Clevios Etch – Technical Guide for Clevios SET S3
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<strong>Clevios</strong> <strong>Etch</strong> <strong>–</strong> <strong>Technical</strong> <strong>Guide</strong> <strong>for</strong> <strong>Clevios</strong> <strong>SET</strong> <strong>S3</strong><br />
Heraeus Deutschland GmbH & Co. KG<br />
Guntermann | HNB-DS | Jan 2015<br />
Seite 1
Patterning by <strong>Clevios</strong> <strong>SET</strong> <strong>S3</strong><br />
<strong>Clevios</strong><br />
Coated Film<br />
Print<br />
<strong>Clevios</strong> <strong>SET</strong> <strong>S3</strong><br />
<strong>Clevios</strong><br />
<strong>Etch</strong><br />
<strong>Clevios</strong> <strong>SET</strong> <strong>S3</strong><br />
Removal<br />
Printed by Screen**<br />
printing<br />
Use a wet layer thickness<br />
of 6-10µm<br />
Dry <strong>for</strong> 1-2 min @ 80°C<br />
<strong>Etch</strong> 60-120 seconds in<br />
10% <strong>Clevios</strong> <strong>Etch</strong><br />
solution*) @ 27°C<br />
Rinse with DI-water<br />
1. Remove with selected solvents(1)<br />
Rinse <strong>for</strong> approx 60 sec @ 20°C -25°C<br />
or<br />
2. Remove with 1.25% ammonia solution(2)<br />
Rinse <strong>for</strong> 2 min @ 25°C or 30-60 sec @40°C<br />
Wash with rinsing DI-water and dry <strong>for</strong> 2min@100 °C<br />
* <strong>Etch</strong>ing time based on <strong>Clevios</strong> F ET coating. <strong>Etch</strong>ing time <strong>for</strong> other <strong>for</strong>mulations can be different .<br />
** 355 mesh/inch; 31 µm Polyester yellow<br />
(1) MEK-Ethanol 25:75 <strong>–</strong> 20:80 or Acetone<br />
(2) For improved stripping results we recommend to add a small amount of e.g Triton X-100 ( 1% by weight on Ammonia sol.)<br />
Guntermann | HNB-DS | Jan 2015<br />
Page 2
CLEVIOS ETCH<br />
CLEVIOS <strong>SET</strong> <strong>S3</strong> <strong>–</strong> GNU 1676<br />
Solid Content :ca 25 %<br />
Viscosity : ca 2-3 Pa.s<br />
Dilution : MMB (3-Methoxy-3-methyl-1-butanol) B.P 174°C<br />
Printing conditions : 355 mesh/inch<br />
For Finelines > 400 mesh/inch<br />
Drying : 1-2 minutes @ 80°C<br />
Screen Cleaning : with Acetone<br />
Guntermann | HNB-DS | Jan 2015<br />
Page 3
η in Pas<br />
ROTO VISCO RV1 <strong>–</strong> CONE / PLATE<br />
Viscosity<br />
<strong>Clevios</strong> <strong>SET</strong> <strong>S3</strong><br />
3,00<br />
2,50<br />
2,00<br />
1,50<br />
GNU 1676<br />
1,00<br />
0,50<br />
0,00<br />
0,00 200,00 400,00 600,00 800,00 1000,00 1200,00 1400,00 1600,00 1800,00 2000,00<br />
1/s<br />
Guntermann | HNB-DS | Jan 2015<br />
Seite 4
CLEVIOS <strong>SET</strong> S 3<br />
Troubleshooting Bubbles<br />
How to avoid/reduce bubbles<br />
Flash-off time be<strong>for</strong>e drying 2 minutes <strong>–</strong> don´t dry immediately after printing<br />
<strong>Clevios</strong> <strong>SET</strong> <strong>S3</strong> can be diluted with MMB (3-Methoxy-3-methyl-1-butanol)<br />
reducing the viscosity will decrease the bubble <strong>for</strong>mation<br />
Don´t Re-use <strong>Clevios</strong> <strong>SET</strong> <strong>S3</strong>.<br />
Using a trampolin screen (metal mesh) similar to fineline screen<br />
Guntermann | HNB-DS | Jan 2015<br />
Seite 5
PRINTING<br />
Typical Printing Parameter<br />
Mesh<br />
Heraeus<br />
Thread Diameter 31µm<br />
355 mesh/inch<br />
Or higher e.g VA400<br />
Material<br />
Polyester<br />
Squeegee durometer 70-75<br />
Squeegee angle 10° = 80°<br />
Flood bar angle 0°<br />
Trampoline VA400<br />
Print speed<br />
Snap off<br />
86 mm/sec<br />
5 mm<br />
Flash off time 60-120“<br />
Drying<br />
Screen Cleaning<br />
80°C/1-2min<br />
Acetone<br />
Guntermann | HNB-DS | Jan 2015<br />
Seite 6
PRINTING<br />
Lineprofiles (Trampoline VA400 )<br />
# Dektak 150<br />
# Z<strong>S3</strong> on PET, silk-screen print<br />
L/S 300 / 100 200 / 100 100 / 100 200 / 80 100 / 80<br />
Position Line Separation Line Separation Line Separation Line Separation Line Separation<br />
Width (µm) Width (µm) Width (µm) Width (µm) Width (µm)<br />
297 106 190 112 110 94 208 83 121 70<br />
282 111 198 100 111 96 200 69 112 64<br />
284 117 196 99 108 90 211 66 107 71<br />
Guntermann | HNB-DS | Jan 2015<br />
Page 7
Preparation of an etching solution<br />
Dissolve <strong>Clevios</strong> <strong>Etch</strong> at room temperature in water<br />
After stirring <strong>for</strong> 30 minutes, remove residues by filtration, filter type 5-10 µm<br />
polypropylene or Whatman filter paper Grade 595 or 602<br />
Use etching solution within 48 h<br />
NEVER STORE THE ETCHING SOLUTION IN A CLOSED BOTTLE !!<br />
If stored <strong>for</strong> more than 48 h, storage temperature should be lower than 23°C<br />
Used solution should be disposed within short time.<br />
See also additional In<strong>for</strong>mation<br />
Guntermann | HNB-DS | Jan 2015<br />
Page 8
<strong>Clevios</strong> <strong>Etch</strong>ing Process<br />
Contact angle<br />
• Best results are obtained if the contact angle (water) of the coating is in a range of<br />
40°-60°. Otherwise longer etching time maybe needed. Use test samples to determine<br />
etching time.<br />
Resolution<br />
• In case of using <strong>Clevios</strong> <strong>SET</strong> S the maximum resolution is approximately 50µm<br />
• Finer lines may also be possible, but may need longer etching time<br />
Crosslinking<br />
• Highly solvent resistant coatings may need longer etching time. Use test samples to find<br />
the right balance.<br />
Temperature of the <strong>Etch</strong>ing bath<br />
• For etching the temperature should be in range of 25-30°C.<br />
• After etching the solution should be cooled below 23°C.<br />
Guntermann | HNB-DS | Jan 2015<br />
Page 9
<strong>Etch</strong>ing process (detailed description)<br />
Products needed : <strong>Clevios</strong> F ET, <strong>Clevios</strong> <strong>SET</strong> <strong>S3</strong> and <strong>Clevios</strong> <strong>Etch</strong><br />
Film preparation<br />
• Coat <strong>Clevios</strong> F ET and dry at 120°C <strong>for</strong> 5 min.<br />
• Print the <strong>Clevios</strong> <strong>SET</strong> <strong>S3</strong> material with approx. 6-10µm wet film thickness<br />
• Flash off time be<strong>for</strong>e drying <strong>–</strong> 2 minutes<br />
• Dry at 80°C <strong>for</strong> 1-2 minutes<br />
<strong>Etch</strong>ing<br />
• Dip the film in a 10% solution of <strong>Clevios</strong> <strong>Etch</strong> (pH 5.7-7 @20°C) <strong>for</strong> 1-2 minutes @ 27°C with circulation<br />
• Wash the film under rinsing water and dry @ 100°C <strong>for</strong> 2 minutes<br />
Removal<br />
• Dip the film in a 1.25% ammonia solution (pH 9-11 @20°C) <strong>for</strong> 2 minutes at RT or <strong>for</strong> 30-60 sec @ 40°C<br />
• Additional washing in 1% sulfuric acid recovers the conductivity<br />
• Alternative solution: remove the <strong>Clevios</strong> <strong>SET</strong> <strong>S3</strong> with rinsing MEK-Ethanol or Acetone <strong>for</strong> 30-60 Seconds<br />
• Wash with water again and dry the film <strong>for</strong> 2 minutes @ 100°C<br />
Guntermann | HNB-DS | Jan 2015<br />
Page 10
<strong>Clevios</strong> <strong>Etch</strong><br />
<strong>Clevios</strong> <strong>Etch</strong> releases: OCl - D ClO 3<br />
-<br />
D HOCl D Cl 2<br />
First studies suggest:<br />
- HOCl / Cl 2 may be active species<br />
- a halogenated intermediate may be involved<br />
PEDOT oxidation <strong>–</strong> possible intermediates<br />
O<br />
S<br />
O<br />
O<br />
S<br />
O<br />
O<br />
O<br />
O O<br />
S<br />
O O<br />
S<br />
O<br />
H<br />
O<br />
O<br />
S<br />
O<br />
O<br />
S<br />
O<br />
H<br />
O<br />
S<br />
O<br />
O<br />
S<br />
O<br />
Cl<br />
O<br />
S<br />
O<br />
O<br />
Cl<br />
S<br />
O<br />
H<br />
O<br />
Cl<br />
S<br />
O<br />
O<br />
S<br />
O<br />
H<br />
n<br />
Other possible deactivation mechanisms / effects<br />
- disruption/rearrangement of conductivity pathways (e.g. via reaction with binder/PSS)<br />
- Macroscopic effects: outer layer of gel particles may be partially deactivated<br />
Guntermann | HNB-DS | Jan 2015<br />
Page 11
<strong>Etch</strong>ing Results of <strong>Clevios</strong> <strong>Etch</strong><br />
10% Solution<br />
Guntermann | HNB-DS | Jan 2015<br />
Page 12
Ohm/sq.<br />
CLEVIOS ETCH<br />
<strong>Etch</strong>ing time @ 20°C <strong>–</strong> of <strong>Clevios</strong> F ET (12µm wet)<br />
1,00E+09<br />
1,00E+08<br />
1,00E+07<br />
1,00E+06<br />
1,00E+05<br />
1,00E+04<br />
1,00E+03<br />
1,00E+02<br />
30 sec<br />
60 sec<br />
90 sec<br />
120 sec<br />
150 sec<br />
180 sec<br />
210 sec<br />
1,00E+01<br />
1,00E+00<br />
0 after 24h after 48h<br />
Storage time of 10% Solution<br />
Guntermann | HNB-DS | Jan 2015<br />
Page 13
Ohm/sq.<br />
CLEVIOS ETCH<br />
<strong>Etch</strong>ing time @ 22.5°C <strong>–</strong> of <strong>Clevios</strong> F ET (12µm wet)<br />
1,00E+09<br />
1,00E+08<br />
1,00E+07<br />
1,00E+06<br />
1,00E+05<br />
1,00E+04<br />
1,00E+03<br />
1,00E+02<br />
30 sec<br />
60 sec<br />
90 sec<br />
120 sec<br />
150 sec<br />
180 sec<br />
210 sec<br />
1,00E+01<br />
1,00E+00<br />
0 after 24h after 48h<br />
Storage time of 10% Solution<br />
Guntermann | HNB-DS | Jan 2015<br />
Page 14
Ohm/sq.<br />
CLEVIOS ETCH<br />
<strong>Etch</strong>ing time @ 26.5°C <strong>–</strong> of <strong>Clevios</strong> F ET (12µm wet)<br />
1,00E+09<br />
1,00E+08<br />
1,00E+07<br />
1,00E+06<br />
1,00E+05<br />
1,00E+04<br />
1,00E+03<br />
1,00E+02<br />
30 sec<br />
60 sec<br />
90 sec<br />
120 sec<br />
150 sec<br />
180 sec<br />
210 sec<br />
1,00E+01<br />
1,00E+00<br />
0 after 24h after 48h<br />
Storage time of 10% Solution<br />
Guntermann | HNB-DS | Jan 2015<br />
Page 15
Chlorine Formation<br />
Guntermann | HNB-DS | Jan 2015<br />
Page 16
dm³<br />
CLEVIOS ETCH<br />
Chlorine <strong>for</strong>mation during storage<br />
of 1000 ml <strong>Clevios</strong> <strong>Etch</strong> (concentration in water: 10%)<br />
1<br />
0,9<br />
0,8<br />
0,7<br />
0,6<br />
Storage temperature: < 23°C<br />
0,5<br />
0,4<br />
0,3<br />
0,2<br />
0,1<br />
0<br />
0 10 20 30 40 50 60 70 80<br />
hours<br />
Guntermann | HNB-DS | Jan 2015<br />
Page 17
dm³<br />
Chlorine <strong>for</strong>mation during storage<br />
of 1000 ml <strong>Clevios</strong> <strong>Etch</strong> (concentration in water: 10%)<br />
1,8<br />
1,6<br />
1,4<br />
1,2<br />
1<br />
Storage temperature: 27 °C<br />
0,8<br />
0,6<br />
0,4<br />
0,2<br />
0<br />
0 2 3 4 5 6 7 8 25 26 27 28 32 48 72 96 168<br />
hours<br />
Guntermann | HNB-DS | Jan 2015<br />
Page 18
Disposal<br />
Sodiumthiosulfate deactivates the active ingredients of <strong>Clevios</strong> <strong>Etch</strong> and is oxidized<br />
to sulfate.<br />
Disposal of <strong>Etch</strong>ing Solution<br />
4 NaClO + Na2S2O3 + 2 NaOH → 4 NaCl + 2 Na2SO4 + H2O<br />
For 100g of a 10% etching solution<br />
• Prepare a solution of 3.94g of Na2S2O3 (sodium thiosulfate) in 100g water<br />
• Add the thiosulfate solution to the etching solution slowly under stirring (temp.<br />
control) exothermic reaction !<br />
• The pH of the solution will change from 6.5 to 0.12.<br />
• Slowly add a 26% solution of sodium hydroxide (NaOH) until the pH exceeds a<br />
value of 11.<br />
• No further smell of chlorine should be observed.<br />
Dispose the obtained solution in accordance with local laws.<br />
Guntermann | HNB-DS | Jan 2015<br />
Page 19