiccant
Moisture ingress can be determined for a variety of structures, and equations set in place to model
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Example:
30*40 mm2 OLED
2 25*14 mm2 DryFlex®
Test condition:
T=60 ° CRH=90%
29 SAES Getters S.p.A.
Hybrid organic-inorganic gettersL ���� L ���� S
L L S
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� surface properties� rheological properties� curing properties
deposition processes
� functional properties
solidification processes
30 SAES Getters S.p.A.
Degradation of Organic Electronic Devices dispensable dryers (hybrid getters)
anode
glass sheet
getter filmgetter filmgetter filmgetter filmreactive edge sealantreactive edge sealantreactive edge sealantreactive edge sealant
d
anode
glass sheet
reactive fillerreactive fillerreactive fillerreactive filler
d
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glass substrateanode
cathode organic EL layer
glass substrate
cathode organic EL layer
BOTTOM EMISSIONBOTTOM EMISSIONBOTTOM EMISSIONBOTTOM EMISSION TOP EMISSIONTOP EMISSIONTOP EMISSIONTOP EMISSION
Formulation Dispensing Curing Solid coating
31 SAES Getters S.p.A.
Hybrid organic-inorganic gettersL ���� L ���� S
Non transparent Transparent
Nano-ZeolitesOxide systems Other chemistry
Organic Electronics
DisplaysPlastic ElectronicsSolar Cells
Thermal / UV Curing Thermal / UV Curing
T i
m e
L
i n e
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Thermal Curing
Active Barriers
Thermal / UV Curing Thermal / UV Curing
DryPaste ®Glue
Gel
Paste
Polymer systemsT
i m
e
L i n
e
32 SAES Getters S.p.A.
SAES approach
Polymerization
Step polymerization
Polyaddition (hydrosilylation)
Polymer begins
• Controlled reactivity
• No by-products
• Gel-elastomer polymers with lower cross-link density
APPLICATION
FILLER
with high dispersingproperties
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Polymerization process
Chain Polymerization
Radical polymerization
Cationic polymerization
• Polymer begins to form immediately
• Chain growth is very rapid under low UV dose
i) UV curable filler (low dose)
ii) thermal curablefiller (low temp.)
UV curable edgesealant
• UV curing under high energy dose
• better properties like adhesiveness
33 SAES Getters S.p.A.
Consolidation mechanism
Polymerization
Step polymerization
Polyaddition (hydrosilylation)
Polymer begins
• Controlled reactivity
• No by-products
• Gel-elastomer polymers with lower cross-link density
APPLICATION
FILLER
with high dispersingproperties
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Polymerization process
Chain Polymerization
Radical polymerization
Cationic polymerization
• Polymer begins to form immediately
• Chain growth is very rapid under low UV dose
i) UV curable filler (low dose)
ii) thermal curablefiller (low temp.)
UV curable edgesealant
• UV curing under high energy dose
• better properties like adhesiveness
34 SAES Getters S.p.A.
Hydrosilylation reaction for gel scavenger production
Filler
� Gels are solids featuring fluid characteristics� A filler gel provides mechanical protection and high instantaneous
deformation� Dampening with good cohesion assures high dryer loading
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FILLER
OLED Stack
Filler
35 SAES Getters S.p.A.
DryPaste1-Ga gel filler for OLED devices
Aluminum cathodeOLED in bottom emission configuration
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Organic stackDryPaste-G in direct contact with stack and cathode
36 SAES Getters S.p.A.
1This material and its associated products are covered by a PCT patent application deposited by SAES Getters S.p.A.; DryPaste is a registered trademark by SAES Getters S.p.A.
Polyaddition (hydrosilylation)
Ethylenically unsaturated polydiorganosyloxanes can be cured by addition reaction where the curing agent for a organosilicon mixture is an organo-hydrogensiloxane containing an average of more than two silicon bonded hydrogen atoms per molecule.
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Working on cross-link density, it is possible to induce gel-like or elastomeric characteristics.
37 SAES Getters S.p.A.
DryPaste-G
� DryPaste-G is a solventless dispersion of a chemical dryer in a siliconic matrix.
� It can be used as a film (10-500 µm) or as a patterned desiccant.� It is supplied in syringes sealed under protected atmosphere.� Mixing is not necessary.� Deposition can be performed by syringe, screen printing and blading
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� Deposition can be performed by syringe, screen printing and blading (40.000-50.000 cP @ shear rate 45s-1 ).
� Deposition can be carried out in air.� DryPaste-G can also be used on flexible substrates.� Thermal curing (120°C for 3h) also possible (gel � solid).
38 SAES Getters S.p.A.
DryPaste flow curve at 25 °C
1000000
10000000
Substrate C.A.glass 72.6 ± 3.6EVA 73.8 ± 2.7PET 70.0 ± 2.3
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0.01 0.10 1.00 10.00 100.00 1000.00
Á in 1/s
10000
100000ƒ in
mP
as
HAAKE RheoWin 4.10.0007
39 SAES Getters S.p.A.
DryPaste-G
Opening
IN AIR OR DRY GAS
DryPaste-G Process Flow
Device sealing
IN GLOVE BOX
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Deposition
DryPaste-Guncured film
Curing DryPaste-G film
120 oC x 3 hours or 160 oC x 1 hour
40 SAES Getters S.p.A.
DryPaste-G: thermal stability
The weight loss in dry nitrogen flux is < 0,2%wt during thermal treatment at 120 °C for 5h.
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The cured DryPaste-G film is stable up to 185 °C in dry nitrogen flux, weight loss at 240 °C is <1%. No weight loss is observed before 185 °C.
41 SAES Getters S.p.A.
DryPaste-G sorption performance at 25 oC / 55% RH
Curing at 160 oC x 1 h under nitrogen
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DryPaste-G performance(after an exposure time of 3 hours at 25 oC / 55% RH conditions)
Sorption capacity after 3 hours exposure
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Sorption capacity after 3 hours exposure in clean room air @ RT: > 10% wt
43 SAES Getters S.p.A.
Optimized composition to tune moisture sorption kinetics
LMEAN=360 µmunsaturated
1 week at 85 oC / 85% RH
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ABS range (absorbance)
completely saturated
Red-completely saturatedBlue-unsaturated
44 SAES Getters S.p.A.
Ageing at 85 oC / 85% RH
330hLMEAN=400 µµµµm
670hLMEAN=700µµµµm
170hLMEAN=180 µµµµm
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Consolidation mechanism
Polymerization
Step polymerization
Polyaddition (hydrosilylation)
Polymer begins
• Controlled reactivity
• No by-products
• Gel-elastomer polymers with lower cross-link density
APPLICATION
FILLER
with high dispersingproperties
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Polymerization process
Chain Polymerization
Radical polymerization
Cationic polymerization
• Polymer begins to form immediately
• Chain growth is very rapid under low UV dose
i) UV curable filler (low dose)
ii) thermal curablefiller (low temp.)
UV curable edgesealant
• UV curing under high energy dose
• better properties like adhesiveness
46 SAES Getters S.p.A.
Low energy dose for transparent dryer
� Transparent dryer is applied in direct contact with the organic stack� UV curing of transparent dryer involves OLED stack exposure � Strong constraint for low energy dose has to be considered in order to
avoid OLED degradation� A low-energy polymerization process has to be selected
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Transparent Dryer in FILLER configuration
OLED Stack
Filler
47 SAES Getters S.p.A.
Radical polymerization
Every step is essential for the modelling and optimization of produced polymer matrix
1. Initiation
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auto-acceleration
4. Chain-transfer
2. Propagation
3. Termination
Initiation needs very low energy
48 SAES Getters S.p.A.
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49 SAES Getters S.p.A.
AqvaDry®
� AqvaDry1 is a transparent, UV-curable or thermally curable solution of an active moisture scavenger in an organic matrix.
� Can be used as a film or as a filler.
� It is supplied in syringes sealed under protected atmosphere.
� Deposition can be performed by syringe, blading, spin coating and jet dispensing.
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and jet dispensing.
� Deposition must be carried out in dry
nitrogen.
� AqvaDry can be used also with flexible
substrates (Tg = 7 oC).
1This material and its associated products are covered by a PCT patent application deposited by SAES Getters S.p.A.; AqvaDry is a registered trademark by SAES Getters S.p.A.
50 SAES Getters S.p.A.
AqvaDry
OpeningDevice sealing before or after UV curing depending on configuration
Storage at 2-5°C
UV AqvaDry Process Flow
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Deposition
AqvaDryuncured film
UV curing Thermal curingAqvaDrycured film
IN GLOVE BOX
on configuration
100mW/cm2 for 15 s λ λ λ λ = 365 nm
51 SAES Getters S.p.A.
AqvaDry
Opening
IN GLOVE BOX
Thermal AqvaDry Process Flow
Storage at 2-5°C
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Deposition
AqvaDryuncured film
Thermal curingAqvaDrycured film
Mixing
IN GLOVE BOX
Device sealing possible before curing
70 oC x 20 min
52 SAES Getters S.p.A.
AqvaDry: ODF compatibilityand thermal stability
Uncured AqvaDry film weight loss under different vacuum conditions: perfect compatibility with the ODF process.
Pressure(mbar)
Process Time(h)
wt% loss
1 2 0,1910-2 2 0,1910-3 2 0,19
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The uncured material is stable up to 85 °C.
Cured AqvaDry is stable up to 180 °C where a decomposition process starts in the organic matrix.
53 SAES Getters S.p.A.
Thermal expansion coefficient and wettability
Temperature (°°°°C) CTE (1/°°°°C)20 6.9x10-3
60 6.9x10-3
100 4.8x10-2
CTE evaluated by Dynamic Mechanical Thermal Analysis (DMTA).
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100 4.8x10-2
Contact angle values measured through the sessile drop method.
Substrate C.A.glass 30.7 ± 1.6stainless steel 51.0 ± 2.1PET 28.7 ± 2.1
glass PET Stainless
steel
54 SAES Getters S.p.A.
Transmittance > 95% for a 100 µm thick filmRefractive index = 1.50
Transmittance spectrum after curing
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UV curing / thermal curing
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Isothermal scan at 70°C (curing: 30 min)
UV Curing dose: 1.5 J/cm2
56 SAES Getters S.p.A.
AqvaDrysorption performance @ 25 oC / 55% RH
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Consolidation mechanism
Polymerization
Step polymerization
Polyaddition (hydrosilylation)
Polymer begins
• Controlled reactivity
• No by-products
• Gel-elastomer polymers with lower cross-link density
APPLICATION
FILLER
with high dispersingproperties
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Polymerization process
Chain Polymerization
Radical polymerization
Cationic polymerization
• Polymer begins to form immediately
• Chain growth is very rapid under low UV dose
i) UV curable filler (low dose)
ii) thermal curablefiller (low temp.)
UV curable edgesealant
• UV curing under high energy dose
• better properties like adhesiveness
58 SAES Getters S.p.A.
Cationic polymerization for adhesive barrier composites
Edge sealant
� Polymerization reaction needs longer time and higher UV dose.� Curing conditions are not suitable for direct OLED stack exposure.
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OLED Stack
Edge sealant
59 SAES Getters S.p.A.
Cationic polymerization
� Initiation reaction generally involves Brönsted and Lewis acids.� The inital step needs a high energy dose.
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A reactive edge sealant: ZeoGlue®®
A dispensable dryer based on� surface-modified nano-sized LTA zeolite� UV-curable and/or thermally-curable epoxy
formulation
Main properties� no phase segregation due to chemically tailored
particle surface (class-I materials from non-reactive capping agents, class-II hybrid materials
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reactive capping agents, class-II hybrid materials from reactive capping agents)
� no leaking pathways within the substrate/scavenger interphase due to particles wetting
� transparency of films in the visible range due to reduced discontinuity of refraction index across the particle/matrix intephase (class-II hybrids)
� excellent adhesive properties due to particles wetting
� good sorption properties (capture rate, capacity, energetics: low H2O vapour pressure)
61 SAES Getters S.p.A.
ZeoGlueparticle size distribution
5,00
10,00
15,00
20,00
25,00
30,00
f(d
) (%
)
XRD LTA POD
0
100
200
300
400
500
600
700
800
900
5 7 9 11 13 15 17 19 21 23 25 27 29 31 33 35 37 39 41 43 45 47 49
2 θ
Inte
nsi
ty
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� Mean particle size: 100-300 nm� Very sharp particle size distribution
� inkjettable scavengers� smooth coatings� thin coatings (2-3 µm)� transparent coatings
100 nm
0,00
5,00
0 4 23 133 750 4237
d (nm)
2 θ
62 SAES Getters S.p.A.
ZeoGluedifferent formulations for different deposition techniques
1,0E+03
1,5E+03
2,0E+03
Vis
cosi
ty (
cP)
SPIN COATING
SCREEN PRINTING
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Mean particle size and particle size distribution enable getter inks for patterning and local protection
0,0E+00
5,0E+02
5 10 15 20 25
Component A (% wt)
Vis
cosi
ty (
cP)
INK-JET
SPIN COATING
ZeoGlue
C.A. glass 79.7 ± 1.6
C.A. stainless steel 76.5 ± 2.1
C.A. PET 68.7 ± 2.1
63 SAES Getters S.p.A.
Photocalorimetric analysis
UV 365 nm
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ZeoGlueWVTR, breakthrough time, lag time
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ZeoGluebreakthrough time (85 °C / 85% RH)
reactive edge sealantreactive edge sealantreactive edge sealantreactive edge sealant
glass substrateglass substrateglass substrateglass substrateanodeanodeanodeanode
glass sheetglass sheetglass sheetglass sheet
cathodecathodecathodecathode
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dtransversal widthtransversal widthtransversal widthtransversal width
66 SAES Getters S.p.A.
ZeoGluediffusion kinetics
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FTIR 3D map of moisture diffusion front (transmittance of OH)
67 SAES Getters S.p.A.
ZeoGluediffusion kinetics
0,80
1,00
1,20
1,40
1,60
Area
ratio
Area
ratio
Area
ratio
Area
ratio
Glue 0h
Glue 24h
Glue 48h
Visible penetration front 24h
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Diffusion profiles from border to center of glass-to-glass ZeoGlue aged @ 85 °C / 85% RH. Absorbance ratio OH peak area on epoxy CH3 combination peak to normalize on film thickness.
0,00
0,20
0,40
0,60
0,00 1,00 2,00 3,00 4,00 5,00 6,00 7,00 8,00 9,00
Distance from side to center (mm)Distance from side to center (mm)Distance from side to center (mm)Distance from side to center (mm)
Area
ratio
Area
ratio
Area
ratio
Area
ratio
Visible penetration front 48h
68 SAES Getters S.p.A.
Conclusions
� Even considering the use of the most performing materials today available to seal or protect the displays (glues, barriers, etc.) and the best lay-out, , the introduction of a suitable dryer is mandatory to prevent moisture contamination inside OLEDs.
� Dispensable getter materials properties can be designed by
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� Dispensable getter materials properties can be designed by considering the final application requirements
� The integration of novel dispensable SAES getter materials and concepts provide a lifetime insurance for Organic Electronics applications.
69 SAES Getters S.p.A.
Hybrid Polymer Lab.R&D SAES
� Paolo Vacca, PhD
Macromolecular Chemistry, OrganicElectronics
� Dr.ssa Alessandra Colombo
Dispensing, encapsulation, formulations,physico-chemical characterization
� Marco Mudu
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� Marco Mudu
Formulations and sampling
� Giorgio Macchi, PhD
Sol gel chemistry, microencapsulation
� Jiabril Gigli, PhD
Rheology, filler/polymer interfacialinteractions, Experimental Design
� Andrea Ravasio, PhD
Polymer waveguides, OrganometallicChemistry
70 SAES Getters S.p.A.
Thanks for your attention
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SAES® Getters is a registered trademark of SAES Getters S.p.A.