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Title: Institute of Solid State Physics, Bulgarian Academy of Sciences,


1
PRODUCTION OF HIERARCHICALLY ORGANIZED MICRO- AND
NANOMETER SCALE SURFACES DEVELOPMENT OF NOVEL
TECHNOLOGY FOR IMPLANT COATINGS AND CELLS
GROWTH PRAMATAROVA Lilyana., Assoc. Prof. Dr.
Institute of Solid State Physics, Bulgarian
Academy of Sciences, 72 Tzarigradsko
Chaussee, bulv., 1784 Sofia, Bulgaria tel
359-2-7144265 fax 359-2-9753632 E-mail
lpramat_at_issp.bas.bg Web page www.issp.bas.bg

2
PARTICIPANTS
1. Institute of Solid State Physics, Bulgarian
Academy of Sciences, Assoc. Prof. Dr. L.
Pramatarova, Development of in-vitro systems and
production of hydroxyapatite (HA), RTD, Bulgaria
Address Assoc. Prof. Dr. L. Pramatarova
Institute of Solid State Physics, Bulgarian
Academy of Sciences 72 Tzarigradsko Chaussee
blvd., 1784 Sofia, Bulgaria, tel. 359-2-7144265,
fax 359-2-9753632 e-mail lpramat_at_issp.bas.bg ,
web page www.issp.bas.bg 2. Pulslight Ltd.,
Bulgaria (MS. I. Kostadinov), Laser systems and
laser processing, (SME), Bulgaria Address
Pulslight Ltd., 72 Tzarigradsko Chaussee,
blvd., 1784 Sofia, Bulgaria, tel 359-2-9743002,
fax 359-2- 9743002 e-mail pulslight_at_issp.bas.b
g, web page www.pulslight.com 3. Base BIO
POSITIONNING, (SME), France Dr Didier Mauroy,
Leader of the Project, Disposable use microchip
for the real-time detection of thrombosis Address
Rue de la Citadelle 11 F-33410 Rions, France
tel. 33 (0) 556 769 301 e-mail
base.be_at_wanadoo.fr

3
The aim of the proposed project is the
development of novel technology based on a
process of laser-liquid-solid-interaction (LLSI)
in simulated body fluids (SBF) and its
optimisation as a model of in vitro system for
the controllable production of samples with
hierarchically organized micro and nanometer
scale surfaces, typical for nature. The process
of LLSI is based on simultaneously
microengineering of beforehand nanostructured
substrate and growth of a layer of hydroxyapatite
(HA) on the surface. The HAP layer will be used
as implant coatings as well as a non viral
carrier in the gene therapy of certain bone
pathologies. For the implementation of the
project the groupe is closely cooperated with a
SME (Pulslight LTD, Sofia), ensures the laser
system (copper bromide pulsed laser, equipped
with a precise scanning system) necessary for the
realization of the LLSI technology.
4
  • METHOD FOR HYDROXYAPATITE GROWTH INDUCED BY THE
    PROCESS OF
  • LASER-LIQUID-SOLID INTERACTION (LLSI)
  • The method of LLSI process employs a deposition
    system and a process, which allows interaction
    between a scanning laser beam and a liquid
    precursor solution (simulated body fluid, SBF),
    and also simultaneous laser illumination of the
    substrate during the laser-liquid interaction,
    thereby stimulating the nucleation and growth of
    hydroxyapatite (HA).
  • Variously modified surfaces serve as substrates
    for the HA growth, induced by a
    laser-liquid-solid interaction process.

5
SCHEME OF AN IN VITRO SYSTEM ON THE BASE ON THE
PROCESS OF LASER-LIQUID-SOLID-INTERACTION (LLSI)

6
LASER PARAMETERS CuBr (copper bromide) laser
?1 511 nm ?2 578 nm P 4.5 W (average
laser power) ? 35 ns (pulse duration) d 50
?m (diameter of laser spot) f 1 19000 Hz
(repetition rate) N 1 19000 pulses/min v
1 2000 mm/s (velocity of scanner)
7

DESIGH OF LASER SCANNING
  • ARGES scanner head equips the pulsed CBL

8

9
Experimental Approach
  • Substrates
  • - stainless steel and titan- materials, widely
    used in orthopedic and dentistry for medical
    implants
  • - silicon- widely used material in
    microelectronics
  • - quartz (or silica glass)- typical
    piezo-electric material
  • - polymers- also find different applications
    as implants
  • Solution
  • SBF, supersaturated with respect to calcium and
    phosphorus aqueous solution resemble the
    composition, ion-concentrations and pH of human
    blood plasma

10
Experimental Approach
  • Methods for surface modification of the
    materials
  • - whole surfase ion implantation
  • - ion implantation through mask
  • - laser irradiation of the surface
  • - nanostructures
  • - porous silicon
  • - poly silicon
  • - deposition of extracellular matrix proteins

11
Results SEM images of hydroxyapatite on modified
by ion implantation of whole surface of SS, S and
SG substrates

12
Results Morphology of HA layer grown on the
surfaces iplanted with Ca and P through the mask
Mask design
  • Substrates
  • Stainless steel (SS)
  • Silicon (S)
  • Silica glass (SG)

13
Results Applying of LLSI process on the
surfaces, implanted by Ca and P ions through a
mask
  • SEM results

Mask design
  • FTIR results

14
Results HRTEM of nanostructured semiconductors
such as Si or CdSe nanopaticals in SiOx material

The method includes surface modification of
substrates by subsequent physical vapor
deposition of SiOx and CdSe at room temperature
in two different regimes or thermal Si
nanoparticle growth in SiO (xlt2) films.
15
Results SEM , Raman and FTIR studies of
nanostructured CdSe in SiOx thin films after
applying of LLSI
16
Results SEM and EDX studies Formation of NaCl
crystals and hydroxyapatite layer on
nanostructured CdSe in SiOx thin films after
applying LLSI process
17
Results SEM of porous Silicon (PS)
PS has been shown to be an excellent candidate
biomaterial, following studies establishing its
biostability and non-toxicity. These favourable
properties, coupled with the ease of its
topographical manipulation, make it an ideal
material for the growth of hydroxyapatite (HA)
for use as an artificial bone material. The
method includes surface modification by
electrochemical and laser induced chemical
etching. orientation (111) orientation
(100)
18
Results Formation of hydroxyapatite layer on
Porous Silicon after applying the process of
laser-liquid-solid interaction (LLSI)

19
Amorphous, nano- and polycrystalline silicon films
The films are deposed by magnetron sputtering and
metal induced crystallization at low temperatures
(lt550oC). Facilities deposition system Dion.
20
Results Formation of hydroxyapatite on
polycrystalline silicon films
21
Results Extracellular matrix (ECM) proteins

The method includes surface modification of the
substrates by their coating with ECM proteins -
to promote interactions with bone-forming cells.
ECM was observed to act as a matrix for the
growth of HA and leads to more homogeneous layer
distribution on the surface and a better arranged
structure.

22
List of recent publications 1. L. Pramatarova,
E. Pecheva, D. Nesheva, Z. Levi, Z. Aneva, R.
Pramatarova, U. Bismayer, T. Petrov, Study of
modified solid surfaces by nanostructured CdSe in
SiOx thin films, physica status solidi c, v. 0(3)
(2003) 1070-1074 2.E. Pecheva, L. Pramatarova,
M. F. Maitz, M. T. Pham, Study of the calcium
phosphate layer grown on AISI 316 stainless steel
from simulated body fluid, Journal of Materials
Science Materials in Electronics 14 (2003)
775-776 3.L. Pramatarova, E. Pecheva, T. Petrov,
N. Minkovski, A. Kondyurin, R. Pramatarova, Ion
beam modified surfaces as substrates for
hydroxyapatite growth induced by
laser-liquid-solid interaction, Proceedings of
SPIE, v. 5449 (2004) 41-45 4.L. Pramatarova, E.
Pecheva, T. Petrov, N. Minkovski, A. Kondyurin,
R. Pramatarova, Enhancement of hydroxyapatite
formation by laser-liquid-solid interaction,
Proceedings of SPIE, v. 5449 (2004) 46-50 5.L.
Pramatarova, E. Pecheva, M. F. Maitz, M. T. Pham,
A. Kondyurin, Ion beam patterning of solid
surfaces for hydroxyapatite deposition, Vacuum,
Vol 76/2-3 pp 335-338 (2004) 6.L. Pramatarova,
E. Pecheva, T. Petrov, A. Kondyurin, R.
Pramatarova, N. Minkovski, Ion beam and laser
processing for hydroxyapatite formation, Vacuum,
Vol 76/2-3 pp 339-342 (2004) 7.L. Pramatarova,
E. Pecheva, D. Dimova-Malinovska, R. Pramatarova,
U. Bismayer, M. Kamenova, T. Petrov, N.
Minkovski, Porous silicon as a substrate for
hydroxyapatite growth, Vacuum, Vol 76/2-3 pp
135-138 (2004) 8.E. Pecheva, L. Pramatarova, M.
F. Maitz, M. T. Pham, A. Kondyurin, Extracellular
matrix used in an in-vitro model system for
hydroxyapatite formation, Annals of
Transplantation 9 (1A) (2004) 58-60 9.L.
Pramatarova, E. Pecheva, M. F. Maitz, M. T. Pham,
A. Kondyurin, Growth of hydroxyapatite layers on
solid surfaces patterned by ion implantation,
Annals of Transplantation 9 (1A) (2004) 40-42
10.E. Pecheva, L. Pramatarova, M. F. Maitz, M.
T. Pham, A. Kondyuirin, Kinetics of
hydroxyapatite deposition on solid substrates
modified by sequential dual implantation of Ca
and P ions. Part I. FTIR and Raman spectroscopy
study, Applied Surface Science 235 (1-2) (2004)
176-181 11.E. Pecheva, L. Pramatarova, M. F.
Maitz, M. T. Pham, A. Kondyuirin, Kinetics of
hydroxyapatite deposition on solid substrates
modified by sequential dual implantation of Ca
and P ions. Part II. Morphological, composition
and structure study, Applied Surface Science 235
(1-2) (2004) 170-175 12.L. Pramatarova, E.
Pecheva, , M. F. Maitz, M. T. Pham, A. Kondyurin,
R. Pramatarova, P. Montgomery, Analysis of
hydroxyapatite films grown on whole-surface ion
implanted substrates for studying the process of
biomineralization, Nanoscience and
Nanotechnology, eds. E. Balabanova, I. Dragieva.
Heron Press, Sofia, issue 4 (2004) 295-298 13.L.
Pramatarova, E. Pecheva, R. Presker, M.
Stutzmann, M. Hanzlik, Patterned surfaces for
hydroxyapatite in vitro growth, Journal of
Optoelectronics and Advanced Materials, Vol. 7,
No. 1, June 2005, p 469-472
23
Conference Participation 2004 1. E. Pecheva,
L. Pramatarova, George Altankov, Investigation of
the fibroblast behavior on different material
surfaces, abstract presented at the 9th Ceramics,
Cells and Tissues Meeting, 28 September 1
October 2004, Faenza, Italy. 2. L. Pramatarova,
E. Pecheva, T. Petrov, R. Presker, M. Stutzmann,
Hydroxyapatite kinetic deposition on solid
substrates induced by laser-liquid-solid
interaction, paper presented at the XIII ISQE
2004 International School on Quantum Electronics
Laser Physics and Applications, 20-24 September
2004, Bourgas, Bulgaria 3. L. Pramatarova, E.
Pecheva, D. Dimova-Malinovska, R. Presker, M.
Stutzmann, U. Schwarz, R. Kniep, A novel
laser-liquid-solid interaction process for
hydroxyapatite formation on porous silicon, paper
presented at the XIII ISQE 2004 International
School on Quantum Electronics Laser Physics and
Applications, 20-24 September 2004, Bourgas,
Bulgaria. 4. L. Pramatarova, E. Pecheva, D.
Nesheva, Z. Aneva, A. L. Toth, E. Horvath, F.
Riesz, Hydroxyapatite growth on glass/CdSe/SiOx
nanostructures, paper presented at the European
Material Research Society Fall Meeting 06 10
September 2004, Warsaw, Poland. 5. L.
Pramatarova, E. Pecheva, R. Presker, U. Schwarz,
R. Kniep, Natural opal as a model system for
studying the process of biomineralization, paper
presented at the European Material Research
Society Fall Meeting 06 10 September 2004,
Warsaw, Poland. 6. L. Pramatarova, E. Pecheva,
R. Presker, M. Stutzmann, M. Maitz, M. Pham,
Patterned surfaces for hydroxyapatite in vitro
growth, abstract presented at NATO Advanced Study
Institute Nanostructured and advanced materials
for applications in sensor, optoelectronic and
photovoltaic technology, 6-17 September 2004,
Sozopol, Bulgaria. 7. L. Pramatarova, E.
Pecheva, D. Dimova-Malinovska, R. Presker, M.
Stutzmann, U. Schwarz, R. Kniep, Mechanism of
hydroxyapatite formation on porous silicon in
simulated body fluid, abstract presented at NATO
Advanced Study Institute Nanostructured and
advanced materials for applications in sensor,
optoelectronic and photovoltaic technology, 6-17
September 2004, Sozopol, Bulgaria. 8. L.
Pramatarova, E. Pecheva, R. Presker, M.
Stutzmann, M. Maitz and M. Pham, Patterned
surfaces for hydroxyapatite in vitro growth,
paper presented at the 13th International School
on Condensed Matter Physics, 30 August-3
September 2004, Varna, Bulgaria. 9. L.
Pramatarova, E. Pecheva, R. Presker, M.T. Pham,
M.F. Maitz, M. Stutzmann, Hydroxyapatite growth
induced by native extra cellular matrix
deposition on solid surfaces, paper presented at
the European Cells and Materials Conference,
28-30 June 2004, Davos, Switzerland. 10. E.
Pecheva, L. Pramatarova, G. Altankov, Fibroblast
interaction with different material surfaces,
extended abstract presented at the European Cells
and Materials Conference, 28-30 June 2004, Davos,
Switzerland. 11. L. D. Pramatarova E. Pecheva,
R. Presker, Novel processing technology for
production and use of hydroxyapatite
nanostructures, Sixth Workshop on NANOSCIENCE
NANOTECHNOLOGY - November 24-27, 2004, Sofia,
Bulgaria .
24
Profile of the Pulslight LTD, Laser systems and
laser processing, SME, Bulgaria
  • MS. I. Kostadinov, President
  • Address
  • 72 Tzarigradsko chaussee bulv., 1784 Sofia,
    Bulgaria
  • tel. 359 2 9743002
  • fax 359 2 9743002
  • e-mail pulslight_at_issp.bas.bg
  • http//www.pulslight.com
  • Abstract Pulslight Ltd. is interested in the
    development and manufacturing of Copper Bromide
    (CuBr) lasers, which are high power devices that
    generate pulses of radiation at two wavelengths
    in the visible region of the spectrum, at 511 and
    578 nanometers (nm) as well as in a scientific
    research and development. Pulslight has
    scientific collaboration with the Metal Vapor
    Laser Group at the ISSP, BAS. (Academic N.
    Sabotinov) and as a result company has high
    expertise, well developed technology and a good
    market realization. Pulslight is a partner in two
    RD projects (EC funded COPERNICUS Project and
    NATO funded SCIENCE FOR PEACE Project). The last
    two years Pulslight Ltd has scientific
    collaboration with the Assoc. Prof. Dr L.
    Pramatarova at the ISSP, BAS, leader of the
    project Development of in vitro system for
    growing of hydroxyapatite as an implant coating.
  • The interest for EU project is.
  • Application of a CuBr laser MOPA
    (master-oscillator-power amplifier) system for
    precision processing of various hard materials,
    drilling of micro-holes, and for the marking and
    cutting of materials.
  • Application of a CuBr laser in a novel method of
    laser-liquid-solid-interaction (LLSI) for
    production of hydroxyapatite coatings on
    variously modified surfaces of implants.

25
Profile of the Base BIO POSITIONNING Disposable
use microchip for the real-time detection of
thrombosis
  • Dr Didier Mauroy, Leade of the Project
  • Address
  • Rue de la Citadelle 11 , F-33410 Rions, FRANCE
  • tel. 33 (0) 556 769 301
  • e-mail base.be_at_wanadoo.fr
  • Abstract A small French firm has created a new
    bioelectronic technology able to identify with
    precision the risk of thrombosis from three
    electrochemical components a consumable made of
    a microchip equipped with silicon sensors and a
    container (capacity equal to a few milliliters),
    a microchip reader, and a data processing unit
    (software computer). The firm is also
    specializes in bioelectronic techniques for
    aqueous environment.
  • Base is a start-up developing a biochip
    (microsystem technology) for the plasma
    measurement. The methodology consist in the
    simultaneous measurement of tree essential
    electro-chemical parameters to give a fine
    position on 3 axes or 3D of the biological field.
    The use of the future biochip will give real time
    measurement at low cost.
  • The interest for EU project is
  • quality control for each plasma like batch
  • biocompatibility between in vitro and in vivo
    conditions
  • adequation between in vitro bio resorbable
    condition and recipient biological field
  • position of the plasma like with human thrombosis
    risk

26
Acknowledgements
This research is supported by Marie Curie
grant No HPMT-CT-2000-00182 of the EC and by
the Bulgarian National Scientific Research Fund
through Grant L1213. Assistance provided by
the staff of PULSSVET Ltd, Sofia and FZR,
Dresden, Germany In cooperation with U.
Bismayer, Hamburg University, Germany M.
Stutzmann, Radina Presker, TU-Munich, Walter
Schottky Institute F. Riesz, Hungarian
Academy of Sciences, Hungary, A. Medvids,
Latvian Academy of Sciences, Latvia D. Nesheva
and T. Petrov- ISSP, BAS, Bulgaria D.
Dimova-Malinovska, CLSENE, BAS, Bulgaria
Special thanks to my PhD student E. Pecheva
27
  • Workingprogramme area(s)
  • (FP6-2003-NMP-TI-3-main) Nanotechnologies and
    Nanosciences
  • Priority 3 - NMP
  • Type of Instruments
  • Specific Targeted Research Project (STREP)
  • Integrated project dedicated to SMEs (IPs-SMEs)
  • Property Rights Submitted for Bulgarian patent
  • Stage of Development Experimental development
    stage (laboratory prototype)
  • Subject Description Health economics, Medicine,
    Technology, Coatings, Cells, Inspection, Testing
  • Subject Index Codes Medicine, Health,
    Processing, Information, Technological Systems,
    Measurement Methods
  • Subject Class Medicine, Physics, Materials,
    Industrial manufacturing technologies
  • Market Applications Orthopedic implants,
    Production of lasers, Diagnostic reagents
  • Research Interest Biomineralization,
    Biomaterials, Material technology,
    Hydroxyapatite, Growth, Simulated body fluids,
    Thin films (coatings), Surface modification
    (patterning), Micro- and Nanostructured surfaces,
    Laser interaction.
  • Country Any Country
  • Experts
  • We are seeking partners having an experience in
    following fields chemistry and online testing of
    the solutions, growth of thin films and coatings,
    modification and functionalization of the
    surfaces, biomaterials, surface engineering,
    especially partners with well established
    methodologies for chemical/physical analysis.
  • We are seeking partners with existing projects or
    new projects that are still looking for suitable
    eastern partners.

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