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Polymer sample preparation techniques

Sputter coating

A sputter coater may be purchased that deposits single layers of gold, gold-palladium, tungsten, chromium, platinum, titanium, or other metals in a very controlled thickness pattern. It is possible, and desirable, to coat only a few nm’s of metal onto the sample surface.

Spin coating

Many polymer films are depositing via a spin coater which spins a substrate (often ITO glass) and drops of polymer liquid are dispersed an even thickness on top of the substrate.


Another option for polymer sample preparation is staining the sample. Stains act in different ways, but typical stains for polymers are osmium tetroxide (OsO 4 ), ruthenium tetroxide (RuO 4 ) phosphotungstic acid (H 3 PW 12 O 40 ), hydrazine (N 2 H 4 ), and silver sulfide (Ag 2 S).


Comb-block copolymer (microstructure of cast film)

  • Cast polymer film (see [link] ).
  • To view interior structure, the film was cut with a microtome or razor blade after the film was frozen in liquid N 2 and fractured.
  • Stained with RuO 4 vapor (after cutting).
  • Structure measurements were averaged over a minimum of 25 measurements.
SEM micrograph of comb block copolymer showing spherical morphology and long range order. Adapted from M. B. Runge and N. B. Bowden, J. Am. Chem. Soc. , 2007, 129 , 10551. Copyright: American Chemical Society (2007).

Polystyrene-polylactide bottlebrush copolymers (lamellar spacing)

  • Pressed polymer samples into disks and annealed for 16 h at 170 °C.
  • To determine ordered morphologies, the disk was fractured (see [link] ).
  • Used SEM to verify lamellar spacing from USAXS.
SEM image of a fractured piece of polymer SL-1. Adapted from J. Rzayev, Macromolecules , 2009, 42 , 2135. Copyright: American Chemical Society (2009).

Swnts in ultrahigh molecular weight polyethylene

  • Dispersed SWNTs in interactive polymer.
  • Samples were sputter-coated in gold to enhance contrast.
  • The films were solution-crystallized and the cross-section was imaged.
  • Environmental SEM (ESEM) was used to show morphologies of composite materials.
  • WD = 7 mm.
  • Study was conducted to image sample before and after drawing of film.
  • Images confirmed the uniform distribution of SWNT in PE ( [link] ).
  • M W = 10,000 Dalton.
  • Study performed to compare transparency before and after UV irradiation.
SEM images of crystallized SWNT-UHMWPE films before (left) and after (right) drawing at 120 °C. Adapted from Q. Zhang, D. R. Lippits, and S. Rastogi, Macromolecules , 2006, 39 , 658. Copyright: American Chemical Society (2006).

Nanostructures in conjugated polymers (nanoporous films)

  • Polymer and NP were processed into thin films and heated to crosslink.
  • SEM was used to characterize morphology and crystalline structure ( [link] ).
  • SEM was used to determine porosity and pore size.
  • Magnified orders of 200 nm - 1 μm.
  • WD = 8 mm.
  • M W = 23,000 Daltons
  • Sample prep: spin coating a solution of poly-(thiophene ester) with copper NPs suspended on to ITO coated glass slides. Ziess, Supra 35
SEM images of thermocleaved film loaded with nanoparticles with scale bar 1 μm. Adapted from J. W. Andreasen, M. Jorgensen, and F. C. Krebs, Macromolecules , 2007, 40 , 7758. Copyright: American Chemical Society (2007).

Cryo-sem colloid polystyrene latex particles (fracture patterns)

  • Used cryogenic SEM (cryo-SEM) to visualize the microstructure of particles ( [link] ).
  • Particles were immobilized by fast-freezing in liquid N 2 at –196 °C.
  • Sample is fractured (-196 °C) to expose cross section.
  • 3 nm sputter coated with platinum.
  • Shapes of the nanoparticles after fracture were evaluated as a function of crosslink density.
Cryo-SEM images of plastically drawn polystyrene and latex particles. Adapted from H. Ge, C. L. Zhao, S. Porzio, L. Zhuo, H. T. Davis, and L. E. Scriven, Macromolecules , 2006, 39 , 5531. Copyright: American Chemical Society (2006).


  • H. Ge, C. L. Zhao, S. Porzio, L. Zhuo, H. T. Davis, and L. E. Scriven, Macromolecules , 2006, 39 , 5531.
  • J. Rzayev, Macromolecules , 2009, 42 , 2135.
  • J. W. Andreasen, M. Jorgensen, and F. C. Krebs, Macromolecules , 2007, 40 , 7758.
  • M. B. Runge and N. B. Bowden, J. Am. Chem. Soc. , 2007, 129 , 10551.
  • P. J. Goodhew, J. Humphreys, and R. Beanland, Electron Microscopy and Analysis , Taylor&Francis Inc., New York (2001).
  • Q. Zhang, D. R. Lippits, and S. Rastogi, Macromolecules , 2006, 39 , 658.

Questions & Answers

what does nano mean?
Anassong Reply
nano basically means 10^(-9). nanometer is a unit to measure length.
do you think it's worthwhile in the long term to study the effects and possibilities of nanotechnology on viral treatment?
Damian Reply
absolutely yes
how to know photocatalytic properties of tio2 nanoparticles...what to do now
Akash Reply
it is a goid question and i want to know the answer as well
characteristics of micro business
for teaching engĺish at school how nano technology help us
Do somebody tell me a best nano engineering book for beginners?
s. Reply
what is fullerene does it is used to make bukky balls
Devang Reply
are you nano engineer ?
fullerene is a bucky ball aka Carbon 60 molecule. It was name by the architect Fuller. He design the geodesic dome. it resembles a soccer ball.
what is the actual application of fullerenes nowadays?
That is a great question Damian. best way to answer that question is to Google it. there are hundreds of applications for buck minister fullerenes, from medical to aerospace. you can also find plenty of research papers that will give you great detail on the potential applications of fullerenes.
what is the Synthesis, properties,and applications of carbon nano chemistry
Abhijith Reply
Mostly, they use nano carbon for electronics and for materials to be strengthened.
is Bucky paper clear?
so some one know about replacing silicon atom with phosphorous in semiconductors device?
s. Reply
Yeah, it is a pain to say the least. You basically have to heat the substarte up to around 1000 degrees celcius then pass phosphene gas over top of it, which is explosive and toxic by the way, under very low pressure.
Do you know which machine is used to that process?
how to fabricate graphene ink ?
for screen printed electrodes ?
What is lattice structure?
s. Reply
of graphene you mean?
or in general
in general
Graphene has a hexagonal structure
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what is biological synthesis of nanoparticles
Sanket Reply
what's the easiest and fastest way to the synthesize AgNP?
Damian Reply
types of nano material
abeetha Reply
I start with an easy one. carbon nanotubes woven into a long filament like a string
many many of nanotubes
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I'm interested in nanotube
what is nanomaterials​ and their applications of sensors.
Ramkumar Reply
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Sravani Reply
what is system testing?
preparation of nanomaterial
Victor Reply
how did you get the value of 2000N.What calculations are needed to arrive at it
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advantages of NAA
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