PMID- 19957975
OWN - NLM
STAT- PubMed-not-MEDLINE
DCOM- 20100601
LR  - 20100310
IS  - 1520-5827 (Electronic)
IS  - 0743-7463 (Linking)
VI  - 26
IP  - 6
DP  - 2010 Mar 16
TI  - How to dip-coat and spin-coat nanoporous double-gyroid silica films with 
      EO19-PO43-EO19 surfactant (Pluronic P84) and know it using a powder X-ray 
      diffractometer.
PG  - 4357-67
LID - 10.1021/la903443p [doi]
AB  - Previously, the synthesis of highly oriented pure double-gyroid nanoporous silica 
      films has been demonstrated using evaporation-induced self-assembly (EISA) and 
      dip-coating with a specialty triblock surfactant (PEO-PPO-alkyl) as the template. 
      For these films, grazing-incidence small-angle X-ray scattering (GISAXS) was used 
      to determine orientation and structure. However, GISAXS is not widely available, 
      and we have observed significant batch-to-batch variability in the PEO-PPO-alkyl 
      surfactants used. Here, we show for the first time: (1) synthesis of highly 
      oriented pure double-gyroid nanoporous silica films using freely available 
      EO(19)-PO(43)-EO(19) surfactant (Pluronic-P84) as the nanostructure-directing 
      agent, (2) the use of spin-coating and dip-coating EISA to fabricate the 
      double-gyroid films, and (3) the use of theta-theta X-ray diffractometers 
      (commonly available and typically used for powder X-ray diffraction, PXRD) to 
      identify the double-gyroid phase. Processing diagrams for P84 using dip-coating 
      and spin-coating are shown in order to map the dependency of the nanostructure on 
      solution composition, relative humidity, and solution aging time. In addition, an 
      effect of the rate of evaporation during EISA is observed via dependence on the 
      angular velocity in spin-coating. Also, through quantitative comparison of the 
      GISAXS patterns with corresponding PXRD patterns, previously unexplained 
      diffraction peaks in the PXRD patterns are shown to result from diffraction from 
      crystallographic planes that are not parallel to the substrate (typically not 
      observed in PXRD) due to the small angles involved and the nonzero acceptance 
      angle of the PXRD Soller slits. These peaks provide a means to distinctly 
      identify the double-gyroid phase using PXRD. The same trends relating 
      aging-time-before-coating to the phase that forms via EISA are observed with 
      EO(19)-PO(43)-EO(19) as was the case in previous studies using 
      EO(17)-PO(14)-C(12). This shows the generality of use of aging time to synthesize 
      nanoporous silica films with nonionic surfactants. Finally, a list of "tips and 
      tricks" is provided to facilitate easy reproducible synthesis of double-gyroid 
      nanoporous silica thin films in other laboratories.
FAU - Tate, Michael P
AU  - Tate MP
FAU - Urade, Vikrant N
AU  - Urade VN
FAU - Gaik, Steven J
AU  - Gaik SJ
FAU - Muzzillo, Christopher P
AU  - Muzzillo CP
FAU - Hillhouse, Hugh W
AU  - Hillhouse HW
LA  - eng
PT  - Journal Article
PL  - United States
TA  - Langmuir
JT  - Langmuir : the ACS journal of surfaces and colloids
JID - 9882736
EDAT- 2009/12/05 06:00
MHDA- 2009/12/05 06:01
CRDT- 2009/12/05 06:00
PHST- 2009/12/05 06:00 [entrez]
PHST- 2009/12/05 06:00 [pubmed]
PHST- 2009/12/05 06:01 [medline]
AID - 10.1021/la903443p [doi]
PST - ppublish
SO  - Langmuir. 2010 Mar 16;26(6):4357-67. doi: 10.1021/la903443p.