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Characterization of light-emittingpolymers
Light-emitting polymer technology is set to open a complete new world of applications for a wide range ofproducts, such as small (and eventually large) flat screen displays, warning signs, decorative lighting andilluminated advertising 1,2. The active layer of polymer-LEDs can be prepared by simple coating methods,such as spin coating. All colors are now available for these displays which can be made as thin as onemillimeter. High brightness can be achieved at low power consumption and long life times of more than
30000 hours. Light emitting polymers are organic, conjugated, macromolecules of very high molecularweight. An important example are phenyl-substituted poly(p-phenylene vinylene) (PPV). To make themsoluble and to process them into thin films they are modified, for example, byintroducing alkyl or alkoxy side chains. Figure 1 shows the structure of acommercially available phenyl alkoxyphenyl PPV copolymer. The compound issoluble in aromatic hydrocarbons, cyclic ethers and certain ketons.The qualityof the film coating process (and thus also the resulting polymer-LED) stronglydepends on the polymerization and the resulting molecular weightdata/molecular weight distribution. The latter parameters can be monitored
Kevin TreacherHeinz Goetz
Figure 2
Overlay of chromatograms obtained simultaneously by diode-
array and refractive index detection setting/evaluation
Conditions
Sample preparationSamples were dissolved in stablized THFand filtered (concentration 0.1 %)Column3 PLGel mixed C, 7.5 300 mm, 5 m(Agilent p/n 79911GP-MXC)Polymer standardsPolystyrene EasyCal vial standards(Agilent p/n 5064-8281)Flow rate1 ml/min
Column compartment temperature20 CInjection volume100 l
Absorbance [mAU]
0
1200
Poly (p-phenyl vinylene)
Time [min]0 5 10 15 20 25 30
nRIU
-2500
15000
Solvent
ingredients
Additives, oligomers
n
ORRO
R = *
OMe
m
ORRO
Figure 1
Structure of phenyl alkoxyphenyl PPV copolymer
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easily and precisely by GPC with Agilent Technologies PLgel columns andtetrahydrofuran as eluent. Figure 2 shows an overlay of the diode array andrefractive index detector signals of a phenyl alkoxyphenyl PPV copolymeranalysis. The chromatograms and the GPC report obtained with theChemStation GPC data analysis software (figure 3) show the high qualityresulting from:
broad molecular weight distribution ranging from about 103 to 7106 Dalton large polydispersity D of about 3.7 very high molecular weight averages, e.g. Mw is larger than 800000 Dalton low concentration of additives and other compounds (figure 2) the purity of the polymer peak as proven by the overlay of UV-visible
spectra acquired at various retention times (figure 4)
Agilent 1100 Series
GPC-SEC system
consisting of
vacuum degasser for
efficient degassing of the
mobile phase
Isocratic pump with large
solvent cabinet
Autosampler with single
valve design
Thermostatted column
compartment for precise
column temperatures
Refractive index detector
with automatic recycle
valve
ChemStation Plus with GPC-
SEC data analysis software
1.Nu Yu, H. Becker, CovionTechnology Bulletin,http://www.covion.com/techsum.html
2.H. Becker, H. Spreitzer, W.Kreuder, E. Kluge, H. Schenh, I.Parker, Y. Cao, Adv. Mater., 12(1),42(2000)
Kevin Treacher is research chemist at
Covion Organic Semiconductors
GmbH, Frankfurt/Main, Germany
Heinz Goetz is an application chemist
at Agilent Technologies, Waldbronn,
Germany
For more information on our products
and services, visit our worldwide
website at
http://www.agilent.com/chem
Equipment
Copyright 2000 Agilent Technologies
Released 10/2000
Publication Number 5988-0116EN
Method
information
Molar mass
distribution
Molecular
weight data
Sample :
Calibration file :
Integration from: Integration to :
MHK - A (Cal.): MHK - K (Cal.):
Eluent : Flowrate :
Concentration : Inject volume :
Detector 1 : Delay volume :
Detector 2 : Delay volume :
Operator : Acquisition interval :
D:\ApplNotes\3PLMIXC2\3PLmixCEasiDADPoly3Jan20.CAL
12.081 ml 22.858 ml
1.000E+0 0.000E+0 ml/g
THF +BHT 1.000 ml/min
0.000 g/l 100.000 ul
DAD A, Sig=260,10 Ref=off 0.000 ml
RID A, Refractive Index Signal 0.197 ml
Heinz G. 0.400 sec
0.0
0.2
0.4
0.6
0.8
Molar mass
104
105
106
107
g/mol
W(log M)
HP GPC-Addon Rev. A.01.03
dad1A rid1A
Mn :
Mw :
Mz :
Mv :
D :
[n]:
Vp :
Mp :
A :
10%
30%
50%
70%
90%
2.1652e5
8.1317e5
1.7186e6
8.1317e5
3.7557e0
0.000000
1.5434e1
7.5494e5
4.4348e3
1.0190e5
2.8114e5
5.2638e5
9.2617e5
1.9051e6
2.3055e5
8.4313e5
1.7654e6
8.4313e5
3.6571e0
0.000000
1.5394e1
7.7939e5
6.3271e4
1.0937e5
2.9857e5
5.5312e5
9.6022e5
1.9571e6
g/mol
g/mol
g/mol
g/mol
ml/g
ml
g/mol
ml*V
g/mol
g/mol
g/mol
g/mol
g/mol
Path :
Date : Sign :
D:\APPLNO~1\3PLMIXC2\SY-02.D
Wednesday 08/30/00 08:22:43
300 350 400 450 500 550
Wavelength [nm]
0
1500
Norm
References
Figure 4
Proof of PPV peak
purity by overlay of
seven spectra
acquired at different
retention times
Figure 3
Single page GPC report including method parameters, molar mass
distribution and molecular weight data