“photoneece ”” dl-1000 - toray.jp · 1 positive-tone photosensitive polyimide for insulation...
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PositivePositive--Tone Photosensitive PolyimideTone Photosensitive Polyimidefor Insulation Layer in OLED/PLEDfor Insulation Layer in OLED/PLED
PhotoneecePhotoneeceTMTM DLDL--10001000
Toray Industries, Inc.
Comparison between DL-1000 and Novolak-resist / Acryl-resist
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Spacer Structures in OLED
*Spacer means a generic name of insulating layer, bank layer and wall.
Insulation LayerInsulation Layer
Insulation Layer shape requirementsRound edge shapeLow tapered angle (20-40)Thickness 1um
AnodeRib layer (Negative photoresist)
CathodeEmitting layer
AnodePlanarization layer
TFT
Glass Glass
Emitting layer
Cathode
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DL-1000 vs. Other Materials
DL-1000 is the best material for an insulation layer in OLED/PLED
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Patterning performance
Electrical performance
Thermal stability(Outgas)
Adhesion to substratesPixel shrinkage
Low tapered angle
Solution stability
DL-1000 Acryl Novolak PR
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Material solution for Pixel Shrinkage
Initial
72hr
80/Dry
Torays polyimide Acrylic resin Novolak resin
Pixel shrinkage 0% 47% 64%
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1. Developability with alkaline solution (2.38% TMAH)
2. High resolution: 1um line/space @1m thickness
3. Low temperature cure (230/30min in air)
4. Controllable side wall angle
5. Stable electrical and chemical properties
6. Excellent thermal stability (Lower outgas)
7. Good adhesion to various substrates
8. Good UV-O3 & O2-plasma resistance
9. Good solution stability
10. Compatible with existing display process tools
1. Developability with alkaline solution (2.38% TMAH)
2. High resolution: 1um line/space @1m thickness
3. Low temperature cure (230/30min in air)
4. Controllable side wall angle
5. Stable electrical and chemical properties
6. Excellent thermal stability (Lower outgas)
7. Good adhesion to various substrates
8. Good UV-O3 & O2-plasma resistance
9. Good solution stability
10. Compatible with existing display process tools
Features of DL-1000
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Family of PhotoneeceTM DL-1000
OLED(Low molecular EL)
PLED(Polymer EL)
DL-1000
Features
Target thickness 1-2 m 1-2 m 1-2 m 2-4 m
Tapered angle 35-45 degree 35-45 degree 20-30 degree 45-60 degree
Standard grade
30, 44 mPa s 40 mPa s 40 mPa s
Target coaterSpin
SlitSpinSpin Spin Spin
Photosensitivity Excellent Good Excellent Good
Good
SL-1900 SL-3000 SL-1100-4
Wide developing process margin Low tapered angle
High Tapered Angle
Viscosity
Process margin(developing)
40-50 mPa s
Excellent Good Good
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OLED PLED
DL-1000 SL-1900 SL-3000 SL-1100-4
Features Standard grade Wide developmarginLow Tapaered
AngleHigh Tapered
Angle
Thickness 12 m 1-2 m 1-2 m 2-4 m
Viscosity 30, 44 mPa s 40 mPa s 40 mPa s 50, 160 mPa s
Coater Spin, Slit&Spin Spin Spin Spin, Slit&Spin
Prebaking Hotplate 1202min 1203min
Exposure Broad Band (at I-line) 70mJ/cm2 60mJ/cm2 50mJ/cm2 150mJ/cm2
Reagent TMAH 2.38% TMAH 2.38%
Time 30s 60s 60s 45s
Oven 23030min (in air)23030min
(in air)
Hotplate 16015min23015min 16015min23015min
Residual thickness ratioat unexposured part
77% 90% 88% 94%
Properties Tapered Angle 35-45 35-45 20-30 45-60
Curing
DevelopmentCondition
Application
Details of DL-1000 Family
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10um L&S (x20k)
Cross Sectional Views
For OLED For PLED
10um L&S (x3k)
10um L&S (x20k) 10um L&S (x20k)
Thickness: 1umRound shapeLow tapered angle
(20-40)
Thickness: 2umHigh tapered angle
(45-60)
25 35 50
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Dielectric Breakdown Strength (Thermal Stability)Holding at 85
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100
150
200
250
300
350
400
0 5 10 15 20
Days (at 85)
Die
lectr
ic S
trengt
h (kV
/m
m)
DL-1000
Acryl
Novolak
Cure: 230 for 30min (in air)Holding: 85 (in air)Measurement: JIS C 2110
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Dielectric Breakdown Strength (Light Stability)
Cure: 230 for 30 min (in air) Irradiation: Xe Longlife Fademeter (Suga)
irradiance(300-400nm) 37W/m2, illuminance(400-700nm) 7,300lxMeasurement: JIS C 2110
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50
100
150
200
250
300
350
400
0 5 10 15 20
Irradiation Time (day)
Die
lectr
ic S
trengt
h (
kV/m
m)
DL-1000
Acryl
Novolak
Under irradiation
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Thermal Stability (Outgas): TGA Analysis
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60
70
80
90
100
110
0 100 200 300 400 500
Temperature ()
Norm
aliz
ed w
eig
ht
(%)
DL-1000
Acryl
Novolak
Cure: 230 for 30min (in air)Measurement: TGA analysis (r.t.->400, in N2)
Heating from r.t. to 400 after 230 cure
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Holding at 120 after 230 cure
Cure: 230 for 30min (in air)Annealing: at curing temp(230) for 10min in the TG-MS apparatusMeasurement: at 120 for 4 hr
Outgas Components of DL-1000: TG-MS
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2
4
6
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10
0 50 100 150 200 250 300
Time (min)
Am
ount
of ga
s evolu
tion (w
tppm
)
m/z 18
m/z 42
m/z 44
m/z 54
m/z 94
m/z 99
total gas
at 120
No OutgasNo Outgas
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0
500
1000
1500
2000
2500
3000
0 50 100 150 200
Temperature (C)
Vola
tile
H2O
wei
ght
(ppm
)
DL-1000 Acryl Novolak
Water Absorption in the Atmosphere
Curing condition: 230C for 30min (in air)Storage: 24 hr in the atmosphere (25C, 60%RH)Measurement: monitoring the weight loss by TGA analysis
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Film Properties of DL-1000
Cure: 230 for 30min (in air)
Tensile Strength 120 MPa
Elongation 10 %
Youngs Modulus 3 GPa
Coefficient of Thermal Expansion 36 ppm/K
Glass Transition Temperature (Tg) 200oC
Dielectric Constant (25) 3.1 /kHz
Volume Resistivity 4.0x1016 . cmElectrical Properties
Thermal Properties 5% Weight Loss Temperature 350oC
Surface Resistivity 1.0x1015
Dielectric Breakdown Strength 350 kV/mm
Mechanical Properties
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Chemical Resistance
Dipping Time (at r.t.)Organic Solvent
IPA 1.35 1.35 1.35PGME 1.35 1.35 1.35
EL (Ethyl lactate) 1.35 1.35 1.35GBL (-Butyrolactone) 1.35 1.35 1.35
Organic solvent
NMP (N-methyl-2-pyrrolidone) 1.35 1.35 1.35
PGMEA 1.35 1.35 1.35Toluene, Xylene 1.35 1.35 1.35
HCl (4wt%; pH=1.0) 1.35 1.35 1.35Inorganic acid
H2SO4(1wt%; pH=1.0) 1.35 1.35 1.35Organic acid CH3COOH (67wt%; pH=0.9) 1.35 1.35 1.35
0 min 5 min 10 min
Cured Film Thickness (m)*
*Cure condition: 230C for 30min in air
The thickness shows no change against the various chemicals.
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Adhesion to various substrates
DL-1000 Acryl Novolak-PR
ITO >500hr 50hr 100hr
Glass(corning 1737)
>500hr 100hr 50hr
SiO2 >500hr 200hr 50hr
* Until the above adhesive time, the crosscut film is retained on the substrates without peeling. **The longer the adhesive retention time is, the higher the adhesion to the substrates is.
Cure condition: 230 for 30min (in air)PCT (Pressure Cooker Test) condition: 121, 2.0x105Pa (2.0atm), 100%RHMeasurement : Crosscut the cured film in 1mmx1mmx100pieces on the substrates
Scotch tape peel test (JIS K 5600)
Tape-pull adhesion test with PCT treatment
Cured film sample
Scotch tape
Substrate
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UV-O3 Treatment Resistance
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0 20 40 60
UV-O3 Time (min)
Thic
kness
Reduction (um
)
DL-1000
Acryl
Novolak
Cure condition: 230 for 30min (in air)UV-O3 treatment: O3 concentration 100+-50ppm
Gap to lamp 25mmIlluminance 15mW/cm2 (at 254nm)
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O2-plasma Treatment Resistance
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1.0
1.2
1.4
1.6
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O2-Plasma Time (min)
Thic
kness
Red
uct
ion (um
)
DL-1000
Acryl
Novolak
Cure condition: 230 for 30min (in air)O2-plasma Treatment: Power 300W
Degree of vacuum 0.4TorrSWR
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Patterning Process Condition for DL-1000
An example for patterning process
Thickness Measurement Apparatus: DNS LambdaSTM-602
1. Solution viscosity 44 mPas (25)
2. Substrate ITO; 100mmx100mmx0.7mm
3. Spin coating 500rpm/10sec + 1200rpm/30sec
4. Edge back rinse OK73thinner (PGME/PGMEA)
5. Prebaking 120/120sec (Hot plate) [Thickness 1.52 um]
*Measure surface temp. at the top of a glass substrate
6. Exposure 70mJ/cm2 (Broad band, ghi mixed line)
or 200mJ/cm2 (I-line stepper)
7. Development (Dipping) 30sec (2.38TMAH) and 30sec (H2O Rinse)
[Thickness 1.34 um]
8. Curing 1) Oven: 230/30min (in air)
2) Hot Plate: 160/15min + 230/15min [Thickness 1.03 um]
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650mm
550mm
Coating Thickness Uniformity of DL-1000 (30mPas)
Viscosity: 30cPSPIN: 1300rpm for 8sec, slit&spin (19.2g)Vacuum dry: Slow vacuum for 5sec Main vacuum 40MPa (0.3Torr) for 63secEdge Rinse: OK73thinner (PGMEA/PGME)
MAX value 1.6838 umMIN value 1.6205 umMEAN value 1.6442 umRange 0.0633 um (1.92%)
MAX value 1.6838 umMIN value 1.6205 umMEAN value 1.6442 umRange 0.0633 um (1.92%)
Using a DNSs Coating System
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Solution Viscosity in the Shelf Life
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10
20
30
40
50
0 10 20 30
Storage days (at 23)
Vis
cosi
ty (m
Pa s
)
No Change
Holding at 23
No Change
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1
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3
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0 20 40 60 80Storage days (at 23)
Def
ect D
ensi
ty (p
artic
les/
cm2)
Measurement apparatus: Hitachi LD-5000 (particle size > 0.27um)
Holding at 23
No particle
Particles in the Shelf Life
No particle
Spacer Structures in OLEDDL-1000 vs. Other MaterialsMaterial solution for Pixel ShrinkageFeatures of DL-1000Family of PhotoneeceTM DL-1000Details of DL-1000 FamilyCross Sectional ViewsDielectric Breakdown Strength (Thermal Stability)Dielectric Breakdown Strength (Light Stability)Thermal Stability (Outgas): TGA AnalysisOutgas Components of DL-1000: TG-MSWater Absorption in the AtmosphereFilm Properties of DL-1000Chemical ResistanceAdhesion to various substratesUV-O3 Treatment ResistanceO2-plasma Treatment ResistancePatterning Process Condition for DL-1000Coating Thickness Uniformity of DL-1000 (30mPas)Solution Viscosity in the Shelf LifeParticles in the Shelf Life