GRACE: Developing electrical characterisation methods

for future graphene electronics

L. Callegaro1 , C. Cassiago1 , A. Cultrera1 , V. D’Elia1 , D. Serazio1 , M. Ortolano1, 2 , M. Marzano1, 2 ,
O. Kazakova3 , C. Melios3 , F. Raso4 , L. Matı́as4 , A. Zurutuza5 , A. Centeno4 , A. Redo-Sanchez6 , A. Kretinin7 ,
K. Sann-Ferro8 , A. Fabricius8 , G. Weking9 , W. Bergholz9 N. Fabricius9 ,
1 INRIM - Istituto Nazionale di Ricerca Metrologica, Strada delle Cacce 91, 10135 Torino, Italy
2 Politecnico di Torino, Corso Duca degli Abruzzi 24, 10129 Torino, Italy
3 NPL - National Physical Laboratory, Teddington TW11 0LW, United Kingdom
4 CEM - Centro Espaņol de Metrologı́a, C/del Alfar 2, 28760 Tres Cantos, Madrid, Spain
5 Graphenea, 76 Donostia San Sebastı́an, Spain
6 Das-Nano, Poligono Industrial Talluntxe II, Calle M-10, 31192 Tajonar, Navarra, Spain
7 The University of Manchester, Manchester M13 9PL, United Kingdom
8 VDE – Association for Electrical, Electronic & Information Technologies,

Stresemannallee 15, 60596 Frankfurt am Main, Germany

9 ISC - International Standards Consulting GmbH & Co. KG, Rubensweg 11, D-32584 Löhne

Abstract— GRACE — Developing electrical characterisation
methods for future graphene electronics is a 2016 Normative
Joint Research Project of the European Metrology Programme
for Innovation and Research. The project focuses on the mea-
surement of the electrical properties of graphene. Its objectives
are to develop validated measurement methods and protocols,
including fast-throughput examples. The work is performed in
collaboration with international standardisation committees, with
an aim to initiate and develop dedicated documentary standards.
Index Terms—Electric variables, Electronics industry, Metrol-
ogy, Standardization, Conductive films, Graphene.
I. I NTRODUCTION
Graphene, a 2-dimensional lattice of carbon atoms discov-
ered in 2004 (see [1] for a review), is being extensively
investigated by industry as a potential new material for elec-
tronics. The difficulty in growing of large areas of high-quality
graphene with uniform and reproducible electric and electronic
properties is the main barrier presently limiting the adoption
of graphene as an electronic industrial product. Accurate
and reproducible characterisation methods adapted to the 2D
nature of graphene, both as test samples and in production
lines, are absolutely crucial. These methods are presently
underdeveloped; guidelines for the proper implementation of
the methods in the industrial environment are lacking.
The issue has been considered by international standardis-
ation organizations, which have initiated working groups and
normative projects devoted to the problem. It is unclear yet
how the different approaches, in particular high-throughput
methods, can be compared and mutually validated. The Eu-
ropean normative bodies CEN and CENELEC1 have listed,
1 CEN - Comité Européen de Normalisation; CENELEC - Comité Européen
de Normalisation Électrotechnique.
978-1-5386-0974-3/18/$31.00
2018 IEEE
in a recent STAIR EMPIR2 survey have listed, the need of
initiating a metrology research project at the European level.
GRACE - Developing electrical characterisation meth-
ods for future graphene electronics is a Normative (code
16NRM01) Joint Research Project (JRP) of the European
Metrology Programme for Innovation and Research (EMPIR).
The project has a duration of three years (Jul 2017 –
Jul 2020). Its partners include National Metrology Institutes,
an academic research center, private companies producing
graphene and measuring instrumentation, a large technical and
scientific association and a consulting company dealing with
standardisation.
Methods for electrical characterisations of graphene include
contact methods, such as in-line, four-contact resistivity
probes, van der Pauw methods and S-parameter measure-
ments on coplanar waveguides (CPW);
non-contact methods, such as scanning probe microscopies
(SPM) (including Scanning Kelvin Probe Microscopy,
SKPM, and Scanning Capacitance Microscopy, SCM),
microwave resonant cavity methods and time-domain
THz waves spectroscopy.
Many of these methods pose problems in their practical ap-
plication to an atomically-thin material like graphene, in terms
of the verification of the underlying assumptions, traceability
to the SI, and the expression of the measurement uncertainty.
In particular, non-contact methods, which are suitable for high-
speed characterisations in an industrial environment, are not
well developed and require additional validation compared to
more established contact methods.
2 The European Metrology Programme for Innovation and Research
(EMPIR) is the main programme for European research on metrology,
managed by the European Association of National Metrology Institutes
(EURAMET). STAIR - STAndardization, Innovation and Research is a joint
working group of EURAMET and CEN/CENELEC.
c
 Project​ ​GRACE
include both inhomogeneities and overall conductance mean values. Figure 1 shows a mosaic
composed​ ​of​ ​individual​ ​sample​ ​maps​ ​showing​ ​different​ ​sheet​ ​conductance​ ​features.

ONYX provides a map of the sheet conductance of the graphene and, therefore, it provides a
measure of the homogeneity of the deposition process. The maps are obtained in a non-contact and
non-destructive​ ​manner​ ​without​ ​sample​ ​preparation.

mS
Fig. 1. Graphical representation of the interaction between the four work-
packages of the project.
Figure​ ​1:​ ​Mosaic​ ​of​ ​the​ ​sheet​ ​conductance​ ​of​ ​the​ ​wafer​ ​composed​ ​of​ ​individual​ ​sample​ ​maps​ ​showing
Fig. 2. different​
Electrical ​sheet​
conductivity
Sample​ ​25
​conductance​
of ​fgraphene
eatures​ ​at​ samples
​100​ ​�m​ ​resolution.
produced by Graphenea.
Furthermore, to date no inter-laboratory studies have been The image is a mosaic of terahertz-wave scans, performed by Das-Nano, on
individual dice samples, cut from a graphene wafer. The samples have been
performed on graphene, in terms of comparing the measure- distributed to the project partners, which will perform traceable measurements
ments from different methods for a single property. Therefore, with different methods. Figure​ ​7:​ ​Sheet​ ​conductance​ ​m
the uncertainty, accuracy and reliability of the measurements
of each method are unknown.
deposited on copper and transferred onto a quartz wafer. The
wafer is diced into individual samples of 10 mm × 10 mm.
II. P ROJECT STRUCTURE AND OBJECTIVES
[CONFIDENTIAL] ​Box​ ​number​
4.4​A conductivity map of the​4 set has been produced by one of 1/21
The project is structured in four workpackages, interacting the partners (Das-Nano) with a THz scanning system (Onyx),
as shown in Fig. 1. see Fig. 2.
The specific objectives of the project are: The samples were distributed among the other partners and
1) To develop an accurate and traceable approach for the will be measured with the different methods available. The
electrical characterisation of graphene through the de- measurement results will be compared and a first determi-
velopment and comparison of different methodologies nation of the compatibility of the various outcomes will be
for both contact measurement and non-contact electrical assessed.
measurement of its properties, with traceability to the
electrical SI units. This will include the improvement of IV. ACKNOWLEDGEMENTS
established techniques as well as the development of new
This project has received funding from the EMPIR pro-
methods.
gramme co-financed by the Participating States and from
2) To develop a high-throughput approach for the electrical
the European Union Horizon 2020 research and innovation
characterisation of graphene, with the development of
programme.
novel methodologies for non-contact electrical character-
isations and their validation with established techniques.
R EFERENCES
3) To disseminate the metrology and methodologies estab-
lished in this project in the form of Good Practice Guides [1] J. B. W. Lu, P. Soukiassen, Ed., Graphene: fundamentals and function-
alities, ser. MRSBulletin, vol. 37, no. 12. Materials Research Society,
and input to documentary standards. Dec. 2012.
4) To contribute to the standards development work of the
technical committee IEC/TC 1133 through the initiation
and development of new written standards for the elec-
Sample​ ​32
trical characterisation of graphene based on the Good
Practice Guides developed within the project.

III. P RESENT S TATUS

At the present date (January 2018), a first set of samples
has been produced by one of the partners (Graphenea). The
set consists of chemical vapour deposition (CVD) graphene
3 IEC — International Electrotechnical Commission. TC 113: Technical
Committee 113 Nanotechnology for electrotechnical products and systems.