Portfolio. Chemical supply. systems. Bulk and. special gas distribution. Engineering, design and development. Service and operation
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1 Thin Film Solutions
2 Portfolio Chemical supply Bulk and systems special gas distribution Engineering, design and development Service and operation Process vacuum and exhaust systems
3 Global Structure EUROPE HQ, R&D, Manufacturing Service Hub Dresden GER Erfurt GER AMERICAS ASIA PACIFIC Sales and Project Execution Service Hub and Sales Greater China, South East Asia Trading Partners Taiwan Japan, Korea
4 Thin-Film Solutions HiBarSens Special equipment for thin film deposition (excerpt ) DEZn supply for ZnO TCO layers TMAl supply for AlOx backside passivation PECVD for barrier layers HMDSO Enabling III/V on Si Special liquid Indium-MO source supply systems for IGZO LED supply systems for MO-III (TMGa)
5 Water Vapor Permeation Measurement System
6 Summary: Starting point Food industry Pharmaceutical industry Anorganic solar cells Organic solar cells Vacuum isolation paneele Organic LED Water transmission rate WVTR g[h 2 O] m -2 d ,1 0,01 1E-3 1E-4 1E-5 1E currently measurable by standard methods?
7 WVTR of 10 x g m -2 d -1 is equivalent to:??? One water drop at a sample area of: Vatican City Soccer field Industry standard (MOCON) Ping-pong table Beer coaster Confetti WVTR Chessboard Crown cork Dresden Zwinger + park Tennis court per day!
8 Market forecast for ultra barrier films Billion US$ Photovoltaics Electrophoretic* OLED light* OLED Billboard etc* OLED display* Year Harry Zervos: "Barrier Films for Flexible Electronics: Needs, Players &Opportunities". IDTechEx Ltd., December 2008)
9 HiBarSens HiBarSens Basics BASICS
10 Measuring modes: dynamic vs. static Measuring setup: dynamic (isostatic) static (quasi isostatic) Typical chart Calculation of WVTR Water vapor mass flux j / g m -2 d Sample 2 Sample 1 Time t / h WVTR Water vapor volume fraction j / ppm Time t / h WVTR WVTR V& Purge M = R T A H O sample 2 p j 1-j WVTR - n& sorp = Vcell R T M A H O 2 sample p Dj Dt j Water vapor volume fraction (measured by LDS)
11 The LASER as a sensor Tunable diode laser absorption spectroscopy (TDLAS) Limit of Detection LOD(H 2 O): 100 ppb m Measuring setup: dynamic static Sample size Chamber volume Accumulation time Purge flow Optical path length 100 cm 2 0,1 l - 10 h 0,01 slm - 1 m WVTR < 10-4 g m -2 d -1 are measurable ~ 10-5 g m -2 d -1 ~ 10-6 g m -2 d -1!Theoretical estimations!
12 Balance equation for dynamic n sorption@sample n permeation General balance equation ( n& in + n& perm + n& sorpt + n& leak - nout ) Dt no n = & + n sorption@cell V purge; n in n n out n& sorption p - n - n Steady-state conditions p 0 0 = n& = 0 = desorption - n& = 0 ( n& - n& ) Dt = const. perm out adsorption n = amount of substance (moisture) N adsorp sample cell V& Purge M WVTR = R T A H O Sample 2 p j 1-j Adsorption isotherm p H2O Mass flux j H2O / g m -2 d Sample 2 Sample 1 Calculation of WVTR ( n& perm - nout ) Dt no n = & + Time t / h
13 Balance equation for static setup n sorption@sample n permeation General balance equation n = & + ( n& in + n& perm + n& sorpt + n& leak - nout ) Dt no n sorption@cell N adsorp n in Adsorption isotherm n = amount of substance (moisture) sample cell p H2O Water vapor volume fraction j / ppm n n out Time t / h n& sorption = n& n& in = n& adsorption non constant conditions out - n& = 0; n& desorption perm = const > 0; p - p Calculation of WVTR n = & + 0 > ( n& perm + n sorpt ) D t n o WVTR = n& perm V cell WVTR = R T WVTR - n& sorp M A Sample M A H 2 H O 2 O Sample Vcell = R T Dn = Dt M A p Dj Dt M A H 2 O Sample H 2 Sample 0 O p Dj Dt
14 Static measurement: Background level Water vapor volume fraction j / ppm GRA, Quasi-isostatisch_neu_GM_12_06_07, purge quasi isostatic measurement Time t / hh Measured background level (sample: stainless 38 C / 90% r.h. WVTR qis = 2,5 x 10-6 g m -2 d -1
15 Dynamic vs. Static: background level Dynamic setup Static setup Water vapor mass velocity / g m -2 d -1-2 SCHA, H2O_Konzmessung_Leermessung_isostatisch, Water vapor volume fraction j / ppm GRA, Quasi-isostatisch_neu_GM_12_06_07, Time t / DDD Time t / hh WVTR qis = 5x 10-5 g m -2 d -1 WVTR qis = 2,5x 10-6 g m -2 d -1 Measured background level (sample: stainless 38 C / 90% r. H.
16 HiBarSens PPRODUCT IMPLEMENTATION
17 Sensitivity of a WVTR measurement N 2 + H 2 O Sensor sensitivity Adsorption / desorption of moisture H 2 O N 2 Sealing of the test cell
18 Parameters for tuning the sensitivity c N 2 + H 2 O Optical path length Carrier gas flow à c Sample area à c Selection of absorption line H 2 O N 2 I ( l ) - ln = e l I ( l ) o c d Theoretical sensitivity LOD = 150 ppb m dynamic setup
19 Tuning sensitivity: optical path length Multipath design in HiBarSens 2 m optical path length by multi 20 reflections
20 Tuning sensitivity: Carrier gas flow WVTR / g[h 2 O] m -2 d Purge flow V* / sccm 10-4 WVTR Purge gas flow Time t / hours 10 0 Carrier gas flow 3 sccm - 50 sccm Boost the sensitivity by factor 16!
21 Sensitivity of WVTR measurement Sensor sensitivity: the laser as a sensor Further advantages High dynamic range: ppb - % ( g m -2 d -1 ) Very high selectivity Immune to high concentrated moisture Long time stable, no drift, no hysteresis Low-maintenance Change of target permeate by change of the laser diode Allows the realization of a compact design Easy to use Tunable Diode Absorption Spectroscopy (TDLAS) is a non-invasive, high sensitive, high selective sensor for detection of moisture traces!
22 Adsorption / desorption of moisture Sensitivity of WVTR measurement N 2 + H 2 O j Mass flux Dm [ g] j system x = WVTR + é g ù ê = 2 m d ú ë û A x j cell H 2 + O j [ m²] Dt sample [ d] + j tubes H 2 O N 2 Mass flux j H2O / g m -2 d Sample 2 j cell = j sample = j tubes = 0 j system = WVTR (dj/dt = 0) 10-4 Sample 1 Time t / h
23 Sensitivity of WVTR measurement Adsorption / desorption of moisture H 2 O N 2 + H 2 O N 2 Steady state conditions are required As small as possible surface area of the cell in contact with moisture Ultra smooth surfaces Avoid any problematic materials inside the cell Highest temperature stability HiBarSens - realization Volume and surface vs. sample area optimized cell design Electro-polished surfaces Temperature stability < 0,5 C Sensor is placed inside the test cell
24 Sensitivity of WVTR measurement Sealing of test (measuring) cell Mass flux: j = WVTR + j system cell j leakage Sample clamping has to follow the requirement for leakage rates of 2.4E-9 mbar*l/s Substitution of the classical concept (polymer O-rings) by the concept of an active sealing Purge channels prevent ambient moisture diffusion into the cell
25 HiBarSens at work 10-2 Mass flux (H 2 O) / g m -2 d x 10-5 g m -2 d -1 Measured background level (sample: stainless steel) Time t / d 10-1 WVTR / g m -2 d -1 WVTR-measurement of ultra barrier sample (Fraunhofer POLO) ,2 Adjusting the gas flow 4,1 x 10-4 g m -2 d -1 00:00 24:00 48:00 72:00 96:00 120:00 144:00 168:00 Time t / h ln(wvtr / g m -2 d -1 ) (@ 85 % RH) Temperature dependence of ultra barrier sample (for photovoltaic) -7,6-8,0-8,4 3,12 3,14 3,16 3,18 3,20 3,22 3,24 3,26 3,28 3, /Temperature / K -1
26 compact & easy to use device Permeation cell - tempered - integrated moisture generator - Gentle clamping of the test sample Purifier valve Sample N 2 purge gas in /out Rel. Humidity controller Connectors for thermostat Flow controller Measurement Place sample Close test cell Adjust rel. Humidity purge flow, temperature Print report
27 Summary HiBarSens HiBarSens HiBarSens laser based sensor technology for highly sensitive determination of water vapor transmission rates of ultra barrier samples provides reliable measurements of WVTR down to 10-5 g m -2 d -1 with the potential to 10-6 g m -2 d -1 is available as a compact, easy to use table top device
28 Acknowlegment Johannes Grübler Kurt Pietsch responsible for manufacturing and sales Harald Beese Wulf Grählert
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