<< Chapter < Page Chapter >> Page >

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

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
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 ?
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
On having this app for quite a bit time, Haven't realised there's a chat room in it.
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
what is the k.e before it land
what is the function of carbon nanotubes?
I'm interested in nanotube
what is nanomaterials​ and their applications of sensors.
Ramkumar Reply
what is nano technology
Sravani Reply
what is system testing?
preparation of nanomaterial
Victor Reply
Yes, Nanotechnology has a very fast field of applications and their is always something new to do with it...
Himanshu Reply
good afternoon madam
what is system testing
what is the application of nanotechnology?
In this morden time nanotechnology used in many field . 1-Electronics-manufacturad IC ,RAM,MRAM,solar panel etc 2-Helth and Medical-Nanomedicine,Drug Dilivery for cancer treatment etc 3- Atomobile -MEMS, Coating on car etc. and may other field for details you can check at Google
anybody can imagine what will be happen after 100 years from now in nano tech world
after 100 year this will be not nanotechnology maybe this technology name will be change . maybe aftet 100 year . we work on electron lable practically about its properties and behaviour by the different instruments
name doesn't matter , whatever it will be change... I'm taking about effect on circumstances of the microscopic world
how hard could it be to apply nanotechnology against viral infections such HIV or Ebola?
silver nanoparticles could handle the job?
not now but maybe in future only AgNP maybe any other nanomaterials
I'm interested in Nanotube
this technology will not going on for the long time , so I'm thinking about femtotechnology 10^-15
can nanotechnology change the direction of the face of the world
Prasenjit Reply
how did you get the value of 2000N.What calculations are needed to arrive at it
Smarajit Reply
Privacy Information Security Software Version 1.1a
Berger describes sociologists as concerned with
Mueller Reply
advantages of NAA
Sai Reply
how I can reaction of mercury?
Sham Reply

Get the best Physical methods in ch... course in your pocket!

Source:  OpenStax, Physical methods in chemistry and nano science. OpenStax CNX. May 05, 2015 Download for free at http://legacy.cnx.org/content/col10699/1.21
Google Play and the Google Play logo are trademarks of Google Inc.

Notification Switch

Would you like to follow the 'Physical methods in chemistry and nano science' conversation and receive update notifications?