NIST Special Publication 1200-17

Strategies for scanning electron microscopy 

sample preparation and characterization of 

multiwall carbon nanotube polymer composites

Version 1.0 

András E. Vladár 

This publication is available free of charge from: 

http://dx.doi.org/10.6028/NIST.SP.1200-17 
NIST Special Publication 1200-17

Strategies for scanning electron microscopy 

sample preparation and characterization of 

multiwall carbon nanotube polymer composites

Version 1.0 

András E. Vladár 

Engineering Physics Division

Physical Measurement Laboratory 

This publication is available free of charge from: 

http://dx.doi.org/10.6028/NIST.SP.1200-17

July 2015 

U.S. Department of Commerce 

Penny Pritzker, Secretary 

National Institute of Standards and Technology 

Willie May, Acting Under Secretary of Commerce for Standards and Technology and Acting Director 

Certain commercial entities, equipment or materials may be identified in this 

document in order to describe an experimental procedure or concept adequately. 

Such identification is not intended to imply recommendation or endorsement by the 

National Institute of Standards and Technology, nor is it intended to imply that the 

entities, materials or equipment are necessarily the best available for the purpose.

National Institute of Standards and Technology Special Publication 1200-17

Natl. Inst. Stand. Technol. Spec. Pub. 1200-17, 21 pages (July 2015) 

CODEN: NSPUE2 

This publication is available free of charge from: 

http://dx.doi.org/10.6028/NIST.SP.1200-17
ii

FOREWORD

This special publication is one in a series stemming from the National Nanotechnology Initiative 

(NNI) Nano-EHS Research Strategy which identified Nanomaterial Measurement Infrastructure 

as one of the essential areas of research needed in order to develop an effective risk assessment 

and management plan regarding various aspects of nanotechnology in consumer products as it 

pertains to human health, exposure and the environment. The National Institute of Standards and 

Technology (NIST) was identified as a lead agency in the development of measurement 

strategies for the detection and characterization of nanomaterials within commercial products. 

Carbon nanotubes in commercial products, the focus for this special publication, were one of the 

nanomaterials identified in the Nano-EHS research strategy. 

This guideline presents methods for the preparation and investigation of samples of multiwall 

carbon nanotube-polymer composites by scanning electron microscopy. It is focused on 

multiwall carbon nanotube epoxy composite, but the strategy should be generally applicable to 

other types of polymer nanocomposite materials. Updates to this protocol may be released in the 

future. Visit http://nist.gov/mml/np-measurement-protocols.cfm to check for revisions of this 

protocol, or new protocols in the series. We also encourage users to report citations to published 

work in which this protocol has been applied. 
1 

1. Introduction

Carbon nanotubes (CNTs) combined with polymers produce composite materials with 

significantly improved mechanical, electrical or thermal properties. Compared to carbon fibers 

CNTs offer considerable advantages, for example, it is estimated that millions of tons of 

kerosene fuel could be saved if CNTs were used for making the body of airplanes. The scientific 

and industrial interest in CNTs growing, so is global CNT production and the number of CNTcontaining consumer products [1-3]. The need to reliably detect and characterize nanocomposite 

materials during their lifecycle (from production to end their of existence) is also increasing. 

Detection and characterization of CNTs in commercial products and in the environment are

difficult tasks that require sophisticated instrumentation and measurement methods. The type, 

surface functionalization, concentration of CNTs, and the additives used in the polymer matrix 

influence the efficacy of these analytical methods. 

To help the detection and characterization of CNTs in nanocomposite materials, the 

National Institute of Standards and Technology (NIST) has developed a set of guidelines 

describing essential procedures for sample material fabrication, preparation, and nanomaterial 

investigation using several widely available measurement techniques and methods. 

The procedures in these NIST guidelines focus on a simple nanocomposite system of multiwall carbon nanotubes (MWCNT) and epoxy, one of the most widely used ones. The sample 

preparation and measurement procedures are relevant to essentially all types of CNTs and 

polymers used to produce nanocomposite materials. 

2. Principles and Scope

Scanning electron microscopy (SEM) is one of the main techniques for nanomaterial 

characterization, due to its ability to provide morphological details of materials at nanometer 

resolution. It can differentiate carbon nanotubes from other similar structures or particles with 

similar sizes. The highest resolution SEMs can reveal fine details of nanotube structures, 

including the number of carbon layers in their walls, and characterize surface coating or 

functionalization of tubes. With proper settings, the SEM can “see” into CNT-epoxy structures 

via charge-based subsurface imaging, and reveal the presence and allow for measurements of 

individual CNTs on the surface and inside composite materials. SEMs can also work in scanning 

transmission electron microscopy mode to reveal three-dimensional structure of embedded 

CNTs. The purpose of this special publication is to provide a detailed procedure for fabricating 

nanocomposite samples suitable for SEM investigations. Detailed discussion of SEM, 

transmitted electron microscopy (TEM) and focused ion beam (FIB) theory and operation can be 

found in the following references [4-7].

3. Terminology

Carbon nanotubes – Seamless cylinders of one or more layers (single-wall, SWCNT, or multiwall, MWCNT) of graphene with open or closed ends 

Nanocomposites – Composite material formed by incorporating nanomaterial as fillers into a 

polymer matrix 
2

Scanning Electron Microscope (SEM) – Type of electron microscope that produces images of a 

sample by scanning it with a focused beam of electrons 

Transmission Electron Microscope (TEM) – Type of electron microscope that produces images 

by the interaction of the electrons transmitted through the ultra-thin sample

SEM sample stub or SEM pin stub – Mounting hardware used to hold samples to be investigate

in a SEM. Shape and size of a stub varies depending on the make and model of the instrument 

used; they are usually made of aluminum.

4. Materials, equipment and instrumentation

4.1 Materials

4.1.1 Epoxy/MWCNT composite sample

4.1.2 Double-sided conductive tape or conductive paint

4.1.3 Aluminum sample stub for mounting the nanocomposite sample

4.1.4 3 mm diameter Cu grid for mounting thin nanocomposite sample

4.2 Sample preparation equipment

4.2.1 Stereo microscope for mounting the nanocomposite sample onto the sample stub

4.2.2 Sputter coater for deposition of nm thin osmium (Os) conductive layer

4.2.3 Tweezers

4.2.4 Razor blade

4.2.5 Latex or nitrile gloves

4.2.6 Personal protection devices

4.3 Instrumentation

4.3.1 High-resolution scanning electron microscope

5. Sample Preparation for SEM investigation of CNT nanocomposites

5.1 Sample size and geometry

Concentration of CNTs in commercial nanocomposites is relatively low (< 5 wt. %) and 

many CNT nanocomposites are poor electrical conductors unless they are specifically engineered 

to be conductive. To prevent excessive charging of the specimen under electron beam 

investigation, it is recommended that the sample size be minimized (5 mm or less in lateral 

dimensions).

5.2 Sample preparation

A small piece of material can be readily cut from the bulk material using a razor blade or a 

microtome machine. Additionally, having a relatively flat and planar geometry (e.g. small piece 
3

of nanocomposite film) will facilitate easier specimen preparation and measurement. Another 

method for preparing cross sections of CNT-nanocomposites is cryo-fracturing. Carefully 

immersing the sample into liquid nitrogen and handling it with protective gloves, one can shatter 

it into small pieces. Pairing the fractured parts makes investigation on two sides of the fractured 

location possible. Cryo-fracturing generally results in less distortion than the use of shear forces 

and room temperature fracturing.

5.3 Bulk sample mounting

Sample mounting hardware/stub varies depending on the type of SEM used. The preferred 

method to secure the small piece of nanocomposite is the use of a couple thin phosphor bronze 

springs and small-size screws that apply only small forces. In this case there is no need for 

adding a conductive layer at the bottom. Alternatively, the sample can either be attached to the 

stub using a double-sided conductive tape (e.g., carbon tape or copper tape) or using a 

conductive paint such as carbon paint or silver paint. If using a conductive paint, use small 

amount of paint to prevent the paint from wicking over the sample. In these cases one should 

wait for a longer period of time (up to an hour) for the conductive tape to “settle” or for the paint 

to completely dry, otherwise, the sample could drift and/or get contaminated by the outgassing 

solvent. See Figure 1 for a schematic illustration of mounting of a bulk nanocomposite sample.

Figure 1. Sample mounting using an Al stub; the preferred method (spring and screw) is 

depicted on the left, in which case the conductive tape or paint is omitted

5.4 Thin slice sample mounting on TEM holders

For STEM imaging and measurements in the SEM CNT-epoxy samples must be prepared 

by cutting about 100 nm thin slices for the bulk sample. This can be done with a microtome 

machine. The slices must be sufficiently electron transparent at the landing energies used. On 

approximately 100 nm thin CNT-epoxy samples even 5 keV electron beam could give useful 

images, so some experimentation is required to arrive at the optimal thickness and landing 

energy of the SEM. The thin slices should be mounted on TEM standard 3 mm Cu grids or other 

special TEM sample holders. The thin slice readily adheres to the surface of the Cu grid, so 

generally no other treatment or adhesive is required. It is important to prevent the layers from 

overlapping. The goal is to have several windows covered by a single layer of the thin slice. 

Figure 2 shows an example of Cu grid-mounted thin MWCNT-epoxy sample. The slice is dark 

over the brighter Cu surface.

Conductive tape or paint

Al sample stub Nanocomposite sample 

Sub-surface imaging region Spring

Screw
4

It is advantageous to use a very sharp knife to avoid rippled sample surface, e.g. stripes left 

behind by the uneven edge of the blade microtome machine. Conductive coating of the mounted 

thin nanocomposite sample is not necessary if Cu or other conductive grid is used.

Figure 2. Thin slice of MWCNT-epoxy sample mounted on Cu TEM sample holder 

5.5 Sample coating

Coating the mounted nanocomposite sample with a thin layer of conductive material is not 

recommended for charge-based imaging, as it will defeat it. For high-resolution imaging of 

individual or set of CNTs special osmium (Os) coating is recommended [8]. With osmium 

coaters one can achieve conductivity at a thickness of slightly less than 1 nm, but in some cases a 

somewhat thicker layer might be needed for completely charge-free imaging of CNT-epoxy 

composites.

Traditional coatings, such as Au, Au/Pd, Pt, etc. are not recommended, because these layers 

are generally too thick and develop disturbing structures over the surface of the sample. In some 

cases samples coated this way could still reveal useful information, but uncertain measurement 

errors with small-diameter CNTs with an unknown, possibly several nm thick metal layer around 

them are unavoidable.
5

6 SEM imaging

CNT-nanocomposites are not conductive enough to allow for imaging that is completely 

free of sample charging, but -except for very low (< 0.01 wt %) CNT concentrations- might be

conductive enough for charge-based SEM imaging. This type of SEM imaging is unique to 

CNT-nanocomposites. It is governed by a set of complex charging phenomena, and in many 

cases makes it possible to “see” into the sample, in some instances down to several hundreds of 

nanometer depths [9]. It is generally agreed that the contrast of subsurface CNTs arises from 

changes in secondary electron (SE) yield due to charge contrast [10]. Due to the shallow escape 

depth of SEs, direct SE emission from CNTs much beyond about 7 nm to 10 nm depths should 

not be detectable [6]. Charge contrast of CNT-nanocomposites is still not a completely settled 

matter; there are several explanations for it at the various landing energies SEM can be used for 

the investigation of CNT-nanocomposites [10].

Three-dimensional charge-contrast imaging is also possible, and good quality information 

can be gained about the sub-surface distribution of CNTs. Charge-based imaging is time- and 

dose-dependent, and depending on the particular CNT-nanocomposites may require some 

experimentation to find out the best pre-charging and imaging landing energies (accelerating 

voltages). Simply changing the settings of the SEM one may get images that show two different 

types of charge-based images. Positive charging is more common, on these SEM images that 

areas that have less CNT are brighter, in negative charging darker than the rest of the sample.

One nm or so thin metal coating of the surface of CNT-nanocomposites makes highresolution imaging at 100 000 times or higher magnifications feasible. The thin metal, preferably

Os coating allows for the assessment of the size and distribution of CNT-rich areas, and for the 

establishment of the correlation between coated and uncoated, charged-based images, which may 

eliminate the need for metal coating of samples in high throughput measurements of CNT 

loading and distribution in CNT-nanocomposites.

6.1 Charge-based SEM imaging

SEM images of uncoated CNT-nanocomposites may look very different depending on the 

landing energy (accelerating voltage) used for their imaging. Figure 3 shows a 5 wt. % MWCNT 

CNT-nanocomposite sample imaged with 0.3, 1, 2, 3, 15 and 30 keV electron landing energy.

These images were taken on the surface of the sample; contrast reversal for the 1 keV image 

turns some areas darker or brighter, depending on the local state of the sample charging on the 

surface and deep in the sample. The higher landing energy images show areas that are CNT-rich 

darker than the bright epoxy-rich areas.

Figure 4 shows a 5 wt. % MWCNT CNT-nanocomposite sample imaged with 15, 10, 5, 3, 2 

and 0.8 keV electron landing energy. The secondary electron images of the same area of the 

cross section show varying contrast, even slight contrast reversal for the 0.8 keV image on the far 

right. Lager energies (2 keV and up) show embedded CNT-rich areas as dark spots, and the 

CNTs that come to the surface and stand above it also vary in their appearance. These contrast 

differences are due to the varying landing energy, i.e., the extent of the penetration of the 

electron beam, and a complex internal system of conductive and non-conductive areas around the 

CNTs.
6

Figure 3. Charge-based SEM images taken on the top of a 5 wt. % MWCNT CNTnanocomposite sample with various electron landing energies, 1.27 mm HFV

Figure 4. Charge-based SEM images taken on a 5 wt. % MWCNT CNT-nanocomposite sample 

with 15 keV (leftmost), 10, 5, 3, 2 & 0.8 keV (rightmost) electron landing energy, 6.35 μm HFV

Charge-based SEM imaging of CNT-nanocomposite samples is a time-dependent 

phenomenon, reaching a stable state may requires pre-charging of the sample. Figure 5 illustrates 

the gradual charge-up of a 1 % wt. MWCNT-nanocomposite sample. These are tilted images to 

show the side also and the flat top. They show gradual charge build-up and the stable patterns of 

the charged epoxy-rich and MWCNT-rich areas. The top patterns are bright as they reached their 

stable charging state fast, and remains essentially unchanged. The exposed left wall of the 

sample charges up at a slower rate due to its weaker dose of electrons; the gradual stabilization 

of the patterns is observable there also. 

300 

eV

1 

keV

2 

keV

5 

keV

15 

keV

30 

keV
7

Figure 5. Fast (on top) and slow (at the side) gradual charge-up of a 1 % wt. MWCNTnanocomposite sample. 608 μm HFV

Figure 6 shows how charge contrast can reveal the MWCNT- and epoxy-rich areas. Tilted, flat 

and cross-sectional 1 wt. % MWCNT-nanocomposite sample images show that charge build-up

yields patterns of brighter epoxy-rich and darker MWCNT-rich areas. The image on right was 

taken immediately after the left one, which essentially got double dose of electrons.

Figure 6. Charge contrast reveals the MWCNT- and epoxy-rich areas. Charge build-up yields 

patterns of brighter epoxy-rich and darker MWCNT-rich areas. The image on right was taken 

immediately after the left one. 195 μm HFV

Figure 7 shows the unique phenomenon of charge-contrast that allows for “seeing” into the 

bulk material.

In this instance the SEM images taken on a 1 wt. % MWCNT-epoxy nanocomposite sample

show that the CNTs are mostly in small-size clumps with uneven distribution. The brightest ones 

are closer to the surface, and there are a fewer of these there than deeper in.
8

Figure 7. Charge-contrast of small-size MWCNT clumps with uneven distribution in bulk 

MWCNT-epoxy sample. There are fewer of these closer to the surface, than deeper in. 2.54 μm

HFV

6.2 Stereo sub-surface charge-based SEM imaging

Taking charge-based SEM images from different angles allow for the three-dimensional 

(3D) imaging and measurements of the CNT distribution at moderately high magnifications. As 

an example, Figure 8 on the top shows an image pair of 0.5 wt. % SWCNT-epoxy sample tilted 

at -50 (left) and +50 (right) angles. On the bottom is a 3D SEM image generated with these. The 

red arrows point to a CNT very close to the surface, the blue ones point to a CNT embedded at 

an estimated depth of 260 nm. [10]
9

Figure 8. Top: 28 kV SEM image pair of a 0.5 % SWCNT-epoxy sample tilted at -50 (left) and 

at -50 (right) angles, 10.6 μm HFV. Bottom: 3D SEM image generated with these images. The 

red arrows point to a CNT very close to the surface, the blue ones to a CNT embedded at an 

estimated depth of 260 nm.

6.3 SEM imaging of non-charging samples

A couple of nanometer thin layer of metal can eliminate strong sample surface charging by 

draining excess electrons to ground, and keeping the sample surface potential at the same 

potential as the ground. It does not, cannot eliminate charging inside the sample, so some charge 

contrast within the bulk of the sample can still be observed. Figure 9 shows a cryo-fractured 1 

wt. % MWCNT-nanocomposite sample at locations where the clumped up CNTs broke in half, 

and individual CNTs are on the surface. Thin Os coating was applied to the sample, which 
10

allows for charging artifact-free imaging at high magnification. The energetic electron beam 

penetrates the thin CNTs and produces higher SE yields where they cross. This can be observed 

especially well on the left where several CNTs are protruding over a darker area. The image on 

the right confirms that there are individual CNTs also, not just those that clumped up.

Figure 9. Cryo-fractured 1 wt. % MWCNT-nanocomposite sample with thin Os coating. Left: 

the energetic electron beam penetrates the thin CNTs and produces higher SE yields where they 

cross. The right image confirms that there are individual CNTs also. 6.35 μm HFV

Figure 10 shows the top of the 2 nm Os-coated sample of Figure 4 with darker areas clearly 

discernable where 1 wt. % MWCNTs clumped into 5 μm to 10 μm-size globulae. Fine details of 

the sample surface are also clearly visible. The sample charges inside to different charging states 

at the CNT-rich and the epoxy-rich areas, and the charge difference leads to different SE yields.

A comparison of Os-coated and non-coated areas indicates that CNT loading and 

distribution in MWCNT-nanocomposite samples can be estimated without sample coating.

Figure 11 shows the tip of the sample shown on Figure 5 before Os coating on the left and after 

coating on the right. The bright areas on the non-coated samples are epoxy-rich, while the dark 

areas are CNT rich, there carbon nanotubes limit sample charging and SE emission. The Oscoated image reveals further fine details and also structures on the top surface that cannot be seen 

otherwise.
11

Figure 10. Sample of Figure 5 after 2 nm Os coating. The dark areas are CNT rich. 127 μm HFV

Figure 11. The sample of Figure 5 before Os coating (left) and after (right). The bright areas on 

the non-coated samples are rich in epoxy, the dark ones are in CNT. 50.8 μm HFV
12

6.4 SEM imaging in transmitted electron modes

Slicing the MWCNT-epoxy samples into about 100 nanometer thin layers offers the 

possibility of investigating the sample in transmitted electron imaging mode. Dedicated 

TEM/STEM instruments have better resolution, but it is easier to work with the SEM in STEM 

mode, and even at 10 keV landing energy sufficient transmission might be possible. Bright-field 

(BF), dark-field (DF) and high-angle annular dark-field (HAADF) STEM imaging certainly adds 

useful information to the secondary electron (SE) mode imaging. The contrast of these imaging 

modes may vary substantially, so experimentation is necessary. The signals coming from very 

small volumes are inherently weak, especially because high primary electron beam currents can 

ruin the sample. To achieve sufficiently noise-free image, several minute-long acquisition times 

are typical. SE imaging mode offers more surface-related information, while the various TEM 

modes provide information on the whole cross section of the sample. DF and HAADF modes 

images use (highly) scattered transmitted electrons, and may reveal the presence of otherwise not 

perceptible structures. Figure 12 shows the SE and HAADF images of the same sample, which 

were acquired at simultaneously.

Figure 12. Simultaneously acquired SE (left) and HAADF SEM (right) images of a thin slice of 

an MWCNT-epoxy sample. Note the different contrast. 635 μm HFV

In many cases the BF and DF images are inverses one another, but subtle differences can be 

seen and it might be easier to detect some sample feature in one or in the other. Figure 13 shows 

a high-resolution image pair of a 1% MWCNT sample. CNT rich areas and individual CNTs are 

clearly visible, and the wall of some of the CNTs as well. To some extent the threedimensionality of the CNTs can be ascertained, CNTs give stronger or weaker contrast as they 

curve up or down. In some cases some embedded material may show up within the CNTs. It is 

important to corroborate these information to ensure proper interpretation of the SEM/STEM 

images, possibly with dedicated TEM/STEM investigation, or with other techniques.
13

Figure 13. DF (left) and BF (right) STEM images of a thin slice of a 1% MWCNT-epoxy

sample. 1.21 μm HFV for both.

HAADF imaging could prove to be the most sensitive to reveal the distribution of CNTs in 

thin slices of CNT-epoxy samples. Figure 14 shows an HAADF image of a 1% MWCNT-epoxy

sample. The MWCNT distribution is typical; there are a lot of CNTs in large quantities together, 

and some dispersed across the field of view. The darker stripes (angled at about 28 degrees) are 

coming from the microtome knife, due its not perfectly sharp edge, the top and the bottom of the 

slice are not completely even, and give some contrast.
14

Figure 14. HAADF STEM image of a thin slice of a 1% MWCNT-epoxy sample. 12.7 μm HFV

6.5 Stereo sub-surface SEM imaging in transmitted electron mode

Slicing the MWCNT-epoxy samples into about 100 nanometer thin layers offers another 

possibility: the investigation of the sample in transmitted electron imaging mode to reveal the 3D 

distribution of MWCNTs at high magnifications. At these magnifications the individual CNTs 

are well visible, so are the catalytic and other materials. Figure 15 shows a BF STEM image pair 

of a thin slice of a 1 % MWCNT-epoxy sample. The left image was taken at -50, the right one at 

-50 tilt. The 2560 horizontal pixel resolution allows for seeing various MWCNTs with varying 

number of walls, and catalytic residues as small as 3 nm or so adhering to the walls. The CNTs 

turn, curl up and intertwine, the ones that are standing close to parallel to the direction of the

primary electron beam (perpendicular to the image), turn dark as there are more carbon atoms 

that stand in the way of the electron beam, causing a dark contrast. The epoxy surrounds the 

CNTs almost completely uniformly, but there are a few locations where the epoxy appears 

uneven.

Figure 15. BF STEM image pair of a thin slice of a 1 % MWCNT-epoxy sample. The left image 

was taken at -50, the right one at +50 tilt. 1.587 μm HFV

All these are better perceptible by the human vision in 3D. Figure 16 shows a red-cyan

color-coded 3D representation of the MWCNT sample generated by using a portion of the DF 

STEM image pair of Figure 15. To see the scene in 3D, red-cyan glasses are necessary. The 

image portions of the right half of the images were turned counter-clockwise, i.e., -900 to align 

them properly for 3D viewing in one of the suitable several software packages [11], which can 

perform the steps necessary to turn a stereo image pair into color-coded 3D image. The 3D 

image reveals more information out of the information present in the two images, than the image 

pair without 3D visualization. It may take a little time for the eyes and the brain to truly see 

things in 3D with the red-cyan glasses, but once they do, the scene is amazing.
15

Figure 16. Red (right) – cyan (left) coded 3D representation of the MWCNT sample generated 

using a portion of the DF STEM image pair of Figure 15. To see the scene in 3D, red-cyan 

glasses are necessary. 1.11 μm HFV

7 Abbreviations

CNT carbon nanotube

SWCNT single-walled carbon nanotube

MWCNT multi-walled carbon nanotube

SEM scanning electron microscopy

TEM transmission electron microscopy

keV kilo electron volt

HFV horizontal field of view

HFW horizontal field width

BF STEM bright-field transmission electron microscopy

DF STEM dark-field transmission electron microscopy

HAADF STEM high-angle annular dark-field transmission electron microscopy

8 Acknowledgements
16

I would like to thank Debra Kaiser for her direction and vision in the characterization of 

nanomaterials in consumer products, from which the development of this protocol derived.

9 References

1. National Nanotechnology Initiative: Environmental, Health and Safety Research Strategy. 2012, 

Presidents Council of Advisors on Science and Technology: National Science and Technology Council 

Committee on Technology: Washington, DC. 

2. De Volder, M.F.L., Tawfick, S.H., Baughman, R.H. & Hart, A.J. (2013) “Carbon Nanotubes: Present and 

Future Commercial Applications”, Science, 339, 535-539 doi: http://dx.doi.org/10.1126/science.1222453

3. Kingston, C., Zepp, R., Andrady, A., Boverhof, D., Fehir, R., Hawkins, D., Roberts, J., Sayre, P., 

Shelton, B., Sultan, Y., Vejins, V. & Wohlleben, W. (2014) “Release characteristics of selected carbon 

nanotube polymer composites”, Carbon, 68, 33-57. doi: http://dx.doi.org/10.1016/j.carbon.2013.11.042

4. Ayache, J., Beaunier, L., Boumendil, J., Ehret, G., Laub, D. “Sample Preparation Handbook for 

Transmission Electron Microscopy Techniques” Ed. Springer, 2010 338 p ISBN 978-1-4419-5975-1

5. Echlin, P. “Handbook of Sample Preparation for Scanning Electron Microscopy and X-Ray 

Microanalysis” Ed. Springer, 2009 330 p ISBN 978-0-387-85731-2

6. Goldstein, J., Newbury, D., Joy, D., Lyman, C., Echlin, P., Lifshin, E., Sawyer, L. & Michael, J. (2003) 

Scanning Electron Microscopy and X-Ray Microanalysis, 3rd Ed. Springer

7. Giannuzzi, F.A. “Introduction to Focused Ion Beams” 2005 358 p Ed. Springer ISBN 978-0-387-23313-0

8. Osmium plasma coaters http://www.2spi.com/catalog/osmi-coat.html

9. Lillehei, P.T., Kim, J.W., Gibbons, L.J. and Park C., 2009, Nanotechnology, 20, 325708 doi: 

http://dx.doi.org/10.1088/0957-4484/20/32/325708

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J.S., Vladár, A.E. and Liddle, A.J., “New Insights into Subsurface Imaging of Carbon Nanotubes in 

Polymer Composites via Scanning Electron Microscopy” 2015 Nanotechnology doi:

http://dx.doi.org/10.1088/0957-4484/26/16/169601

11. SEM-imaging 3D software examples: ImageJ Fiji, Alicona MeX, Digital Surf Mountains, Olympus 

Scandium, Adobe Photoshop, etc.