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NREL’s	
  e-­‐Ca	
  Test	
  


                                                                                     Energy	
  Innova5on	
  Portal	
  Webinar	
  

                                                                                     Arrelaine	
  A.	
  Dameron	
  

                                                                                     March	
  27,	
  2012	
  

NREL	
  is	
  a	
  na*onal	
  laboratory	
  of	
  the	
  U.S.	
  Department	
  of	
  Energy,	
  Office	
  of	
  Energy	
  Efficiency	
  and	
  Renewable	
  Energy,	
  operated	
  by	
  the	
  Alliance	
  for	
  Sustainable	
  Energy,	
  LLC.	
  
Characteriza5on	
  of	
  Water	
  Permea5on	
  Barriers	
  
                                               Vapor	
  adsorbs	
  and	
  
                                               dissolves	
  into	
  
                  Ambient	
  Environment	
     barrier	
  	
  

                           Barrier	
           Vapor	
  diffuses	
  

                  Sensi*ve	
  Components	
     Vapor	
  desorbs/
                                               outgasses	
  

•  Barrier	
  manufacturers	
  
   need	
  a	
  characteriza5on	
  
   method	
  that	
  is:	
  
   –  Reproducible	
  
   –  Highly	
  sensi*ve	
  
   –  Easy	
  to	
  use	
  
   –  Scalable	
  
                                                                      2	
  
Application Specific Tolerable Water Permeation
                                   Volume	
  in	
  1	
  m2	
   WVTR	
  	
  
                                                                  	
  
                                      	
  a]er	
  20	
  yrs	
   (g/m2/day)	
  
                                              ~7	
  L	
  	
       1 	
      	
  Food	
  Packaging	
  	
  	
  
                                                                       	
   	
  	
  
Gravimetric	
  Test	
  Limit	
                                  0.1	
         	
  LCDs	
  
ASTM	
  E96	
                                                   	
  
(1	
  ×	
  10-­‐1)	
                                            0.01          	
  	
  
                                                                       	
     	
  TFTs	
  
                                                                10-­‐3         	
  	
  
Isosta5c	
  Test	
  Limit	
  
                                                                       	
     	
  CdTe	
  /Thin	
  Film	
  
ASTM	
  F1249	
  
                                             ~7	
  mL	
  	
     10-­‐4         	
  	
  
(5	
  ×	
  10-­‐4)	
  
                                                                       	
     	
  CIGS	
       	
  	
  
                                                                10-­‐5         	
  	
  	
  

                                                                       	
     	
                	
             	
  	
  
                                             ~7	
  uL	
  	
     10-­‐6         	
  OPV	
  &	
  OLEDs	
  	
  
Ca	
  Test	
  Limit	
  
                                                                	
  
(5	
  × 10-­‐7)	
  
                                                                10-­‐7	
  
                                                                                                                          3	
  
NREL’s	
  e-­‐Ca	
  Test	
  


                                                                                  Ca	
  +2H2O(g)	
  →	
  Ca(OH)2	
  +H2	
  




Ca	
  transforms	
  from	
  opaque,	
  conduc*ve	
  metal	
  to	
  transparent,	
  resis*ve	
  oxide	
  upon	
  exposure	
  
                                                    to	
  water	
  

                                                                                                                Barrier	
  Film	
  
                                                                                                                	
  
                                                                                                                Edge	
  Seal	
  
                                                                                                                	
  
                                                                                                                Spacer	
  
                                                                                                                	
  
                                                                                                                Test	
  Card	
  
                                                                                                                	
  
                                                                                                                Edgecard	
  
                                                                                                                	
  Connector	
  
                                                                                                                   4	
  
Ca	
  Test	
  Components	
  
•  Computer	
  for	
  Data	
  collec5on	
  
      o    Custom	
  so[ware	
  
            –  Data	
  collec*on	
  real-­‐*me	
  WVTR	
  display	
  and	
  calcula*ons	
  
•  Commercial	
  digital	
  mul5meter	
  
      o    6.5	
  digit	
  accuracy	
  
•  Mul5plexing	
  Distribu5on	
  Hardware	
  
      o    Combina*on	
  of	
  commercially	
  available	
  and	
  custom	
  assembled	
  instrumenta*on	
  
      o    Current	
  configura*on	
  can	
  measure	
  up	
  to	
  128	
  samples	
  
•  Ca	
  Test	
  Assembly	
  
      o    Cables	
  between	
  electronics	
  and	
  Ca	
  assembly	
  
      o    Commercial	
  edgecard	
  connector	
  for	
  easy/fast	
  
           connect/disconnect	
  
      o    Custom	
  Test	
  Card	
  with	
  Ca	
  and	
  Au	
  traces	
  
             –  Evaporated	
  contacts	
  using	
  shadow	
  mask	
  
                onto	
  glass	
  substrate	
  
      o    Commercial	
  edgeseal	
  (extensive	
  tes*ng	
  done)	
  
      o    Custom	
  diffusion	
  spacer	
  element	
  
             –  Machined	
  aluminum	
  block	
  
      o    Barrier	
  Film	
  
                                                                                                               5	
  
Test	
  Card	
  
•  Ca	
  Traces	
  are	
  fabricated	
  separate	
  from	
  the	
  barrier	
  film	
  
•  3	
  redundant	
  4-­‐pt	
  measurements	
  of	
  Ca	
  resistance	
  as	
  a	
  func5on	
  of	
  5me	
  
•  Witness	
  line	
  monitors	
  edgeseal	
  integrity	
  and	
  provides	
  internal	
  standard	
  
   of	
  sensi5vity	
  limits	
  
•  Inert	
  contacts	
  pass	
  signal	
  to	
  the	
  outside	
  of	
  the	
  assembly	
  and	
  fit	
  into	
  
   standard	
  edgecard	
  connector	
  
•  Test	
  cards	
  can	
  be	
  produced	
  in	
  bulk	
  (and	
  stored	
  in	
  inert	
  environment)	
  
   prior	
  to	
  obtaining	
  barriers	
  to	
  be	
  tested	
  




                                                                                                              6	
  
Why	
  Incorporate	
  a	
  Diffusion	
  Spacer?	
  
•  Worst	
  Case	
  Scenario:	
  Ca	
  traces	
  are	
  deposited	
  onto	
  the	
  barrier	
  but	
  the	
  
   barrier	
  has	
  a	
  pinhole	
  defect:	
  
         t0	
                          t1	
                           t2	
  




                    t3	
                            t4	
                           t5	
  




•  Resultant	
  measurement	
  is	
  not	
  reflec5ve	
  of	
  the	
  average	
  WVTR!	
  
•  For	
  Accurate	
  Test:	
  diffusion	
  distance	
  approx.	
  equal	
  to	
  area	
  of	
  the	
  Ca	
  
                                                                                                                7	
  
Spacer	
  Advantages	
  


                                                                                                                 Glass/barrier	
  




                                        (a) Flat               (b) Trench              (c) “O” Ring              sealing	
  surface	
  
                                                                                                                 (d) Al Ridge


•  The	
  ra5o	
  of	
  apertures	
  controls	
  the	
  sensi5vity	
  range	
  by	
  adjus5ng	
  the	
  
   barrier	
  area	
  rela5ve	
  to	
  the	
  Ca	
  area	
  	
  
     o    Some	
  ra*os	
  that	
  we	
  can	
  use	
  presently	
  are	
  9x,	
  30x,	
  60x,	
  700x	
  	
  
•  The	
  sealing	
  surface	
  design	
  allows	
  for	
  reproducible	
  areas,	
  and	
  also	
  limits	
  
   the	
  influence	
  of	
  the	
  edgeseal	
  materials	
  on	
  the	
  measurement	
  
•  The	
  spacer	
  also	
  allows	
  the	
  Ca	
  Test	
  to	
  be	
  assembled	
  quickly	
  with	
  a	
  
   mechanical	
  press	
  


                                                                                                                            8	
  
Measured	
  Sensi5vity	
  of	
  e-­‐Ca	
  Test	
  
 Actual	
  measured	
  data	
  from	
  a	
  barrier	
  film	
  provided	
  by	
  a	
  commercial	
  partner	
  shows	
  
                       steady	
  state	
  permea*on	
  at	
  ~3	
  ×	
  10-­‐5	
  g/m2/day.	
  	
  


                                                                                                                                  Commercial	
  
                                                                                                                                   Test	
  Limit	
  




This	
  data	
  is	
  well	
  above	
  the	
  sensi*vity	
  limits	
  of	
  NREL’s	
  e-­‐Ca	
  test	
  and	
  well	
  below	
  what	
  
                         can	
  be	
  measured	
  using	
  a	
  commercially	
  available	
  test.	
  
                                                                                                                                           9	
  
Possible	
  Market	
  Integra5on	
  of	
  e-­‐Ca	
  Test	
  

•  Integra5on	
  of	
  capabili5es	
  at	
  a	
  test	
  lab	
  
    o    Provide	
  tes*ng	
  services	
  
    o    NREL	
  receives	
  requests	
  for	
  tes*ng	
  constantly	
  
          –  Several	
  ongoing	
  commercial	
  partners	
  
•  Instrumenta5on/Laboratory	
  Equipment	
  
    o    Source	
  the	
  instrumenta*on	
  and	
  required	
  deposi*on	
  
         designs	
  
          –  Lab	
  scale	
  
          –  Commercial	
  quality	
  control	
  scale	
  
    o    Source	
  the	
  consumables	
  
          –  Test	
  cards	
  
          –  spacers	
  


                                                                               10	
  

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Nrel’s e ca test

  • 1. NREL’s  e-­‐Ca  Test   Energy  Innova5on  Portal  Webinar   Arrelaine  A.  Dameron   March  27,  2012   NREL  is  a  na*onal  laboratory  of  the  U.S.  Department  of  Energy,  Office  of  Energy  Efficiency  and  Renewable  Energy,  operated  by  the  Alliance  for  Sustainable  Energy,  LLC.  
  • 2. Characteriza5on  of  Water  Permea5on  Barriers   Vapor  adsorbs  and   dissolves  into   Ambient  Environment   barrier     Barrier   Vapor  diffuses   Sensi*ve  Components   Vapor  desorbs/ outgasses   •  Barrier  manufacturers   need  a  characteriza5on   method  that  is:   –  Reproducible   –  Highly  sensi*ve   –  Easy  to  use   –  Scalable   2  
  • 3. Application Specific Tolerable Water Permeation Volume  in  1  m2   WVTR        a]er  20  yrs   (g/m2/day)   ~7  L     1    Food  Packaging             Gravimetric  Test  Limit   0.1    LCDs   ASTM  E96     (1  ×  10-­‐1)   0.01        TFTs   10-­‐3     Isosta5c  Test  Limit      CdTe  /Thin  Film   ASTM  F1249   ~7  mL     10-­‐4     (5  ×  10-­‐4)      CIGS       10-­‐5                 ~7  uL     10-­‐6  OPV  &  OLEDs     Ca  Test  Limit     (5  × 10-­‐7)   10-­‐7   3  
  • 4. NREL’s  e-­‐Ca  Test   Ca  +2H2O(g)  →  Ca(OH)2  +H2   Ca  transforms  from  opaque,  conduc*ve  metal  to  transparent,  resis*ve  oxide  upon  exposure   to  water   Barrier  Film     Edge  Seal     Spacer     Test  Card     Edgecard    Connector   4  
  • 5. Ca  Test  Components   •  Computer  for  Data  collec5on   o  Custom  so[ware   –  Data  collec*on  real-­‐*me  WVTR  display  and  calcula*ons   •  Commercial  digital  mul5meter   o  6.5  digit  accuracy   •  Mul5plexing  Distribu5on  Hardware   o  Combina*on  of  commercially  available  and  custom  assembled  instrumenta*on   o  Current  configura*on  can  measure  up  to  128  samples   •  Ca  Test  Assembly   o  Cables  between  electronics  and  Ca  assembly   o  Commercial  edgecard  connector  for  easy/fast   connect/disconnect   o  Custom  Test  Card  with  Ca  and  Au  traces   –  Evaporated  contacts  using  shadow  mask   onto  glass  substrate   o  Commercial  edgeseal  (extensive  tes*ng  done)   o  Custom  diffusion  spacer  element   –  Machined  aluminum  block   o  Barrier  Film   5  
  • 6. Test  Card   •  Ca  Traces  are  fabricated  separate  from  the  barrier  film   •  3  redundant  4-­‐pt  measurements  of  Ca  resistance  as  a  func5on  of  5me   •  Witness  line  monitors  edgeseal  integrity  and  provides  internal  standard   of  sensi5vity  limits   •  Inert  contacts  pass  signal  to  the  outside  of  the  assembly  and  fit  into   standard  edgecard  connector   •  Test  cards  can  be  produced  in  bulk  (and  stored  in  inert  environment)   prior  to  obtaining  barriers  to  be  tested   6  
  • 7. Why  Incorporate  a  Diffusion  Spacer?   •  Worst  Case  Scenario:  Ca  traces  are  deposited  onto  the  barrier  but  the   barrier  has  a  pinhole  defect:   t0   t1   t2   t3   t4   t5   •  Resultant  measurement  is  not  reflec5ve  of  the  average  WVTR!   •  For  Accurate  Test:  diffusion  distance  approx.  equal  to  area  of  the  Ca   7  
  • 8. Spacer  Advantages   Glass/barrier   (a) Flat (b) Trench (c) “O” Ring sealing  surface   (d) Al Ridge •  The  ra5o  of  apertures  controls  the  sensi5vity  range  by  adjus5ng  the   barrier  area  rela5ve  to  the  Ca  area     o  Some  ra*os  that  we  can  use  presently  are  9x,  30x,  60x,  700x     •  The  sealing  surface  design  allows  for  reproducible  areas,  and  also  limits   the  influence  of  the  edgeseal  materials  on  the  measurement   •  The  spacer  also  allows  the  Ca  Test  to  be  assembled  quickly  with  a   mechanical  press   8  
  • 9. Measured  Sensi5vity  of  e-­‐Ca  Test   Actual  measured  data  from  a  barrier  film  provided  by  a  commercial  partner  shows   steady  state  permea*on  at  ~3  ×  10-­‐5  g/m2/day.     Commercial   Test  Limit   This  data  is  well  above  the  sensi*vity  limits  of  NREL’s  e-­‐Ca  test  and  well  below  what   can  be  measured  using  a  commercially  available  test.   9  
  • 10. Possible  Market  Integra5on  of  e-­‐Ca  Test   •  Integra5on  of  capabili5es  at  a  test  lab   o  Provide  tes*ng  services   o  NREL  receives  requests  for  tes*ng  constantly   –  Several  ongoing  commercial  partners   •  Instrumenta5on/Laboratory  Equipment   o  Source  the  instrumenta*on  and  required  deposi*on   designs   –  Lab  scale   –  Commercial  quality  control  scale   o  Source  the  consumables   –  Test  cards   –  spacers   10