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MANUNET transnational call 2017 · MNET17/NMCS-0114

OLIDIGRAPH

Optical limiter device based on innovative graphene-derived materials

A Romanian–Norwegian research project (2018–2020) on graphene-based materials that limit the intensity of laser beams, and on a prototype optical limiter that protects eyes and optical sensors.

ResultsConsortium
months
24
partners
5
countries
2

01

The project

Acronym
OLIDIGRAPH
Full title
Optical limiter device based on innovative graphene-derived materials
Call
MANUNET transnational call 2017
Contract
MNET17/NMCS-0114
Topic
New manufacturing methods, components and systems
Keywords
Hybrid manufacturing processes · Nanotechnologies · Surfaces
Duration
24 months, March 2018 to February 2020
Start date
1 March 2018
Coordinator
INOE 2000, National Institute of Research and Development for Optoelectronics
Contact person
Ileana Cristina Vasiliu

Abstract

Lasers are currently indispensable for many military and civil applications, and there is a considerable need for a material that can be built into a device for the laser damage prevention of optoelectronic devices and for the protection of people.

The overall objectives of the project are (1) to validate a laboratory-scale technology for the synthesis of an innovative class of graphene-based nonlinear optical materials for the visible and infrared domains, and (2) to build a device that incorporates the synthesized materials. Silico-phosphate (SP) composites with graphene oxide (GO), as bulk materials and films, and GO / reduced GO (rGO) films, prepared by sol-gel, will be investigated.

These materials lower their optical transmittance when the intensity of the incident laser beam rises above a threshold value, keeping the intensity of the transmitted beam constant and thus preventing damage to the human eye and to optical sensors. Z-scan investigations will explore the nonlinear optical properties and the optical limiting performance of these materials all along the technological chain, and will allow the best-performing material to be selected for the final prototype device.

Incident intensity →Transmitted intensity →thresholdlinear materialoptical limiter
Schematic: below a threshold the material transmits light normally; above it, its transmittance drops, so the transmitted intensity stays at a safe level.
chemical reductionor thermal treatmentGOrGO
Graphene oxide (GO) and reduced graphene oxide (rGO): chemical reduction or thermal treatment removes most of the oxygen groups.

02

Objectives

General objectives

  1. 1

    To elaborate, evaluate and validate at laboratory level a technology for the synthesis of an innovative nonlinear optical material with optical limiting properties in the visible and infrared domains.

  2. 2

    To build a prototype device that incorporates the material with the best performance.

Specific objectives

  • To develop surface-functionalized, well-dispersed graphene oxide (GO) and reduced graphene oxide (rGO), giving homogeneous, stable and reproducible suspensions for two types of nonlinear optical materials: GO/rGO-based composites and GO/rGO coatings.
  • To develop a laboratory sol-gel synthesis technology for silico-phosphate composites with graphene oxide.
  • To develop an alternative laboratory sol-gel synthesis technology for GO and rGO films on glass/ITO substrates.
  • To explore the optical properties of the innovative silico-phosphate composites with graphene and the GO/rGO films prepared by sol-gel, for laser damage prevention. The optical limiting function of the synthesized materials is investigated by the Z-scan and I-scan methods.
  • To build a prototype device that incorporates the best-performing material and demonstrates the protection of optical sensors (CCD, CMOS, etc.) by testing it under high-intensity laser beams.

03

Work packages

  1. WP1

    Development of well-dispersed GO and/or rGO in organic media

  2. WP2

    Development of sol-gel derived SiO₂–P₂O₅ glass composites with GO/rGO

  3. WP3

    Fabrication and characterization of GO/rGO thin films on glass substrates

  4. WP4

    Evaluation of nonlinear optical properties

  5. WP5

    Design, demonstration and testing of the prototype device

  6. WP6

    Project management and dissemination

04

Results

Stage I

2018

Results

  • Report on the experimental variants for preparing silico-phosphate films doped with GO, and structural characterization of the prepared structures
  • Test structures of silico-phosphate films doped with rGO
  • Report on the optical limiting function of GO/rGO suspensions, silico-phosphate composite films with GO/rGO and GO/rGO films
  • Report on the concept and development of the opto-mechanical parts of the graphene-based optical limiter
Activities (8)›
  1. Design and synthesis of GO/rGO embedded in silico-phosphate films by the sol-gel method
  2. Structural, optical and morphological characterization of sol-gel composite films of GO/rGO embedded in a silico-phosphate matrix (FTIR, Raman and UV-VIS-NIR spectroscopy)
  3. SEM and TEM investigations of silico-phosphate composite films with GO/rGO
  4. Investigation of the optical limiting function of GO/rGO suspensions
  5. Investigation of the optical limiting function of silico-phosphate composite films with GO/rGO
  6. Optical limiting function of GO/rGO films prepared by the Norwegian partners
  7. Design of the general concept of the optical limiter system
  8. Development of the opto-mechanics, with the related mechanical devices and internal parts of the graphene-based optical limiter

Stage II

2019

Results

  • Report on the production flowsheet for GO/rGO suspensions and functionalized GO/rGO
  • Report on the technological parameters for the sol-gel synthesis of GO- and rGO-doped silico-phosphate materials
  • Report on the surface functionalization of GO/rGO
  • Report on the fabrication of GO/rGO thin films on glass substrates by the sol-gel method
  • Report on the optical limiting function of GO/rGO suspensions, silico-phosphate composites with GO and rGO, and GO-doped polymer films
  • Report on the development of the opto-mechanical parts of the graphene-based optical limiter
  • Test structures: silico-phosphate materials doped with rGO and GO, rGO/GO films, polymer films doped with rGO/GO
Activities (9)›
  1. Experiments to define the technological parameters for the sol-gel synthesis of GO- and rGO-doped silico-phosphate materials with optical limiting properties
  2. Structural, optical and morphological characterization of the sol-gel GO- and rGO-doped silico-phosphate composite films and layers (FTIR, Raman and UV-VIS-NIR spectroscopy)
  3. SEM investigations of silico-phosphate composite materials with GO and rGO
  4. Fabrication and characterization of functionalized GO/rGO
  5. Investigation of the optical limiting function of functionalized GO/rGO suspensions
  6. Investigation of the optical limiting function of silico-phosphate composite materials with GO and rGO
  7. Optical limiting function of GO/rGO films
  8. Investigation of the optical limiting function of organic polymers doped with GO
  9. Development of the opto-mechanics and internal parts of the graphene-based optical limiter

Stage III

2020

Results

  • Report on the development of well-dispersed GO and/or rGO in organic media
  • Report on the development of sol-gel derived SiO₂–P₂O₅ glass composites with GO/rGO
  • Report on the fabrication and characterization of GO/rGO thin films on glass substrates
  • Report on the evaluation of nonlinear optical properties
  • Report on the design, demonstration and testing of the prototype device
Activities (11)›
  1. Testing the stability and homogeneity over time of the synthesized GO and rGO suspensions and dispersions
  2. Optimization of the synthesis route and production of the best-performing silico-phosphate films and bulk composites with rGO
  3. Optimization of the fabrication route for functionalized GO/rGO
  4. Optimization of the fabrication parameters for GO/rGO films
  5. Investigation of the optical limiting function of GO/rGO suspensions
  6. Investigation of the optical limiting function of silico-phosphate composite films with GO/rGO
  7. Investigation of the optical limiting function of bulk silico-phosphate composites with GO/rGO
  8. Optical limiting function of GO/rGO films
  9. Investigation of laser-induced damage in the best-performing synthesized materials under high-power laser beams
  10. Prototyping of the opto-mechanical parts integrated into a workable system
  11. Testing and characterization of the optical limiter demonstrator in operation

05

Dissemination

2018

  • Conference

    Graphene applications for photo sensing devices development

    D. Ulieru, O.-M. Ulieru, X. Vila, A. Topor

    European Microwave Week 2018, Sensors and Remote Systems, 23–28 September 2018, IFEMA, Feria de Madrid, Spain

  • Conference

    Optoelectronic modules for optical limiters integrated into laser systems

    D. Ulieru, X. Vila, O.-M. Ulieru, A. Topor

    Industrial Technologies 2018: Innovative industries for smart growth, workshop “Photonics for Industrial Production”, 29–31 October 2018, Messe Wien Exhibition & Congress Center, Vienna, Austria

2019

  • Training course

    Modern packaging technologies for biomedical applications

    D. Ulieru

    Training course “Prototyping for biomedical applications”, bTB Test workshop, SITEX and ECAS Electronics, Bucharest, Romania, 15 January 2019

  • Exhibition

    The human eye protection by application of optical limiter devices

    D. Ulieru, X. Vila, O.-M. Ulieru, A. Topor

    MedTec exhibition, 23–25 May 2019, Nuremberg, Germany

  • Conference

    Optical limiting potential of reduced graphene oxide based films, solutions and silico-phosphate composites

    A. Petris, C. Vasiliu, S. Mei, J. Yang, S. Etemadi, R. Wendelbo, P. Gheorghe, L. Ionel, L. Rusen, A. M. Iordache, M. Elisa

    E-MRS Spring Meeting 2019, Symposium V: Laser interactions with materials: from fundamentals to applications

  • Conference

    Developing and implementation of a new generation of nano safety assessment tools

    D. Ulieru, O.-M. Ulieru, X. Vila, A. Topor

    EuroNanoForum 2019, paper H04, 12–14 June 2019, Palace of the Parliament, Bucharest, Romania

  • Poster

    The optical limiter based on application of innovative graphene-derived materials by photodetecting device integration

    D. Ulieru, F. Babarada, O.-M. Ulieru, X. Vila, A. Topor

    Sensor+Test 2019, SITEX booth 5/411, 25–27 June 2019, Nuremberg, Germany

  • Conference

    Passive optical limiting in graphene-based nonlinear materials

    A. Petris, P. Gheorghe, L. Ionel, L. Rusen, C. Vasiliu, A. M. Iordache, M. Elisa, C. Simon, S. Mei, J. Yang, K. Thorshaug, B. Wabende, R. Wendelbo, S. Etemadi

    14th International Conference “Correlation Optics 2019”, Chernivtsi, Ukraine

2020

  • Patent application

    Integrated electronic device for optical limiting of laser beam intensity

    D. Ulieru, I. C. Vasiliu, A. Petris

    Patent application A/90/21.02.2020

  • Journal article

    Graphene oxide-based silico-phosphate composite films for optical limiting of ultrashort near-infrared laser pulses

    A. Petris, I. C. Vasiliu, P. Gheorghe, A. M. Iordache, L. Ionel, L. Rusen, S. Iordache, M. Elisa, R. Trusca, D. Ulieru, S. Etemadi, R. Wendelbo, J. Yang, K. Thorshaug

    Nanomaterials 10 (9), article 1638, September 2020

    DOI 10.3390/nano10091638

06

Consortium

07

Contact

INOE 2000

National Institute of Research and Development for Optoelectronics

Contact person

Ileana Cristina Vasiliu