Ultrasonically Deposited Nanoparticle Coatings on Polymeric Biomaterials for Medical Applications

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1 Laboratory of Nanostructures INSTITUTE OF HIGH PRESSURE PHYSICS Ultrasonically Deposited Nanoparticle Coatings on Polymeric Biomaterials for Medical Applications Julia Rogowska-Tylman, MSc Eng. Research Associate, Laboratory of Nanostructures, IHPP PAS, Poland

2 Institute of High Pressure Physics Laboratories: Metal forming under pressure Semiconductors Crystal Growth Nanostructures + X-Ray Lab Tunable laser diodes Superconductors High Pressure Food and Soft Matter Processing Protein Biophysics High Pressure Equipment - Unipress Equipment (UE) Ceramics and Glass Terahertz Laboratory (TeraGaN) Semiconductors Characterization Molecular Beam Epitaxy Optoelectronic Devices NL-1 NL-2 NL-3 NL-4 NL-5 NL-6 NL-7 NL-8 NL-9 NL-10 NL-11 NL-12 NL-14 NL-15

3 RESEARCH AREAS: Microwave Reactors Characterization of Nanomaterials Ultrasonic Coating Electrospinning of Nanofibers Nanoparticles High-Pressure Forming Our lab has a team of well-educated, highly experienced scientists and technicians. We are able to solve your scientific problems or provide customer directed testing and analysis.

4 CHARACTERIZATION OF NANOMATERIALS We are the only laboratory in Poland certified with the Quality Management System, according to the norm ISO/EIC General requirements for the competence of testing and calibration laboratories, for specific nanomaterials characterization methods: Particle size analysis - Dynamic light scattering (DLS) ISO 22412:2008 Methods for Zeta potential determination in collidal systems ISO :2012 Particle Size Distribution of Nanomaterials in Suspension by Nanoparticle Tracking Analysis (NTA) ASTM E Determination of density by volumetric displacement - Skeleton density by gas pycnometry ISO 12154:2014 Determination of the specific surface area of solids by gas adsorption - BET method ISO 9277:2010

5 MICROWAVE STOP-FLOW REACTORS Current works: Commercialisation of reactor technology (reactors design) Production and sales of nanopowders with taylored on demand properties Advantages of Hydrothermal/Solvothermal syntheis: Synthesis occurs without sintering of the nanoparticles Easy doping of elements during crystal growth Liquid-suspended nanoparticles solution on demand Unique structures obtained extremaly hard to mimic by other methods Intensive mixing of reagents is caused by internal turbulence of liquid

6 MSS1 Reactor (UNIPRESS-ITE-ERTEC) MSS2 Reactor (UNIPRESS-ITE-ERTEC) Stop-flow system: Maximum Pressure 4 MPa Maximum Temperature 300ºC Chamber volume 150 ml Stop-flow next generation: Fully automatic proces control Manual/Automatic work mode Maximum Temperature 260 C Maximum Pressure 6 MPa Chamber volume 470 ml No contact of reagents with metallic parts (teflon, Al 2 O 3 only!) Silver medal. High Technologies Innovations - Investments. VI Exhibition and Congress, 2009, St. Petersburg, Russia The Poznan International Fair in the category INNOVATION and TECHNOLOGY MACHINE

7 MICROWAVE SYNTHESIS OF NANOPARTICLES

8 Hydroxyapatite Inorganic component of bone and teeth Bone: 70% wt HAp 22% wt protein 8% wt water Applications: Ceramic implants Composites (polymer- ceramic) Coatings Pastes/ Bone cements Nanotechnology: Boning up on biology T. Andrew Taton Nature 412, (2 August 2001)

9 When our interest in Hydroxypatite Production Started? Bio-Implant Project Computed Tomography (CT-scaning) Creating 3D model 3D printing Polymeric scaffold structures Source: Faculty of Materials Science and Engineering, Warsaw University of Technology

10 Tumor location Virtual operation planning Precise extraction of tumor and surrounding tissues Taylor-made implant Defect Reconstruction Source: Faculty of Materials Science and Engineering, Warsaw University of Technology

11 Highly biocompatible Nanohydroxyapatite (GoHAP with controlled grain size) NON-TOXIC by-product Name Specific Surface Area (BET) [a s ±σ.m 2 /g] Density [ρ±σ.g/cm 3 ] Size [d±σ.nm] GoHAP Type ± ± 0,02 8±1 GoHAP Type ± ± 0,02 10±1 GoHAP Type ± ± 0,02 15±1 GoHAP Type 4 88 ± ± 0,02 23±2 GoHAP Type 5 64 ± ± 0,02 30±3 GoHAP Type 6 49 ± ± 0,02 43±4 S. Kuśnieruk et al., Influence of hydrothermal synthesis parameters on the properties of hydroxyapatite nanoparticles, Beilstein Journal of Nanotechnology, 11,4, 2016 D. Smoleń et al., Highly biocompatible, nanocrystalline hydroxyapatite synthesized in a solvothermal process driven by high energy density microwave radiation International Journal of Nanomedicine 8, 653, 2013

12 Intenisty/counts GoHAP properties 6 types of GoHAP It was shown that by changing the synthesis parameters, the diameter of HAp nanoparticles could be controlled. GoHAP type 1 GoHAP type 2 GoHAP type 3 XRD analysis GoHAP type 4 GoHAP type 5 GoHAP type Theta/ Type 6 Type 5 Type 4 Type 3 Type 2 Type 1

13 Human bone-derived cells (HBDC) response on the material (A) XTT assay and (B) DNA assay for GoHAP and commercial material Microscopic images of in vitro cell culture on the GoHAP (D - 1day, H 7days, and L 14 days) after FDA/PI staining. D. Smoleń et al., Highly biocompatible, nanocrystalline hydroxyapatite synthesized in a solvothermal process driven by high energy density microwave radiation International Journal of Nanomedicine 8, 653, 2013

14 Materials of extremely high purity and narrow particle size distribution NANOPARTICLES: TiO 2 hydroxyapatite GoHAP (6 types) ZnO ZrO 2 (doped with Eu) ZrO 2 (doped with Mn, Co) nanocomposites: ZnO+ Ag Batch on demand: in the form of powder or suspension! Sales contact:

15 ELECTROSPINNING Lab and semi-industrial scale production of fibers for various applications We are able to produce more than 1.5 m 2 of the material per day due to unique setup designed by our experts. Bulk fibers Hollow fibers V Core-shell fibers Surface-decorated fibers Nanoparticles coated fibers Syringe pump Rotating collector

16 Ultrasonically Deposited Nanoparticle Coatings on Polymeric Biomaterials for Medical Application Julia Rogowska-Tylman a,d,bartosz Woźniak a,agnieszka Chodara a,jacek Wojnarowicz a, Tadeusz Chudoba a,vita Zalite b,janis Locs b,ilze Salma b,mara Pilmane c, Wojciech Święszkowski d,aharon Gedanken e, Witold Łojkowski a a) Laboratory of Nanostructures, Institute of High Pressure Physics, Polish Academy of Sciences, Warsaw, Poland b) Rudolfs Cimdins Riga Biomaterials Innovations and Development Centre, Institute of General Chemical Engineering, Faculty of Materials Science and Applied Chemistry, Riga Technical University, Riga, Latvia c) Faculty of Anatomy and Anthropology, Riga Stradins University, Riga, Latvia d) Faculty of Materials Science and Engineering, Warsaw University of Technology, Warsaw, Poland e) Department of Chemistry, Bar-Ilan University, Ramat Gan, Israel

17 The power of sound We are operting in this area

18 Throwing Stones in situ synthesis and coating with NPs Ultrasound Radiation as a Throwing Stones Technique for the Production of Antibacterial Nanocomposite Textiles Perelshtein, G. Applerot, N. Perkas, J. Grinblat, E. Hulla, E. Wehrschuetz-Sigl, A. Hasmann, G. Guebitz and A. Gedanken* Kanbar Laboratory for Nanomaterials, Department of Chemistry, Institute of Nanotechnology and Advanced Materials, Bar-Ilan University, Ramat-Gan 52900, Israel Institut für Umweltbiotechnologie, Petersgasse 12, 8010 Graz, Austria

19 Ultrasonic acoustic cavitation in liquid basics of coating The ultrasonic generator creates an alternating electrical field whose energy is transformed into mechanical energy by piezoelectric transducers and transmitted into the solution. This creates pressure changes in the liquid: Bubble jet collapsing speed 200m/s

20 Particles present in vicinity of the collapsing bubble jet are naturally speed up to the coated surface direction, which result in uniform coverage of the surface with nanoparticles layer of nanometric thickness. Ultrasonic horn Ultrasonic cavitation phenomena Unstable bubble Initial collapse Jetting BEFORE Solid/liquid interface Nanoparticles Vessel with nanoparticles suspension in liquid medium

21 Glass Polymeric meshes Ceramics Natural fibers Titanium 21

22 Glass needles

23 Titanium Screws

24 Ceramic scaffolds BEFORE AFTER Hydroxyapatite layer substrate substrate

25 Polymeric fibers Woven structures 3D-printed structures Cross-section

26 Sonosca Project FP7 ERA-NET SONOSCA MATERA/BBM ( ) - Sonochemical technology for bioactive bone regeneration scaffold production

27 Ceramic scaffolds 3D printed polymer scaffold

28 Ultrasonic coating method of materials dedicated for implantology technology patented by the members of Laboratory of Nanostructures is PL (B1) METHOD FOR MANUFACTURING BONE IMPLANT AND BONE IMPLANT

29 NanoLigaBond Project Orthopaedic Appication of the Coatings Source:

30 Nanoligabond Project POIR /16- Artificial tendons and ligaments fixation to bone tissue using nanotechnological approach Microwave synthesis of GoHAP nanohydroxyapatite Mixing Reagents Microwave Reaction Ultrasonic coating with GoHAP NPs Suspension Ultrasonic horn Surface-modified synthetic implants Cell culture in vitro test Animal model in vivo implantation Bone Fixation screw Implant attachment Prototype Implant Source:

31 We Offer: - Certified Characterization of Nanomaterials - Synthesis of Nanopowders - Materials Coating Services - Scientific Experise (Future: ISO certified medical nanohydroxyapatite production) We are looking for: - International Projects Partners - Collaboration with Industry - Commercialization Advisors

32 Our Team

33 Contact Information: INSTITUTE OF HIGH PRESSURE PHYSICS PAS LABORATORY OF NANOSTRUCTURES Warsaw / Poland Aleja Prymasa Tysiąclecia 98 Phone: Web: w.lojkowski@labnano.pl Experts in Nano