OLEM Presentation at Sichuan Delegation n Sofia, 07.September 2018

NANOTECHNOLOGY RESEARCH

at the Open Laboratory on Experimental

Micro&Nano Mechanics (OLEM)Institute of Mechanics-BAS

Prof. Rumiana Kotsilkova, D.Sc.

Head of OLEM

http://www.imbm.bas.bg

http://www.imbm.bas.bg/index.php/en_US/olem

Open Laboratory of Experimental Micro & Nano Mechanics (OLEM)

Development, Characterization and Application of Polymer Nanocomposites with Graphene and CNTs

OLEM researchers have created in 2013 the Spin-off Company NanoTechLab Ltd. to bring the nanotechnology research at OLEM to prototyping and product validation.

OLEM is found in 2010, within the Research Infrastructure Project D-02-53, supported by the Bulgarian SF. OLEM is fully equipped from this RI project and several other EU Projects.

OLEM is operating as Open Laboratory at National level for Nanomaterials Research, Education and Training. 60% of research time is used for own projects and 40% - for external services (towards other BAS Institutes, Universities and SMEs)

About OLEM

Research Topics

Spin-off Company NanoTechLab

Expertise of OLEM:

• Fabrication of Polymer Nanocomposites by

novel Processing Methods.

• Nanocomposite Design based on Rheology-

Structure-Property Relations.

• Study Mechanical Properties of Nanomaterials

at Macro-Micro-Nanoscale.

• Produce novel Nanocomposite Materials with

extraordinary Mechanical Properties, Electrical

and Thermal Conductivity, Electromagnetic

Shielding and Lightness.

NANOCOMPOSITE PROCESSING LABORATORY• Ultrasonic mixing• High shear mechanical• Filament extrusion• 3D Printing

X400 PRO 3D printerGerman Rep Rap

MICRO&NANOMECHANICS LABORATORY

Nano Indentation, Nanoscratch,AFM Indentation (Bruker)

Tribology, Friction & Wear, Creep, Adhesion (Bruker)

RHEOLOGY & THERMAL ANALYSIS LABORATORY

AR-G2

DSC - Q20

TGA - Q50

(TA Instruments)

Laboratories and Research Facilities of OLEM

Projects of OLEMProject oriented research in OLEM. Since 2010, OLEM is involved in 5 European

projects, funded by Horizon'2020 and FP7.

Running Projects

H2020-MSCA-RISE-734164 Graphene 3D (2017-2020)

(Coordinator); http://graphene3d.imbm.bas.bg/

FP7- Graphene Flagship (2014-2016);

H2020-Graphene Flagship Core 1 (2016-2018)

H2020-Graphene Flagship Core 2 (2018-2020)

Completed Projects:

FP7- NMP- NanoXCT "Compact X-ray computed tomography system“ (2013-2015);

FP7-INCO-BY NanoERA "Industrial developments of applied nanoelectronics" (2011-2013)

F7-NMP-NAPOLYNET "Setting up research intensive clusters across the EU on characterization of polymer nanostructures“ (2010-2012)

OLEM is the COORDINATOR of H2020-MSCA-RISE-Graphene 3D ProjectTitle: MULTIFUNCTIONAL GRAPHENE-BASED NANOCOMPOSITES WITH ROBUST

ELECTROMAGNETIC AND THERMAL PROPERTIES FOR 3D-PRINTING APPLICATION

Partners of Graphene 3D Project:

IMech-BAS, Bulgaria

CNR-IPCB, Italy

NARRANDO SRL - Italy

UNamur, Belgium

UniSa, Italy

NanoTecLab, Bulgaria

SIPT, Georgia

INP-BSU, Belarus

SKLPME, SICHUAN Uni. P.R.China

MackGraph - Brazil

Partner: Sichuan University Prof. Hesheng XiaSKLPME, Polymer Research InstituteSichuan, China

POLYMER NANOCOMPOSITE

DEVELOPMENTS at OLEM

We offer well characterized PROTOTYPES of Nanocomposite Materials for

various Applications:

Novel Nanocomposite Materials for 3D printers (FDM and SLS) with

high Electrical and Thermal Conductivity, 100% Electromagnetic

Shielding efficiency and Mechanical Reinforcement – market needs:

(1) Nanocomposite Filament of Biodegradable Polylactic Acid (PLA) with Graphene and Carbon Nanotubes for 3D Printers (FDM) - better than

the only commercial filament with GNP - Black Magic (USA).

(2) Nanocomposite Filament of High Density Polyethylene (HDPE) with

Graphene and Carbon Nanotubes for 3D printers (FDM) –with no commercial analog on market

(3) Conductive HDPE Powder wrapped with Graphene and Carbon

Nanotubes for 3D printers (SLS) – with no commercial analog on market.

POLYMER NANOCOMPOSITE

DEVELOPMENTS at OLEM

Polypropylene (PP) Nanocomposite with Carbon nanotubes

and Nanoclay for PACKAGING FILMS - with high Mechanical

strength, Thermal Stability and Barrier Properties.

PROTECTIVE COATINGS of Epoxy Nanocomposites with

Carbon Nanotubes with high Electrical Conductivity and

Electromagnetic Shielding Efficiency.

1. WE PROPOSE WELL CHARACTERISED PROTOTYPES OF THOSE

NANOMATERIALS WITH TUNABLE PROPERTIES.

2. WE ARE LOOKING FOR PROJECT SUPPORT AND TECHNOLOGY

TRANSFER FOR OUR NANOMATERIALS DEVELOPMENTS.

Application of Multifunctional Nanocomposite

Materials developed at OLEM

Electrical and thermal

conductive parts and

EM Absorbers for power

electronics.

- Electromagnetic shielding screens

- Protective wall plates, boxes and

coatings.

- Radiation protection in MHz, GHz

and THz wave regions

Examples

- 3D printed Cellular Structures.

- 3D printed Construction Details.

- Packaging Films.

with tunable mechanical and

physical properties and lightness.

1. Nanocomposite Filament of Biodegradable Polylactic Acid

(PLA) with Graphene and Carbon Nanotubes for 3D Printers (FDM)

PLA - monofiller and bifiller Nanocomposite Filaments for 3D printing (FDM)

HDPE- monofiller and bifiller Nanocomposite Filaments for 3D printing (FDM)

Well characterized properties – Materials Technical Specifications.

Properties:

100% Electromagnetic shielding efficiency in GHz and THz region (absorbance 40-60% / reflection 40-60%/ transmission 0%).

High electrical conductivity (≤ 5 S/m). High thermal conductivity (≤ 0.7 W/mK). Mechanical reinforcement: Increased hardness (40%) and Young’s modulus (30%)

Robust Design for optimization of the

best Nanocomposite Material

Standard Extruder Processing

Better than Black Magic (USA) in

properties and lower price.

Good printability

0 3 6 9 12 15

2

3

4

5

Nanocomposite loading, %

Young's

Modulu

s,

GP

a

PLA

1.5GNP1.5MWCNT

4.5GNP1.5MWCNT

1.5GNP4.5MWCNT

3GNP3MWCNT

3GNP6MWCNT

6GNP3MWCNT

9GNP3MWCNT

3GNP9MWCNT

6GNP6MWCNT

0 3 6 9 12 15

100

150

200

250

Nanocomposite loading, %

Hard

ness,

MP

a

PLA

1.5GNP1.5MWCNT

4.5GNP1.5MWCNT

3GNP3MWCNT

1.5GNP4.5MWCNT

3GNP6MWCNT

6GNP3MWCNT

9GNP3MWCNT

3GNP9MWCNT

6GNP6MWCNT

PROPERTIES OF MULTIFUNCTIONAL PLA/GNP/CNT FILAMENT

2. Conductive HDPE Powder Wrapped with Graphene and MWCNTs for 3D printers (SLS)

HDPE powder coated with MWCNTs/GNP by dry wrapping technology.

Conductive network of GNP/MWCNTs around polymer particles = conductive 3D printed parts

95

96

97

98

99

100

101

4%M

WCNT

3%M

WCNT

2%M

WCNT

1%M

WCNT

0,5%

MW

CNT

0%M

WCNT

Conta

ct A

ngle

[o] -W

ate

r

0

5

10

15

20

25

30

4%M

WCNT

3%M

WCNT

2%M

WCNT

1%M

WCNT

0,5%

MW

CNT

0%M

WCNT

Sur

face

Fre

e E

nerg

y [m

J/m

2 ]

Dispersive Component (d)

Polar Component (p)

Surface Free Energy

High electrical conductivity and mechanical reinforcement of 3D printed parts.

By wrapping of HDPE particles with MWCNT/GNT we increase their hydrophobicity:

Low surface contamination of 3D printed parts.

Decreased wettability of surfaces of 3D printed structures.

94

96

98

100

102

104

106

2%G

NP

2%M

WC

NT

1,5%

GN

P

1,5%

MW

CN

T

1%G

NP

1%M

WC

NT

0,5%

GN

P

0,5%

MW

CN

T

0,25

%G

NP

0,25

%M

WC

NT

0%G

NP

0%M

WC

NT

Conta

ct A

ngle

[o] -W

ate

r

3. PP Nanocomposites with MWCNTs and Nanoclay for

PACKAGING FILMS with high Mechanical strength,

Thermal stability and Barrier properties

Properties:

• Low filler content: 1-3 wt% MWCNTs and Nanoclay in PP;

• 10-40% increased tensile strength, hardness and elastic

modulus. The elongation at break is similar to the neat PP;

• 25% decreased coefficient of friction;

• 50oC increased thermal stability in N2;

• Electromagnetic shielding >80% (at < 1 mm thickness);

250 300 350 400 450

0

20

40

60

80

100

TGA Air -10oC/min

Va

lue

[%

]

Ts [°C]

PPMA

PPMA1CNT3(I.44P)

PPMA1CNT3(I.34TCN)

PPMA1CNT3(I.31PS)

PPMA1CNT3OC

Three-phases

5. PROTECTIVE COATINGS of Epoxy Nanocomposites with

MWCNTs with High Electrical conductivity and

Electromagnetic shielding efficiency

• Very low content (< 0.1-0.3wt%) of MWCNT in Epoxy resin;

• Low percolation threshold.

• Electrostatic properties: dc-conductivity: < 10-3 S/m.

• Controlled Electromagnetic Shielding by film thickness:

EMI 55-95% at thickness ≥ 1 mm

• Nanocomposites are applicable for protective films and coatings

The research results obtained in OLEM in last 5 years are published in: Many peer review publications in Impact Factor Journals 1 Book; 4 Book Chapters.

Publication activities of OLEM

OLEM Team: 8 Researchers

1 Full Professor; 1 Associate Professor; 3 Research Assistants;

and 3 PhD students

Prof. DSc. Rumiana Kotsilkova

Prof. Dr. Evgeni Ivanov

Res. Assist. Dr. Ivanka Petrova

Res. Assist. Dr. Verislav Angelov

Res. Assist. Dr. Dzhihan Menseidov

Hristiana Velichkova - PhD student

Polya Angelova - PhD student

Radost Ivanova - PhD student

Contacts:

Prof. DSc. Rumiana Kotsilkova

OLEM at Institute of Mechanics

Bulgarian Academy of Sciences

Acad. G. Bonchev, Block 4

1113 Sofia, Bulgaria

E-mails: kotsilkova@yahoo.com

kotsilkova@imbm.bas.bg

http://www.imbm.bas.bg/index.php/en_US/olem

Thanks for your attention!