The area of research of the working group includes:

-       Methods of synthesis of nanopowders,

-       Development of high pressure reactors for nanopowders synthesis

-        Characterisation of nanopowders

-       Their applications

Nanopowders are powders with particle size below 100 nm. Nanopowders are produced in industrial scale since long time, e.g., carbon black, silica, titania etc. However, recently much interest is in nanopowders of high commercial value due to their specific optical and magnetic properties that result from nano-size.. Furthermore, from nanopowders, or using nanopowders, one can produce nanocrystalline materials or nanocomposites  of radically improved strength. Nanopowders do already play an important role in many industrial fields, and the field of their application will continuously increase in future.

1. One of major barriers in the science and technology of nanopowders is that high value nanopowders need to be produced with well controlled and narrow grain size distribution, and these parameters are difficult to control and measure.

2. Wet chemistry methods for their production are usually cheap, but after such synthesis processes nanoparticles are frequently coated with a layer of untreated reaction precursors. Therefore a major issue is to obtain nanoparticles of high degree of crystallinity.

3. It is worth developing technology of nanopowders with engineered magnetic or optical properties. An efficient method to add to nanopowders controlled magnetic or optical properties is to dope them with ions of metals which have themselves magnetic or optical properties. These ions are then protected from the environment since they are embedded in a stable oxide lattice, and at the same time this particle is so small, that it can be embedded in various materials like polymers, textiles, other ceramics, dispersed in fluids, or used  for imaging cells. Adding value to nanoparticles requites synthesis methods that permit to dope the nanoparticles to high level with such ions, without their segregation as clusters.

4. It is important to be able to coat the nanopowders with functional layers which enhance their sintering into usable mechanical parts or dispersion in fluids, or attaching to selected surfaces. . Such a process is impossible in high temperature production processes.

5. Therefore, there is a need for innovative synthesis methods that would permit to scale up production of nanopowders and at the same time meet all the above criteria, and for commonly agreed characterisation procedures to ensure delivery of quality nanopowders.

The above issues have been addressed by our working group and solutions found will be reported bellow.

1. We have developed a method to estimate the grain (or crystallite) size distribution of nanopowders based solely on an analysis of the shape of XRD peaks. The peaks must be measured according to well defined procedures and can be analysed using an analytical formula.
2. We introduced density measurements as an important tool for characterisation of nanopowders. Density tells us about the thickness of the layers on the powders surface. We could optimise the synthesis process so that such layers thickness is the minimum possible under given thermodynamic conditions.
3. Competence we acquired in characterisation of nanopowders and nanoceramics nanostructure permitted us to edit a first Nanometrology report focussed on Nanoparticles and nanomaterials, published as a prestigious Nanoforum report at the European nanotechnology web page www.nanoforum.org
4. We have found that solvothermal and hydrothermal  synthesis, i.e., a method where reagents in solution are heated above the boiling point at atmospheric pressure (and this is made possible because the fluids are in a high pressure vessel) is a method that permits to incorporate in the lattice  of ZnO a relatively large amount of metal ions: Al³⁺, Mn²⁺, Ni²⁺¸Co²⁺¸Cr³⁺ without formation of measurable clusters or precipitates. It was found that addition of Al ions in the range 0f 0.4 mol %n is possible. And this leads to increase of luminescence by more than one order of magnitude. As far as magnetic ions, the material obtained was paramagnetic. Absence of ferromagnetism indicates that ZnO doped with Mn²⁺ is not a suitable material for spintronics, contrary to many claims. Probably the magnetic properties of material obtained by other methods is caused by segregation of Mn clusters.
   Also doping of Zirconia with rare earth ions was very successfully performed, and nanoparticles emitting under excitation by laser, UV or X-ray radiation emit a range of colours have been produced.
5. We produced hydroxyapatite powders coated with collagen, which could be sintered into biocompatible material with very good mechanical properties; combined strength and ductility. Such material can be sued in tissue engineering.
6. Our studies show a range of advantages of the solvothermal method, and in particular when microwaves are used for heating:
   - comparing to high temperature methods high levels of doping are possible, and non volatile ions can be doped.
   - comparing to precipitation/ calcination or sol-gel methods, no high temperature annealing is necessary for nanopowders production, and the powders can stay all the time in closed vessels.
   
   A drawback of solvothermal synthesises that high pressure vessels are slow to heat up and cool down due to high thermal inertia. Furthermore, contact with heating elements or  steel parts of the vessel should be avoided and highly pure products can be obtained. This can be achieved by heating the reagents using microwaves, which act across a Teflon vessel where the reagents are enclosed.  In addition to that, if microwaves are used, the process of synthesis is shortened about 5 times or more, because the thermal inertia of the vessel is not limiting hating rates. However, such Teflon lined reactors are not suitable for processes at temperatures above 300^oC. 
7. We compared all the methods available in our group, and based on a SWOT analysis, we have developed two production processes:
   Stopped – flow microwave – pressure reactor, capable of producing about 1 kg of zinc oxide nanopowders per day, at pressure up to 4 MPa and temperature up to 250^oC. .
   
   Continuous synthesis of YAG nanopowders in supercrical water, at temperature about 450^oC and pressure about 40 MPa. The process includes also a thermal annealing of the powders at 600^oC to obtain a good density. Contrary to precipitation/calcination methods powders prepared in that way do not form aggregates. We have also shown several advantages of the present method over the claimed in the literature synthesis methods of YAG in continuous flow reactors.
   Both reactors are unique world wide, and give the opportunity of industrial production of nanopowders. There are some patents pending.

In summary, the results of our working group collaboration are as follows:

1. Obtaining new information about synthesis of nanopowders with the use of  microwave and pressure reactors. It was found that these techniques are especially well suited to produce  doped nanopowders of ZnO and ZrO2 as well as hydroxyapatite powders coated with organic material.
2. Scaling up of the nanopowders production using high pressure and/or microwave reactors. It was found that scaling up to industrial production is feasible. New concepts for such reactors have been developed.
3. Developing procedures for characterisation of nanopowders. We developed two new procedures, but still a lot has to be done in this field.
4. First steps towards understanding basic phenomena which take place during synthesis and sintering. This field of research is now a hot topic, since important data have been gathered and need to be explained.
5. Ready for applications. The powders produced can now be tested in various applications. Prototype devices need to be developed to convince industry about advantages of nanopowders based nanotechnology.

The general conclusion is that: “High Pressure Technology for production and processing nanopowders is now a fact that needs to be taken into account by the scientific and industrial communities”

WG D30/003    Papers

1. Study of Grain Size Distribution in Nanocrystalline Iron Oxides Synthesized by Hydrothermal Method, Solid State Phenomena 94, 239 (2003),
R. Fedyk , T. Chudoba , A. Presz , W. Lojkowski and. K. Kurzydlowski

2. New hydroxyapatite based nanomaterials for potential use in medical field, Annals of Transplantation, 9, 20 (2004),  R. M. Piticescu, G.C. Chitanu. M.L. Popescu, W. Lojkowski, A. Opalinska, T. Strachowski,

3. Biocompatibility of hydroxyl-apatite thin films obtained by pulsed laser depositionReviews on Advanced Materials Science, 8,: 164,  (2004), M.L Popescu. R.M., Piticescu , S. Petrescu, L.Zdrentu, I.Mihailescu, G.Socol, W.Lojkowski

4. Hybrid HAp-maleic anhydride copolymer nanocomposites obtained by in-situ functionalisation, Solid State Phenomena:  6, 47  (2005), R.M. Piticescu, C.C. Chitanu, M.  Albulescu, M. M. Giurginca, L. Popescu, W. Lojkowski,

5. Application of image analysis for characterization of powdersMaterials Science - Poland, 23, 79, (2005), J. Michalski, T.Wejrzanowski, R.Pielaszek, K. Konopka, W.Lojkowski, K.J. Kurzydlowski.

6. Chemical Synthesis of nanostructured Powders and Films with controlled Properties, Proceedings of the International Conference on Materials Science and Engineering, Brasov, Romania, 24-26 February 2005, ISBN 973-635-454-7, R. M Piticescu., R. R.Piticescu, V.Badilita, C.Monty,  F.Sibieude  and W. Lojkowski

7. Quantitative methods for nanopowders characterization, T,. Wejrzanowski R, . Pielaszek  A. Opalinska, H. Matysiak, Lojkowski W,. K.J. Kurzydlowskx, APPLIED SURFACE SCIENCE,  253: 204-208 (2006)

8. Effect of Pressure on Synthesis of Pr-Doped Zirconia Powders Produced by Microwave-Driven Hydrothermal Reaction, Journal of Nanomaterials,  Volume 2006, Article ID 98769, Pages 1–8, A. Opalinska, C. Leonelli, W. Lojkowski, R. Pielaszek, E. Grzanka T. Chudoba, H. Matysiak, T.Wejrzanowski, and K. J. Kurzydlowski

9. Magnetic properties of ZnMnO nanopowders solvothermally grown at low temperature from zinc and manganese acetate, Applied Physics Letters 89, 242102 (2006), A. Tomaszewska-Grzeda, A. Opalińska, E. Grzanka, and W. Łojkowski, A. Gedanken, M. Godlewski, S. Yatsunenko V. Osinniy, and T. Story

10. Synthesis of nanoparticulate yttrium aluminum garnet in supercritical water–ethanol mixtures, J. of Supercritical Fluids 40, 284  (2007) , A Cabanas., Jun Li, P., Blond, T.Chudoba, W.Lojkowski, M. Poliakoff, E.Lester

11. Nanometrology. Editors Witold Łojkowski et al, Nanoforum report 2007,   www.nanoforum,org

12. Zirconia Based Nanomaterials for Oxygen Sensors – Generation, Characterisation and Optical Properties, J.D. Fidelus, W.Lojkowski, D. Millers, L. Grigorjeva, K. Smits, and R.R. Piticescu, Solid State Phenomena 141, Vol. 128, (2007)

13. Morphology and luminescence properties of zinc oxide nanopowders doped with aluminium ions obtained by hydrothermal and vapour condensation methods., J. Applied Physics, in Press., T. Strachowski, E. Grzanka, W. Lojkowski, A. Presz M. Godlewsk, S. Yatsunenko, H. Matysiak, R.R. Piticescu, C.J. Monty

14. Solvothermal synthesis of submicron zinc oxide doped with Mn2+, Ni2+, Co2+ and Cr2+ ions by means of a microwave reactor, A. Gedanken, W. Łojkowski, A. Tomaszewska Grzęda, A. Opalińska, E. Grzanka, M. Godlewski, J of Phys Chem of Solids, submitted

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25. [CEPT] Studies of nanoparticles size distribution
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32. Welcome address
33. Otwarcie NanoInfoDay, Powitanie
34. Characteristic of hydroxyapatite dense nanoceramic produced by The High Pressure Consolidation  
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44. Nanosafety - challenge of nowadays
45. Influence of heat treatment on luminescence of ZrO₂ + Eu nanopowders
46. Solvothermal synthesis of doped nano zinc oxide for the project NanoFATE.
47. Podsumowanie
48. Solwotermalna synteza domieszkowanego nano tlenku cynku dla projektu NanoFATE.
49. Hydrothermal Synthesis of Zinc Oxide Nanopowders
50. Optyczny sensor tlenu na bazie nanokrystalicznego ZrO₂
51. Solvothermal synthesis of nonstoichiometric hydroxyapatite nanoparticles
52. Solvothermal synthesis of nonstoichiometric hydroxyapatite nanoparticles
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54. Oferty nanoproszków - Laboratorium Nanostruktur, Instytut Wysokich Ciśnien PAN
55. Nanofotonika dla małych i średnich przedsiębiorstw - mapy dorogowe i analizy SWOT  najważniejszych technologii.
56. Otwarcie konferencji
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58. Nowe mikrofalowe reaktory do syntez nanocząstek - wybrane zagadnienia badawcze i przykłady zastosowań
59. ZrO₂:Tb nanopowders obtained by coprecipitation method
60. ZnFe₂O₄/ZnO core-shell particles obtained by coprecipitation route
61. Hydrothermal Synthesis of ZnAl₂O₄ Spinel
62. Localization of rare-earth dopants in the lattice of nanocrystalline ZrO₂ - EXAFS study
63. Advanced nanoporous yttria-stabilized zirconia ceramics for luminescent oxygen sensors
64. Excitation transfer in zirconia nanocrystals and ceramics
65. Eu Luminescence in zirconia nanocrystals
66. ZnO ceramic sintering and luminescence properties
67. Oferta zaawansowanych materiałów w perspektywie 5 - 20 lat
68. Strategia rozwoju badań nanoproszków
69. Error bars in powder diffraction
70. Synthesis of doped ZnO nanopowders in microwave hydrothermal reactors
71. Characterization of nanopowders
72. Synthesis of Al doped ZnO nanopowders and their enhanced luminescence
73. Synthesis of nanopowders in supercritical water in a continuous flow reactor
74. Summary of activities of Working Group D30/003 "Synthesis and Processing of Nanopowders"
75. Doped zirconia nanopowders made in microwave – pressure reactor
76. Combining microwave and pressure techniques for hydrothermal synthesis of ZnO and ZrO₂ nanopowders doped with a range of metal ions
77. Luminescence properties of zinc oxide nanopowders doped with Al ions obtained by the hydrothermal and vapour condensation methods.
78. Mechanical property of nano-TiO2 dispersed Al65Cu20Ti15 amorphous/nanocrystalline matrix bulk composite prepared by mechanical alloying and high pressure sintering
79. Microwave technique applied on the hydrothermal synthesis and sintering of calcia stabilized zirconia nanoparticles
80. Luminescence properties of cerium doped Y₃Al₅O₁₂ nanopowders and nanoceramic
81. Yttrium-Aluminum Garnet Synthesized in the Medium of Supercritical Fluids
82. Advanced nanostructural zirconia ceramics for optical oxygen sensors
83. Study of undoped and doped zirconia nanocrystals luminescence
84. Doping of ZnO nanopowders with Mn, Ni and Cr In an ultrasound and microwave driver hydrothermal reaction
85. Localization of rare-earth dopants in the lattice of nanocrystalline ZrO₂ - EXAFS study
86. Zirconia-based nanomaterials for oxygen sensor - generation, characterisation and optical properties
87. Production of doped and non doped ceramics nanoparticles for optical applications
88. Synthesis, sintering and properties of doped nanocrystalline powders of zirconia, zinc oxide and yttrium aluminum garnet (YAG)
89. Characterization of nanocrystalline ZrO₂ doped with Rare-Earth elements synthesized via High Pressure Hydrothermal Method
90. Particle Size Distribution of ZrO₂:Pr³⁺- Influences of pH, High Power Ultrasound, Surfactant and Dopant Quantity
91. Time-Resolved Luminescence Characteristics of Doped YAG and YAP Nanopowders
92. Cathodoluminescence of Al doped ZnO nanopowders
93. Morphology of Al doped Zinc Oxide Obtained using Hydrothermal and Vapour Condensation Methods
94. Luminescence and structural properties of rare-earth doped YAG nanoceramics
95. Optimization of conditions of preparation of YAG nanopowders for sintering of translucent ceramics
96. The influence of ZrO₂ containing 10% Eu ³⁺ on the polyurethane hard domain structure of nano-composites with luminescence properties
97. Growth and properties of ytterbium doped KY(WO₄)₂ nanocomposites
98. Investigations on the utilization of nano zinc oxides synthesized by hydrothermal method in rubber compounds
99. Doping of ZnO nanopowders with Mn and Cr in an ultrasound and microwave driven hydrothermal reaction
100. Investigations of phase composition and grain size distribution in Pr doped ZrO2
101. Nasze wyniki, zdania i sposoby ich realizacji
102. Morphology of Al doped zinc oxide obtained by the vapour condensation method
103. The comparison of the properties of YAG obtained by coprecipitation and SCR method
104. Synthesis of nanopowders at elevated pressure and their characterisation - summary of work of the WG-002
105. Accuracy of XRD size measurements of nanocrystals
106. Morphology of Al-Doped Zinc Oxide Obtained by the Vapour Condensation Methods
107. SWOT analysis of various reactors used for synthesis of nanopwoders in our Working Group
108. Preliminary research on zirconia based optical oxygen sensor
109. Preparation and electrical properties of the BaTiO3 nanoceramics
110. Current trends in the development of metallic nanomaterials: results of a study carried out within the EC project Nanoroad SME
111. Microstructural Evolution in Mechanical Alloying and Hot Pressing of Aluminium and 316 Stainless Steel Powder Blend
112. Time-resolved luminescence of nanostructured ZnO
113. Prediction of degree of localisation of misfit dislocation cores in intercrystalline interfaces based on interfacial adhesion
114. Kinetic and thermodynamic factors leading to dissolution of cementite in pearlitic steel subjected to severe plastic deformation under pressure
115. Yttria stabilized zirconia nanocrystals luminescence
116. Application of XRD diffraction methods for determination of grain size distribution in nanoparticles
117. Optical investigations of RE-doped YAG nanoceramics
118. Electrical properties of nanocrystalline ZrO2 at high-pressure
119. High-pressure Induced Structural Decomposition of RE-doped YAG Nanoceramics
120. Synthesis of Al-doped ZnO nanomaterials with controlled luminescence properties
121. Combination of ECAP and Hydrostatic Extrusion for ultra-fine grain (UFG) microstructure generation in 99.98% nickel.
122. Mechanical properties and deformation behaviour of ultra-fine grained nickel.
123. Grain Size and Grain Size Distribution of Nanocrystalline Pr-doped Zirconia Powders Obtained in High Pressure Microwave Reactor
124. Influence of synthesis conditions on the particles size and the morphology of zinc oxide nanopowders
125. Measuring the Grain Size Distribution of Pr-doped Zirconia Nanopowders obtained by Microwave Driven Hydrothermal Synthesis
126. Excellent mechanical properties of UFG metals and alloys, subjected to combination of severe plastic deformation methods.
127. An FT-IR Spectroscopic Investigation of Hydroxide Groups in Nano-Crystals of ZrO2.
128. Development of microstructure and mechanical properties in nickel deformed by hydrostatic extrusion
129. Structural and luminescence properties of yttrium-aluminum garnet (YAG) nanoceramics
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131. Hybrid HAp- maleic anhydride copolymer nanocomposites obtained by in situ functionalisation
132. Fabrication and electrical properties of Eu³⁺:BaTiO₃ nanoceramics for SOFC
133. Luminescence of ZrO₂ nanocrystals
134. Molecular impurities in the luminescent ZnO nanocrystals
135. X-Ray investigations of the natural and artificial White Etching Layer
136. Diffusion and diffusion induced defects in GaN
137. Excellent Mechanical Properties of Nickel Processed by High Pressure Techniques
138. Microwave driven hydrothermal synthesis of iron oxide - the effect of process parameter on the properties of the nanopowders
139. Relaxation processes in ZrO2 at high pressures
140. Luminescence of ZrO2 and ZnO nanocrystals
141. Zinc oxide nanopowders obtained by the microwave-hydrothermal route
142. Microwave driven hydrothermal synthesis of Pr-doped zirconia nanopowders
143. New hydroxyapatite based nanomaterials for potential use in medical fields
144. Correlation between high-pressure ZrO2 electrical properties and crystallite size
145. Precise determination of full Grain Size Distribution from diffraction peak profile as a result of kinematical theory of diffraction for polidispersive nanomaterials
146. Pressure Effect on Grain Boundary Diffusion in Al Bicrystals
147. Microstructure of Surface Layers of Raiways After Heavy Exploatation
148. Normal Grain Growth in 2-d Strips of Polycrystalline Aluminium Under High Pressure
149. Reaction Diffusion in Metallic Systems under High Pressure
150. High Pressure Effect on Grain Boundary Wetting in Aluminium Bicrystals
151. Pressure Effect on Interface Energy, Diffusion and Reactions
152. Microwave-Hydrothermal Synthesis of Nanostructured Pr-Doped Zirconia Powders
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156. Structure, Morphology and Luminescence Properties of Pr-doped Nanocrystalline ZrO2 Obtained by Hydrothermal Method
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158. Hydrothermal Synthesis of Zinc Oxide Nanopowders with Microwaves Applications
159. Microwave Driven Hydrothermal Synthesis of Iron Oxide Nanopowders
160. Indentation Technique for Determination if Mechanical Behavior of Nanomaterials (Bulk and Coatings)