COLLOID AND POLYMER SCIENCEKOLLOID-ZEITSCHRIFT & ZEITSCHRIFT FOR POLYMERE
OFFICIAL JOURNAL OF THE KOLLO1D-GESELLSCHAFT
Volume 253 July 1975 Number 7
Polymer Science • Polymere
Twente University of Technology, Enschede (The Netherlands), andMiddle East Technical Universify, Ankara (Turkey)
A preparation technique for examination of wet-spun polymer fibersin a scanning electron microscope
D. M. Koenhen, M. A. deJongh, C. A. Smolders
N. Yiicesoy*)With 8 figures
(Received November 29, 1973)
In the investigation of morphological struc-tures by a scanning electron microscope(SEM) the factors which effect the resolutionpower and magnification can be derided intotwo groups. Those factors connected withthe design of the instrument will depend onthe specification provided by the manufac-turer. On the other hand, sample properties,sample preparation and conditions during ex-amination in the microscope form a group ofvery important variables. Therefore with theinstrument available, much attention should bepaid to the last group of variables.In our laboratory we are studying coagula-tion phenomena of polymer solutions incontact with non-solvents.Especially the changes in morphologyduring coagulation of the polymer phaseare relevant to polymer membrane and fiberstructure and properties.In order to study the morphology during allstages of coagulation of a spinning fiber, wetried to use the freeze-shock and freeze-etching technique in combination with trans-mission electron microscopy (1). Difficultiesin obtaining a satisfactory cleavage surface
*) Research Associate at Twente University duringthe academic year 1971--1972.
with the freeze ultramicrotome for severalpolymer species, forced us to look for adifferent method. The present study of morph-ological structures makes use of the largedepth of field of the SEM. Sample preparationconsists essentially of cryogenic breaking of awet-spun fiber, followed by a low temperatureand low pressure freeze drying (or etching)treatment.To prevent charging up of the sample in themicroscope a coating is given with a chargeconducting layer.
2. Sample preparation
Previously (2, 3, 4) methods have beendeveloped for the examination of externalfiber surfaces and fatigue broken fiber ends byscanning electron microscopy. Attention waspaid to coating techniques, by vapour deposi-tion of carbon and metals like Ag, Au and Pt.A cryogenic breaking technique has alsobeen employed earlier, for the investigation ofdry polymer membranes (5) and biologicalmaterials (6).In the present work excellent fracture sur-faces Of freshly coagulated wet-spun fibershave been obtained through breaking underliquid nitrogen or liquid propane. To revealthe coagulation structure of the polymer, thespecimen is then freeze-dried (or etched) at low